CN115010745A - Method for effectively removing high-boiling-point impurities in dimethyldichlorosilane - Google Patents
Method for effectively removing high-boiling-point impurities in dimethyldichlorosilane Download PDFInfo
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- CN115010745A CN115010745A CN202210663032.4A CN202210663032A CN115010745A CN 115010745 A CN115010745 A CN 115010745A CN 202210663032 A CN202210663032 A CN 202210663032A CN 115010745 A CN115010745 A CN 115010745A
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- parts
- dimethyl
- dimethyldichlorosilane
- impurities
- high boiling
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- 239000012535 impurity Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 27
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 40
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 28
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- 238000009835 boiling Methods 0.000 claims abstract description 16
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 15
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 13
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims abstract description 12
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 12
- 239000010948 rhodium Substances 0.000 claims abstract description 12
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 10
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 239000010703 silicon Substances 0.000 claims abstract description 8
- 230000003197 catalytic effect Effects 0.000 claims abstract description 7
- 238000013021 overheating Methods 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000007669 thermal treatment Methods 0.000 claims 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000460 chlorine Substances 0.000 abstract description 5
- 229910052801 chlorine Inorganic materials 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 18
- 239000005046 Chlorosilane Substances 0.000 description 9
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 9
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- 150000002431 hydrogen Chemical class 0.000 description 7
- 239000000178 monomer Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- VNJCDDZVNHPVNM-UHFFFAOYSA-N chloro(ethyl)silane Chemical compound CC[SiH2]Cl VNJCDDZVNHPVNM-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N trimethylsilyl-trifluoromethansulfonate Natural products C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- KTQYJQFGNYHXMB-UHFFFAOYSA-N dichloro(methyl)silicon Chemical compound C[Si](Cl)Cl KTQYJQFGNYHXMB-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
Images
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 System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
-
- 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 System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a method for effectively removing high-boiling point impurities in dimethyldichlorosilane, which comprises the following steps: preheating dimethyl obtained by an organic silicon rectification process, carrying out overheating treatment, and then, allowing dimethyl and an accelerant to enter a catalytic reactor for catalytic reaction to convert ethyl hydrochlorosilane impurities into dimethyl; the accelerant is hydrogen chloride gas or chlorine; the catalyst for the catalytic reaction is an aluminum chloride system, wherein the parts of aluminum chloride are 80-90 parts, the parts of platinum are 3-6 parts, and the parts of rhodium are 3-6 parts.
Description
Technical Field
The invention belongs to the technical field of organic silicon, and particularly relates to a method for effectively removing high-boiling-point impurities in dimethyldichlorosilane.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
At present, in the organosilicon monomer industry, in addition to a target product dimethyldichlorosilane (dimethyl, which accounts for about 85%), a large amount of other chlorosilane byproducts still exist in a methylchlorosilane monomer mixture (crude monomer), wherein the chlorosilane monomer mixture mainly comprises monomethyltrichlorosilane (monomethyl), trimethylmonochlorosilane (trimethyl), methylhydrodichlorosilane (monomethyl contains hydrogen), dimethylhydrogenmonochlorosilane (dimethyl contains hydrogen), low-boiling-point substances, high-boiling-point substances and the like. The crude monomer needs further rectification and purification to obtain dimethyl.
Through years of research, the inventor finds that the boiling point of one of the ethylchlorosilane impurities in the crude monomer is close to that of dimethyl, and the ethylchlorosilane impurity is difficult to remove by means of rectification, so that the quality of the final product of the target product dimethyl is influenced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for effectively removing high-boiling-point impurities in dimethyldichlorosilane, namely, a raw material product is heated and vaporized, a small amount of promoter is added, then the raw material product enters a reactor with a catalyst, the impurities are converted into normal products through catalytic reaction under certain temperature and pressure conditions, and the normal products enter a subsequent system, so that the purity of dimethyl is favorably improved.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for effectively removing high-boiling-point impurities in dimethyldichlorosilane comprises the following steps:
dimethyl obtained by the organic silicon rectification process is preheated and superheated, and then enters a catalytic reactor together with an accelerant for catalytic reaction, so that ethyl hydrochlorosilane impurities are converted into substances with higher boiling points, and the separation of dimethyl and dimethyl is facilitated;
the accelerant is hydrogen chloride gas or chlorine;
the catalyst for the catalytic reaction is an aluminum chloride system, wherein the parts of aluminum chloride are 80-90 parts, the parts of platinum are 3-6 parts, and the parts of rhodium are 3-6 parts.
The beneficial effects of the invention are as follows:
the ethyl hydrochlorosilane impurities in dimethyl can be effectively removed through the over-catalysis reaction, and the purity of dimethyl is improved.
Through research and development, the inventor firstly converts and removes high-boiling impurities close to dimethyl through catalytic reaction under certain reaction conditions, and finally obtains a dimethyl product with higher purity. Therefore, the quality of the dimethyl product can be improved, the quality of subsequent products is correspondingly improved, and the market competitiveness of the products is improved.
The hydrogen chloride gas or chlorine gas promoter has the functions of promoting the breaking of bonds and increasing the selection of chlorine elements.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic diagram of a system for removing high boiling impurities from dimethyldichlorosilane in accordance with one or more embodiments of the present invention.
In the figure: the mutual spacing or size is exaggerated to show the position of each part, and the schematic diagram is only used for illustration;
wherein, the method comprises the steps of 1-preheater, 2-superheater, 3-catalytic reactor, 4-filter and 5-condenser.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
A method for effectively removing high-boiling-point impurities in dimethyldichlorosilane comprises the following steps:
dimethyl obtained by an organic silicon rectification process is preheated and superheated, and then enters a catalytic reactor together with an accelerant to perform catalytic reaction, so that ethyl hydrochlorosilane impurities are converted into substances with higher boiling points;
the accelerant is hydrogen chloride gas or chlorine;
the catalyst for the catalytic reaction is an aluminum chloride system, wherein the parts of aluminum chloride are 80-90 parts, the parts of platinum are 3-6 parts, and the parts of rhodium are 3-6 parts.
In the catalyst, the functions of the components are respectively as follows:
aluminum chloride: as the main carrier of the catalyst, the catalyst mainly provides enough chlorine element to realize ion exchange, generate and obtain a target product and facilitate separation.
Platinum: it is suitable for the occasions of silicon addition and hydrosilylation.
Rhodium: generally, the catalyst is used together with platinum to accelerate the reaction.
In some embodiments, the catalyst comprises 80 to 85 parts aluminum chloride, 4 to 5 parts platinum, and 4 to 5 parts rhodium.
In some embodiments, the post-dimethyl superheat temperature from the silicone rectification process is greater than 120 ℃.
In some embodiments, the volume fraction of promoter added to the dimethyl is 0.1% or less.
In some embodiments, the temperature of the catalytic reaction is 125-135 ℃ and the reaction pressure is 0.1-0.25 MPa.
Preferably, the temperature for the catalytic reaction is 128-.
In some embodiments, the gas velocity in the catalytic reactor is from 0.2 to 0.5m/s and the reaction time is from 5 to 30 s.
The invention is further illustrated by the following examples in conjunction with the drawings.
Example 1
As shown in figure 1, in the dimethyl material, the content of chromatographic detection impurity peaks is about 0.0015%, the dimethyl material is overheated to about 129 ℃ through a heater 2 after being vaporized by a steam preheater 1, hydrogen chloride supplied by a hydrogen chloride cylinder in a laboratory is used as a promoter, and the hydrogen chloride and the overheated dimethyl gas enter a catalytic reactor 3 together, the adding amount of the hydrogen chloride is 0.1% of the volume of the dimethyl material, the reactor is heated by a jacket, the reaction temperature is controlled between 128-131 ℃, and the reaction pressure is 0.2 MPa. In the catalyst, the parts of aluminum chloride, platinum and rhodium are respectively 85 parts, 5 parts and 5 parts.
The reactor adopts ceramic balls as catalyst supports, the catalyst is dried and dehydrated before operation, and in addition, the catalyst cannot be packed tightly and needs to have certain looseness. The reaction time is not less than 30s, impurities are filtered by a filter 4 after being discharged from the bottom of the reactor, and pure liquid dimethyl material is obtained after condensation and recovery by a condenser 5. The impurity peak (ethyl hydrogen chlorosilane) of the finally obtained dimethyl product through chromatographic detection shows that the impurity peak is 0.000 percent.
Example 2
The difference from example 1 is that: the catalyst was prepared in the same manner as in example 1 except that the catalyst was changed to 81 parts by weight of aluminum chloride, 4 parts by weight of platinum and 6 parts by weight of rhodium. The impurity peak (ethyl hydrogen chlorosilane) of the finally obtained dimethyl product through chromatographic detection shows that the impurity peak is 0.000 percent.
Example 3
The difference from example 1 is that: the catalyst was prepared in the same manner as in example 1 except that the amount of aluminum chloride was 90 parts, the amount of platinum was 6 parts, and the amount of rhodium was 3 parts. The impurity peak (ethyl hydrogen chlorosilane) of the finally obtained dimethyl product through chromatographic detection shows that the impurity peak is 0.000 percent.
Comparative example 1
The difference from example 1 is that: the catalyst was the same as in example 1 except that platinum was omitted. The impurity peak (ethyl hydrogen chlorosilane) of the finally obtained dimethyl product through chromatographic detection shows that the impurity peak is 0.0012%.
Comparative example 2
The difference from example 1 is that: the catalyst was the same as in example 1 except that rhodium was omitted. The impurity peak (ethyl hydrogen chlorosilane) of the finally obtained dimethyl product through chromatographic detection shows that the impurity peak is 0.001 percent.
Comparative example 3
The difference from example 1 is that: the catalyst was the same as in example 1 except that platinum and rhodium were omitted. The impurity peak (ethyl hydrogen chlorosilane) of the finally obtained dimethyl product through chromatographic detection shows that the impurity peak is 0.0014%.
Comparative example 4
The difference from example 1 is that: the promoter hydrogen chloride was omitted, and the procedure was otherwise the same as in example 1. The impurity peak (ethyl hydrogen chlorosilane) of the finally obtained dimethyl product through chromatographic detection shows that the impurity peak is 0.0011 percent.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for effectively removing high-boiling point impurities in dimethyldichlorosilane is characterized by comprising the following steps: the method comprises the following steps:
preheating dimethyl obtained by an organic silicon rectification process, carrying out overheating treatment, and then, allowing dimethyl and an accelerant to enter a catalytic reactor for catalytic reaction to convert ethyl hydrochlorosilane impurities into dimethyl;
the accelerator is hydrogen chloride gas or chlorine gas;
the catalyst for the catalytic reaction is an aluminum chloride system, wherein the parts of aluminum chloride are 80-90 parts, the parts of platinum are 3-6 parts, and the parts of rhodium are 3-6 parts.
2. The process for the efficient removal of high boiling impurities in dimethyldichlorosilane as claimed in claim 1 wherein: in the catalyst, the parts of aluminum chloride are 80-85 parts, the parts of platinum are 4-5 parts, and the parts of rhodium are 4-5 parts.
3. The process for the efficient removal of high boiling impurities from dimethyldichlorosilane as claimed in claim 1, wherein: the temperature of dimethyl obtained by the organic silicon rectification process after the dimethyl thermal treatment is more than 120 ℃.
4. The process for the efficient removal of high boiling impurities in dimethyldichlorosilane as claimed in claim 1 wherein: the temperature of the dimethyl heat treatment obtained by the organic silicon rectification process is 125-140 ℃.
5. The process for the efficient removal of high boiling impurities in dimethyldichlorosilane as claimed in claim 1 wherein: the volume fraction of the accelerator added to the dimethyl is 0.1% or less.
6. The process for the efficient removal of high boiling impurities in dimethyldichlorosilane as claimed in claim 5, wherein: the volume fraction of the accelerator added to the dimethyl is 0.01-0.1%.
7. The process for the efficient removal of high boiling impurities in dimethyldichlorosilane as claimed in claim 6 wherein: the volume fraction of the accelerator added into the dimethyl is 0.05-0.1%.
8. The process for the efficient removal of high boiling impurities in dimethyldichlorosilane as claimed in claim 1 wherein: the temperature of the catalytic reaction is 125-135 ℃, and the reaction pressure is 0.1-0.25 MPa.
9. The process for the efficient removal of high boiling impurities in dimethyldichlorosilane as claimed in claim 8, wherein: the temperature of the catalytic reaction was 128-131 ℃.
10. The process for the efficient removal of high boiling impurities in dimethyldichlorosilane as claimed in claim 1 wherein: the gas velocity in the catalytic reactor is 0.2-0.5m/s, and the reaction time is 5-30 s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210663032.4A CN115010745A (en) | 2022-06-13 | 2022-06-13 | Method for effectively removing high-boiling-point impurities in dimethyldichlorosilane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210663032.4A CN115010745A (en) | 2022-06-13 | 2022-06-13 | Method for effectively removing high-boiling-point impurities in dimethyldichlorosilane |
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| CN115010745A true CN115010745A (en) | 2022-09-06 |
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| CN202210663032.4A Pending CN115010745A (en) | 2022-06-13 | 2022-06-13 | Method for effectively removing high-boiling-point impurities in dimethyldichlorosilane |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4985579A (en) * | 1989-10-16 | 1991-01-15 | Dow Corning Corporation | Removal of hydrogen-containing silanes from organosilane mixtures |
| US5292912A (en) * | 1993-07-19 | 1994-03-08 | Dow Corning Corporation | Catalytic conversion of direct process high-boiling component to chlorosilane monomers in the presence of hydrogen chloride |
| US5292909A (en) * | 1993-07-14 | 1994-03-08 | Dow Corning Corporation | Catalytic conversion of direct process high-boiling component to chlorosilane monomers in the presence of hydrogen chloride and hydrogen |
| CN113444121A (en) * | 2021-06-08 | 2021-09-28 | 天津大学 | Method for removing ethyl dichlorosilane impurities in dimethyl dichlorosilane |
| CN113845542A (en) * | 2021-10-29 | 2021-12-28 | 新疆晶硕新材料有限公司 | Method and system for removing ethyl hydride in crude dimethyldichlorosilane |
-
2022
- 2022-06-13 CN CN202210663032.4A patent/CN115010745A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4985579A (en) * | 1989-10-16 | 1991-01-15 | Dow Corning Corporation | Removal of hydrogen-containing silanes from organosilane mixtures |
| US5292909A (en) * | 1993-07-14 | 1994-03-08 | Dow Corning Corporation | Catalytic conversion of direct process high-boiling component to chlorosilane monomers in the presence of hydrogen chloride and hydrogen |
| US5292912A (en) * | 1993-07-19 | 1994-03-08 | Dow Corning Corporation | Catalytic conversion of direct process high-boiling component to chlorosilane monomers in the presence of hydrogen chloride |
| CN113444121A (en) * | 2021-06-08 | 2021-09-28 | 天津大学 | Method for removing ethyl dichlorosilane impurities in dimethyl dichlorosilane |
| CN113845542A (en) * | 2021-10-29 | 2021-12-28 | 新疆晶硕新材料有限公司 | Method and system for removing ethyl hydride in crude dimethyldichlorosilane |
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