CN111072967A - Method for preparing organic silicon by hydrolyzing and condensing chlorosilane in isopropanol - Google Patents
Method for preparing organic silicon by hydrolyzing and condensing chlorosilane in isopropanol Download PDFInfo
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- CN111072967A CN111072967A CN201911337280.4A CN201911337280A CN111072967A CN 111072967 A CN111072967 A CN 111072967A CN 201911337280 A CN201911337280 A CN 201911337280A CN 111072967 A CN111072967 A CN 111072967A
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- chlorosilane
- isopropanol
- organic silicon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a method for preparing organic silicon by hydrolyzing and condensing chlorosilane in isopropanol, which adopts isopropanol solution to replace toxic solvents such as toluene, xylene and the like to carry out hydrolysis and condensation reaction, thereby not only reducing the post-treatment cost of the product and improving the production efficiency, but also meeting the requirement of environmental protection, and leading the organic siloxane product to have the excellent performances of low viscosity (less than or equal to 16cP) and low free Cl content (less than or equal to 6ppm), and the quality to be stable and controllable.
Description
Technical Field
The invention belongs to the technical field of chemical industry, relates to the technical field of organic silicon production, and particularly relates to a method for preparing organic silicon by hydrolyzing and condensing chlorosilane in isopropanol.
Background
The organochlorosilane is converted into the intermediate oligomeric organosiloxane with a linear or cyclic structure through hydrolysis and polycondensation, and is the basis for synthesizing silicone oil, silicone rubber and silicone resin. In the prior art, most of organic silicon resins produced are subjected to hydrolysis condensation reaction in organic solvents with high toxicity, such as toluene, xylene and the like, and harm is caused to the environment and operators.
Disclosure of Invention
The invention aims to develop a method for preparing organic silicon by hydrolyzing and condensing chlorosilane in isopropanol in order to reduce the use of toxic solvents and reduce the post-treatment cost of products.
The invention is realized by the following scheme:
a method for preparing organic silicon by hydrolyzing and condensing chlorosilane comprises the following steps:
(1) adding deionized water, isopropanol and chlorosilane in a mass ratio of (2-6) - (1-4) - (0.3-3) into a reaction kettle, controlling the temperature at 25-40 ℃, and stirring to form a homogeneous solution;
(2) adding chlorosilane into a reaction kettle, uniformly stirring, and continuously reacting for 4 hours;
(3) standing, removing an acid water layer, repeatedly washing the hydrolysate to be neutral by water, and then transferring the hydrolysate into a polycondensation kettle;
(4) preparing organic silicon at 60-100 ℃ under reduced pressure, and recovering to room temperature.
On the basis of the technical scheme, the chlorosilane RSiCl is prepared by the method3、RR’SiCl2RR 'R "SiCl wherein R, R', R" is one of phenyl, methyl, ethyl, propyl, isopropyl aliphatic and aromatic groups.
Further, the mass ratio of the deionized water, the isopropanol and the chlorosilane in the step (1) is preferably 4:2: 2.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, an isopropanol solution is adopted to replace toxic solvents such as toluene and xylene to carry out hydrolysis condensation reaction, so that the product post-treatment cost is reduced, the production efficiency is improved, the use of the toxic solvents is reduced, the green environmental protection requirement is met, and the organosiloxane product has the excellent performances of low viscosity (less than or equal to 16cP) and low free Cl content (less than or equal to 6ppm), and is stable and controllable in quality.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the purpose of facilitating understanding of the present invention and should not be construed as specifically limiting the present invention.
Unless otherwise specified, various starting materials of the present invention are commercially available; or prepared according to conventional methods in the art. Unless defined or indicated 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. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention.
Example 1
A method for preparing organic silicon by hydrolyzing and condensing chlorosilane in isopropanol comprises the following steps:
(1) adding deionized water, isopropanol and chlorosilane in a mass ratio of 4:2:2 into a reaction kettle, controlling the temperature at 35 ℃, and stirring to form a homogeneous solution;
(2) adding chlorosilane into a reaction kettle, uniformly stirring, and continuously reacting for 4 hours;
(3) standing, removing an acid water layer, repeatedly washing the hydrolysate to be neutral by water, and then transferring the hydrolysate into a polycondensation kettle;
(4) preparing organic silicon at 80 ℃ under reduced pressure, and recovering to room temperature.
Example 2
A method for preparing organic silicon by hydrolyzing and condensing chlorosilane in isopropanol comprises the following steps:
(1) adding deionized water, isopropanol and chlorosilane in a mass ratio of 5:2:1 into a reaction kettle, controlling the temperature at 35 ℃, and stirring to form a homogeneous solution;
(2) adding chlorosilane into a reaction kettle, uniformly stirring, and continuously reacting for 4 hours;
(3) standing, removing an acid water layer, repeatedly washing the hydrolysate to be neutral by water, and then transferring the hydrolysate into a polycondensation kettle;
(4) preparing organic silicon at 80 ℃ under reduced pressure, and recovering to room temperature.
Example 3
A method for preparing organic silicon by hydrolyzing and condensing chlorosilane in isopropanol comprises the following steps:
(1) adding deionized water, isopropanol and chlorosilane in a mass ratio of 2:1:0.5 into a reaction kettle, controlling the temperature at 35 ℃, and stirring to form a homogeneous solution;
(2) adding chlorosilane into a reaction kettle, uniformly stirring, and continuously reacting for 4 hours;
(3) standing, removing an acid water layer, repeatedly washing the hydrolysate to be neutral by water, and then transferring the hydrolysate into a polycondensation kettle;
(4) preparing organic silicon at 80 ℃ under reduced pressure, and recovering to room temperature.
The applicant states that on the basis of the above-mentioned examples, the specific content point values of the components in the above-mentioned examples are combined with the technical solutions in the summary of the invention, so as to generate a new numerical range, which is also one of the described ranges of the present invention, and the present application does not list these numerical ranges again for the sake of brevity.
Claims (3)
1. The method for preparing the organic silicon by hydrolyzing and condensing the chlorosilane in the isopropanol is characterized in that the hydrolysis and condensation reaction comprises the following steps:
(1) adding deionized water, isopropanol and chlorosilane in a mass ratio of (2-6) - (1-4) - (0.3-3) into a reaction kettle, controlling the temperature at 25-40 ℃, and stirring to form a homogeneous solution;
(2) adding chlorosilane into a reaction kettle, uniformly stirring, and continuously reacting for 4 hours;
(3) standing, removing an acid water layer, repeatedly washing the hydrolysate to be neutral by water, and then transferring the hydrolysate into a polycondensation kettle;
(4) preparing organic silicon at 60-100 ℃ under reduced pressure, and recovering to room temperature.
2. The process for preparing organosilicon by hydrolytic condensation of chlorosilane in isopropanol as claimed in claim 1, wherein the chlorosilane RSiCl is added to the reaction mixture3、RR’SiCl2RR 'R "SiCl wherein R, R', R" is one of phenyl, methyl, ethyl, propyl, isopropyl aliphatic and aromatic groups.
3. The method for preparing organosilicon by hydrolytic condensation of chlorosilane and isopropanol as claimed in claim 1, wherein the mass ratio of the deionized water, the isopropanol and the chlorosilane in step (1) is 4:2: 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911337280.4A CN111072967A (en) | 2019-12-23 | 2019-12-23 | Method for preparing organic silicon by hydrolyzing and condensing chlorosilane in isopropanol |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911337280.4A CN111072967A (en) | 2019-12-23 | 2019-12-23 | Method for preparing organic silicon by hydrolyzing and condensing chlorosilane in isopropanol |
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| Publication Number | Publication Date |
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| CN111072967A true CN111072967A (en) | 2020-04-28 |
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| CN201911337280.4A Pending CN111072967A (en) | 2019-12-23 | 2019-12-23 | Method for preparing organic silicon by hydrolyzing and condensing chlorosilane in isopropanol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113248710A (en) * | 2021-06-29 | 2021-08-13 | 山东硅科新材料有限公司 | (2,4, 4-trimethyl amyl) silane oligomer and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6107505A (en) * | 1997-12-26 | 2000-08-22 | Chisso Corporation | Process for production of polyorganosiloxane |
| CN102675642A (en) * | 2012-04-20 | 2012-09-19 | 杭州硅畅科技有限公司 | Method for preparing solid organic silicon resin by utilizing chlorosilane high-boiling residue |
| CN103408758A (en) * | 2013-07-10 | 2013-11-27 | 江苏大学 | Preparation method of ethyl phenyl silicone oil |
-
2019
- 2019-12-23 CN CN201911337280.4A patent/CN111072967A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6107505A (en) * | 1997-12-26 | 2000-08-22 | Chisso Corporation | Process for production of polyorganosiloxane |
| CN102675642A (en) * | 2012-04-20 | 2012-09-19 | 杭州硅畅科技有限公司 | Method for preparing solid organic silicon resin by utilizing chlorosilane high-boiling residue |
| CN103408758A (en) * | 2013-07-10 | 2013-11-27 | 江苏大学 | Preparation method of ethyl phenyl silicone oil |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113248710A (en) * | 2021-06-29 | 2021-08-13 | 山东硅科新材料有限公司 | (2,4, 4-trimethyl amyl) silane oligomer and preparation method and application thereof |
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Application publication date: 20200428 |
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