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Silicone resin with oxime groups in its side groups, and its preparation method and application

The technology of polysiloxane resin and ketoxime group is applied in the fields of polysiloxane resin containing ketoxime group in side group, preparation and application thereof, and can solve the problems of low mechanical strength of cross-linked products and achieve temperature resistance performance. Excellent, high quality residual rate, high crosslinking density effect

Inactive Publication Date: 2013-06-19
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The deoxime type crosslinking agent currently used is mainly trifunctional or tetrafunctional ketoxime silane, such as methyl triacetone oximino silane, methyl tributyl ketoxime silane, phenyl tributyl ketoxime silane, tetrabutyl The disadvantage of small molecular compounds such as ketoximosilane is that the mechanical strength of the cross-linked product is low

Method used

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  • Silicone resin with oxime groups in its side groups, and its preparation method and application
  • Silicone resin with oxime groups in its side groups, and its preparation method and application
  • Silicone resin with oxime groups in its side groups, and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Preparation of polysiloxane resin (PMKS) containing acetone oxime group in side group:

[0031] Raw materials: methyl hydrogen-containing silicone oil with a hydrogen content of 1.6mol / 100g; acetone oxime is selected as the ketoxime; tetrahydrofuran is selected as the solvent; tetramethylammonium hydroxide is selected as the catalyst.

[0032] Conditions: Add 50g of methylhydrogen silicone oil, 100g of acetone oxime, 400g of tetrahydrofuran, and 1.0g of tetramethylammonium hydroxide into a three-necked flask, and react for 12 hours at a reaction temperature of 25°C.

[0033] The synthetic product is liquid at room temperature, and it is characterized by infrared. Compared with the infrared spectrum of the raw material methyl hydrogen-containing silicone oil, the 2169cm -1 The characteristic peak at disappears, indicating that the Si-H group is reacted; 1650cm -1 New characteristic peaks appear, indicating Si-ON=C(CH3) 2 Group generation.

[0034] synthesized products...

Embodiment 2

[0039] Preparation of Polysiloxane Resin Containing Butanone Oxime Group in Side Group

[0040] Raw materials: methyl hydrogen-containing silicone oil, hydrogen content 1.66mol / g; ketone oxime chooses butanone oxime; solvent chooses toluene; catalyst chooses alkali glue.

[0041] Conditions: Add 50g of methyl hydrogen-containing silicone oil, 120g of butanone oxime, 300g of gasoline, and 1.0g of alkali glue into a three-necked flask, and react for 18 hours at a reaction temperature of 20°C.

[0042] The synthetic product is liquid at room temperature. It is also proved by infrared characterization and nuclear magnetic characterization that under the preparation method of the present invention, the raw material methyl hydrogen-containing silicone oil has been transformed into a polysiloxane resin with a side group containing butanone oxime group. Its structural formula for:

[0043]

[0044] Where: X 1 、X 2 Both are methyl groups, m is 30, and n is 0.

Embodiment 3

[0046] Preparation of Polysiloxane Resin Containing Diacetyl Oxime Group in Side Group

[0047] Raw materials: methyl hydrogen-containing silicone oil, hydrogen content 0.01mol / 100g; dimethylglyoxime is selected as the ketoxime; a mixture of acetone and cyclohexane is selected as the solvent; basic ion exchange resin is selected as the catalyst.

[0048] Conditions: Add 50g of methyl hydrogen-containing silicone oil, 10g of dimethylglyoxime, 120g of acetone, 100g of cyclohexane, and 2.5g of basic ion exchange resin into a three-necked flask, and react for 24 hours at a reaction temperature of 35°C.

[0049] The synthetic product is liquid at room temperature, and it is also proved by infrared characterization and nuclear magnetic characterization that under the preparation method of the present invention, the raw material methyl hydrogen-containing silicone oil has been transformed into a polysiloxane resin with a diacetyloximine group in the side group, which The structural f...

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Abstract

The invention discloses a silicone resin with oxime groups in its side groups, and its preparation method and application. The silicone resin has a structural formula as described in the specification; in the structural formula, R1, R2, R3 and R4 is methyl groups, ethyl groups, methy ketoxime groups and phenyl groups or hydrogen groups, X1 and X2 is methyl groups or hydroxy groups, m is no less than 1 and no more than 1200, and n is no less than 0 and no more than 6000; the silicone resin with oxime groups in its side groups is prepared from methyl hydrogen silicone fluid, oximes, a solvent and a catalyst under certain conditions. The silicone resin with oxime groups in its side groups can react with moisture in air under the condition of room temperature or heating, and changes from a liquid state into a solid state to form matrix resin with excellent temperature resistance for a sealing material; the silicone resin can also be used as a cross-linking agent for cross-linking of hydroxyl terminated polysiloxanes, and a resultant of crosslinking has improved performance compared to a resultant of crosslinking with a micromolecular oxime cross-linking agent. The silicone resin has agood application prospect in the aspects of composite materials, paints, adhesives, sealants, cross-linking agents, etc.

Description

Technical field: [0001] The invention relates to a polysiloxane resin whose side group contains ketoxime group, a preparation method and application thereof. Background technique: [0002] With the development of aviation, aerospace, construction and other industries, people have higher and higher requirements for high temperature resistant resins, adhesives and sealing materials. For example, materials are required to have a higher temperature limit to meet the needs of special environments. Materials are required to be On-site curing to meet construction needs, etc. [0003] Although traditional inorganic sealants, such as silicates and phosphates, can withstand high temperatures, their chemical resistance is not good and they are easily eroded by chemicals, and the curing speed of inorganic sealants is slow, so they cannot It is beneficial to on-site construction; the existing high-temperature polymer sealing materials, such as epoxy resin, polyurethane, etc., generally ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/388C08L83/08C08L83/06
Inventor 张军营蔡喜庆
Owner BEIJING UNIV OF CHEM TECH