CN105330683A - Industrial preparation method for t-butyldimethylsilane - Google Patents
Industrial preparation method for t-butyldimethylsilane Download PDFInfo
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- CN105330683A CN105330683A CN201410389184.5A CN201410389184A CN105330683A CN 105330683 A CN105330683 A CN 105330683A CN 201410389184 A CN201410389184 A CN 201410389184A CN 105330683 A CN105330683 A CN 105330683A
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- Prior art keywords
- rectifying tower
- preparation
- silane
- tower
- dmcs
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- ILMRJRBKQSSXGY-UHFFFAOYSA-N tert-butyl(dimethyl)silicon Chemical compound C[Si](C)C(C)(C)C ILMRJRBKQSSXGY-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 20
- BCNZYOJHNLTNEZ-UHFFFAOYSA-N tert-butyldimethylsilyl chloride Chemical compound CC(C)(C)[Si](C)(C)Cl BCNZYOJHNLTNEZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000009835 boiling Methods 0.000 claims abstract description 9
- 238000006462 rearrangement reaction Methods 0.000 claims abstract description 7
- 239000011521 glass Substances 0.000 claims abstract description 4
- 239000002841 Lewis acid Substances 0.000 claims abstract description 3
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 3
- 150000007517 lewis acids Chemical class 0.000 claims abstract description 3
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 28
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 14
- 239000000945 filler Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 235000005074 zinc chloride Nutrition 0.000 claims description 7
- 239000011592 zinc chloride Substances 0.000 claims description 7
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 claims description 4
- 229910015900 BF3 Inorganic materials 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 17
- 239000000463 material Substances 0.000 abstract 2
- 239000000919 ceramic Substances 0.000 abstract 1
- KTQYJQFGNYHXMB-UHFFFAOYSA-N dichloro(methyl)silicon Chemical compound C[Si](Cl)Cl KTQYJQFGNYHXMB-UHFFFAOYSA-N 0.000 abstract 1
- 239000005048 methyldichlorosilane Substances 0.000 abstract 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 28
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 14
- 239000000203 mixture Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000002904 solvent Substances 0.000 description 7
- 238000004821 distillation Methods 0.000 description 6
- 239000005055 methyl trichlorosilane Substances 0.000 description 6
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- GIXWDMTZECRIJT-UHFFFAOYSA-N aurintricarboxylic acid Chemical compound C1=CC(=O)C(C(=O)O)=CC1=C(C=1C=C(C(O)=CC=1)C(O)=O)C1=CC=C(O)C(C(O)=O)=C1 GIXWDMTZECRIJT-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000012280 lithium aluminium hydride Substances 0.000 description 1
- -1 lithium aluminum hydride Chemical compound 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 125000001981 tert-butyldimethylsilyl group Chemical group [H]C([H])([H])[Si]([H])(C([H])([H])[H])[*]C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
Abstract
The invention discloses an industrial preparation method for t-butyldimethylsilane. The method comprises the following steps: subjecting tert-butylchlorodimethylsilane and methyldichlorosilane to a rearrangement reaction at 35 to 45 DEG C under the catalysis of Lewis acid; and then carrying out rectification in a rectifying tower until a boiling state is reached and taking fractions obtained at a temperature of 81 to 83 DEG C, wherein a filling material in the rectifying tower is a structured ceramic or glass filling material, the height of the rectifying tower is 7 to 11 m, the internal diameter of a column of the rectifying tower is 45 to 55 cm, and the interior of the rectifying tower is sealed and dry. The method provided by the invention has the advantages of mild reaction conditions, a high conversion rate and high product purity.
Description
Technical field
The invention belongs to organosilicon technical field, particularly a kind of method of preparation of industrialization t-butyldimethyl silane.
Background technology
T-butyldimethyl silane, No. CAS is 29681-57-0, and molecular formula is C6H15Si, is a kind of hydrogenation reagent, because have active si-h bond in molecule, can provide hydrogen atom in the reaction.At present, in the synthetic method of t-butyldimethyl silane, have and use lithium aluminum hydride to make reductive agent, also have and use red aurin tricarboxylic acid as reductive agent, these methods are all only limitted to laboratory and prepare t-butyldimethyl silane, still can not realize suitability for industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of method of preparation of industrialization t-butyldimethyl silane, to solve the above-mentioned problems in the prior art.
For achieving the above object, technical scheme of the present invention is as follows:
A method for preparation of industrialization t-butyldimethyl silane, comprises the steps:
By TERT-BUTYL DIMETHYL CHLORO SILANE and dimethyl dichlorosilane (DMCS) under lewis acidic catalysis, at 35 ~ 45 DEG C, carry out rearrangement reaction;
Rearrangement reaction product is carried out rectifying to boiling by rectifying tower, gets the cut of 81 ~ 83 DEG C, obtain t-butyldimethyl silane;
Wherein, the filler in described rectifying tower is regular pottery or glass filler, and the tower height of rectifying tower is 7 ~ 11m, and rectifying tower column internal diameter is 45 ~ 55cm, hermetically drying in tower.
Preferably, the mol ratio of described TERT-BUTYL DIMETHYL CHLORO SILANE and dimethyl dichlorosilane (DMCS) is 1:(2 ~ 6).
Preferably, the tower height of described rectifying tower is 9m.
Preferably, described king-post internal diameter is 50cm.
Preferably, the temperature of described rearrangement reaction is 40 DEG C.
Preferably, described Lewis acid is the one in zinc chloride, aluminum chloride, iron(ic) chloride and boron trifluoride.
Preferably, the mol ratio of described TERT-BUTYL DIMETHYL CHLORO SILANE and dimethyl dichlorosilane (DMCS) is 1:(3 ~ 5).
Preferably, the mol ratio of described TERT-BUTYL DIMETHYL CHLORO SILANE and dimethyl dichlorosilane (DMCS) is 1:4.
The present invention to conversion unit and reaction conditions less demanding, can suitability for industrialized production be realized, not adopt tetrahydrofuran (THF) as solvent, avoid the problem of azeotropic.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but protection scope of the present invention is not only confined to embodiment.
The method of embodiment 1 one kinds of preparation of industrialization t-butyldimethyl silane, the method comprises following operation:
Zinc chloride is added after 151kg TERT-BUTYL DIMETHYL CHLORO SILANE being mixed with 210kg dimethyl dichlorosilane (DMCS), react 10 hours at 35 DEG C, obtain the mixture of METHYL TRICHLORO SILANE and t-butyldimethyl silane, this mixture is dropped into rectifying tower, and (tower height of rectifying tower is 7m, rectifying tower column internal diameter is 55cm, filler is regular pottery, hermetically drying in tower.) in, be heated to boiling and carry out atmospheric distillation, get the cut of 81 ~ 83 DEG C, obtain t-butyldimethyl silane product, product purity is 99.98%.
The present invention to conversion unit and reaction conditions less demanding, can suitability for industrialized production be realized, not adopt tetrahydrofuran (THF) as solvent, avoid the problem of azeotropic.
The method of embodiment 2 one kinds of preparation of industrialization t-butyldimethyl silane, the method comprises following operation:
Aluminum chloride is added after 151kg TERT-BUTYL DIMETHYL CHLORO SILANE being mixed with 690kg dimethyl dichlorosilane (DMCS), react 10 hours at 45 DEG C, obtain the mixture of METHYL TRICHLORO SILANE and t-butyldimethyl silane, this mixture is dropped into rectifying tower, and (tower height of rectifying tower is 7m, rectifying tower column internal diameter is 45cm, filler is glass, hermetically drying in tower.) in, be heated to boiling and carry out atmospheric distillation, get the cut of 81 ~ 83 DEG C, obtain t-butyldimethyl silane product.Product purity is 99.97%.
The present invention to conversion unit and reaction conditions less demanding, can suitability for industrialized production be realized, not adopt tetrahydrofuran (THF) as solvent, avoid the problem of azeotropic.
The method of embodiment 3 one kinds of preparation of industrialization t-butyldimethyl silane, the method comprises following operation:
Zinc chloride is added after 151kg TERT-BUTYL DIMETHYL CHLORO SILANE being mixed with 460kg dimethyl dichlorosilane (DMCS), react 8 hours at 40 DEG C, obtain the mixture of METHYL TRICHLORO SILANE and t-butyldimethyl silane, this mixture is dropped into rectifying tower, and (tower height of rectifying tower is 11m, rectifying tower column internal diameter is 45cm, filler is regular pottery, hermetically drying in tower.) in, be heated to boiling and carry out atmospheric distillation, get the cut of 81 ~ 83 DEG C, obtain t-butyldimethyl silane product.Product purity is 99.99%.
The present invention to conversion unit and reaction conditions less demanding, can suitability for industrialized production be realized, not adopt tetrahydrofuran (THF) as solvent, avoid the problem of azeotropic.
The method of embodiment 4 one kinds of preparation of industrialization t-butyldimethyl silane, the method comprises following operation:
Zinc chloride is added after 151kg TERT-BUTYL DIMETHYL CHLORO SILANE being mixed with 345kg dimethyl dichlorosilane (DMCS), react 10 hours at 35 DEG C, obtain the mixture of METHYL TRICHLORO SILANE and t-butyldimethyl silane, this mixture is dropped into rectifying tower, and (tower height of rectifying tower is 9m, rectifying tower column internal diameter is 50cm, filler is regular pottery, hermetically drying in tower.) in, be heated to boiling and carry out atmospheric distillation, get the cut of 81 ~ 83 DEG C, obtain t-butyldimethyl silane product.Product purity is 99.96%.
The present invention to conversion unit and reaction conditions less demanding, can suitability for industrialized production be realized, not adopt tetrahydrofuran (THF) as solvent, avoid the problem of azeotropic.
The method of embodiment 5 one kinds of preparation of industrialization t-butyldimethyl silane, the method comprises following operation:
Zinc chloride is added after 151kg TERT-BUTYL DIMETHYL CHLORO SILANE being mixed with 460kg dimethyl dichlorosilane (DMCS), react 8 hours at 45 DEG C, obtain the mixture of METHYL TRICHLORO SILANE and t-butyldimethyl silane, this mixture is dropped into rectifying tower, and (tower height of rectifying tower is 7m, rectifying tower column internal diameter is 55cm, filler is regular pottery, hermetically drying in tower.) in, be heated to boiling and carry out atmospheric distillation, get the cut of 81 ~ 83 DEG C, obtain t-butyldimethyl silane product.Product purity is 99.99%.
The present invention to conversion unit and reaction conditions less demanding, can suitability for industrialized production be realized, not adopt tetrahydrofuran (THF) as solvent, avoid the problem of azeotropic.
The method of embodiment 6 one kinds of preparation of industrialization t-butyldimethyl silane, the method comprises following operation:
Zinc chloride is added after 151kg TERT-BUTYL DIMETHYL CHLORO SILANE being mixed with 575kg dimethyl dichlorosilane (DMCS), react 10 hours at 35 DEG C, obtain the mixture of METHYL TRICHLORO SILANE and t-butyldimethyl silane, this mixture is dropped into rectifying tower, and (tower height of rectifying tower is 9m, rectifying tower column internal diameter is 50cm, filler is regular pottery, hermetically drying in tower.) in, be heated to boiling and carry out atmospheric distillation, get the cut of 81 ~ 83 DEG C, obtain t-butyldimethyl silane product.Product purity is 99.97%.
The present invention to conversion unit and reaction conditions less demanding, can suitability for industrialized production be realized, not adopt tetrahydrofuran (THF) as solvent, avoid the problem of azeotropic.
Last it is noted that above embodiment only in order to illustrate the present invention and and unrestricted technical scheme described in the invention; Therefore, although this specification sheets with reference to each above-mentioned embodiment to present invention has been detailed description, those of ordinary skill in the art should be appreciated that and still can modify to the present invention or equivalent to replace; And all do not depart from technical scheme and the improvement thereof of the spirit and scope of the present invention, it all should be encompassed in right of the present invention.
Claims (8)
1. a method for preparation of industrialization t-butyldimethyl silane, is characterized in that, comprises the steps:
By TERT-BUTYL DIMETHYL CHLORO SILANE and dimethyl dichlorosilane (DMCS) under lewis acidic catalysis, at 35 ~ 45 DEG C, carry out rearrangement reaction;
Rearrangement reaction product is carried out rectifying to boiling by rectifying tower, gets the cut of 81 ~ 83 DEG C, obtain t-butyldimethyl silane;
Wherein, the filler in described rectifying tower is regular pottery or glass filler, and the tower height of rectifying tower is 7 ~ 11m, and rectifying tower column internal diameter is 45 ~ 55cm, hermetically drying in tower.
2. preparation method according to claim 1, is characterized in that: the mol ratio of described TERT-BUTYL DIMETHYL CHLORO SILANE and dimethyl dichlorosilane (DMCS) is 1:(2 ~ 6).
3. preparation method according to claim 1, is characterized in that: the tower height of described rectifying tower is 9m.
4. preparation method according to claim 1, is characterized in that: described king-post internal diameter is 50cm.
5. preparation method according to claim 1, is characterized in that: the temperature of described rearrangement reaction is 40 DEG C.
6. preparation method according to claim 1, is characterized in that: described Lewis acid is the one in zinc chloride, aluminum chloride, iron(ic) chloride and boron trifluoride.
7. preparation method according to claim 2, is characterized in that: the mol ratio of described TERT-BUTYL DIMETHYL CHLORO SILANE and dimethyl dichlorosilane (DMCS) is 1:(3 ~ 5).
8. preparation method according to claim 7, is characterized in that: the mol ratio of described TERT-BUTYL DIMETHYL CHLORO SILANE and dimethyl dichlorosilane (DMCS) is 1:4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410389184.5A CN105330683A (en) | 2014-08-08 | 2014-08-08 | Industrial preparation method for t-butyldimethylsilane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410389184.5A CN105330683A (en) | 2014-08-08 | 2014-08-08 | Industrial preparation method for t-butyldimethylsilane |
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| CN105330683A true CN105330683A (en) | 2016-02-17 |
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| CN201410389184.5A Pending CN105330683A (en) | 2014-08-08 | 2014-08-08 | Industrial preparation method for t-butyldimethylsilane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108948063A (en) * | 2018-08-09 | 2018-12-07 | 洛阳中硅高科技有限公司 | The preparation method of tetramethylsilane |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4593112A (en) * | 1984-04-17 | 1986-06-03 | Shin-Etsu Chemical Co., Ltd. | Method for the preparation of a tert-hydrocarbyl silyl compound |
-
2014
- 2014-08-08 CN CN201410389184.5A patent/CN105330683A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4593112A (en) * | 1984-04-17 | 1986-06-03 | Shin-Etsu Chemical Co., Ltd. | Method for the preparation of a tert-hydrocarbyl silyl compound |
Non-Patent Citations (2)
| Title |
|---|
| H WESTERMARK 等: ""Infrared Spectra of Alkylsilanes. I"", 《ACTA CHEMICA SCANDINAVICA》 * |
| THOMAS J. BARTON等: ""Sterically Hindered Silyl Perchlorates as Blocking Reagents"", 《CHEMISCHER INFORMATIONSDIENST》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108948063A (en) * | 2018-08-09 | 2018-12-07 | 洛阳中硅高科技有限公司 | The preparation method of tetramethylsilane |
| CN108948063B (en) * | 2018-08-09 | 2020-10-02 | 洛阳中硅高科技有限公司 | Preparation method of tetramethylsilane |
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Application publication date: 20160217 |