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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 viscosity of the product and reduce the storage stability. At the same time, it is not easy to remove Cl, which is very harmful to many applications (such as microelectronic packaging). - ion

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

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1, the preparation of polysiloxane polymer

[0024]In a 250mL three-necked flask, add 96.2g of monomeric methylhydrogensiloxane cyclic body, 34.5g of methylvinylcyclotetrasiloxane and 1.87g of tetramethyldivinyldisiloxane (the In the reaction system, the molar ratio of methyl hydrogen siloxane ring body and methyl vinyl cyclotetrasiloxane is 1:4; The molar ratio of alkane ring body and the total amount of monomer units of methyl vinyl cyclotetrasiloxane is 1:100); under magnetic stirring, add 0.39g CF 3 SO 3 H (which accounts for 0.3% of the total mass of the methylhydrogensiloxane ring body and the methylvinylcyclotetrasiloxane siloxane monomer) and 0.015g deionized water, stirred and reacted for 3 hours in an oil bath at 65°C Viscosity After there is no obvious change, after feeding sufficient amount of ammonia gas, the low boiling matter is removed under vacuum at 140-150°C; after filtering through a G3 sand core funnel, 115g of colorless transparent liq...

Embodiment 2

[0025] Embodiment 2, the preparation of polysiloxane polymer

[0026] In a 1000mL three-necked flask, add 451g methylhydrogensiloxane ring body, 215g methylvinylcyclotetrasiloxane and 4.66g end-capping agent tetramethyldivinyldisiloxane (in this reaction system, The molar ratio of methyl hydrogen siloxane ring body and methyl vinyl cyclotetrasiloxane is 3:1; The molar ratio of the total substance amount of base vinyl cyclotetrasiloxane is 0.5:100); under magnetic stirring, add 0.78g CF 3 SO 3 H (which accounts for 0.1% of the total mass of the siloxane monomer of the methyl hydrogen siloxane ring body and the methyl vinyl cyclotetrasiloxane), stirred and reacted for 4 hours in an oil bath at 65° C., and introduced a sufficient amount of ammonia After degassing, remove the low boiler under vacuum under reduced pressure at 140-150°C; after filtering through a G3 sand core funnel, obtain 143g colorless transparent liquid (yield 89%), as shown in formula (I), wherein, x is 0.75...

Embodiment 3

[0027] Embodiment 3, the preparation of polysiloxane polymer

[0028] In a 1000mL three-necked flask, add 361g methylhydrogensiloxane ring body, 433g methylvinylcyclotetrasiloxane and 1.87g end-capping agent tetramethyldivinyldisiloxane (in this reaction system, The molar ratio of methyl hydrogen siloxane ring body and methyl vinyl cyclotetrasiloxane is 1.2:1; The molar ratio of the total substance amount of base vinyl cyclotetrasiloxane is 0.2:100); under magnetic stirring, add 0.86g CF 3 SO 3 H (which accounts for 0.11% of the total mass of siloxane monomers of methylhydrogensiloxane ring body and methylvinyl cyclotetrasiloxane) and 0.086 deionized water, stirred and reacted at 65°C in an oil bath for 4 hours, After feeding a sufficient amount of ammonia, remove the low boilers under vacuum at 140-150° C., and filter through a G3 sand core funnel to obtain 590 g of a colorless transparent liquid (yield 75%), as shown in formula (I) , wherein, x is 0.55, y is 0.45, z is 0,...

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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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