CN111808129A - Preparation method of trimethylsilanol - Google Patents
Preparation method of trimethylsilanol Download PDFInfo
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- CN111808129A CN111808129A CN202010686915.8A CN202010686915A CN111808129A CN 111808129 A CN111808129 A CN 111808129A CN 202010686915 A CN202010686915 A CN 202010686915A CN 111808129 A CN111808129 A CN 111808129A
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- trimethylsilanol
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- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical compound C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 44
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 26
- 229960000583 acetic acid Drugs 0.000 claims abstract description 22
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000004821 distillation Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims 7
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000002699 waste material Substances 0.000 abstract 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- 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
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0836—Compounds with one or more Si-OH or Si-O-metal linkage
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses a preparation method of trimethylsilanol, which has the technical scheme that: the method specifically comprises the following steps: s1, selecting raw materials: selecting the following components in parts by weight for later use: 550 parts of hexamethyldisilazane, 450-55 parts of glacial acetic acid and 90-110 parts of water; s2, mixing: adding water and glacial acetic acid into a 1000ml four-mouth bottle, uniformly stirring after mixing, and then heating the mixed solution to 60-70 ℃; s3, reaction: adding hexamethyldisilazane dropwise into the mixed solution obtained in the step S2, and reacting for 2-3 h; s4, rectification: distilling the solution obtained in the step S3 to obtain trimethylsilanol with the purity of more than 98%; the preparation method of trimethylsilanol has the advantages of simple raw materials, short manufacturing process, less production waste and the like.
Description
Technical Field
The invention relates to the field of trimethylsilanol preparation, and particularly relates to a preparation method of trimethylsilanol.
Background
Trimethylsilanol has a CAS number of 1066-40-6, also known as trimethylsilanol, trimethylhydroxysilane, trimethylsilanol 25G.
Trimethylsilanol having a boiling point of 100 ℃, a self-ignition point of 395 ℃ and a relative density of 0.8112(20/4 ℃, refractive index of 1.3880(20 ℃), which is easily dehydrated and condensed into hexamethyldisiloxane, can be hydrolyzed from trimethylchlorosilane.
Reference can be made to the existing chinese patent publication No. CN109438499A, which discloses a method for preparing trimethylsilanol, comprising the following steps: s1: adding hexamethyldisilazane and phosphoric acid into a reaction kettle under the stirring condition, wherein the molar ratio of the hexamethyldisilazane to the phosphoric acid is 1: 1-3; s2: after the reaction is carried out for a period of time under the condition of heat preservation, stirring and washing by using a solvent; s3: and standing for layering and then separating to obtain trimethylsilanol.
The above-mentioned method for producing trimethylsilanol has the advantage of less by-products, but the above-mentioned method for producing trimethylsilanol still has some disadvantages, such as: firstly, the controllability is poor during reaction; secondly, the raw materials are relatively complex to use and are more in dosage; thirdly, some byproducts still exist, so that the environmental protection property is not good enough; fourthly, the process is relatively complex and requires post-treatment steps.
Disclosure of Invention
In view of the problems mentioned in the background art, the present invention aims to provide a method for preparing trimethylsilanol, which solves the problems mentioned in the background art.
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of trimethylsilanol specifically comprises the following steps:
s1, selecting raw materials: selecting the following components in parts by weight for later use: 550 parts of hexamethyldisilazane, 450-55 parts of glacial acetic acid and 90-110 parts of water;
s2, mixing: adding water and glacial acetic acid into a 1000ml four-mouth bottle, uniformly stirring after mixing, and then heating the mixed solution to 60-70 ℃;
s3, reaction: adding hexamethyldisilazane dropwise into the mixed solution obtained in the step S2, and reacting for 2-3 h;
s4, rectification: and distilling the solution obtained in the step S3 to obtain trimethylsilanol with the purity of more than 98%.
Preferably, the ammonia gas generated during the S3 reaction is absorbed by a tail gas recovery device.
Preferably, when the raw material is selected in S1, the following components by weight are selected for use: 500 parts of hexamethyldisilazane, 50 parts of glacial acetic acid and 100 parts of water.
Preferably, the yield of trimethylsilanol obtained from the rectification of S4 is 85-90%.
Preferably, when mixing the S2, water and glacial acetic acid are added to a 1000ml four-necked flask, and after mixing and stirring the mixture uniformly, the mixture is heated to 63 to 68 ℃.
Preferably, when the S3 reaction is performed, the HNMR detection means is used to determine that trimethylsilanol is formed.
Preferably, the S4 distillation is carried out by controlling the distillation temperature to be 103-105 ℃ and then condensing.
Preferably, in the mixing of S2, a thermometer is inserted into one of the four-necked bottles, and the mixture is stirred and mixed continuously with a stirring rod in one of the four-necked bottles.
In summary, the invention mainly has the following beneficial effects:
firstly, the process produces and produces trimethylsilanol by four steps of selecting raw materials, mixing, reacting and rectifying, and has simple production process and less post-treatment steps;
secondly, the process is carried out in a titration mode during reaction, the controllability is high, and the production is easy to expand;
thirdly, no solid waste is generated during production of the process, and a small amount of generated waste gas is convenient to treat;
fourthly, the process adopts single raw material, is simple and easy to obtain, and has small dosage.
Drawings
FIG. 1 is a process flow diagram for the purposes of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1, a method for preparing trimethylsilanol specifically includes the following steps:
s1, selecting raw materials: selecting the following components in parts by weight for later use: 450 parts of hexamethyldisilazane, 45 parts of glacial acetic acid and 90 parts of water;
s2, mixing: adding water and glacial acetic acid into a 1000ml four-mouth bottle, uniformly stirring after mixing, and then heating the mixed solution to 60 ℃;
s3, reaction: adding hexamethyldisilazane dropwise into the mixed solution obtained in the step S2, and reacting for 2 hours;
s4, rectification: distilling the solution obtained in S3 to obtain trimethylsilanol with purity of more than 98%.
Wherein ammonia gas generated during the S3 reaction is absorbed by a tail gas recovery device.
Wherein, when S3 reacts, HNMR detection means is used to determine that trimethylsilanol is generated.
Wherein, in the S4 distillation, the distillation temperature is controlled to be 103 ℃ and then condensation is carried out.
In the case of the mixing in S2, a thermometer was inserted into one of the four-necked bottles, and the mixture was stirred and mixed by a stirring rod continuously at one of the four-necked bottles.
The analysis shows that the process produces the trimethylsilanol by four steps of selecting raw materials, mixing, reacting and rectifying, the production process is simple, and the post-treatment steps are few; the process is carried out in a titration mode during reaction, has high controllability and is easy to expand production; in addition, no solid waste is generated during production, and a small amount of waste gas generated is convenient to treat; moreover, the process adopts single raw material, is simple and easy to obtain, and has less consumption.
Example 2
Referring to fig. 1, a method for preparing trimethylsilanol specifically includes the following steps:
s1, selecting raw materials: selecting the following components in parts by weight for later use: 480 parts of hexamethyldisilazane, 45 parts of glacial acetic acid and 100 parts of water;
s2, mixing: adding water and glacial acetic acid into a 1000ml four-mouth bottle, uniformly stirring after mixing, and then heating the mixed solution to 65 ℃;
s3, reaction: adding hexamethyldisilazane dropwise into the mixed solution obtained in the step S2, and reacting for 2.4 hours;
s4, rectification: distilling the solution obtained in S3 to obtain trimethylsilanol with purity of more than 98%.
Wherein ammonia gas generated during the S3 reaction is absorbed by a tail gas recovery device.
Wherein, when S3 reacts, HNMR detection means is used to determine that trimethylsilanol is generated.
Wherein, in the S4 distillation, the distillation temperature is controlled to be 103 ℃ and then condensation is carried out.
In the case of the mixing in S2, a thermometer was inserted into one of the four-necked bottles, and the mixture was stirred and mixed by a stirring rod continuously at one of the four-necked bottles.
Example 3
Referring to fig. 1, a method for preparing trimethylsilanol specifically includes the following steps:
s1, selecting raw materials: selecting the following components in parts by weight for later use: 520 parts of hexamethyldisilazane, 45 parts of glacial acetic acid and 100 parts of water;
s2, mixing: adding water and glacial acetic acid into a 1000ml four-mouth bottle, uniformly stirring after mixing, and then heating the mixed solution to 68 ℃;
s3, reaction: adding hexamethyldisilazane dropwise into the mixed solution obtained in the step S2, and reacting for 3 hours;
s4, rectification: distilling the solution obtained in S3 to obtain trimethylsilanol with purity of more than 98%.
Example 4
Referring to fig. 1, a method for preparing trimethylsilanol specifically includes the following steps:
s1, selecting raw materials: selecting the following components in parts by weight for later use: 550 parts of hexamethyldisilazane, 45 parts of glacial acetic acid and 110 parts of water;
s2, mixing: adding water and glacial acetic acid into a 1000ml four-mouth bottle, uniformly stirring after mixing, and then heating the mixed solution to 70 ℃;
s3, reaction: adding hexamethyldisilazane dropwise into the mixed solution obtained in the step S2, and reacting for 2 hours;
s4, rectification: distilling the solution obtained in S3 to obtain trimethylsilanol with purity of more than 98%.
Example 5
Referring to fig. 1, a method for preparing trimethylsilanol specifically includes the following steps:
s1, selecting raw materials: selecting the following components in parts by weight for later use: 450 parts of hexamethyldisilazane, 55 parts of glacial acetic acid and 110 parts of water;
s2, mixing: adding water and glacial acetic acid into a 1000ml four-mouth bottle, uniformly stirring after mixing, and then heating the mixed solution to 60 ℃;
s3, reaction: adding hexamethyldisilazane dropwise into the mixed solution obtained in the step S2, and reacting for 3 hours;
s4, rectification: distilling the solution obtained in S3 to obtain trimethylsilanol with purity of more than 98%.
Example 6
Referring to fig. 1, a method for preparing trimethylsilanol specifically includes the following steps:
s1, selecting raw materials: selecting the following components in parts by weight for later use: 450 parts of hexamethyldisilazane, 55 parts of glacial acetic acid and 90 parts of water;
s2, mixing: adding water and glacial acetic acid into a 1000ml four-mouth bottle, uniformly stirring after mixing, and then heating the mixed solution to 65 ℃;
s3, reaction: adding hexamethyldisilazane dropwise into the mixed solution obtained in the step S2, and reacting for 3 hours;
s4, rectification: distilling the solution obtained in S3 to obtain trimethylsilanol with purity of more than 98%.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A preparation method of trimethylsilanol is characterized in that: the method specifically comprises the following steps:
s1, selecting raw materials: selecting the following components in parts by weight for later use: 550 parts of hexamethyldisilazane, 450-55 parts of glacial acetic acid and 90-110 parts of water;
s2, mixing: adding water and glacial acetic acid into a 1000ml four-mouth bottle, uniformly stirring after mixing, and then heating the mixed solution to 60-70 ℃;
s3, reaction: adding hexamethyldisilazane dropwise into the mixed solution obtained in the step S2, and reacting for 2-3 h;
s4, rectification: and distilling the solution obtained in the step S3 to obtain trimethylsilanol with the purity of more than 98%.
2. The method according to claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: and (3) absorbing the ammonia gas generated in the S3 reaction by using a tail gas recovery device.
3. The method according to claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: when the S1 selects the raw materials, the following components by weight are selected for later use: 500 parts of hexamethyldisilazane, 50 parts of glacial acetic acid and 100 parts of water.
4. The method according to claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: the yield of trimethylsilanol obtained during the S4 rectification was 85-90%.
5. The method according to claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: when mixing the above S2, water and glacial acetic acid were added to a 1000ml four-necked flask, and after mixing and stirring, the mixture was heated to 63 to 68 ℃.
6. The method according to claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: and when the S3 is reacted, determining that trimethylsilanol is generated by the reaction by using an HNMR detection means.
7. The method according to claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: and during the S4 distillation, the distillation temperature is controlled to be 103-105 ℃, and then condensation is carried out.
8. The method according to claim 1, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: in the mixing of S2, a thermometer was inserted into one of the four-necked bottles, and the mixture was stirred and mixed by a stirring rod continuously at one of the four-necked bottles.
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|---|---|---|---|
| CN202010686915.8A CN111808129A (en) | 2020-07-16 | 2020-07-16 | Preparation method of trimethylsilanol |
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| CN202010686915.8A CN111808129A (en) | 2020-07-16 | 2020-07-16 | Preparation method of trimethylsilanol |
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| CN202010686915.8A Withdrawn CN111808129A (en) | 2020-07-16 | 2020-07-16 | Preparation method of trimethylsilanol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112662185A (en) * | 2020-12-07 | 2021-04-16 | 合盛硅业(嘉兴)有限公司 | Method for preparing liquid silicone rubber-based adhesive by using hexamethyldisilazane |
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2020
- 2020-07-16 CN CN202010686915.8A patent/CN111808129A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112662185A (en) * | 2020-12-07 | 2021-04-16 | 合盛硅业(嘉兴)有限公司 | Method for preparing liquid silicone rubber-based adhesive by using hexamethyldisilazane |
| CN112662185B (en) * | 2020-12-07 | 2022-06-07 | 合盛硅业(嘉兴)有限公司 | Method for preparing liquid silicone rubber-based adhesive by using hexamethyldisilazane |
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Application publication date: 20201023 |
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| WW01 | Invention patent application withdrawn after publication |