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A dealcoholized room temperature vulcanized silicone rubber rosin modified organosilane crosslinking agent and preparation method thereof

A technology for organosilane and rosin modification, which is applied in chemical instruments and methods, organic chemistry, compounds of group 4/14 elements of the periodic table, etc., and can solve the problem of poor mechanical properties of condensation-type room temperature vulcanized silicone rubber and silicone rubber molecules. The problems of high chain flexibility and small intermolecular force can be achieved to make up for the poor mechanical properties of silicone rubber, simple preparation and improved mechanical properties.

Active Publication Date: 2018-09-11
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the condensation type room temperature vulcanized silicone rubber prepared by ethyl orthosilicate, methyl orthosilicate, and methyl triethoxysilane has poor mechanical properties, which is due to the high flexibility of the silicone rubber molecular chain and the intermolecular interaction. Due to weak force
Although the mechanical properties of condensation-type room temperature vulcanized silicone rubber prepared by phenyltriethoxysilane have been improved, the process is complex and expensive, and it will cause potential environmental damage during the synthesis process, use process and disposal. Also consumes petrochemical raw materials

Method used

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  • A dealcoholized room temperature vulcanized silicone rubber rosin modified organosilane crosslinking agent and preparation method thereof
  • A dealcoholized room temperature vulcanized silicone rubber rosin modified organosilane crosslinking agent and preparation method thereof
  • A dealcoholized room temperature vulcanized silicone rubber rosin modified organosilane crosslinking agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 50 parts of refined rosin glycidyl ester and 31 parts of aminopropyltriethoxysilane into a three-necked flask, and react at 60°C for 1.5 h under nitrogen protection and stirring at 300 rpm to synthesize refined rosin glycidyl ester. Aminopropyltriethoxysilane crosslinker.

[0025] FT-IR spectrum identification of refined rosin glycidyl ester and refined rosin glycidyl ester modified aminopropyltriethoxysilane crosslinking agent:

[0026] Refined rosin glycidyl ester: 1726cm -1 Carbonyl characteristic absorption peak, 765cm -1 、859cm -1 、910cm -1 It is the characteristic absorption peak of epoxy group; refined rosin glycidyl ester modified aminopropyl triethoxysilane crosslinking agent: 3319cm -1 It is the characteristic absorption peak of nitrogen-hydrogen bond, 1079cm -1 It is the characteristic absorption peak of silicon oxygen carbon bond, 957cm -1 It is the characteristic absorption peak of ethoxy group. From the comparative analysis of the characterist...

Embodiment 2

[0029] Weigh 50 parts of dehydroabietic acid glycidyl ester and 31 parts of aminopropyltriethoxysilane into a three-necked flask, and react at 40°C for 3 hours under nitrogen protection and stirring at 300 rpm to synthesize dehydroabietic acid glycidyl ester Glyceride modified aminopropyltriethoxysilane crosslinker.

[0030] Dehydroabietic acid glycidyl ester modified aminopropyltriethoxysilane crosslinking agent 13 CNMR spectrum identification: in the range of 120-145ppm, it belongs to the C=C characteristic chemical shift peak in the phenanthrene ring structure of the rosin structure, 178ppm belongs to the C=O characteristic chemical shift peak, 67ppm belongs to the O-C characteristic chemical shift peak, 58 and 18ppm respectively It belongs to the characteristic chemical shift peak of Si-O-C-C, and 48ppm belongs to NH-CH 2 The characteristic chemical shift peak, 10-55ppm belongs to the characteristic chemical shift peak of other carbon atoms in the rosin structure. pass ...

Embodiment 3

[0032] Weigh 50 parts of hydrogenated rosin glycidyl ester and 31 parts of aminopropyltriethoxysilane into a three-necked flask, and react at 35°C for 6 hours under nitrogen protection and stirring at 300 rpm to synthesize hydrogenated rosin glycidyl ester modified Aminopropyltriethoxysilane crosslinker.

[0033] Hydrogenated rosin glycidyl ester modified aminopropyltriethoxysilane crosslinking agent 13 CNMR spectrum identification: 120 and 146ppm belong to the CH=C characteristic chemical shift peak in the phenanthrene ring structure of the rosin structure, 178ppm belongs to the C=O characteristic chemical shift peak, 70ppm belongs to the O-C characteristic chemical shift peak, 58 and 18ppm belong to Si -O-C-C characteristic chemical shift peak, 48ppm belongs to NH-CH 2 The characteristic chemical shift peak, 10-55ppm belongs to the characteristic chemical shift peak of other carbon atoms in the rosin structure. pass 13 CNMR spectrogram analysis, the results show that hydr...

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Abstract

The invention discloses a dealcoholizing type room temperature vulcanized silicone rubber rosin modified organosilane crosslinking agent and a preparation method thereof. The preparation method of the crosslinking agent comprises the following step of enabling epoxy-based rosin and organosilane to react for 0.5 to 8h at the temperature of 20 to 60 DEG C, so as to obtain the dealcoholizing type room temperature vulcanized silicone rubber rosin modified organosilane crosslinking agent, wherein the molar ratio of the organosilane to the epoxy-based resin is (1 to 1) to (1 to 2). The preparation method of the dealcoholizing type room temperature vulcanized silicone rubber rosin modified organosilane crosslinking agent has the advantages that the raw materials are natural resources, the amount is large, the cost is low, the obtaining is easy, and the like; the rosin and a derivative thereof can replace a petrochemical product, the problems of shortage of existing petrochemical resources, high cost, pollution to environment and the like are solved, and a new path is developed for the deep processing of the rosin; the synthesizing technology is simple, the environment-friendly, green and regenerating effects are realized, and the requirement of sustained development is met; the defect of poor mechanical property of silicone rubber is overcome.

Description

technical field [0001] The invention relates to a dealcoholized room temperature vulcanized silicone rubber rosin-modified organosilane crosslinking agent and a preparation method thereof, belonging to the field of crosslinking agents. Background technique [0002] The basic composition of one-component condensation type RTV silicone rubber includes: base polymer, crosslinking agent, catalyst and filler. The crosslinking agent is the core component of one-component room temperature vulcanizing silicone rubber. The more commonly used one is the dealcoholization room temperature vulcanization silicone rubber crosslinking agent. The dealcoholization room temperature vulcanization silicone rubber crosslinking agent includes orthosilicate Acetate methyl ester, methyl triethoxysilane, phenyl triethoxysilane, etc. Among them, the condensation type room temperature vulcanized silicone rubber prepared by ethyl orthosilicate, methyl orthosilicate, and methyl triethoxysilane has poor ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/544C07F7/18C08L83/06C08K13/02
CPCC07F7/1804C07F7/1888C08K5/544C08K13/02C08L2312/08C08L83/04
Inventor 刘鹤李侨光宋湛谦商士斌宋杰
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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