Polysiloxane polymer and preparation method thereof

A technology of polysiloxane and polymer, applied in the field of polysiloxane polymer and its preparation, can solve problems such as difficult removal, increase product viscosity, reduce storage stability, etc., achieve less side reactions, simple reaction, low The effect of viscosity

Active Publication Date: 2012-05-09
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the preparation by hydrolysis and polycondensation, it is easy to cause microgel and some branched structures in the reaction process, which will increase the viscosit

Method used

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  • Polysiloxane polymer and preparation method thereof
  • Polysiloxane polymer and preparation method thereof
  • Polysiloxane polymer and preparation method thereof

Examples

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Example Embodiment

[0023] Example 1. Preparation of polysiloxane polymer

[0024] In a 250 mL three-necked flask, add 96.2 g of monomer methyl hydrogen siloxane ring, 34.5 g of methyl vinyl cyclotetrasiloxane and 1.87 g of tetramethyl divinyl disiloxane as a blocking agent. In the reaction system, the molar ratio of methyl hydrogen siloxane ring body and methyl vinyl cyclotetrasiloxane is 1:4; the capping agent unit tetramethyl divinyl disiloxane and methyl hydrogen siloxane The molar ratio of the alkane ring body to the total amount of the monomer units of methyl vinyl cyclotetrasiloxane is 1:100); under magnetic stirring, add 0.39 g of CF 3 SO 3 H (it accounts for 0.3% of the total mass of methyl hydrogen siloxane ring body and methyl vinyl cyclotetrasiloxane siloxane monomer) and 0.015 g deionized water, stirred and reacted for 3 hours at 65°C in an oil bath. Viscosity After there is no obvious change, after passing in enough ammonia gas, the low-boiling matter is removed under vacuum and reduce...

Example Embodiment

[0025] Example 2. Preparation of polysiloxane polymer

[0026] In a 1000 mL three-necked flask, add 451 g of methyl hydrogen siloxane ring, 215 g of methyl vinyl cyclotetrasiloxane and 4.66 g of capping agent tetramethyl divinyl disiloxane (in the reaction system, The molar ratio of methyl hydrogen siloxane ring body and methyl vinyl cyclotetrasiloxane is 3:1; the end-capping agent tetramethyl divinyl disiloxane and methyl hydrogen siloxane ring body and a The molar ratio of the total amount of the base vinyl cyclotetrasiloxane is 0.5: 100); under magnetic stirring, 0.78 g of CF is added 3 SO 3 H (it accounts for 0.1% of the total mass of the siloxane monomers of methyl hydrogen siloxane ring body and methyl vinyl cyclotetrasiloxane), stir and react for 4 hours at 65°C in an oil bath, and pass in sufficient ammonia After gasification, the low-boiling matter was removed under vacuum at 140-150°C; after filtering by G3 sand core funnel, 143g of colorless transparent liquid (yield 8...

Example Embodiment

[0027] Example 3. Preparation of polysiloxane polymer

[0028] In a 1000 mL three-necked flask, add 361 g of methyl hydrogen siloxane ring, 433 g of methyl vinyl cyclotetrasiloxane and 1.87 g of capping agent tetramethyl divinyl disiloxane (in the reaction system, The molar ratio of methyl hydrogen siloxane ring body and methyl vinyl cyclotetrasiloxane is 1.2:1; the end-capping agent tetramethyl divinyl disiloxane and methyl hydrogen siloxane ring body and a The molar ratio of the total amount of the base vinyl cyclotetrasiloxane is 0.2: 100); under magnetic stirring, 0.86 g of CF is added 3 SO 3 H (which accounts for 0.11% of the total mass of the siloxane monomer of methyl hydrogen siloxane ring body and methyl vinyl cyclotetrasiloxane) and 0.086 deionized water, stirred and reacted for 4 hours at 65°C in an oil bath, After a sufficient amount of ammonia gas is introduced, the low-boiling substances are removed under vacuum and reduced pressure at 140-150°C, and filtered throug...

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Abstract

The invention provides a polysiloxane polymer and a preparation method thereof. The polysiloxane polymer is shown in formula (I). The preparation method of the polymer comprises the following step: carrying out ring-opening polymerization reaction on methyl hydrogen cyclosiloxane and methyl vinyl cyclosiloxane, or methyl hydrogen cyclosiloxane, methyl vinyl cyclosiloxane and monomer A in the presence of organic silicon blocking agent and cationic polymerization initiator, thus obtaining the polysiloxane polymer, wherein the monomer A is dimethyl cyclosiloxane, methyl phenyl cyclosiloxane or R'-substituted methyl hydrogen cyclosiloxane; R' is methyl, phenyl, CH2CH2Ph, CH2CH2CN, CH2CH2CO2CH3, CH2CH2CO2C4H9, CH2CH(CH3)CO2CH3 or CH2CH2OR''; and R'' is C1-20 alkyl, cycloalkyl, ether or alcohol.

Description

technical field [0001] The invention relates to a polysiloxane polymer and a preparation method thereof, and belongs to the field of high-temperature-resistant thermosetting resins and the preparation thereof. Background technique [0002] Precursor pyrolysis conversion method to prepare ceramic technology (PDC) has attracted much attention due to its excellent practicability and designability, which can be used to prepare materials with ceramic properties by a processing and molding process close to organic resins. Research hotspots in the field of preparation of ceramic matrix composites. Precursor pyrolysis conversion method to prepare ceramic materials, the first step is to design and synthesize precursor polymers with excellent processability and high ceramic yield, and then pyrolyze them to obtain ceramic materials. Silicon carbon oxide (Si-C-O) ceramics prepared by precursor polysiloxane have excellent properties such as high temperature resistance, oxidation resista...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/26
Inventor 陈阳李永明吴纪全徐彩虹王丁王秀军
Owner INST OF CHEM CHINESE ACAD OF SCI
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