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. ~ ERDA/JPL 954343-70/1 DISTRIBUTION CATEGORY UC-6J
PROCESS FEASIBILITY STUDY IN SUPPORT OF SILICON MATERIAL TASK I
QUARTERLY TECHNICAL PROGRESS REPORT (I)
MARCH, 1978
C.S. Fang, Keith C. Hansen, J~seph W. Miller, Jr. and Carl L. Yaws
LAHAR UNIVERSITY Chemical Engineering Department
P.O. Box 10053 Be.at!!Uont, Texas 77710
~::.:':::;:.'-------- ---'\\
ii JPL COI,~tract No. 954343
Contractual Ackn~~l.:dgement
The JPL Low-Cost Silicon Solar Array Project is sponsored by the U. S. Department of Energy and fortns part of' the Solar-:Photovoltaic Conversion Porgram to initiate a major effort toward the dev~lopment of low-cost solar arrays. This work was perfonned for the Jet pi'opulsi0n Laboratory, California Institute of Technology by agreement betwe~n NASA and DoE.
?prOVal Signature ea..-S. ~ .~~~~ "
,: '.
https://ntrs.nasa.gov/search.jsp?R=19780015618 2020-07-05T17:28:41+00:00Z
,Disclaimer
"This ;'l.-eport was prepared as an account of work sponsored by the United states~, Government. Neither the United States nor th~ United States Departmentof" EnergY" nor any of their employees, nor any of their contractors, subcontractors, or their employees, makes any warranty, express or implied, or assumes any legal liability or ref,p()!lsibility for the accllracy, completeness or usefulness of anyinfol-matiori, apparatus, product or process disclosed, or represents that its'use would not infringe privately owned rights."
Graduate-student Assistruit Acknowleogernent
The authors wish to acknowledge the valuable help and contributions of the following graduatestudent assistants in the performance of this work:
JOHN HERA, JR. KAREN S. HYATT LESLIE A. LANDRY
': PRABODH M. PATEL PRAFUL N. SHAH JOHN R. SITZMAN CHOLTICHA RUNGAROONTHAIKUL
ABSTRACT
Major actlviticf; durinC] this reporting period centerl...·d on process system properties, chemical engineering and economic analyses.
In analyses of process system properties, major efforts focused on properties of silicon tetrachloride which is the source iuat~rial for s~veral alternate processes under consideration for solar cell grade silicon production. The status and progress are reported for physi~al, thermodynamic and transport property data.
Experimental determination of gaseous thermal condutivity of silicon source materials was continued. Initial results for gas thermal conductivity of silicon tetrafluoride and trichlorosilane are reported in respective tem-
. - j,lerature ranges of 25 to 400 C and 50 to 400 C. There have been no previously reported experimental values for the thermal conductivity of trichlorosilane in this temperature range.
For Chemical engineering analyses, the preliminary precess design for the original silane process of union Carbide was completed for cases A and B, Regular and t1inimum Process Storage. Two cases were presented becaus.:: of the large recycle requirements for this process, necessitating considerable tankago:: for material storage. Included are raw material useage, utility requirements, major process equipment list, and production labor requirements. seventy-six major pieces of process equipment are required for Case A versus fifty-eight for Case B.
The pr~liminary process design results for Cases A and B were used for economic analyses. Because of the large differences in surge tankage between major unit operations the fixed capital investment varied from $19,094,000 to $11,138,000 for Cases A and B, respectively. The product cost for Case A is $5.5.4/1b of silane versus $4.58/lb of silane for Case B.
For the ;silane process, Uuion Carbide engineering-research personn~l revised their original flowsheet for a more optimum arr~)gement of major equipment, raw materials and operating conditions. The initial issue of the revised flowsheet (Case C) for the silane process indicated favorable cost benefits over the ol:iginal schem.::. This includes higher pressure silicon tetrachloride hyrogenation for incresed trichlorosilane yield with lower recycle requirements, higher pressure distillation net requiring expensive low temperature refrigeration, and improved raw materials not requiring hydregen chloride purchase.
The revised silane process (Case C) should provid~ the following cost benefits:
-lower capital ccst -lower raw material costs -lower operating labor costs
3
TABLE OF CONTENTS
I. PROCESS SYSTEM PROPERTIES ANALYSES (TASK 1) •..•.•••••••.•••••.•• 5 A. SILICON TETRACHLORIDE PROPERTIES............................ 5 B. THE~mL CONDUCTIVITY INVESTIGATION •••••••••••••••••••••••.•• 6
II. CHEMICAL ENGINEERING ru~AYLSES (TASK 2) ....•.•.....•......••..... 11 A'. SILANE PROCESS (UNION CARBIDE) ••••••• , •.•.••••••.••••••..••• 11
1. Case A - Regular Process Storage ........................ 12 2. Case B - r.-.ir.irnwr. Process Storage ........................ 29 3. Case C - Revised' Process... . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 45
B. OTHER PROCESSES .............................................. 47
,II!. ECONOMIC ANALYSES (TASK 3)...................................... 48 A. SILANE PROCESS (UNION CARBIDE) •••••••••••••••••••••••••••••• 48
1. Case A - Regular Process Storage ........................ 49 2. Case B - 11inirnurn Process Storage ...............•.......• 61
,3. Case C - Revised Process................................ 73 B. OTHER PROCESSES....... • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • • •• 74
IV. SUNMARY - CONCLUSIONS •••••••••• " •••••••••••••••••••••••••••••••• 75
V. PLANS ••••••••••••••••••••••••.•••••••.•••••••••••••••••••••••• " 77 REFERENCES. • • • • • • • • • • • • • • • • • • • • • • • • . • • • • • • • • • • • • • • • • • • • • • • • • • • •• 78 MILESTONE CHART
:-: j:., PROCESS SYSTEM PROPERTIES ANALYSES (TASK 1)
A.. SILICON TETRACHLORIDE PROPERTIES I
Analyses of process system properties of silicon source materials was continued during this reporting period.
Primary efforts were devoted to properties of silicon tetrachloride which is under consideration for solar cell grade silicon production in several alternate processes. Progress in areas of data collection, analysis, estimation and correlation are summarized below for those properties required in the performance of the chemical engineering analyses:
Prior Current l. Vapor Pressure, Pv 80% 90% 2. Heat of Vaporization, llHv 60% 70% 3. Gas Heat Capacity, Cp 80% 90% 4. Liquid He~t Capacity, Cp 45% 60% 5. Density, PL 45% 60% 6. Surface Tension, °L 459; 60% 7. Gas Viscosity, nG 45% 60% 8. Liquid Viscosity( nL 45% 60% 9. Gas Thermal Conductivity, AG 45% 60%
10. Liquid Thermal Conductivity, AL 45% 60% II. Heat of Formation, t.Hf
0 45% 60% 12. Gibb's Free Energy of Formation, t.Gf
0 4S!!> 60%
5
B. THEm-tAL CONDUCTIVrry INVESTIGATION
During this repc1rting period the experimental determination .:>f gaseous thermal conductivity of silicon source materials was continued.
Tho'thermal conductivity of silicon tetraflouride (SiF4) has been determined between 25° and 400°C ('i.'able IB-3 and Figure IB-G). The values
.. obtained in this study agree to wi.'chin ±3% with previously reported experimental data for silicon tetrafluoride (ref. 40).
The thernal conductivity of trichlorosiland (SiHCl 3) has been detarmin~d between SO°C and 400°C (T~le IB-4 and Fighre IB-7). There have been no previously reported experimental data for gaseous thermal conductivity· of trichlorosilane.
6
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II. CHEHICAL ENGINEERING ANALYSES ('i'ASK 2)
A. SILANE PROCESS (UNION CARBIDE)
The completion of the preliminary process design of the Union Carbide Silane Process a~ characterized by the original flowsheet received was a rn.;;:;jor accomplishment this reporting pe:dod. Sine.:: th~ amount of recycle r~quired for this process is large, the rEgular surge t a nkag(' requirements required for recycl(! mat.:rial can effect the plant investment significantly. Therefore, two cases for t:1e preliminary process design were considered for the original flowsh .. et:
Case A - Regular Process Storage
Case B - ~linimum Process Storage
In additional activities for the silane process, Union Carbide engineering-research personnel revised their original flowsheet. The revisea process (Case C) involves a more optimum arrangement of major process equipment, raw material requirements and operations conditions:
Case C - R~vised Process
Initial review of the revised flowsheet suggests favorable improvements over the original scheme.
Each of these Cases (A, E and C) are discussed separately in the following sections.
11
1. CASE A - Regular Process Storage
A summation of the salient features of Case A is presented in a tabular format as follows:
CASE A
Process ...•..•..................•...•.........•.. Silane (Union Carbide) Plant Size .••..•.....•.........•..•.............. 1270 MT/year of Silane Process Flowsheet ..••..•.....•..••...••...•...... Original received from Union C~~~" Process Chemistry and Equilibrium .••........•...• From Union Carbide Intermediate Product Storage Considerations •...•• Regular Major Process Equipment .....•...• : .........•..•..• 76 pieces of process equipment
The status of prelimin~ry process design activities inVOlving Case A, including progress since the last reporting period, is given below for key items:
Prior Current
Proctss- Flow Diagram 10M 100% Mat(~r'ial Balance 100% 100% Energy Balance
'r':-100% 100%
Property Data 85% 100% Equipment Design 85% 100% Production Labor 75% 100%
The detailed status sheet is shown in Table IIA-l.OA, and is representative of the various subitems that make up the preliminary design activity. The flowsheet used for the design is shown in Figure IIA-l.GA. This flowsh(~t was received from Union Carbide.
The results from the preliminary process design are presented in a tabular format similar to J?revious design results for alternate processes to produce silicon. Note that in this process results are per pound of silane versus other processes represented as per kilogram of silicon. The sildne plant size assumes a 90% conversion of silane to silicon.
The quide to the tables for Case A is given below:
Be\se Case Conditions .•......•.••.••.•• Table IIA-l.lA Reaction Chemistry .....••.•.....•...•• Table IIA-l.2A RedistrL?uticn Equilibrium ..•..•..•..• Figure IIA-l.lA Raw Material Requirement •........••..• Table I!A-l.3A Utility Requirements ..•........•...•.• Table IA-l.4A Major Process Equipment ..•.•..•...•... 1able IIA-l.5A Production Labor Requirements •..•...•. Table IIA-l.oA
.... w
CA
SE
A
TAB
LE
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CT
IVIT
IES
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R
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AN
E
PRO
CES
S -
CA
SE
A
(UN
ION
C
AR
BID
E)
Pre
l.
Pro
cess
U
esig
n
Acti
vit
y
1.
Sp
ecif
y
Bas
e C
ase
Co
nd
itio
ns
1.
Pla
nt
Siz
e
2.
Pro
du
ct
sp
ecif
ics
3.
Ad
dit
ion
al
Co
nd
itio
ns
2.
De
fin
e
Reacti
on
C
hem
istr
y
3.
1.
Reacta
nts
, P
rod
ucts
2
. E
qu
ilib
riu
m
Pro
cess
F
low
D
iag
ram
1
. F
low
Seq
uen
ce,
Un
it O
pera
tio
ns
2.
Pro
cess
C
on
dit
ion
s (~,
P,
etc
.)
3.
En
vir
on
men
tal
4.
Com
pany
In
tera
cti
on
(T
ech
no
log
y
Ex
chan
ge)
4.
Mate
rial
Bal
ance
C
alc
ula
tio
ns
1.
Raw
M
ate
rials
2
. P
rod
ucts
3
. B
y-P
rod
uct
s
5.
En
erg
y
Bal
ance
C
alc
ula
tio
ns
1.
Hea
tin
g
2.
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oli
ng
3
. A
dd
itio
nal
6.
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pert
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Dat
a 1
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hy
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2.
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erm
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yn
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dd
itio
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Sta
tus
• • • • • • • • • • • • • • • • • • • • • • • •
Pre
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cess
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esig
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cti
vit
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7.
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men
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esig
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1.
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Vess
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nit
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(p,
T,
rate
, etc
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8.
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t o
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qu
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CASE A
TABLE IIA-lolA
BASE CASE CONDITIONS FOR SILANE PROCESS - CASE A (Union Carbide)
1. Plant Size - Allow for 10% losses of silane in production of silicon - 1270 metric tons/year of silane - Solar cell grade si~icon
2. Hydrogenation Reaction - Metallurgical grade silicon, hydrogen L to~roduce trichlorosilane (TCS)
make-up hydrogen chloride used and. recycle silicon tetrachloride(T~T) - Copper" eatalyzed . . - Fluidized bed - 55DoC, 50 PSIG. - 15.B% conversion of SiC14 (Union Carbide flowsheet)
3. TCS Redistribution Reaction - TCS from hydrogenation produces dichlorosilane (DeS) - Catalytic redistribution of TCS with tertiary amine ~on exchange resin.
Liquid phase 50 PSIG, BOoC. - Conversion a function of inlet co~centration per Figure iIA-2
(Union Carbide equilibrium) - Conversion from pure TCS feed is about 10% to nes (example)
4. nes Redistribution Reaction - DCS produces SiH4 (silane)
Catalytic redistribution of DCS with tertiary amine ion exchange resin. - Gas phasti GO-BOoC - Conversion a function of inlet concentration per Figure II~.l
(Union Carbide equilibrium), - Conversion from pure JJCSfeed is about 14% to Silane (example)
5. Recycles - unreacted chlorosilanes separated by distillation and recycled
G. Silane Purific ,in - Chlorosi1ane~-'-~emov~dby absorption in _40°C SiC1
4 (Tet)
~Tiace contaminants removed by carbon adsorption
7. Operating Ratio.,. - .~pproximately 90% utilization - Approximately, 7SS0"hvur/year production
8. Storage Considerations - Feed materials (two week supply) - Product (two week supply) - Process (several days)
15
CASE A
TABLE IIA~ . 2A
REACTIW CHEMISTRY FOR SILANE PROCESS - CASE A (UNION CARBIDE)
1. Hydrogenation Re~~
2. Trichlorosilane Redistribution Reaction
3 ~- Dichlorosilane Redistribution Reaction
~'SiH2C12 Distill~tion) 25iHC13
+ 5iH4
Note
1. Reaction 1 Product contains H2 , SiC14 , SiHC13, SiH2C12 (trace), othel: trace chlorides
2. Reaction 2 Product contains SiHe13 , SiC14 , SiH2Cl2
, SiH3Cl
3. Reaction 3 Product contains SiH2C12, SiHC1
3, SiCl
4, SiH
3Cl, SiH
4
16
OR!1'RODUCIBILITY nn .THl:'I J.\,IGIN ,-,.t' 11,
:r AL PAGE IS POOfi CASE A
Figure IIA-l.IA Redistribution Equilibrium For Silane Process .- CASE A (Provided by union Carbide)
17
CASE A --.-
TABLE IIA-I.3A
RAW MATERIAL REQUI~NTS FOR SILANE PROCESS - CASE A (UNION CARBIDE)
Requirement Raw Material fb/lb of Silane
1- Anhydrous Hel 1.239
2. Hydrogen .362
3. caustic (50%) 2.448
4. M. G. Silicon 1.11
18
CASE A
TABLE IIA-1.4 A
UTILITY REQUIRF~mNTS FOR SILANE PROCESS - CASE A (UNION CARBIDE)
Utility/Function
1.. E1ectricty 1. All p\lmp and compressor
motors (24)
2. Stea.m 250 PsiD 1. #1 Distillation Column Preheater 2. #1 Distillation Column Reboi1er 3. #2 Distillation Column Reboiler 4. #2 Redistribution Reactor Preheater 5. #3 Distillation Column Preheater 6. 113 Distillation Column Reboiler 7. 114 Distillation Column Reboiler S. Waste Treatment
3. Cooling Water (lO-120°F) 1. #1 Distillation Column Condenser 2. 112 Distillation Column Condenser
4. Process Water (90°F) 1. Waste Troatment
5. Refrigerant (23°F) 1. #4 Distillation Column Feed Tank
6. Refrigerant (5°F) 1. #3 Distillation Column Overhead
Receiver
7. Refrigerant (-7°F) 1. #4 Distillation Column OVerhQad
Receiver
S. Refrigerant (-20°F) ~_. 113 Distillation Column Condenser 2. 114 Distillation Column Condenser
19
~equirernents/1b of Silane Product
.253 KW-HR
(.253)
(6.96) (81.18) (91. 77) (3.0 ) (3.62) (3.29) ( .41) ( .11)
(146.12) (22.09)
(S.22)
(27.1 )
(79.1 )
(26.4 )
(2058.0) (245.2)
190.34 Ibs
16S~12 gallons
8.22 9allons
27.1 BTU
79.1 BTU
26.4 BTU
2303.2 BTU
CASE A
TABLE IIA-1. 4A . (Continued)
9. Refrigerant (-30°F) 1. ~rcs Reactor Recycle Gas Condenser (30788.0)
10. Refrigerant (-40°F) 1. #2 Redistribution Reactor Con
densate Receiver 2. Silane Product Storage
11. Refrigerant (-50°F) 1. #2 Redistribution Reactor Gas
Condensor 2. Product Silane Condenser 3. Absorbent Cooler
12. High Temperature Heat Exchange Fluid 1.'TCS Reactor Recycle Gas Heater 2. 'HC1 Vaporizer 3. Tet Vaporizer 4. Heat Nitrogen to Regnerate Char.
Adsorbers 5. TCS Reactor
13. Nitrogen 1. Regenerate Charcoal Adsorbers
(192.2) .(88.4)
(2986.0)
(137.9) (379.3)
(6.591 x 103 ) (4.466 x 102) (2.464 x 104 ) (70.95)
(1.491 x 103)
(5.54)
30788.0 BTU
280.6 BTU
3503.2 BTU
3.324 x 104 BTU
5.54 SCF
~
"Tl)
M
.G.
Sil
ico
n
Sto
rag
e H
oppe
r
L (T
2)
Hyd
roge
n S
tora
ge
Tan
k
3.
(T3)
L
iqu
id H
el
Sto
rag
e T
Ank
4.
(T4)
R
ecy
cle
TET
Sto
rag
e
5.
(TS)
TC
S R
eact
or
Off
-G
as F
lash
Tan
k
6.
(T6)
T
CS/
TE
T
St.
ora
ge
7.
(T7
) #
l D
isti
llati
on
C
olum
n C
on
den
sate
A
ccu
mu
lato
r
8.
~Ta)
#1
Red
istr
ibu
tio
n
Rea
cto
r F
eed
Tan
k
9.
(T9)
#
1
Red
istr
ibu
tio
n
Rea
cto
r P
rod
uct
T
ank
CA
SE
A
TA
BLE
11
1\ -
L'~ 5
A
I,1ST
OF
MA
JOR
PRO
CES
S E
QU
IPM
EN
T
FOR
SIL
AN
E
PRO
CES
S -
CA
SE
A
(UN
IGtl
C
AR
BID
E)
Fu
ncti
on
D
uty
.Raw
Mat~ria1 St~rage
2 w
eeks
st
ora
ge
-~~---
Ra
w M
ate
rial
Sto
rag
e
8·h
ou
rs·h
ack
up
fo
r p
ipeli
ne f
ail
ure
P4W
M
ate
rial
Sto
rag
e
2 w
eek
s st
ora
ge
Fo
r T
CS
Rea
cto
r F
eed
2
day
s &
tora
ge
Ph
ase
sep
ara
tio
n
Fee
d D
isti
l1ato
n
Col
umn
#1
Ref
lux
fe
ed
; co
lum
n C
on
tro
l
Ho
ld-u
p a
nd
fe
ed
Reacto
r
Ho
ld-u
p a
nd
fe
ed
#2
D
isti
llati
on
C
olum
n
2 D
ays
ho
ld-u
p
20
min
ute
s h
old
-up
2 d
ays
ho
ld-u
p
2 d
ays
ho
ld-u
p
Mate
rials
S
ize
of
Co
nst
ructi
on
4 1
.36
3 x
1
0
gall
on
s cs
9.1
61
x
10
4 g
all
on
s 2
50
P
SIA
(s
ph
eri
cal)
1.6
12
x
104
gall
on
s 2
50
PS
IA,
-SO
op
(s
ph
eri
cal)
1.9
85
x
10
5 g
all
on
s 65
P
SIA
1 ft.
d
iam
eter
by
4 ft
. lo
ng
, 65
PS
IA, O~F
65
P
SIA
S 1
.96
6
x 1
0 '
g
all
on
s 65
P
ISA
4.8
8
x 1
03
gall
on
s 65
:'
SIA
2.2
66
x
10
5 g
all
on
s 65
PS
IA
2.2
1
x 1
05
g
all
on
s 65
P
SIA
cs
Nic
kel
Ste
el
cs
C5
cs
cs
cs
cs
CA
SE
A
TAB
LE
lIA
-l.S
A
(co
nti
nu
ed)
10
. (T
IO)
#2
Dis
till
ati
on
R
eflu
x
feed
; co
lum
n
Col
umn
Co
nd
ensa
te
Co
ntr
ol
Acc
um
ula
tor
11
. (T
Il)
#2
Red
istr
ibu
tio
n
Rea
cto
r P
eed
Tan
k
12
. (T
12)
#2
Red
istr
ibu
tio
n
Rea
cto
r P
rod
uct
T
ank
13
. (T
13)
#3 D
isti
llati
on
C
olum
n C
on
den
sate
A
ccu
mu
lato
r
N
14
. (T
14)
#3 D
isti
llati
on
N
C
olum
n C
on
den
sate
T
an
k
15
. (T
IS)
#4 D
isti
llati
on
C
olum
n P
eed
Tan
k
16
. (T
16)
#4
Dis
till
ati
on
C
olum
n C
on
den
sate
A
ccu
mu
lato
r
17
. (T
17)
#4
Dis
till
ati
on
C
olum
n C
on
den
sate
T
an
k
IS.
(TIS
) W
aste
Tan
k
19
. (T
19)
Ab
sorb
er
Pee
d
Ta
nk
20
. (T
20)
Sil
an
e s
tora
ge
Ho
ld-u
p a
nd
fe
ed
Rea
cto
r
Ho
ld-u
p a
nd
fe
ed
#3
Dis
till
ati
on
Col
umn
Ref
lux
fe
ed;
ph
ase
Separation~
colu
mn
co
ntr
ol
Ho
ld-u
p a
nd
re
cy
cle
fe
ed to
#2
Red
istr
ibu
ti
on
R
eact
or
Su
rge
bet
wee
n ab
sorb
er
and
dis
till
ati
on
Ref
lux
fe
ed
; co
lum
n co
ntr
ol
Ho
ld-u
p a
nd
recy
cle
to
#2
R
ed
istr
ibu
tio
n
Rea
cto
r
Co
llect
was
te fo
r T
reat
men
t an
d d
isp
osa
l
Fee
d T
ET to
ab
sorb
er
Fin
al
Pro
du
ct s
tora
ge
20 m
inu
tes
ho
ld-u
p
2 d
ays
ho
ld-u
p
2 d
ays
ho
ld-u
p
6.S
x
104
B
TU
/hr
20 m
inu
tes
ho
ld-u
p
2 d
ays
ho
ld-u
p
2. S
l x
10
BT
U/h
r
2 d
ays
ho
ld-u
p
9.6
3 x
10
3 B
TU
/hr
20
min
ute
s h
old
-up
2 d
ays h~ld-up
9.4
x
10
B
TU
/hr
2 w
eek
sto
rag
e
2 d
ays
sto
rag
e
1 w
eek
. st
ora
ge
3. 1
4 x
1
04
BT
U/h
r
746
gall
on
s 65
PS
IA
1.8
91
x
104
g
all
on
s 65
P
SIA
3.4
6 x
1
04
gall
on
s -4
0°F
, 60
P
5IA
19
4 g
all
on
s SO
p,
60
P5I
A
1.7
x
104
gall
on
s 60
P
SIA
, S
op
4.6
9
x 1
03
gall
on
s 60
P
SIA
18
gall
on
s 50
P
SIA
,-7
°p
2.5
5 x
1
03
gall
on
s 50
P
SIA
, _
7°p
1.3
7S
x
104
g
all
on
s 65
P
SIA
2.4
4
x 1
03
gall
on
s 50
P5I
A
1.5
22
x
10
4 g
all
on
s -4
0°F
, 25
0 P
5IA
55
55
55
55
55
55
55
55
CS
5S
55
CA
SE
A
TAB
LE
IIA
-l.5
A(c
on
tin
ued
)
21
. (T
21)
cau
stic
Sto
rag
e
Raw
M
ate
rial
Sto
rag
e
2 w
eek
s st
ora
ge
2.3
04
x
10
4 g
all
on
s SS
22
. (H
l)
TCS
Rea
cto
r H
eat
Rec
ycl
e g
as
and
2
.34
2 x
1
06
BT
U/h
r 75
2 ft2
C
S R
ecy
cle
Gas
H
eate
r H
ydro
gen
to
550°
C
65
PS
IA
23
. (H
2)
HC
1 V
ap
ori
zer
Hea
t R
eact
ant
to
1.5
87
x
105
BT
U/h
r 34
ft2
CS
55
0°C
65
P
SIA
24
. (H
3)
TET
Vap
ori
zer
Hea
t R
eact
ant
to
8.7
55
x
106
BT
U/h
r 23
81 ft2
CS
55
0°C
65
P
SIA
25.
(H4)
TC
S R
eacto
r R
e-P
has
e se
para
tio
n;
1.0
94
x
107
BT
U/h
r 1
88
2 ft2
C
S/S
S
cy
cle
C
on
den
ser
Rec
ycl
e h
yd
rog
en
65
PS
IA
26.
(H5)
#1
D
isti
llati
on
P
reh
eat
dis
till
ati
on
2
.04
4 x
1
06
BT
U/h
r 16
4 ft
2 CS
IV
C
olum
n P
reh
eate
r fe
ed to
bubbl~ p
oin
t 2
50
P
SIA
.....
27
. (H
6)
111
Dis
till
ati
on
P
rov
ide
Ref
lux
to
1
.29
6 x
1
07
BT
U/h
r 31
89 ft
2 CS
C
olum
n C
on
den
ser
Col
umn
65
PS
IA
28.
(H7)
#1
D
isti
llati
on
P
rov
ide
vap
or
to
2.3
82
x
107
BT
U/h
r 28
18 ft2
C
S C
olum
n R
eb
oil
er
Col
umn
250
PS
IA
29.
(H8)
#2
D
isti
llati
on
P
rov
ide
Re fl
ux
1
.96
x
106
BT
U/h
r 95
6 ft
2
CS
/ss
Col
umn
Co
nd
ense
r to
col
umn
65
PS
IA
30
. (H
9)
#2
Dis
till
ati
on
P
rov
ide
Vap
or
2.6
93
x
107
BT
U/h
r 25
14 ft2
C
S C
olum
n R
eb
oil
er
to C
olum
n 25
0 P
SIA
31
. (H
lO)
#2
Red
istr
ibu
tio
n
vap
ori
ze
Reacta
nts
8
.81
x
105
B
TU
/hr
78 ft
2
CS
/SS
R
eacto
r F
eed
fo
r R
eact
or
250
PS
I A
Vap
or.
izet
'
32
. (H
ll)
#2
Red
istr
ibu
tio
n
Con
dens
e V
apo
r fo
r 1
.06
x
106
B
TU
/hr
306
ft2
C
S/S
S
Reacto
r P
rod
uct
ho
ld-U
p s
tora
ge
60
PS
IA
Co
nd
ense
r
33
. (H
12)
#3
Dis
till
ati
on
V
apo
rize
an
d p
reh
eat
1.0
6 x
1
06 B
TU
/hr
66
ft2
C
S/s
s C
olum
n P
reh
eate
r fe
ed
to C
01
W.;
:"ll
25
0 P
SIA
iV
.1>0
CA
SE
A
TAB
LE
IIA
-l.5
A(c
on
tin
ued
)
34
. (H
13)
#3
Dis
till
ati
on
P
rov
ide
Col
umn
Ref
lux
C
olum
n C
on
den
ser
(Part
ial
Co
nd
ense
r)
35
. (H
14)
#3 D
isti
llati
on
P
rov
ide
Vap
or t
o
Col
umn
Reb
oil
er
Col
umn
36
. (H
IS)
Sil
an
e C
on
den
ser
Co
nd
ense
r F
inal
Pro
d
uct
for
sto
rag
e
37
. (H
16)
#4 D
isti
llati
on
P
rov
ide
Ref
lux
38
.
Col
umn
Co
nd
ense
r
(H17
) #4
D
isti
llati
on
C0
1WlU
l R
eb
oil
er
39
. (H
18)
Ab
sorb
er P
re
co
ole
r
40
. (H
19)
Nit
rog
en H
eate
r
41
. (P
I)
TCS
Rea
cto
r O
ff
Gas
R
ecy
cle
Com
p
ress
or
42
. (P
2)
#1 D
isti
llati
on
C
olum
n F
eed
Pum
p
43
. (P
3)
#1 D
isti
llati
on
Pro
vid
e V
apor
to
co
lum
n
Co
ol
TET
for
ab
sorp
ti
on
col
umn
Hea
t N
itro
gen
to
re
gen
era
te C
har
coal
A
dso
rber
s
Cir
cu
late
Rec
ycl
e G
as
to R
eact
or
Fee
d C
olum
n
Pro
vid
e R
eflu
x a
nd
Col
umn
OV
erhe
ads
rem
ove
ov
erh
ead
Pu
mp
pro
du
ct
44
. C
P4)
#1 D
isti
llati
on
C
olum
n B
ott
om
s P
ump
Rem
ove
Bo
tto
ms
Pro
du
ct t
o T
ET
sto
rag
e
tan
k
7.3
12
x
105
BT
U/h
r
9.6
4 x
10
5 B
TU
/hr
4.9
x
104
BT
U/h
r
8.7
1 x
1
04 B
TU
/hr
1.2
x
105
BT
U/h
r
1.3
5 x
10
5 B
TU
/hr
2.5
2 x
10
4 B
TU
/hr
1.3
6 x
10
3 SC
FM
13
6.5
gpm
244
gpm
69
gpm
593
ft2
6
0 P
SIA
84 ft
2
250
PSIA
53
ft2
25
0 P
SIA
84 ft
2
50 P
SIA
13 ft
2
250
PS
IA
35 ft
2
60
PSI
A
14
.1 f
t2
26
.5 H
ors
epo
wer
75
P
SIA
D
isch
arg
e
106
PSI~
14
.5 B
HP
92
.3
PS
I;
22
.5 B
HP
106
PS
I) 7
.3 B
HP
cs/s
s
cs/S
S
cs/s
s
cs/s
s
cs/S
S
CS
/SS
CS
CS*
cs*
CS*
CS*
CASE
A
TAB
LE
IIA
-I.5
A
(co
nti
nu
ed)
45.
(PS)
P
rocess
Wat
er
Fee
d P
roce
ss
Wat
er
48
.6 g
pm
82
.5 P
SI,
4
BHP
CS
· F
eed
Pum
p to
Was
te
Tre
atm
ent
46
. (P
6)
Cau
stic
Fee
d
Fee
d R
aw M
ate
rial
1 gp
m
11
8 P
SI;
?r4
BA
P SS
Pu
mp
to w
aste
tr
eatm
en
t
47
. (P
7)
#1 R
ed
istr
ibu
-F
eed
TC
S to
Rea
cto
r 79
gp
m
106
PS
I,
8.4
BH
P SS
ti
on
Rea
cto
r F
eed
Pum
p
4B.
(PB
) #2
D
isti
llati
on
F
eed
TC
S/D
CS
sti
ll
76
.6 g
pm
92
.3
PS
I,
7.1
BH
P S5
C
olum
n F
eed
Pum
p
49
. (P
9)
#2
Dis
till
ati
on
P
rov
ide
Ref
lux
an
d
37
.3
gpm
9
2.3
PS
I;
3.4
BH
P 5
5
I\J
Col
umn
Ov
erh
ead
s R
emov
e O
Ver
head
Pro
du
ct
VI
Pum
p
50
. (P
IO)
#2
Dis
till
ati
on
R
emov
e B
ott
om
s P
rod
uct
6
6.7
gp
m
10
6.3
PS
I;
7.1
BPH
SS
C
olum
n B
ott
om
s to
TC
S/T
ET
st
ora
ge ta
nk
Pu
mp
5l.
(P
H)
#2
Red
istr
ibu
tio
n
Fee
d n
cs t
o R
eact
or
13
.4 9
pm
130
PS
I.
1.7
BH
P SS
R
eact
or
Fee
d P
ump
52
. (P
12)
#3
Dis
till
ati
on
F
eed
Sil
an
e S
till
12
9Ft
ll 8
7.3
P
SI,
1
BHP
SS
Col
umn
Fee
d P
ump
53
. (P
13)
#3
Dis
till
ati
on
P
rov
ide
Ref
lux
; R
emov
e 9
.7 g
pm
87
.3
PS
I;
1 BH
P SS
C
olum
n O
Ver
head
O
Ver
head
P
rod
uct
Pu
mp
54
. (P
14)
#3
Dis
till
ati
on
R
emov
e B
ott
om
s P
ro-
5.2
gpm
1
06
.3
PS
I; ~ B
HP
SS
Col
umn
Bo
tto
ms
du
ct
to T
CS/
TE
T T
ank
Pum
p
55
. (P
IS)
#4 D
isti
llati
on
F
eed
TET
S
trip
per
1.6
gpr
n 17
.3
PS
I, ~ B
HP
SS
Fee
d P
ump
* In
l!:l
udes
in
cre
men
tal
hig
her
co
st f
or
specia
l p
uri
ty r
eq
uir
em
en
ts.
56
. (P
l6)
#4 D
isti
llati
on
C
olum
n O
Ver
head
Pu
mp
57
. (P
l7)
#4 D
isti
llati
on
C
olum
n B
ott
om
s Pu
mp
58
. (P
18)
#4 D
isti
llati
on
C
on
den
sate
R
ecy
cle
pu
mp
59
. (P
I9):
Sil
an
e P
rod
uct
:~~~,
Co
mp
ress
or
'i' '.
60
. (P
20)
Was
te
Fee
d P
ump
N ~ 61
. (P
21)
TCS
Rea
cto
r F
eed
P
ump
62
. (P
22)
113
Dis
till
ati
on
C
on
den
sate
R
ecy
cle
Pum
p
63
. (P
23)
Was
te C
oll
ecti
on
Pu
mp
64
. (P
24)
Ab
sorb
er F
eed
Pu
mp
65
. (C
l)
#1
D
isti
llati
on
C
olum
n
CA
SE
A
TAB
LE
IIA
-l.5
A
(co
nti
nu
ed)
Pro
vid
e R
efl
ux
, R
emov
e O
Ver
head
P
rod
uct
Rem
ove
Bo
tto
ms
Pro
du
ct
to A
bso
rber
F
eed
TC
lnk
Rec
ycl
e C
on
den
sate
b
ack
.to
#2
R
ed
istr
ib
uti
on
R
eact
or
Liq
uef
y S
ilan
e fo
r st
ora
ge
Dis
till
ati
on
wast
es
to W
aste
Tre
atm
ent
Fee
d T
ET
to
Rea
cto
r
Rec
ycl
e C
on
den
sate
b
ack
to
#2
R
ed
istr
ibu
ti
on
re
acto
r
Dis
till
ati
.:m
wast
es
to
Was
te
Tan
k
Fee
d C
old
TE
T to
A
bso
rpti
on
Col
umn
Sep
ara
te T
ET
fr
om
TCS
1 gp
m
19
prn
1 g
pm
66 S
CF
f.!
19
prn
69
gpm
5.9
gpm
1 gp
m
I gp
m
95
,22
0 Ib
/hr
of
feed
77
.3
PS
I; ~ B
liP
91
.3 P
SI;
~ B
HP
10
6.3
P
SI;
~
BH
P
250
PSIA
D
isch
arg
e 6
.5
HP
76
.3
PS
I; ~flP
92
.3
PS
I;
6.4
B
HP
92
.3
PS
I; ~
BH
P
87
.3
PS
I; ~
BH
P
87
.3
PS
I; ~
BHP
7.5
6 ft
. d
iam
ete
r 1
00
ft
. ta
ll,
50
tray
s
S5
S5
55
55
CS
CS*
5S
CS
SS
CS
~~
..J
66
. (C
2j
67
. (C
3)
68
. (C
4)
69
. (C
S)
70
. (C
6)
#2
Dis
till
ati
on
C
olum
n
#3
Dis
till
ati
on
C
olum
n
#4 D
isti
llati
on
C
olum
n
Sil
an
e A
bso
rber
Ch
arco
al A
dso
rber
71
. (R
l)
.TC
5 F
luid
ized
B
ed
Rea
cto
r
72
. (R
2)
#1
Red
istr
ibu
ti
on
R
eact
or
73
. (R
3)
#2
Red
ir;t
d.b
u
tio
n
Rea
cto
r
74
. (A
I)
Fin
es S
ep
ara
tor
75
. (A
2)
Was
te
Tre
atm
ent
76
. (A
3)
Hyd
roge
n F
lare
CA
SE
A
TAB
LE
IIA
-l.S
A
(co
nti
nu
ed)
Sep
ara
te T
CS
from
D
C5
Sep
ara
te S
ilan
e
fro
m
oth
er
Ch
loro
sila
nes
Str
ip T
ET
for
use
in
ab
sorb
er
Ab
sorb
Ch
loro
sila
ne
from
Sil
an
e
Acti
vate
d
Car
bo
n A
dso
rb
tio
n o
f S
ilan
e t
o re
m
ove
Tra
ce C
hlo
rosi
lan
e
Pro
du
ces
TCS
from
TE
T M
.G.S
ilic
on
, il
nd
H2
Red
istr
ibu
te
TCS
to
DCS
Red
istr
ibu
te
Des
to
S
ilan
e
R~move
Sil
ico
n F
ines
carr
ied
ov
er
wit
h
TCS
Rea
cto
r O
ff-g
as
Dis
char
ge
inn
ocu
ou
s eff
luen
t
Dis
po
se o
f H
ydro
gen
fro
m W
aste
Tre
atm
ent
48
, 32
1 lb
/hr
of
feed
7344
1
b/h
r o
f fe
ed
1007
.7
lb/h
r o
f fe
ed
81
9.3
lb
/hr
of
vap
or
feed
366
lb/h
r o
f v
apo
r fe
ed
10
.6 f
t.
Dia
met
er
136
ft.
tall
, 68
tr
ay
s
2.0
1 ft.
D
iam
etd
: 2
9 ft
. ta
ll,
29
tray
s
1.0
4 ft
. D
iam
eter
2
8.5
ft
. ta
ll,
38
tray
s
0.8
23
ft
. D
iam
eter
12
ft
. ta
ll,
16
tru
ys
1 ft
. D
iam
eter
7
ft.
tall
(2
),
62
3
Ibs
of
carb
on
C5
5S
SS
55
55
6.2
6 ft
. in
dia
mete
r 55
2
6.5
ft
. ta
ll,
481
tub
es
1",
1
6'
lon
g
2'
Dia
me>
ter
by
15
it.
tfll
l S5
10
42
Ibs
cata
lyst
2.3
4'
Dia
met
er
by
35
Et.
tall
55
1
66
7.2
lb
s cata
lyst
Sta
nd
ard
desi
gn
55
3
0"
Dia
met
er
1 co
lwnn
fo
r ab
sorp
tio
n
£S
+ 1
h
eat
exch
ang
er
to
vap
or-
ize
feed
30 ft
. st
ack
6
" D
iam
eter
CS
CASE 11. TABLE UA-'l,.6A
PRODUCTION LABOR REQUIRl~!'lEN,]'S FOR SILANE PROCESS-CASE A:,(UN!O~;CARBIDE)
i'
Skilled Labor,Han Hours , ' Unit Operation !'ype
\\
1. TCS Production B
2. ,Hydrogen Recycle C
3. Raw Material vapori2:ation C
~. TCS Condensation C
5. TCS/TET separation C
6. #1 Redistribution \, C Reactor
7. DCS/'rCS Separation ,', C
8. #2 Redistibui ton C ,aeactor
9,. Silane Distillation C
10. Silane Absorption C
lI. Silane Purification 11 (adsorption)
12. Silane compression B;'
13. Si1an& tondensation B
14. Materials Handling A ,'"'
15. Waste Treatment B
16. Silicon Fines S!-!paration A·.,
TO'rAL
NOTES:
1. A. Batch Process, of Hul tip1e Small Units B, Average Proce,59 c 1t,utomated Proc-e~s
;'.' <."
Per Da}~ .. Per Ib.Sildne
65 .0085
18 .0023
50 .0065
50 .0065
6? .0081
49 .0064
52 .0068
32 .0042,
32 .0042
28 .0036
36 .0047
23 .0::13
23 .0.03 ,
:60-- .0078
IS .002
59S .0776
2. Man hours/day Uni t',from Figure 4-6', Peters and TirnrnerhCl.t1s (7).
'::J.', -'.
28
Semiskilled Labor Per Da:r Per lb.Silane
48 .0063
48 .0063
2. CASE B - Minimum Process Storage
A summation of ~~e important features of CASE B is presented in the following table:
CASE B
Process •••••••••••.•.•••••••••••••••••••••••••. Silane (Union Carbide) Plant Size ••••••••••••••••••.•.•••••..•.••..••• 1270 MT/year of Silane Process Flow Sheet ••••.•••••••.••• ; •••.••••••.. Original Received from Union Carbide Process Chemistry & Equilibrium •••••••••••..••• From Union Carbide Intermediate Product Storage Considerations •.•. Ninimum Maj?r Process Equipmen't ••.••• , •.••..•.••.•••••• 58 pieces of Process Equipment
The status of preliminary process design activi'':ies inVOlving CASE B, including progress since the last reporting period,:i.s given below for key items :
Prier Current Process Flow Diagram 0% 100% Material Balance 100% 100% Energy Balance 0% 100% PrClperty Data 85%
I! 100%
Equipment Design 0% 100% Production Labor 0% 100%
The detailed status sheet is shown in Table IIA-l.OB, and is rep~esentative of all the activities that coropose the preliminary process design. 7.he flowsheet received from Union Carbide, upon which the design is based, is shown in Figure IIA-l.OB.
The results from the preliminary process design (CASE B) are summa:r.ized in a tabular format parallel to those representing CASE A. These tables are represented by the following guide to enable the reader to quickly locate iterns of interest.
Base Case Conditions ••••••••••••••••••••••••.••• Table IIA-l.lB Reaction Chemistry •••••• .-•••••••••••.••••••••••• Table IIA-l.2B Redistributic:,n Equilibrium •••••••••••••••••••••. Table IIA-I. 3B RB,w Material Requiremel!t •••••••••••••••••••••••• Table IIA-1.4B utility Requirements •••••••••••••••••••.•••.•••• Table IIA-l.4B Major Process Equipment ••••••••••••••••••••••••• Table IIA-I.SB Production Labor Requirements ••••••••••.•••••••• Table IIA-l.6B
29
w
o
~
TA
aLE
II
A-I
.OB
C~EMICAL
ENG
INEE
RIN
G
AN
ALY
SES:
P
RE
LIH
INA
RY
P
RO
CE
SS
D
ES
IGN
A
C"r
IVIT
IES
F
OR
S
ILA
NE
P
RO
CE
SS
-C
AS
E
B
(UN
ION
C
AR
BID
E)
Pre
l.
Pro
cess
D
esi
gn
A
cti
vit
y
1.
Sp
ecif
y
Bas
e C
ase
C
on
dit
ion
s 1
. P
lan
t S
ize
2.
Pro
du
ct
Sp
ecif
ics
"3
. A
dd
i tio
nal
Co
nd
i tio
ns
2.
Defi
ne
Reacti
on
C
hem
istr
y
1.
Reacta
nts
, P
rod
ucts
2
. E
qu
ilib
riu
m
" ~
3.
Pro
cess
F
low
D
iag
ram
1
. F
laN
S
eq
uen
ce.
Un
it O
pera
tio
ns
2.
Pro
cess
C
on
dit
ion
s C
T,
P,
etc
.)
,].
En
vir
on
!:le
nta
l '
4 •
CO
o:lp
ar.·
f In
te r
c.c ti
on
(T
ech
no
log
y
r;x
chan
ge)
4.
I'!a
teri
al
E3
1an
ce C
alc
ula
tio
ns
1.
P.aw
H
ate
rials
2
. P
rod
ucts
:
3.
By
-Pro
du
cts
5.
En
erg
y
Bal
.:mr.
<:
Calc
ula
tio
ns
1.
Heati
n'J
2
. C
oo
lin
g
3.
Ad
dit
ion
al
Sta
tus
"
• • • • • • • • I • • I • • • , I • •
Pre
l.
Pro
cess
D
esi
gn
A
cti
vit
y
7.
Eq
uip
men
t D
esi
gn
calc
ula
tio
ns
1.
~torage Vessel~
2.
Un
it O
pera
tio
ns
Eq
uip
men
t 3
. P
rocess
D
ata
(P
, T
, rate
, et·
;.1
4
. M
di t
ion
a I
B.
Lis
t o
f t~a:jor
Pro
cess
E
qu
ipm
en
t
8a.
1.
Siz
e
2.
Ty
pe
3.
Mate
rials
o
f C
on
str
ucti
on
Majo
r T
ech
nic
al
Facto
rs
(Po
ten
tial
Pro
ble
m
Are
as)
1
. H
ate
rials
C
om
pati
bil
ity
2
. P
rocess
C
on
dit
ion
s L
imit
ati
on
s
3.
Ad
di t
ion
al
9.
Pro
du
ctio
n
Lab
or P~quirem0.nt5
1.
i'ro
Cf!
SS
T
ech
no
log
y
2.
Pro
du
cti
on
V
olu
me
W.
Fo
n/a
rd
for
Eco
no
iili
c
i-na
I"! s
is
,5.
Pro
pert
y
Data
• • • •
o P
lan
1
. P
hy
sic
al
2.
The
rmod
ynam
ic
3.
Ad
di t
ion
a1
(jj
In
Pro
gre
ss
• C
om
ple
te
~
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Fig
ure
II
A-l
.OB
Pro
cess
Flo
w S
heet
for
Sil
an
e
Pro
cess
-C
ASE
B
(R
evis
ed,
Pro
vid
ed b
y U
nio
n C
arb
ide)
0:0
~~
~~
~g
~~
QC
"'
~~
r:n
'"C
O
8~
~~
t:j
CASE B
TABLE r::-A-l.lB
BIISE CIISE C"CtlDITIONS FOR SrLA!~E PROCESS-CASE B (Union carbide)
1. Plan t Size - Allow for 10% losses of silane in production of silicon
1270 metric tons/year of silane - Solar cell grade silicon
2. Hydrogenation Reaction - Metallurgical grade silicon, hydrogen,_ to produce trichlorosilane (TCS)
make-up hydrogen chloride used and recycle silicon tetrach10ride(T~T) - Copper catalyzed - F1uidizeCl bed - 550°C. 50 PSIG. - 15.8% cOflversion of SiC14 (Union Carbide :Elowsheet)
3. TCS Redistribution Reaction
4.
s.
6.
7.
8.
- TCS from hydrogenation produces dichlorosilane (DeS) - Catalytic redistribution of TCS with tertiary amine ion exchange resin. - Liquid phase 50 FSIG, 80°C. - Conversion a function of inlet concentration per Figure IIA-2
(Union Carbide equilibrium) - Conversion from pure TCS feed is about 10% to DeS (p.xample) DeS Redistribution Reaction - DeS produces Si!l4 {silane) - Catalytic redistribution of DeS with tertiary amine ion exchange resin. o - Gas phase 60-80 C - Conversion a function of inlet concentration per Figure II~1.1
(union Carbide equilibrium) - Conversion from pure DCS feed is about 14~ to Silane (example) Recycles - Unreacted chlorosilanes separated by distillation and recycled
Silane Purification - Chlorosilanes removed by absorption in _40°C SiC1
4(Tet)
- Trace contaminants removed by carbon adsorption
Operating Ratio - Approximately 90\ utilization - Approximately 7880 hour/year production
Storage Considerations - Feed materials (two week supply) - Product (two week supply) - Process (several days)
32
CASE B
TABLE IIA-l.2B
REACTION CHEMIS'fRY FOR SILANE PROCESS - CASE B (UNION CAFJ3ID~) ri'
1. Hydrogenation Reaction
2. TrichlorosiJ.a.ne Redistribution Reaction
3. Dichlorosilane:Redistribution Reaction (.
Note
3 Siu2
C12
Distillation) 2SiHC13
+ SiP..4
,'j,
1. Reaction 1 Product contains H2
, SiCl4
, SiHCl3
, SiH2
C12
(tl.cace), other trace chlorides
2. Reaction 2 Product contains SiHCl3
, SiCl4
, SiH2
Cl2
, SiH3
Cl
3. Reaction 3 Product contains SiH2
C12
, SiHCl3
, SiCl4
, SiH3
Cl, SiH4
33
CASE B REPRODUCmILITY OF THg ORIGINA!. T':',(e" ;n~r:
t-~'7~'~~'~'I'I'IIIIIIIIIIIIIIIIIIIIIiIlIlIlIlIlIlIlIlIlIlI!II!lill!lilllllilillll!lllilll!!!l1I1 ~~:.t ' ,.,. --' ~ ~':. ::' o r;
Figure IIA-I.l Redistribution Equilibrium For Silane Process-CASE B (Prl11rided by Union Carbide)
CASE B .
TABLE IIA-I. 3 B
RAW MATERIAL RF~UlREMENTS FOR SILANE PROCESS-CASE B (Union Carbide)
Raw Material Requirement
lb/lb of Silane
I. Anhydrous HCI 1.239
2. Hydrogen .362
3. caustic (50%) 2.448
4. M~G. Silicon 1.11
35
CASE B
TABLE IIA - 1.4B
UTILITY REQUIREMENTS FOR SILANE PROCESS - CASE B (UNION CARBIDE)
Utility/F~,~tion
1. Electricity
2.
1. All pump and Compressor t-lotors (16)
Steam 250 Psia 1- #l Distillation Column 2. #l Distillatiol1 ?":olurnn 3. ' #2 Disti lla tion Column
Preheater Reboiler Reboiler
4. #2 Redistribution Reacotr Preheater 5. #3 Distillation Colum.'1 Reboil-ar 6. #4 Distillation Column Reboiler 7. Waste Treatment
3 .. Cooling Water (10-120oF)
4.
5.
6.
7.
8.
1. #1 Distillation Column Condenser 2. #2 Distillation Column Condenser
Process Water (~OoF) 1. Waste Treatment
Refrigerant (-20°F) 1. #3 Distillation Column Condenser 2. #4 Distillation Column Condenser
Refrigerant (-30°F) 1.. TCS Reactor Recycle Gas Condenser
: ° Refrigerant (-40 F) 1. Silane Product,Storage
Refrigerant (-50°F) 1. Product Silane Condenser 2. Abso:cbent Cooler
9. High Temperature Heat Exchange Fluid 1. TCS Reactor Recycle Gas Heater 2. HCl Vaporizer 3. Tet Vaporizer 4. Heat Nitrogen to Regenerate Char.
Adsorbers 5. TCS Reactor
36
Reguirements/lb
.212)
(6.96) (81.18) (91.77)
(3.0) (3.29 ) (0.41) (0.11)
(146.12) (22.09)
(8.22)
(2058.0) (245.2)
(30788.0)
(25.26)
(137.9) (379.3)
(6.591 x 10 3 j (4.46 x 102) ( 2 .464 x 104)
(70.95) (1.491 x 103)
of Silane Product
.212 KW-HR
186.72 Ibs
168.12 gallons
8.22 gallons
2303.2 BTU
30788.0 BTU
25.26 BTU
517.2 BTU
3.324 x 104 BTU
CASE B
TABLE IIA-l.4B (Continued)
Utility/Function Requirements/lb of Silane Product
10. Nitrogen 5.54 SCF 1. Regenerate Charcoal Adsorbers (5.54)
37
~
l-(T
l)
M.G
. S
ilic
on
S
tora
ge H
op
per
2.
(T2)
H
ydro
gen
Sto
rag
e
Tan
k
3.
(T3
) L
iqu
id H
Cl
Sto
rag
e T
ank
4.
(T4)
R
ecy
cle
TET
w
Sto
rag
e
CD
5.
(T5i
TC
S R
p.ac
tor
Off
-G
as
Fla
sh T
ank
6.
(T6)
T
C5/
TE
T
Sto
rag
e
7.
(T7)
11
1 D
isti
llati
on
C
olum
n C
on
den
sate
A
ccu
mu
lato
r
8.
(T8)
#2
D
isti
llati
on
C
olum
n C
on
den
sate
A
ccu
mu
lato
r
9.
(T9
) #3
D
isti
llati
on
C
olum
n C
on
den
sate
A
ccu
mu
lato
r
CA
SE
B
TP.B
LE
IIA
-1
.5B
LIS
T O
P M
AJO
R Pk
OC
ESS
EQU
IPM
ENT
FOR
SILA
NE
PRO
CES
S -
CA
SE
B
(UN
ION
C
AR
BID
E)
Fu
nct
ion
D
uty
Raw
M
ate
rial
Sto
rag
e 2
wee
ks
sto
rag
e
Raw
M
ate
rial
Sto
rag
e 8
ho
urs
b
ack
up
fo
r p
ipeli
ne fa
ilu
re
Raw
I.
w.t
eria
l S
tora
ge
2 w
eek
s st
ora
ge
Fo
r TC
S R
Eac
tor
Fee
d 1
day
st
ora
ge
Ph
ase
Sep
ara
tio
n
Fe~d
Dis
till
ati
on
1
day
h
old
-up
i
Col
umn
III
Ref
lux
fe
ed;
colu
mn
20
min
ute
s h
old
-up
C
on
tro
l
Ref
lux
fe
ed:
colu
mn
20
min
ute
s h
old
-up
co
ntr
ol
Ref
lux
fe
ed;
ph
ase
20
min
ute
s h
old
-up
se
para
tio
n;
colu
mn
co
ntr
ol
Mate
rials
S
ize
of
Co
nst
ructi
on
1.3
63
x
104
g
all
on
s CS
9.1
61
x
104
gall
on
s C
S 25
0 PS
IA
(sp
heri
cal)
1.6
12
x
104
gall
on
s N
ick
el S
teel
250
PS
IA,
-50
°F
(sp
heri
cal)
9.9
23
x
104
gall
on
s CS
65
PS
IA
1 ft
. d
iam
ete
r by
4
ft.
CS
lon
g,
65
PS
IA,
OaF
65
PS
IA
1.9
66
x
105
65
PSIA
4.8
8
x 10
3 g
all
on
s 65
P5
IA
746
gall
on
s 65
PS
IA
194
gall
on
s S
Op.
60
P
5IA
C5
C5
55
55
CA
SE
B
---
TAB
LE
IIA
-l.S
B
(Co
nti
nu
ed)
10
. (T
1D)
~4 D
isti
llati
on
R
eflu
x fe
ed
; co
lum
n 20
m
inu
tes
ho
ld-u
p
18 g
all
on
s S
5 C
olum
n C
on
den
sate
co
ntr
ol
50
PS
IA,
_7°F
T
ank
11
. (T
ll)
Was
te
Tan
k C
oll
ect
was
te
for
2 w
eek
sto
rag
e
1.3
78
x
10
4g
allo
ns
CS
Tre
atm
ent
and
dis
po
sal
65
PS
IA
12
. (T
12)
Sil
an
e S
tora
ge
Fin
al
Pro
du
ct
sto
rag
e
2 d
ays
sto
rag
e
4.3
49
x
103
gall
on
s SS
8
.97
x
103
BT
U/H
r "4
0oF
, 25
0 P
SIJ
\
13
. (T
13)
Cau
stic
Sto
rag
e R
aw
Mate
rial
Sto
rag
e 2
wee
ks
sto
rag
e
2.3
04
x
104
gall
on
s ss
14
. (H
I)
TCS
Rea
cto
r H
eat
Rec
ycl
e g
as
and
2
.34
2
x 10
6 B
TU
/hr
752
ft2
es
Rec
ycl
e G
as
Hea
ter
Hyd
roge
n to
550
0e
65
PSIA
w
\0
1
.58
7
x 10
5 B
TU
/hr
34
Ft2
1
5.
(H2)
H
el
Vap
ori
zer
Hea
t R
eacta
nt
to
CS
55
0°C
65
P
SIA
16
. (H
3)
TE
'f v
ap
ori
zer
Hea
t R
eacta
nt
to
8.7
55
x
106
BT
U/h
r 23
81
ft2
cs
550°
C
65
FS
IA
17
. (H
4)
TCS
Teacto
r R
e-p
has
e se
para
tio
n;
1.0
94
x
107
BT
U/h
r 18
82
ft2
C
S/s
s cj
":::l
e C
on
den
ser
Rec
ycl
e h
yd
rog
en
65
PS
IA
18
. (H
S)
III
Dis
till
ati
on
P
reh
eat
dis
till
ati
on
2
.04
4
x 1
06
BT
U/h
r 1
64
E
t2
CS
Col
umn
Pre
heate
r fe
ed to
b
ub
ble
po
int
250
PS
IA
19
. (H
6)
111
Dis
till
lati
on
P
rov
ide
Ref
lux
to
1
.29
6
x 1
07
BT
U/h
r 31
89
ft2
C
S co
lum
n C
on
den
ser
Col
umn
65
PS
IA
20
. (H
7)
1I1
Dis
till
ati
on
P
rov
ide v
apo
r to
2~3B2
x 1
07
BT
U/h
r 28
18 ft
2
CS
Col
umn
Reb
oil
er
Col
umn
250
PS
IA
.to
o
21
. (H
a)
#2
Dis
till
ati
on
C
olum
n C
on
den
ser
22
. (H
9)
#2
Dis
till
ati
on
C
olum
n R
eb
oil
er
Pro
vid
e R
eflu
x
to c
olum
n
Pro
vid
e V
apor
to
col
unU
l
23
. (H
IO)
#2
Red
istr
ibu
tio
n
Vap
ori
ze
Reacta
nts
R
eacto
r F
eed
fo
r R
p.ac
tor
24
.
._ vap
ori
zer
(Hll
) ~#3
Dis
till
ati
on
C
olum
n C
on
den
ser
25
. (H
12)
#2
Dis
till
ati
on
C
olum
n R
eb
oil
er
26
. (H
I3)
Sil
an
e C
on
den
ser
27
. (H
I4)
#4
Dis
till
at.
ion
C
olum
n C
on
den
ser
28
. (H
I5)
#4 D
isti
llati
on
C
olum
n R
eb
oil
er
29
. (H
I6)
Ab
sorb
er
Pre
co
ole
r
30
. (H
17)
Nit
rog
en
H
eate
r
31
. (P
I)
TC
S
Reacto
r o
ff
Gas
R
ecy
cle
Com
p
ress
or
Pro
vid
e C
olum
n R
eflu
x
(Part
ial
Co
nd
ense
r)
Pro
vid
e V
aPQ
r to
C
olum
n
Co
nd
enso
. F
inal
Pro
d
uct
for
sto
rag
e
Pro
vid
e R
eflu
x
Pro
vid
e V
apor
to
C
olum
n
Co
ol
TET
for
ab
sorp
ti
on
col
umn
Hea
t N
itro
gen
to
re
g
en
era
te
Ch
arco
al
Ad
sorb
ers
Cir
cu
late
P
2cy
cle
Gas
to
R
eact
or
CA
SE
B
TAB
LE
IIA
-l.5
B
(Co
nti
nu
ed)
1.9
6 x
10
6 B
TU
/hr
2.6
93
x
107
BT
U/h
r
8.8
1
x 1
05
BT
U/h
r
7.3
12
x
105
BT
U/h
r
9.6
4
x 10
5 B
TU
/hr
4.9
x
104
BT
U/h
r
8.7
1
x 10
4 B~
J/hr
1.2
x
105
BT
U/h
r
1.3
5
x 10
5 B
TU
/hr
2.5
2
x 10
4 B
TU
/hr
1.. 3
6 x
10
3 SC
FM
956
ft2
65
P
SIA
2514
ft
2
250
PSIA
78
ft2
25
0 PS
IA
593
ft2
60
PS
IA
84
ft2
25
0 P
SIA
53
ftL
25
0 P
SIA
84
ft2
50
PS
IA
13 ft
2
250
PSJA
35
ft2
60
PS
IA
14
.1
ft2
26
.5
Ho
rsep
ow
er
75
PS
IA
Dis
char
ge
CS
/SS
CS
CS
/SS
CS
/SS
CS
/SS
CS
/SS
CS
/SS
CS
/SS
CS
/SS
CS
CS
·
CA
SE
B
TAB
LE
IIA
-1.5
B(C
on
tin
ued
)
32
. (P
2)
ttl
Dis
ti :l
ati
on
F
eed
Col
umn
13
6.5
gp
m
106
PS
I;
14
.5
DH
P C
S·
Col
umn
':"ee
d Pu
mp
33
. (P
3)
III
Dis
tJ,l
lati
on
P
rov
ide
Ref
lux
an
d
244
gpm
9
2.3
P
SI;
2
2.5
BH
P C
S·
Co
lwn
nO
ver
hea
ds
rem
ove
ov
erh
ead
Pu
mp
pro
du
ct
34
. (P
4)
#1
Di5
till
ati
on
R
emov
e B
ott
om
s 69
gp
m
106
PS
I,
7.3
BH
P C
5*
Col
umn
B0
tto
ms
Pro
du
ct to
TET
st
ora
ge
Pum
p ta
nk
3S.
(PS)
P
rocess
\" a
ter
Fee
d
Pro
cess
w
ate
r 4
8.6
gp
m
82
.5
PS
I;
4 B
liP
C5*
F
eed
pu
mf'
to W
aste
Tre
atm
ent
36
. (P
6)
Cau
stic
F
eed
F
eed
R
aw M
ate
rial
1 gp
m
11S
P
SI;
1
/4
BHP
55
~
I-'
37
. (P
7)
#2 D
isti
llati
on
P
rov
ide R
eflu
x
and
3
7.3
gpm
9
2.3
P
SI;
3
.4
BPH
55
C
olum
n O
ver
hea
ds
Rem
ove
Ov
erh
ead
P
rod
uct
Pu
mp
38
. (P
S)
#2
Dis
till
ati
on
R
emov
e B
ott
om
s P
rod
uct
6
6.7
gp
m
10
6.3
PS
I;
7.1
BP
H
55
Col
umn
Bo
tto
ms
to T
CS/
TE
T st
ora
ge
tan
k
Pum
p
39
. (r
9)
#3 D
isti
llati
on
P
rov
ide
Ref
lux
: R
emov
e 9
.7
gpm
8
7.3
P
SI;
1
BliP
S5
C
olum
n O
ver
hea
d
Ov
erh
ead
P
rod
uct
Pu
mp
40
. (P
lO)
#3 D
isti
llati
on
R
emov
e B
ott
om
s P
ro-
5.2
gp
m
10
6.3
P
SI;
1
/2
BliP
SS
C
olum
n B
ott
om
s d
uct
to
TC
S/T
ET
T
ank
Pum
p
..
• In
clu
des
incre
men
tal
hiq
her
co
st
for
specia
l p
uri
ty re
qu
irem
en
ts.
ob
I"
CA
SE a
--'-
-.~;,,
~.
TAB
LE, IIA
-l)~
5B
(Co
nti
nu
ed)
41
. (P
ll)
#4
Dis
till
ati
on
C
oltn
nn O
ver
hea
d
Pum
p
42
. (P
ll)
#4 D
isti
llati
on
C
olum
n B
ott
om
s Pt
nnp
43
. (P
13)
Sil
an
e P
rod
uct
C
om
pre
sso
r
44
. (P
14)
Was
te
Fee
d pu~p
Pro
vid
e R
eflu
x,
Rem
ove
Ov
erh
ead
"P
rod
uct
Rem
ove
Bo
tto
ms
'Pro
du
ct to
Ab
sorb
er
Fee
d T
ank
Liq
uef
y S
ilan
e fo
r S
tora
ge
Dis
till
ati
on
Was
tes
to W
aste
Tre
atm
ent
45
. (P
IS)
TCS'
Rea
cto
r R
eed
Fee
d T
ET to
Rea
cto
r Pu
mp
46
. (P
16)
Was
te C
oll
ecti
on
Pu
mp
47
. (C
l)
#1 D
isti
llati
on
C
olum
n
48
. (C
2)
#2
Dis
till
ati
on
C
olum
n
49
. (e
3)
#3 D
isti
llati
on
C
olum
n
50
. (C
4)
#4 D
isti
llati
on
C
olum
n
51
. (C
5)
Sil
an
e A
bso
rber
Dis
till
ati
on
Was
tes
to
Was
te
Tan
k
Sep
ara
te T
ET
from
TC
S
Sep
ara
te T
CS
from
D
es
sep
ara
te S
ilan
e
fro
m
oth
er
Ch
loro
sila
nes
Str
ip T
ET
for
use
in
ab
sorb
er
Ab
sorb
Ch
loro
sila
ne
from
Sil
an
e
I gp
m
I gp
m
66
SCFM
I'
gp
m
69
gpm
1 gp
m
94
,22
0 lb
/hr
of
feed
,,4
8,3
21
lb
/hr
of
feed
7344
lb
/hr
of
feed
10
07
.7 l
b/h
r o
f fe
ed
81
9.3
/1b
/\1
r o
f v
apo
r fe
ed
* In
clu
des
incre
men
tal
hig
her
co
st fo
r sp
ecia
l p
uri
ty
req
uir
em
en
ts.
77
.3>
PS
I;
1/4
BH
P
91
. 3 1
,PSI
; 1
/4 B
HP
. .
t-·
250
PS
IA b
isch
arg
e
6.5
H
P ,
"
76
.3 P
SI;
1
/4 ,B
HP
92
.3 P
SI;
6
.4,B
HP
, \
'87
.3 psi~
1/4
BH
P'
7.5
6 ft
. d
iam
ete
r IO
cr ,f
t. ta
ll,
"50
tray
s
10
.6 f
t.
Dia
met
er
136
ft.
tall
, 6
8 tr
ay
s
2.0
1 ft.
D
iam
eter
2
9 ft
. ta
ll,
29
tr
ay
s
1.0
4 ft.
D
iam
eter
2
8.5
ft
. ta
ll,
38
tray
s
0.8
23
!ft.
Dia
mete
r 12
,fl
:, ta
ll,
16
tra
ys
SS
SS
55
CS
CS*
CS
C8
C8
SS
SS
88 I
:CA
SEB
--
--\\.
TA
BLE
II
A-l
oS
B
(Co
nti
nu
ed)
52
. {C
6)
Ch
arco
al A
dso
rber
A
cti
vate
d C
arb
on
Ad
sorb
-36
6 lb
/hro
f ti
on
of
Sil
rule
to
rem
ove
vap
Or'
fee
d,
Tra
ce C
hlo
rosi
lan
e
' n
, '
53
. (R
l)
54
. (R
2)
55
. (R
3)
TC
S F
luid
ized
B
ed R
eact
or
#l
Red
istr
ibu
-ti
on
Rea
cto
r (2
)
#2
Red
istr
ibu
-ti
on
Tea
cto
r (2
)
Pro
du
ces
TCS
from
T
ET
,M.G
. S
ilic
on
, an
d
H2 Red
istr
ibu
te
TC5
to
DCS
Red
istr
ibu
te D
es to
S
ilan
e
" "
.t>.
56
. (A
l)
Fin
es
Sep
ara
tor
Rem
ove
Sil
ico
n F
ines
carr
ied
ov
er
wit
h T
CS
Rea
cto
r O
ff-g
as
w
57
. (A
2)
Was
te T
reat
men
t D
isch
arg
e in
no
cuo
us
eff
luen
t
S8
. (A
3)
Hyd
roge
n F
lare
D
isp
ose
of
Hyd
roge
n fr
om w
aste
T
reat
men
t
l,ft.
D
iam
eter
7
ft.
tall
(2
).
623
lbs
of'
car
bo
n
6.2
6 ft
. in
Dia
met
er
26
.5 ft
. ta
ll,
,481
tu
bes
1
" i
16
' lo
ng
'0.';
, '
2' Dian~ter
by
15
ft.
tall
10
42 l
bs
cata
lyst
2.3
4'
Dia
met
er b
y 3
5 ft
. ta
ll 1
66
7.2
lb
s cata
lyst
Sta
nd
ard
desi
gn
3
0"
Dia
mete
r
1 co
lum
n fo
r ad
sorp
tio
n
+ 1
heat
exch
ang
er t
o v
apo
r-iz
e
feed
30 ft
. st
ack
6
" D
iam
eter
55
55
SS
S5
5S
55
cs
CASE B·
TABLE rIA-l.oB
PRODUCTION LABOR REQUIREMENTS FOR SIl..'\NE PROCESS -CASE B (llnion Carbide)
Skilled Unit Operation ~
1. TCS Production B
2. ' . Hydrogen Recycle C
3. Raw Material vaporizat:ion C
II. TCS Condensation C
5. TCS/TET Separation C
0 •. n Redistribution C Reactor
J.'
'7. OCS/TCS Separation C '~ ...
8~ ·412 Redistibuiton C Reactor.
J.,
9. SilanEL Distillation C
" , . ..
10. ' <Silane J\bsorption ::. C ":.' 11. Silane purificatton A
. (adsorption) " "
12. Silane compression B
13, " Silane Conderisation B
' . .:" 14. Materials Handling A
15. Waste Treatment a.
l6~ Silicon Fines Separation A.
;. ,,:.
,. , TOTAL
NOTES:
1. A Batch Process of Multiple Small Units B Average Process c AutomatedcProcess
Per Duy
65
1S
50
SO
62
49
52
32
32
28
36
23
23
60
15
--SQ5
r.abor ,Han Hours Pur lb. Sil ane
.OOSS
.0023
.0065
.0065
.00S1
• (\064
.0068
.0042
.0042
.0036
.00117
.003
.003
.0078
.002
.Q776
2. Man hours/day Unit from l"igure 4-6, Pf)ters alld Timm6rhaus (7).
44
Semiskill ed Labor ~r Day Por lb. Silane
4B .00(53
48 .0063
3. CASE C - Revised Pro~ess
The status cf preliminary process design activities involving Case C is shewn in Table IIA-l.OC, which is representative of all the activities that compose the preliminary process d~sign.
For the silane process, Union Carbide engineering, research and development personnel revised their flowsheet for a more optimum arrangement of major process equipment, raw material requirements a:1d operating conditions. A joint meeing with Union Carbide and Lamar was conducted in late January for initial review of the revised flowsheet and potential lower plant capital investment and lo~er product cost for silane production.
In the revised silane process, the silicon tetrachloride is hydrogenated in a fluidized bed of silicon which is catalyzed by copper. The hydrogenation reaction is conducted at a higher pressure than originally proposed to increase the yeld of desireable trichlorosilane. The gas leaving the fluidized bed reactor is cooled and condensed to recover the liquid chlorosilanes. The hydrogen is recycled.
The condensed liquid chlorosilanes are separated by distillation. The inerts (dissolved gases) are removed in the initial distillation column. The remaining distillation columns separate the liquid chlorosilanes into primarily silicon tetrachloride, trichlorosilane, dichlorosilane and silane. The silicon tetrachloride is recycled back to the hydrogenation reactor. The trichlorosilane and dichlorosilane are sent to the redistribution reactors for rearranement of chlorine/hydrogen bonds to silicon. The final redistribution reactor product is sent to the silane distillation column. The silane is removed from this distillation and sent to product storage.
The initial review of the revised flowsheet for the silane process suggests favorable improvement over the original scheme.
The finalized flowsheet of the revised silane process (Case C) will issue in the next report.
~
0\
CA
SE
C
TA
BL
E
IIA
-1.
OC
C
HE
MIC
AL
E
NG
INE
ER
IUG
lU
1AL
YS
ES
:
PR
EL
IMIN
AR
Y
PR
OC
ES
S
DE
SIG
N
AC
TIV
ITIE
S
FO
R
SIL
AN
E
PR
OC
ES
S-C
AS
E
C
(UN
ION
C
AR
BID
E)
Pre
l.
Pro
cess
D
esig
n A
cti
vit
y
1.
Sp
ecif
y B
ase
Cas
e co
nd
itio
ns
1.
Pla
nt
Siz
e
2.
Pro
du
ct
Sp
ecif
ics
3.
Ad
dit
ion
al
Co
nd
itio
ns
2.
Def
ine
P.e
acti
on
C
hem
istr
y
1.
Reacta
nts
, P
rod
ucts
2
. E
qu
ilib
riu
m
3> P
recess
F
low
D
iag
ram
1
. F
low
Seq
uen
ce,
un
it O
pera
tio
ns
2.
Pro
ces5
Conditio~s
(T,
P,
etc
.)
3.
En
vir
on
men
tal
4.
Com
pany
In
tera
cti
on
(T
ech
no
loT
J E
xch
ang
e)
4.
Mate
rial
Bal
ance
C
alc
ula
tio
ns
1.
Raw
!-
tate
rials
2
. P
rod
ucts
3
. B
y-P
rod
uct
s
5.
En
erT
I B
alan
ce calc
ula
tio
ns
i.
Heati
ng
2
. C
oo
lin
g
3.
Ad
dit
ion
al
6.
Pro
pert
y
Dat
a 1
. P
hy
sical
2.
The
rmod
ynam
ic
3.
Add
i tio
nal
Sta
tus
iii iii
iii iii
iii i iii iii iii 9 iii iii iii iii iii i iii iii
iii iii iii
iii iii iii
Pre
l.
Pro
cess
D
esig
n A
cti
vit
y
7.
Eq
uip
men
t D
esig
n
Calc
ula
tio
ns
S.
Sa.
1.
Stora~e
Vess
els
2
. U
nit
O
pera
tio
ns
Eq
uip
men
t 3
. P
rocess
D
ata
(P,
T,
rate
, etc
.)
4.
Ad
dit
ion
al
Lis
t o
f M
ajo
r P
roce
sS
Eq
uip
men
t 1
. S
ize
2.
Ty
pe
3.
Hate
rials
of
Co
nst
ructi
on
Najo
r T
ech
nic
al
Facto
rs
(Po
ten
tial
Pro
ble
m A
reas
) 1
. H
ate
rials
C
om
pati
bil
ity
2
. P
rocess
C
on
dit
ion
s Limit~tions
3.
Ad
dit
ion
al
9.
Pro
du
cti
on
:'
aho
r R
equ
irem
ents
1
. P
rocess
T
ech
no
log
y
2.
Pro
du
cti
on
'1
olw
ne
10
. F
orw
ard
fo
r E
con
om
ic A
naly
sis
a P
lan
iii
In
Pro
gre
ss
e C
om
ple
te
l>ta
tus
---
o o o o o o o o o o o o o o o o o o
B. OTHER PROCESSES
For other processes under consideration for solar cell grade sificon production, the following technical progress reports are being received and screened;
1. Battelle Process (Zn/SiC14) 2. Union Carbide Process (SiH4) 3. Motorola Process (SiF4/SiF2) 4. Westinghouse Process (Na/SiC14) 5. Dow Process (C/Si02) 6. SRI Process (Na/SiF4) 7. AeroChern Process .' B. J.e. SChumacher'C6. (SiBr4)
47
III. ECONOl-lIC ANALYSES (TASK 3)
A. Silane Process (Union Carbide)
Majoy efforts during thisrepocting period focused on completion of the preliminary economic analysis of the Ur.ion Carbide Silane Process as characterized by the original flowsho:!et received. Two cases are covere,i for the original flowsheet:
Case A - Regular Process Storage
Ca~e B - Minimum Process Storage
In'additional efforts, Union Carbide personnel have revised their original flowsneet for a. more optimumdrrangement of major process equipment, raw mat~rinls and operating conditions:
Case'C -- RcvisE':d Process
Several cost benefits (lower" capital and operating costs) are suggested from initial revie"· of t!te re'vised process.
Each case (A, B'and C) is discussed separately in the following sections.
48
1. CASE A - Regular Process Storage
A summation of ti,~e key results for Cl'.5E A is' presented in the following tahle:
CASE A - Regular Porcess Stol.~age
Process .•...•...........••••...... :'; ' ...•..•.... Silane (Union Plant Size ......••••.•..........•.••... : ......• 1270 MT/year Intermediate Product Storage Consideration ••••. Regular Cost Basis •..•....••.•..•.......••••.•...•.•... 1975 Dollars
Car-bide) Silane
Plant Investment. ..••••.•.•.•..•••......•...••• $19,094,000 . Prod\lct Cost (No Profit) •....•.....••.••••.• ~ .• $5. 54/1b of Silane
The detailed res.u1 ts from the completed preliminary econoni{~ analysis are presented in a tabular format for Case.,'k.-<·Note that all dollar valuEls are given per pound of Silane.instead oi>~r:'--K9~ of sU~con. Th~"gp.ide,~or,. the tabular format is give!} below: . .. , . -, ' -
Preliminary Economic Analysis Activities .... Table IIIA-lo OA Process Design Inputs ..••••....•....••.••••• Table lIIA-l.lA Base Case Conditions •..... , .••..••••.•....... Table IIIA-1.2A Ra~~ Material Cost •..••.•••••.•..•.•.••••••• '. Table IIIA-lo 3A Utility Cost ••. ~ ............................. Table IIIA-1.4A Major Porcess Equipment Cost ......•...•.•• ;.Table IIIA-l.SA Production Labor Cost .••..•......•••••...•.• Table lIIA-1.5A Plant Investment ••..•.•..••••.....•......••• Table IIIA-lo 7A Total Product Cost •••..•.•.......••••••..... Table IIIA-l.BA
49
VI o
CA
SE
A
Tab
le
IlIA
-LO
A
ECO~;oMIC
AN
ALY
SES:
,
PREL
IMIN
AR
Y
ECO
NO
MIC
A
NA
LYSI
S A
CT
IVIT
IES
FOR,~IL1\NE
PRO
C;::S
S C
ASE
A
(U
NIO
N
CA
RB
IDE)
Pre
:!..
Pro
cess
E
con
om
ic A
cti
vit
y
1.
Pro
cess
D
esig
n
Inp
uts
1
. na
.. H
ate
rial
Req
uir
emen
ts
2.
Uti
li ty
R
equ
irem
en ts
3
. E
qu
ipm
ent
Lis
t 4
. l,
ilio
r R
equ
irem
ents
2.
Sp
ecif
y
Bas
e C
ase
Co
nd
itio
ns
1.
Bas
e Y
ear
for
Co
sts
2.
Ap
pro
pri
ate
In
dic
es
for
Co
sts
3.
Ad
dit
ion
al
3.
Ra
w M
ate
rial
Co
sts
1.
Bas
e C
ost
/Lb
. o
f M
ate
rial
2.
Mate
rial
Cast/
lb o
f S
illt
i\e
3.
To
tal
Co
st/l
b o
f S
ilan
e
4.
U~ility
Co
sts
1.
Bas
e C
ost
fo
r E
ach
U
tili
ty
2.
uti
lity
C
ost
/lb
of
Sil
an
e
3.
To
tal
Co
st/l
b o
f S
ila
ne
5.
~Ia~or
Pro
cess
Eq
uip
men
t C
ost
s 1
. In
div
idu
al
Eq
uip
men
t C
ost
2
. co
st
Ind
ex A
dju
stm
ent
Sta
tus
--- • • • • • • • II
• • • • • • • • • • • •
Pre
l.
Pro
cess
E
con
om
ic A
cti
vit
y
6.
Pro
du
ctio
n
Lab
or
Co
sts
1.
Bas
e C
os t
Pe r
Han
H
our
2.
Co
st/
lbS
ilan
e
Per
Are
a 3
. T
ota
l C
os t)l
b S
ilan
e
7.
Est
imati
on
o
f P
lan
t In
vest
men
t 1
. B
att
ery
Lim
its
Dir
ect
Co
sts
2.
Oth
er D
irect
Co
sts
3.
Ind
irect
Cos
ts
4.
Co
nti
ng
ency
5
. T
ota
l P
lan
t In
vest
men
t (F
ixed
Cap
ital)
B.
Est
imati
on
o
f T
ota
l P
rod
uct
Co
at
1.
Dir
ect
Man
ufa
ctu
rin
g C
ost.
2
. In
dir
ect ~ufacturing
Co
st
3.
Pla
nt
Ove
rh
ead
4
. B
y-P
rod
uct
Cre
dit
5
. G
ener
al E
xp
ense
s 6
. T
ota
l C
ost
of
Pro
du
ct
'-:
o P
lan
g
In
Pro
gre
ss
• C
om
ple
te
Sta
tus
• • • • • • • • • • • • • • • • •
TABLE IlIA-lolA
PROCESS DESIGN INPUTS FOR SILANE PROCF.SS - CASE A (UNION CARBIDE)
1. Raw r-laterial Requirements
-!>l.G. Silicon, anhydl-ous HCI, caustic, hydrogen.
-see table for "Raw r-laterial O~st"
2. Utility
-electrical, stearn. cooling water, P~c.
-see table for "Utility Cost"
3. Equipment List
-76 pieces of major process equipment
-process vessels, heat exchangers, reactor. etc.
-see table for "r-lajor Pl-ocessEql'" }ment Cost"
4. Labor Requirements
-pl.'uduction labor for purification, vaporization, product handling, etc.
-see table for "Production Labor Cost"
51
CASE A
TABLE IIIA-1.2A
BASE CASE CONDITIONS FOR SILANE PROCESS-CASE A (UNION CARBIDE)
1'1'. Capital Equipment
-January 1975 Cost lndex for Capital Equipment Cost -January 1974 Cost Inde~ Value = 430
2. Utili ties
-Electrical, Steam, Cooling Water, Nitrogen -January 1975, Cost Index (U.S. Dept. Labor) -Values determined by literatlJre search and sununarized in cost standardization work
3. Raw Material Cost
-Chemical Marketing Reporter -January 1975 Value -Other Sources
4. Labor Cost
-Average for Chemical Petroleum, Coal and Allied Industries (1975) -Skilled $6.90/hr -Semiskilled $4.90/hr
52
Raw Haterial
l. HCl
2. Hydrogen
3. Caustic (50%)
4. M.G. Silicon
CASE A
TABLE II:::A-l. 3A
RAW MATERIAL COST FOR SILANE PROCF.SS - CASE A (UNION CARbIDE)
Requirement S/lb of lb/lb ofSlJ.ane Haterial
1.239 .10
.362 .96
2.448 .0382
1.11 .454
53
Cost $/lb of Silane
.12
.35
.09
.50
l.06/lb Silane
I.
2.
3.
4.
5.
6.
7.
8.
9.
10.
II.
12.
13.
CASE A
TABLE IIIA-1.4 A
UTILITY COST FOR SILANE PROCESS -CASE A (UNION CARBIDE)
Require:nent/lb Cost of Utility of Silane utility
Electricty .253. KW-Hr $ .03/Kw-Hr
Stearn 190.34 lbs 1.25/M lb
Cooling ~-Jater 168.12 gallons .08/M gal
Process water 8.22 gallons .35/M gal
Refrigerant (23 O p) 27.1 BTU 4.75/MM BTU
Refrigerant (Sup) 79.1 BTU 6.40/MM BTU
Ref.z:igerant (_7°p) 26.4 BTU 7.50/MM BTU
Refrigerant (-20o p) 2.3 MBTU 8.70/MM BTU ~. - . .;.'.:"' __ ".0-_:-_-.:,..;;:;
Refrigerant (-30~P) 30.8 M BTU 9.60/MM BTU
Refrigerant (-40op) 369 BTU 10.50/MM.BTU
Refrigerantc (-50o p) 3.5 M BTU 11 .42/MM BTU
High Temperature Heat 3.324 x 104 BTU 3.0/MM BTU Exchange Fluid Nitrogen 5.54 SCP .50/M SCF
54
Cost $/lh of Silane
.0076
.2379
.0134
.0029
.0001
.0005
.0002
.0200
.2957
.0039
.0400
.099
.0028
.724/lb Silane
l.
2.
3.
4.
5.
6.
7.
8.
9.
10.
ii.
12.
13.
14.
15.
16.
17.
18.
19.
20.
2l.
22.
23.
24.
25.
CASE A
TABLE IlIA-1.SA
PURCHASED COST OF MAJOR PROCESS EQUIPMENT FOR SILANE PROCESS -CASE A (UNION CARBIDE)
Equipment (Tl) ~I.G. Silicon Storage Hopper
(T2) Hydrogen Storage Tank
(T3) Liquid HCl Sto=age Tank
(T4) Recycle TET Storage
(T5) TCS Reactor Off-Gas Flash Tank
(T6) TCS/TET Storage
(T7) III Distillation Column Condensate Accumlator
(T8) #1 Redistribution Reactor Feed Tank
(T9) n Redistribution Reactor Product Tank
(TIO), #2 Distillation Column Condensate Accumulator
(Tll) #2 Redistribution Reactor Feed Tank
(T12) #2 Redistribution Reactor Product Tank
(T13) #3 Distillation Column Condensate Accumulator
(T14) #3 Disti llation Column CC'1densate Tank
(TIS)' #4 Distillation Column Feed Tank
(T16) #4 Distillation Column Condensate Accumulator
(TI7) #4 Distillation Column Condensate Tank
(TIS) waste Tank
(T19) Absorber Feed Tank
(T20) Silane Storage
(T21) Caustic storage
(HI) TCS Reactor Recycle Gas Heater
(H2) HC1 Vaporizer
(H3) TET Vaporizer
(H4) TCS Reactor Recycle Condenser
55
Purchased Cost,$lOOO 12.05
179.2
95.27
214,4
0.71
214.4
8.51
244.99
245.0
7.37
76.03
221.17
2.76
'147.44
S3.45
2.76
34.1
17 .01
16.59
255.9
92.15
8.12
1.15
18.48
38.98
CASE A ---
TABLE IIIA-1.5A{continued)
26. (H5) #1 Distillation Column Preheater 3.24
"
27. (H6) , #1 Distillation Column Condenser 22.4
' "
28. (li?) #1 Disdllation ColUmn Reboiler 23.7 p'""
Distiliation 29. (Ha) #2 Column Condenser, 21.08
30. (H9) #2 Distillation Column Reboiler 21.16
31. (HlO) #2 Redistribution Reactor Feed Vaporizer 3 .. 67
32. (HIl)' #2 Redistribution Reactor Product condenser 8.62
33. (H12) #3 Distillation Column Preheater 2.S6
34,. (H13) #3 Distillation Column Condenser 14.95
35". (H14) #3 Disti lla tion Column Reboiler 3.88
36. (HIS) Silane Condenser 2.29
37. (H16) #4 Di~tillation Column Condenser 3.48
3S. (H17) #4 Distillation Column Reboiler 1.33
39. (H18) Absorber Pre-cooler 1. 79 • ,> .,
40. (H19) l-iitrogen Heater .92
41. (PI) TCS Reactor Off~gas Recycle Compressor 35.1
42. (P2) #1 Distillation Column Feed Pump 5.03
43. (P3) #1 Distillation Column Overheads Pump 6.04
44. (P4) #1 Distillation Colum Bottoms Pump 3.5.9
45. (P5) Process Water Feed Pump 2.87
46. (P6) Caustic Feed" Pump 1.25
47. (P7) #1 Redistribution Reactor Feed Pump 4.02
48. (PS) #2 Distillation Column Feed Pump 3.59
49. (P9) #2 Distil1:ltion Column Overheads Pump' 2.57
50. (PIO) #2 Distillation Column Bottoms Pump 3.59
51. (Pll) #2 Redistribution Reactor Feed Pump 2.09
52. (PI2) #3 Distillation Column Feed Pump 1.77
56
TABLE IIIA-1.5A(continued)
53. (P13) #3 Distillation Column .overheads Pump
54. (P14) #3 Distillation Column Bottoms Pump
55. (P1S) #4 Distillation CoJ1.unn. Feed Pump
~,6. (P16:- #4 Distillation Col:umn Overheads Pump
·57. (P17i'. #4 Distillation Column 13ottoms Pump
5S: (P1S) #4 Distillation Condensate Recycle Pump
59. (P19) Silane Product Compressor'
60. (P20) waste Feed Pump
61. (P21) TCS Reactor Feed Pump
62. (P22j #3 Distillation Condensate Recycle Pump
63. (P23) Waste Collection Pump
64. (P24) Absol:'ber Feed Pump
65. (Cl) #1 Distillation Colu~
66. (C2) #2 Distillation Column
67. (C3) #3 Distillation Column
6S. (C4) #4 Distillation Column
69. ,(C5) Silane Absorber
70'. (C6) Charcoal Adsorber
71. (Rl) TCS Fluidized Bed Reactor
72. (R2) #1 Redistribution Reactor
73. (R3) #2 Redistribution Reactor
74. (Al) Fines Separator
75. (A2) waste Treatment
76. '(A3) Hydrogen Flare
TOTAL PURCHASED EQUIPMENT COST
57
1.77
1.47
1.23
1.23.
1,23_: .. ,
1.23
l7.S5
.62
3.31
1.47
.62
1.23
100.66
214.0S
40.19
. 21.14
15.06
lS.0
155.06
13.26
33.14
2.0
18.72
0.10
$3079.31
CASE A
TABLE IlIA-l.6A
PRODUCTION LABOR COST F:OR SILANE PROCESS - CASE A
(UNION CARBIDE),.
Skilled Labor Semiskilled Labor Unit Operation Man-Hrs/l:b Silane Man-Hrs/lb Silane
1- TCS Production .0085 -:,.. ... '
2. Hydrogen Recycle .0023
3. Raw Material Vapo:t'ization .0065
4. TCS Condensation .0065
5~ TCS/TET Separation .0081 .',::: ..
6. #1 Redistribution R~actor .0064
7. DCS/TCS Separation .00G8
8. #2 Redistribution Reactor .0042
9. Silane Distillation .0042 , '
10. Silane Absorption .0036
1l. Silane Purification. (Adsorption) .0047
12. Silane Compression .003
13. Silane Condensation .003
,14. Materials Handling .0063
15. Waste, 'l'reatment .0078
16. Silicon.FiDes Separation " : I· "
,002
TOTAL COST
NOTES
Based"on labor costs of $6.90 skilled, $4. 90 s~..miski11ed. i!
58
Cost Silb of, Silane
.05865
.01587
.04485
.04485
.05589
.04416
, .04692
: .02898
.02898
.02484
.03243
.0207
.0207
.03087
.05382
.0138
$ .'5663/1b of Silane
TABLE UIA -1. 7A
ESTIMATION OF PLANT INVESTMENT FOR SILANE PROCESS - CASE A (UNION CARBIDE)
1. llIhl:C1' PLAllT IN\'I:S1'MENT COSTS 1. ~~ajor Proel'S'; BquipllCnt Cost :2. Installatioll vi ~'<ljor rrocess Equiprrcnt 3. Process Pipill'J, Installed 4. InstrwTentation, In~tal1ed 5. Electrical, Installed 6. Process ~ui1dings, Installed
lao SUB'l~)'rAL FOR 01 Hr.C'l' PLANT INVESTMENT COSTS (PRIMARILY BA'r'!'F.HY LIMIT FACILITIES)
2. O'l1iEH IJIRECT PLANT INVES'l'MENT COSTS 1. Utilities, Installed 2.. General Services, Site Developmnnt,
l-'ire Protection, etc. 3. General Buildings, Offices, Shops, etc. 4. Receiving, Shipping Facilities
2a.. SUI\'ftJ'rr.l, l-'OR Ul'll!::R D1 RECT Pl.I\NT INVESTHENT COSTS (PR: .. :,,\lULY OFFSITE FACILITIES OUTSIDE BATTERY LIMITS)
3. TOTAL DIRECT PLANT INVESTMENT COST, la ~ 2d
4. INDIRECT PLANT INVESTl-\ENT COSTS l~' Engineering, Overhead, e;tc. 2. Normal Cant. for Floods, Strikes, etc.
4a. TOTAL INDIRECT PLANT INVESTMENT COST
5. TOTlIL DIRECT AND INDIRECT PLANT INVESTMENT COST, 3 + 4a
6. OVERALL CONTINGENCY
7. f'IXED CAPITAL INVESTMENT FOR PLANT, 5 + 6
8. WORKING CAPITAL INVES'IMENT FOR PLANT
9. TOTAL PLANT INVESTMENT, 7 + 8
59
Investment $1000
$3079.31 1324.10 2278.69 585.07 307.93 307.93
7883.03
1478.07 369.52
431.10 646.66
2925.35
10808.38
1693.62 2186.31
3879.93
14688.31
4406.49
19094.80
CASE A
TABLE IlIA-I. 8A
ESTIMATION OF TOTAL PRODUCT COST FOR SILANE PROCESS- CASE A (UNION CAlU3IDE)
$/.'lb of Silane
1. Direct Manfacturing Cost (Direct Charges) 1. Raw Materials- from prel. design 2. Dire~t Operating Labor- from prel.
design , 3. Utilities-from prel. design 4. Supervision and Clerical, 5. Maintenance and Repairs.
6. Operating Supplies. 7. Laboratory Charge, 8. Patents and Royalties.
costs
2. Indirect Manufacturing Cost (Fixed Charges) 1. Depreciation 2. Local Taxes 3. Insurance 4. Interest
3. Plant Overhead
4. By-Product Credit- from prel. design
4a. Total Manufacturing Cost, 1 + 2 + 3 + 4
5. General Expenses 1. Administration. 2. Distribution and'Sales.
cost 3. Research and Development,
cost
6. Total Cost of Product, 4a + 5
60
1.06 .5663
.724
.085
.682
.136
.085
.682
.136,
.068
.595
4.819
.289
.289
.145
5~'S4
2. CASE 8 - Minimum P:r:CCti:SS Storage
A summation of the key rtlsults for case B is presented in the following table:
CASE B - Minimum Process storage
Process ..•....•••••••.•••..•.••••••••••••.•••• Silane (Unio11 Carbide) Plant Size ••.•••.•••••••••••.••.•••••••.•••.•• l270 MT/year Silane Intermediate Product Storage Consideration •••• ~linir.:um Cost Bas is .•.••. ' ••••.•.•..•••••.••••.••••••••• 1975 Dollars Plant Investment •••••.•.•.•.••.••••••.•••.•••• $11,l3E,OOO Product Cost (No Prcfit) ..•.•••.•••••..•.••••• $4.58/lb of Silane
The detailed results from the completed preliminary economic analysis are preserlted in a tabular format for Case B. Note tnat all dollc.r values are given per pound of silane instead of per Kg of 8i1i·:;:on. 'lile guide for the tabular format is given below:
preliminary Economic Analysis Activities ••. Tabie IIIA-l.OB Process DeSign Inputs .•..••.••...•.••..•..• Table IIIA-l.IB Base Case Conditions ...•.••.•••••....•.•..• Table lIlA-l.2B Raw Material Cost ...•...•...••..••••••.•.•• Table IIIA-l.3B utili ty Cost •..••••.•....•.•.•.•..•..•.•....• Tal.lle lIlA-I. 4B Major Process Equipment Cost •.•.•..•....••. Table lIIA-l.58 Production Labor Cost ..••••••.••..••....•.. Table lIrA-10GB plant Invcstment •.......•...••••..•••••••.. Table IiIA-l.7B Total Product Cost .•••....•...•.••••..•.••. 'l~able IIIA-l.SB
61
_ CA
SE
B
TABLE-:L~IIA~1.~B
ECO
NO
l-lIC
A
NA
LYSE
S:
PREL
IMIN
AR
Y
ECO
NO
MIC
AN
ALY
SIS
AC
TIV
ITE
S FO
R S
ILA
NE
PRO
CES
S -
CASE
B
(UN
ION
C
AR
BID
E)
CASE B
TABLE IIIA-l.IB
PROCESS DESIGN INPUTS FOR SILANE PROC~S - CASE B (UNION CARBIDE)
1. Raw Material Requirements
~.~.G. Silicon, anhydrous HCl, ca'.lstic, hydrogen.
-see table for "Raw Material Cost"
2. Utility
-electrical, steam, cooling water, etc.
-see table for "Utili ty Cos~"
3. Equipment List
~5a pieces of major process eq~ipment
-process vessels, heat exchanger~~, reactor, etc.
-see table for "Major Process Equi,~ent Cost"
4. Labor R~quirements
-production labor for purification, vaporization, product handling, etc.
-see table for "Production Labor Cost"
63
CASE B
TABLE IIIA-l.2B
BASE CASE CONDITI.JNS FOR
SILANE PROCESS - CASE B (UNION CAR'9IDE)
1. capi tal Equipment
-January 1975 Cost Index for Capital Equipment Cost -January 1976 Cost Index Value = 430
2. Utilities
-Electrical, Steam, Cooling Water, Nitrogen -January 1975 Cost Index (U.S. Dept. Labor) -Values determined by literature search and summarized in cost , standardization work
3. Raw Material Cost
-Chemical ~1arketing Reporter -January 1975 Value -Other Sources
4. Labor Cost
-Average for Chemical Petroleum, Coal and Allied Industries (1975) -Skilled $6.90/hr -Semiskilled $4.90/hr
64
Raw Material
1. HCl
2. Hydrogen
3. Caustic (501t)
·4. ~j ... G. Silicon
CASE B
TABLE IlIA-I. 3B
RAW MATERIAL COS~ FOR SILANE PROCESS-CASE B (UNION CARBIDE)
Requirement $/lb of lb/lb of Silane Material
1.239 .10
.362 .96
2.448 .0382
loll .454
Cost $/lb of Silane
.12
.35
.09
.50
1.06/lb Silane
,~
CASE B
TABLE IIIA-1.4B
UTILITY COST FOR SILANE PROCESS -CASE B (UNION CARBIDE)
Requirement/lb Cost of Utility of Silane Utility
1. Electricty .212 KW-Hr $ .03/KW-Hr
2. Steam 186.72 Ibs 1.25/M 1b
3. Cooling Water 168.12 gallons .08/M gal
4. Process Water 8.22 gallons .35/M gal
5. Refrigerant (-20°F) 2.3 M BTU 8.70/MM BTU
6. Refrigerant (-30°F) 30.8 M BTU 9.60/MM BTU
7. Refrigerant (-40°F) 25.3 BTU 10.SO/MM BTU
8. Refrigerant (-50°F) 517.2 BTU 11.42/MM BTU
9. High Temperature Heat 33.24 M BTU 3.0/MM BTU Exchange Fluid
10. Nitrogen 5.54 SCF .50/M scr
Cost $/lb of Silane
.0064
.2334
.0134
.0029
.0200
.2957
.0003
.0059
.0997
.0028
. 680S/lb Silane
1.
(~., _ .. , .
5 .. (:: ; -. "
( ..
i.
.~ ( l' .. ..
? ! '1" '-:. ~ .
IJ .
. ,., L_.
(" .. ,
14 - (Ii~. ;* .... --
15 , ....... , -- ':'':'1'':,
, , m:l) fT''r'T .1.1;) . ~-, ...
17 {HfJ \ TCS I
16. {H~· ) = .
19 . (i-iG) ;..1
20. (H7) ~l
21- (HS) ;'2
~ :." ". :.. .!.
:·.i
:--
;.. . -. _ ..... ,.; ;:
. '"\ ;..".'
h·";.a::t~_·r F:~ - ---.,; ~,,:..: ... " ... .:.
\,"~I.;:: ri.:::t:-."
REPRoDUClB ,~r "."r 1 ~ li~" :. • 51"-:- ORIGINAL p"lLlTY OF THE
L1GE IS POOR
.'!::.£.
'.~: ~'~'F ;·F~)2:':5~ EQUIPMENT FOR - C'";.~; .. :7, (t.]]~·I~;i~·" CARBI[JE)
~~f"::·".(~~-'ns£!~e ;~ccumulato=-
:~n~ensa~e Accumulator
C:~;·;_j",nsatE: hccumulator
!-leCiter
Purchased Cost, $1000
12.05
.J:i~. 2 .-
95.27
125.55
0.71
214.4
8.51
7.37
2.76
2.76
17.01
82.09
92.15
8.12
1.15
18.48
~~8~C:C~" : < '.-:.~: .::: ~ (,. ';0:1 den SE r 38.98
['·iE-.i 1.::' ':'.": .... C' ~ \.l17~' • P :-e[;eat'2r 3.24
[j...Ls~i~ 1.(",,;. t 1(>.°, C::.,lun!1: COnORTlSer 22.4
Distil lation c-::· 1 u:r.r: Rcl:oi 1 er 23.7
IJis:'':lli!t.!o!~ COlui7'"u'1 Conde::scr 21.08
67
2~. (HE.)
(HI::)
26. (HI::')
*-:. C·.i st.illF1~ion Col U:7'.11
Ci\SF.. B
I. /;
28. (HIS);;~ Distillat!.nn Col'1.l:u1 Reboiler
34. (P4,1 =1 Distillatio:1 C.::.:Lul.!1 Bottclms Pump
36.
37. (P7) "? ,,- Distillation Co 1 UIl'J1 Ovc!:heads Pump
38. (P8) #2 Distillation COIUll:, Bott.oms Fump
39. (?9) #3 Distillation c(·lu;;U1 Overheads Pump
40. (P1O) .:~ ,,~ Distillation Column Bott:oms Pump
4l. (Pll) .... Tr"c! uistillat.:on Col'.l!1U; Overheaas Pwnp
42. (P12) ~4 !:'h:ti llAt ior. Column Bottoms ?ump
43. (P13) Silane Prnnuct COmI!reSSOr
44. (PI4) \'laste Fe(:G Pump
68
21.16
3.67
14.95
3.88
2.29
1. 33
1. 79
.92
35.1
5.03
6.0~
3.59
2.87
1.25
2.57
3.59
1.77
1.47
1.23
1.23
17.55
.62
C.:'SE B
',: ',J1.:' ! ';'J;.-1. C"t, (Continu.-·d)
45. 3.31
46. (PIG} .62
'i -;. (:::] : ~. l.!~,! 11.! ; -. .1, :. 10C·.66
45. (e':) 214.08
49. (C3) <:0.19
50. (C~) 21.14
51- (CS) 15.06
52. (C6) 18.0
53. (Rl i 155.06
s.:;. ( ''', ' r ... _ J 26.52
55. (~.,\
""'I 66.28
5>6. (.Zl.1 ) 2.0
57. (A:) 18.72
58. (,:,3 ) Hydrase:; Fl:ue 0.10
TOTAL PUl-:CH.Zl.5ED EQUIPJ>iENT COST 1796.17
69
CASE B
TABLE I IIl\-l. 6 '~ .
, PR6DUC'l'ION0.Bo~~ COETFDR '·SII ... n.NE PROCES'S -CASE B . ) . (UHrON CARBIDE)'
. ~ I . '
'. ," . ~ .• ' . r' .
."~'
,Ski lle:d Labo!".. . Semiskilled: 'Lithor Uni t Opera U on ... , Han-H rs/l·bSi lane' Man-:Hrs/lb Silane,
1- TCS Production .0065
2~ Hydrogen 'Recycle . .002~ -;t:-
3. Ra ... ~ f-later'ial Vapori::aLion .0005 \'.'j
4; TC'S Condensatioll .0065
5. TCS/TET 'Separation .0081
6. n Redistribu tiClrl. r,eo~~ t· '':: . 0064
7. DC~/TCS Separation .0068
8. #2' Redistribution 'Reactor .0042
9. Silane Distillation .0042
lO. Silane Absorption ;0036
ll. Silane Purification (Adsorption), .0047
l2. Silane Compression . , .003
l3. Silane Condensation .003
L4. Materials Handling .0063
15. Waste:. Treatment .0078
16. Silicon . Fines Separation .002
TOTAL COST
NOTES
Based on labor costs of $6.90 skillad, $4.90 s"'miskilled~
70
Cost S Ill> of Silane
.051865
.01587
.04485
.04485.
.. 05589
.0441&
.04692
.02898
.02898
.02484
.03243
.0207
.0207
.03087
.05382
.0138
$.5663/1b of Silane
l. 2. ., -'.
4. 5. 6.
CASE B
TABLE IIlA-l. 7 8
ES'l'HIlI'l'lOt-: or .1't.tIN1' ) N'.'ES'l'HENT F')R SILANE PROCESS CASE B
(UNION CARBIDE)
r:ajor F ror.c'.~;,-, 1::; Ll t}.:~';.!11 L COS.t Install<lt.icll uf ~I.)jor Process CquiplOOllt
Process Fir ill:1, In~lall0.ci
lnstrurncrltat:icn, lr:!;t,lllco i:lectt"icCll, 1:,!'!;.111t!d
Frocess .D1Jilciiny:>, Irlstal1ed
lao SUBTOTAL F0r~ Dl!'.r:.':T rUIllT W'/ESTI'1Elll' COSTS {PRIH .... rULY BATTE!'Y I.IHIT Fl\CILITIES)
2. OTHER ["lhECT PLi',:,'i' ltr:r.STI·lr.NT COSTS
1. , ~ . 3. 4.
Utilities, tn"f.allca "_~I1\H:ul ~:ervic(~t:, Site L\-:!veloprn.'nt, yile I'rot~·l"li;.m, ctc. ·:;Cp,ul:a.l i 1'.lllulngG, Offices, Shups, e.tc. Rc CC' i ':1n9, f;l: i ['1 in 9 r i1d 1i tics
2 a. SU}!'feTl..!. rOH CTll!.:F 1.'1 PJ.::C'f r'LIINT J N .... 'ES1'HEln COSTS (PRHllIRILY OF1~3lTE FACILITIES ()tJ1'~jI!)G Bl\TTERY LINITS)
3. TOTi\L [;I PoECT PLMl'r nJ\iC:S'fHENT COST, la + 2 a ",
4. {~:(~-'
INDII\ECT Pl.J\Il'(i J:J\'I::;'l~'IENT COSTS 1. Engi:;ceri ng, 1.lverheuc1, o:;tc. 2. NOrtn.ll Cr.Jllt-, for Floods, Strikes, etc.
4a. TOTAL INDIRECT Pl,i\."l'l' INVESTHl:NT COST
5. 'fOTAL DIP.ECT l\l.;() INLJIrmc1' PLlUI'1' IN\'l::STN1Jn COS'i', 3 + 4a
6. OVEHALI, COtl'I'lNGl:NCY
7. FIXED CAPITi\L TNVESTI':ENT FOR PLANT, 5 + 6
8. WOKKING CAPITAL INVESTr-IENT FOR PLANT
9. TOTJU.· PLANT INVES'l'HEN1',. 7 + 8
71
Investmont $11)00
$ 1196.17 772.35
1329.17 341.27 179.62 179.62
4598.2
S62.16 215.54
251.46 377 .20
1706.36
6304.56
9S7.89 1275.28
2263.17
8567.73
2570.32
11138.05
CASE B
TABLE, I,IIA-l. BE:
, ",.-'~!'
ESTlMA1'10N OF TOTAL PRODUCT COST FORSUJ\NE PROCESS -CASE B
nON CARBIDE}
f. Direct Manfacturlng COH (!Hrect Charges) 1., Ra ... ' Materials-, from preL design 2. Direct: Operating Lab,or- from piel.'
design " 3. -Utili,ties-from prel. design 4. "Supervision and Clerica:t; '5. !-lairltcnance and Repairs,
6. Oper~ting Suppl ies, 7. Laboratory Charge, 8. Patents and Royalties,
, costs
2. Indirect Hanufacturing COSl (Fixed Charges) 1. Deereciatfon' 2. Local 'taxes' J. InsU'rance ~. Interest
J!
3. Pllll1 tOverhead,
4. By,:,:Product Cr.edit- from prel. deSign
la. Total l'-ianufacturing Cost, 1 +, 2 + 3 + 4"
5. General E~'Penses L Admini~; t ra tion, cost. 2. Distribution and Sales,
3. Research and Development, cost
Total Cost o( Product, 48 + 5
$/lb of Silane
1.06 .5663
.6805
.0849
.3976
.0795
.0849
.3976
.0795
.0398
, .51
3.9806
.2388
.2388
.1194
4.58
3. CASE C -Revised Process
Initial revi~w of the reviSed silane process (Case C) suggests favorable cost benefits over the original scheme.
Operation of the silicon tetrachloride reaction at higher pressure for increased trichlorosilane yield should lower recycle requirements. Lower.recYcle requirements will lower capital equipment and labor costs. The distillation train as nvw proposed will operate at several hundred pounds pressure compared to original lower pressure. This higher pressure permits use of cooling water in the condensers and does not require expensive low temperature refrigeration as originally proposed. This will provide lower operating (utilities) cost in 3 of the 4 distillation colurr~s. The higher pressure also permits use of smaller diameter columns (vapor loading, density proportional to pressure). The elimination of hydrogen chloride reduces starting material costs. Also, the use of hydrogen from the silane pyrolysis provides additional lower feed materiaLcosts.
The revised silane process (Case C) should provide the following .cost benefits:
-lower capital costs -lower. raw material costs -lower. operating labor costs
73
B. OTHER PReCESSES
The following technical progress reports are baing received and screened for technical information for additional processes under consideration for solar cell grade silicon:
- .' , " '.;\\
, " 1. Battelle Process (Zn!SiC14) 2. Union Carbide Process (SiH4) 3.. Motorola Process (SiF4/siC14) 4. Westinghouse Porcess (Na!SiC14). 5. Dow Proces~(C!Si02) .," 6. SRI prcice~~(Na/SiF 4) 7. AeroChem Process 8. J .C. Schumacher Co. (SiDr4)
74
IV->' SUMMARY - CONCLUSIONS ::..:;. •.. ~
The following suii.mary-conclusions are made as a'result of major activitiesaccomplishad du:i~ing this reporting period:'
::~ Ii : . .~_ Tcisk 1
~~ '~~~~l~sle,:~of pro~ess system pro~~rties, major activitiescfocused on propel:'t:les Of silicQ!1...tetrachloride which is the source material for
], severaValterria'te processe'i;'"'underconsideration for solar cell grade silicon "proCil1dti6ri~:The,s ta tus ~ntl:progre.ss·arerepoited for physical , thermody
namic and transport property data .•
"," .... __ • ,'. I". . • ',:" . Expenmental determination of g&seous thermal conductivity cif silicon sourc~ materials was continued. Initial results 'for gas thermal conductivity of silic,on'tetrafluoride andtrichlorosilane are reported in !espective temperature ranges of,25 to 400°C and 50.to 400 c C.
2. Task 2,:' j, .~:
'. The prelimi~aryprOcess design was completed for the Union Carbide Silane Process' elk characterized.by theo~iginal flowsheet. Two cases were considered for the original floWsheet·: .
• I ".. .
. ... Case A ~ Regular ,proc~ss storage I) :
'. ;\ 'j' , '
~;, ,..Case B -,):1inimum Process Storage ',- ;1
Twd{cases were pr~si:mtedibecause of the large recycle requirements for this process,. necessi tatingconsiderable tankage for mat;erial storage .Th~ major resu;lting differnce between CASES A and B is 76 ver7us 58 pieces of major process equipment. . .
~ , . . ". .',
·-Ti~~1·(;~·:.-:-:-'---~~=--: ':-~, ' ... _"
", Fbr the silane process , union c~rbidEi erigineeri,ng-research persor.itel rev5.sed their flowsheet. The revised process '(Case C) involves a more optImum arrangement 6f major process equipment, raw material requirements
. and'operatirig conditions: . . ,
,& C aseC - Revised Process
A jointmeei.ng with Union Carbide and Lamar was ,conducted during this reporting period for review of the revised flowsheet.·. Initial review results suggest that the revised process. is a fd,vorabl~., ,improvement over the original ,scheme.' "
75'
3. Task 3
The preliminary process design results for Cases A and B were used for economic analyses. Because of the large differences in surge tankage between major unit operations, the fixed capital investment varied from $19,094,000 to $11,138,000 for Cases A and B, respectively. The product cost for Case A is $5.54/1b of silane versus $4.58/lb of silane for Case B.
The initial issue of the revised flowsheet (Case C) for the silane process indicates favorable cost benefits over the original scheme. This includes higher pressure silicon tetrachloride hydrogenation for increased tr j"chlor()silane yield with lower recycle requirements, higher pressure di:i;tillation not requiring expensive low temperature refrigeration, and improved raw material feed requirements. The revised silane process (Case C) should provide the following cost benefits:
-low'er capital cost -lower raw material costs -lower operating labor costs , ,
76
v. PL~S
Plans for the next reporting period are summarized below:
1. Task 1
continue analyses of process system properties for silicon source materials under consideration for solar grade silicon including additional correlation of experimental data.
Experimental thermal ~onductivity data measurements for silicon source materials will be continued with emphasis on chlorinated silanes.
2. Task 2
Continue interactions with Union Carbide on their ·rev:ised silane process (Case C).
Initiate preliminary design of revised silane process using finalized flowsheet.
3. Task 3
Economic analyses will be initiated as preliminary process designs are forwarded.
77
References
l.Bauman, H. C., "Fundamentals of Cost Engineering In the Chemical . Industry ," Reinhold Publishing Corp. ,N. Y. (1964).
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