CN106279237A - A kind of production method of chloropropyl dichlorosilane - Google Patents
A kind of production method of chloropropyl dichlorosilane Download PDFInfo
- Publication number
- CN106279237A CN106279237A CN201610656326.9A CN201610656326A CN106279237A CN 106279237 A CN106279237 A CN 106279237A CN 201610656326 A CN201610656326 A CN 201610656326A CN 106279237 A CN106279237 A CN 106279237A
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- reactor
- low
- reaction
- still temperature
- dichlorosilane
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- VOVKNAOBZXBVMN-UHFFFAOYSA-N dichloro(3-chloropropyl)silicon Chemical compound ClCCC[Si](Cl)Cl VOVKNAOBZXBVMN-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 39
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000009835 boiling Methods 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- 229920002545 silicone oil Polymers 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 9
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 9
- 239000001632 sodium acetate Substances 0.000 claims abstract description 9
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 9
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004821 distillation Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 9
- OWXJKYNZGFSVRC-NSCUHMNNSA-N (e)-1-chloroprop-1-ene Chemical compound C\C=C\Cl OWXJKYNZGFSVRC-NSCUHMNNSA-N 0.000 claims description 7
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000004886 process control Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 3
- 238000001704 evaporation Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000010668 complexation reaction Methods 0.000 abstract description 2
- 229910052697 platinum Inorganic materials 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- GNVPGBIHGALKRR-UHFFFAOYSA-N dichloro-methyl-propylsilane Chemical compound CCC[Si](C)(Cl)Cl GNVPGBIHGALKRR-UHFFFAOYSA-N 0.000 description 5
- 239000005055 methyl trichlorosilane Substances 0.000 description 5
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 5
- 238000004080 punching Methods 0.000 description 5
- 235000021050 feed intake Nutrition 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 239000005046 Chlorosilane Substances 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 1
- -1 chloropropyl Chemical group 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/14—Preparation thereof from optionally substituted halogenated silanes and hydrocarbons hydrosilylation reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/30—Addition reactions at carbon centres, i.e. to either C-C or C-X multiple bonds
- B01J2231/32—Addition reactions to C=C or C-C triple bonds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0238—Complexes comprising multidentate ligands, i.e. more than 2 ionic or coordinative bonds from the central metal to the ligand, the latter having at least two donor atoms, e.g. N, O, S, P
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/82—Metals of the platinum group
- B01J2531/828—Platinum
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
Abstract
The present invention relates to the production method of a kind of chloropropyl dichlorosilane, belong to organic chemistry filed.The present invention uses isopropanol, acetic acid, phenyl silicone oil etc. to react chloroplatinic acid, then sodium acetate is used to be neutralized, and the part isopropyl alcohol conveying platinum complexation is replaced completely by acetic acid in the basic conditions, thus cause the part of catalyst directly to be replaced by acetic acid and phenyl base silicone oil, avoid catalyst to inactivate in addition process with tri-n-butylamine for promoter after replacement；Mixed feeding reaction is used during synthesis, carry out addition at low temperatures, reaction is continued Deng heating up after having reacted major part, now low-boiling products has been distilled at ambient pressure after having reacted, evaporating before distillation the most under vacuum, the chloropropyl dichlorosilane product of available more than 99.5% after evaporating before having distilled, the product yield of present invention synthesis is high, and the advantage such as production capacity is low, by-product is few, equipment requirements is low, and the most fairly simple.
Description
Technical field
The present invention relates to the production method of a kind of chloropropyl dichlorosilane, belong to organic chemistry filed.
Background technology
Silane coupler is the silane that a class has organo-functional group, has energy and inanimate matter the most simultaneously and has
The chemically combined reactive group of machine material, is widely used in the industrial circles such as surface process, filled plastics.Due to chloropropyl three
Chlorosilane is a class γ substituted propyl type silane coupler of main application on market, causes grinding chloropropyl dichlorosilane
The carelessness studied carefully, along with sending out of market is opened, chloropropyl dichlorosilane is along with the raising of people's living standard in fact, its demand
Also increasing.
Summary of the invention
It is an object of the invention to: provide one have yield compared with high, production capacity is high, low cost, energy consumption are little, by-product is few,
The production method of the chloropropyl dichlorosilane of the advantages such as easy industrialized production.
The technical scheme is that
A kind of production method of chloropropyl dichlorosilane, it is characterised in that: it comprises the following steps:
1), the preparation of catalyst
First be quantitatively adding in the reactor with thermometer, condenser and magnetic agitation chloroplatinic acid, acetic acid, phenyl silicone oil and
Isopropanol, under agitation feeds intake, and temperature of reactor rises to after having fed intake 0.5 hour backward reactor of 100 DEG C of stirrings
In be quantitatively adding sodium acetate and react, after reacting 2 hours, cooling is filtered, and directly distills out different after having filtered under 35 DEG C of low temperature
Propanol, is subsequently adding quantitative tri-n-butylamine and stirs 15 minutes, obtain finished catalyst after distillation, standby；
2), additive reaction
(1) after first the air in reactor being drained with nitrogen, then by chloropropene and methyl hydrogen dichlorosilane by after quantitative batch mixing
Together in press-in measuring tank, the most quantitative catalyst adding above-mentioned preparation in reactor；
(2) step (1) starts to warm up after completing, and will start to keep still from bottom feed, fill process after still temperature rise to 35 DEG C
Temperature is between 37 DEG C ~ 39 DEG C；
(3) according to still temperature control charging rate, whole fill process controls at 200 kgs/hour, after charging 37 DEG C ~
Continue reaction 2 hours between 39 DEG C, after completion of the reaction still temperature rise to 87 DEG C is continued reaction 2 hours, by still temperature rise after having reacted
Between 121 DEG C ~ 123 DEG C, open low boiling and receive tank acceptance receipts low-boiling-point substance, until zero discharge；
(4) low boiling starts cooling after having distilled, and opens water and rush pump and heat up, by still temperature rise to 92 DEG C ~ 94 after still temperature drop to 60 DEG C
Until zero discharge, cooling between DEG C, obtain content chloropropyl dichlorosilane more than 99.5%.
The principle of the present invention
The present invention be use homemade catalyst to carry out the addition of chlorosilane, first by isopropanol, acetic acid, phenyl silicone oil etc.
Carry out complex reaction with chloroplatinic acid, then use sodium acetate to be neutralized, and convey the part isopropyl alcohol of platinum complexation at alkalescence bar
Replaced completely by acetic acid under part, thus cause the part of catalyst directly to be replaced, with three after replacement by acetic acid and phenyl base silicone oil
N-butylamine is that promoter avoids catalyst to inactivate in addition process；Use mixed feeding reaction during synthesis, enter at low temperatures
Row addition, waiting heats up after having reacted major part continues reaction, has now distilled low-boiling products at ambient pressure, then exist after having reacted
Evaporate before distillation under vacuum condition, the chloropropyl dichlorosilane product of available content more than 99.5% after evaporating before having distilled.
The advantage of this patent is:
The product that the present invention makes the homemade catalyst of employing synthesize is higher than the product yield that conventional catalyst synthesizes, production capacity is high,
The advantages such as by-product is few, low cost, energy consumption are low, equipment requirements is low, and be easier to implement in industrialized production.System of the present invention
Standby chloropropyl dichlorosilane product can be directly used for esterification, and yield can reach more than 92%.
Specific embodiments
Embodiment 1:
First in the reaction vessel with thermometer, condenser and stirring, add 50g chloroplatinic acid, 500ml acetic acid, 500ml benzene
Base base silicone oil and 500ml isopropanol, under agitation feed intake, and temperature of reactor rises to after having fed intake 100 DEG C of stirrings 0.5
Adding 50g sodium acetate in hour backward reactor to react, after react 2 hours, cooling is filtered, direct at 35 DEG C after having filtered
Distill out 500ml isopropanol under low temperature, add the most wherein after 50ml tri-n-butylamine stirs 15 minutes and obtain 1050ml catalysis
Agent, standby.
After the air in 2T reactor being drained with nitrogen, first by 765kg chloropropene and 1150kg methyl hydrogen dichlorosilane
Proportionally batch mixing is pressed in measuring tank together, then adds above-mentioned standby catalyst 20ml in reactor, then will be anti-
Answering still temperature rise to start to keep still temperature from bottom feed, fill process between 37 DEG C ~ 39 DEG C to 35 DEG C, the too quickly water of the temperature that rises drops
Temperature, whole fill process controls at 200 kgs/hour, continues reaction 2 hours after having fed between 37 DEG C ~ 39 DEG C, and low temperature is anti-
After Ying, still temperature rise to 87 DEG C be continued reaction 2 hours, by between still temperature rise to 121 DEG C ~ 123 DEG C after pyroreaction is complete, beat
Opening low boiling and receive tank, receive low boiling methyl trichlorosilane 70kg, low boiling starts cooling after having accepted, and opens water punching after being cooled to 60 DEG C
Pump also heats up, by between still temperature rise to 92 DEG C ~ 94 DEG C until zero discharge, evaporate methyl-propyl dichlorosilane 74kg before receipts, final
To the product 1769kg of 99.7% content, yield is 92.4%.
Embodiment 2:
50g chloroplatinic acid, 500ml acetic acid, 500ml phenyl base is added in the reaction vessel with thermometer, condenser and stirring
Silicone oil and 500ml isopropanol, under agitation feed intake, and temperature of reactor rises to after having fed intake 100 DEG C and stirs 0.5 hour
Adding 50g sodium acetate in backward reactor to react, after reacting 2 hours, cooling is filtered, and directly steams at 35 DEG C after having filtered
Distillate 500ml isopropanol, add the most wherein after 50ml tri-n-butylamine stirs 15 minutes and obtain 1050ml catalyst.Standby.
After the air in 2T reactor being drained with nitrogen, first by 765kg chloropropene and 1150kg methyl hydrogen dichlorosilane
Proportionally batch mixing is pressed in measuring tank together, then adds the above-mentioned catalyst 20ml prepared in reactor, then will be anti-
Answering still temperature rise to start to keep still temperature from bottom feed, fill process between 37 DEG C ~ 39 DEG C to 35 DEG C, the too quickly water of the temperature that rises drops
Temperature, whole fill process controls at 200 kgs/hour, continues reaction 2 hours after having fed between 37 DEG C ~ 39 DEG C, and low temperature is anti-
After Ying, still temperature rise to 87 DEG C be continued reaction 2 hours, by between still temperature rise to 121 DEG C ~ 123 DEG C after pyroreaction is complete, beat
Opening low boiling and receive tank, receive low boiling methyl trichlorosilane 67kg, low boiling starts cooling after having accepted, and opens water punching after being cooled to 60 DEG C
Pump also heats up, by between still temperature rise to 92 DEG C ~ 94 DEG C until zero discharge, evaporate methyl-propyl dichlorosilane 72kg before receipts, final
To the product 1774kg of 99.7% content, yield is 92.6%.
Embodiment 3:
Degree meter, condenser and stirring reaction vessel in add 50g chloroplatinic acid, 500ml acetic acid, 500ml phenyl base silicone oil and
500ml isopropanol, under agitation feeds intake, after having fed intake, temperature of reactor is risen to 100 DEG C stirring 0.5 hour backward instead
Answering addition 50g sodium acetate in device to react, after reacting 2 hours, cooling is filtered, and directly distills out at 35 DEG C after having filtered
500ml isopropanol, adds the most wherein after 50ml tri-n-butylamine stirs 15 minutes and obtains 1050ml catalyst.Standby.
After the air in 2T reactor being drained with nitrogen, first by 765kg chloropropene and 1150kg methyl hydrogen dichlorosilane
Proportionally batch mixing is pressed in measuring tank together, then adds the above-mentioned catalyst 20ml prepared in reactor, then will be anti-
Answering still temperature rise to start to keep still temperature from bottom feed, fill process between 37 DEG C ~ 39 DEG C to 35 DEG C, the too quickly water of the temperature that rises drops
Temperature, whole fill process controls at 200 kgs/hour, continues reaction 2 hours after having fed between 37 DEG C ~ 39 DEG C, and low temperature is anti-
After Ying, still temperature rise to 87 DEG C be continued reaction 2 hours, by between still temperature rise to 121 DEG C ~ 123 DEG C after pyroreaction is complete, beat
Opening low boiling and receive tank, receive low boiling methyl trichlorosilane 69kg, low boiling starts cooling after having accepted, and opens water punching after being cooled to 60 DEG C
Pump also heats up, by between still temperature rise to 92 DEG C ~ 94 DEG C until zero discharge, evaporate methyl-propyl dichlorosilane 78kg before receipts, final
To the product 1762kg of 99.7% content, yield is 92.6%.
First in the reaction vessel with thermometer, condenser and stirring add 50g chloroplatinic acid, 500ml acetic acid,
500ml phenyl base silicone oil and 500ml isopropanol, under agitation feed intake, and after having fed intake, temperature of reactor rises to 100 DEG C
Stirring addition 50g sodium acetate in 0.5 hour backward reactor to react, after reacting 2 hours, cooling is filtered, after having filtered directly
At 35 DEG C, distill out 500ml isopropanol, obtain 1050ml after adding the stirring of 50ml tri-n-butylamine the most wherein 15 minutes and urge
Agent.Standby.
After the air in 2T reactor being drained with nitrogen, first by 765kg chloropropene and 1150kg methyl hydrogen dichlorosilane
Proportionally batch mixing is pressed in measuring tank together, then adds the above-mentioned catalyst 20ml prepared in reactor, then will be anti-
Answering still temperature rise to start to keep still temperature from bottom feed, fill process between 37 DEG C ~ 39 DEG C to 35 DEG C, the too quickly water of the temperature that rises drops
Temperature, whole fill process controls at 200 kgs/hour, continues reaction 2 hours after having fed between 37 DEG C ~ 39 DEG C, and low temperature is anti-
After Ying, still temperature rise to 87 DEG C be continued reaction 2 hours, by between still temperature rise to 121 DEG C ~ 123 DEG C after pyroreaction is complete, beat
Opening low boiling and receive tank, receive low boiling methyl trichlorosilane 64kg, low boiling starts cooling after having accepted, and opens water punching after being cooled to 60 DEG C
Pump also heats up, by between still temperature rise to 92 DEG C ~ 94 DEG C until zero discharge, evaporate methyl-propyl dichlorosilane 70kg before receipts, final
To the product 1778kg of 99.7% content, yield is 92.8%.
Embodiment 4:
First in the reaction vessel with thermometer, condenser and stirring, add 50g chloroplatinic acid, 500ml acetic acid, 500ml benzene
Base base silicone oil and 500ml isopropanol, under agitation feed intake, and temperature of reactor rises to after having fed intake 100 DEG C of stirrings 0.5
Adding 50g sodium acetate in hour backward reactor to react, after react 2 hours, cooling is filtered, direct at 35 DEG C after having filtered
Under distill out 500ml isopropanol, add the most wherein after 50ml tri-n-butylamine stirs 15 minutes and obtain 1050ml catalyst.Standby
With.
After the air in 2T reactor being drained with nitrogen, first by 765kg chloropropene and 1150kg methyl hydrogen dichlorosilane
Proportionally batch mixing is pressed in measuring tank together, then adds the above-mentioned catalyst 20ml prepared in reactor, then will be anti-
Answering still temperature rise to start to keep still temperature from bottom feed, fill process between 37 DEG C ~ 39 DEG C to 35 DEG C, the too quickly water of the temperature that rises drops
Temperature, whole fill process controls at 200 kgs/hour, continues reaction 2 hours after having fed between 37 DEG C ~ 39 DEG C, and low temperature is anti-
After Ying, still temperature rise to 87 DEG C be continued reaction 2 hours, by between still temperature rise to 121 DEG C ~ 123 DEG C after pyroreaction is complete, beat
Opening low boiling and receive tank, receive low boiling methyl trichlorosilane 64kg, low boiling starts cooling after having accepted, and opens water punching after being cooled to 60 DEG C
Pump also heats up, by between still temperature rise to 92 DEG C ~ 94 DEG C until zero discharge, evaporate methyl-propyl dichlorosilane 70kg before receipts, final
To the product 1778kg of 99.7% content, yield is 92.8%.
Claims (1)
1. the production method of a chloropropyl dichlorosilane, it is characterised in that: it comprises the following steps:
1), the preparation of catalyst:
First be quantitatively adding in the reactor with thermometer, condenser and magnetic agitation chloroplatinic acid, acetic acid, phenyl silicone oil and
Isopropanol, under agitation feeds intake, and temperature of reactor rises to after having fed intake 0.5 hour backward reactor of 100 DEG C of stirrings
In be quantitatively adding sodium acetate and react, after reacting 2 hours, cooling is filtered, and directly distills out different after having filtered under 35 DEG C of low temperature
Propanol, is subsequently adding quantitative tri-n-butylamine and stirs 15 minutes, obtain finished catalyst after distillation, standby；
2), additive reaction:
(1) after first the air in reactor being drained with nitrogen, then by chloropropene and methyl hydrogen dichlorosilane by after quantitative batch mixing
Together in press-in measuring tank, the most quantitative catalyst adding above-mentioned preparation in reactor；
(2) step (1) starts to warm up after completing, and will start to keep still from bottom feed, fill process after still temperature rise to 35 DEG C
Temperature is between 37 DEG C ~ 39 DEG C；
(3) according to still temperature control charging rate, whole fill process controls at 200 kgs/hour, after charging 37 DEG C ~
Continue reaction 2 hours between 39 DEG C, after completion of the reaction still temperature rise to 87 DEG C is continued reaction 2 hours, by still temperature rise after having reacted
Between 121 DEG C ~ 123 DEG C, open low boiling and receive tank acceptance receipts low-boiling-point substance, until zero discharge；
(4) low boiling starts cooling after having distilled, and opens water and rush pump and heat up, by still temperature rise to 92 DEG C ~ 94 after still temperature drop to 60 DEG C
Until zero discharge, cooling between DEG C, obtain content chloropropyl dichlorosilane more than 99.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610656326.9A CN106279237A (en) | 2016-08-12 | 2016-08-12 | A kind of production method of chloropropyl dichlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610656326.9A CN106279237A (en) | 2016-08-12 | 2016-08-12 | A kind of production method of chloropropyl dichlorosilane |
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| Publication Number | Publication Date |
|---|---|
| CN106279237A true CN106279237A (en) | 2017-01-04 |
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| CN201610656326.9A Pending CN106279237A (en) | 2016-08-12 | 2016-08-12 | A kind of production method of chloropropyl dichlorosilane |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4614812A (en) * | 1985-12-31 | 1986-09-30 | Union Carbide Corporation | Novel process for promoting hydrosilation reactions using a second hydrosilane |
| JP2000256372A (en) * | 1999-03-10 | 2000-09-19 | Dow Corning Asia Ltd | Production of aliphatic chlorosilane by hydrosilylation reaction |
| CN102850388A (en) * | 2011-06-29 | 2013-01-02 | 中国蓝星（集团）股份有限公司 | A preparation method of silane coupling agent |
-
2016
- 2016-08-12 CN CN201610656326.9A patent/CN106279237A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4614812A (en) * | 1985-12-31 | 1986-09-30 | Union Carbide Corporation | Novel process for promoting hydrosilation reactions using a second hydrosilane |
| JP2000256372A (en) * | 1999-03-10 | 2000-09-19 | Dow Corning Asia Ltd | Production of aliphatic chlorosilane by hydrosilylation reaction |
| CN102850388A (en) * | 2011-06-29 | 2013-01-02 | 中国蓝星（集团）股份有限公司 | A preparation method of silane coupling agent |
Non-Patent Citations (2)
| Title |
|---|
| 律微波等: "国内苯基硅油产品现状和应用", 《有机硅材料》 * |
| 胡春野等: "氯铂酸-胺体系催化氯丙烯硅氢化反应的研究", 《分子催化》 * |
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