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Maleopimaric acid modified polysiloxane resin and preparation method thereof

A technology of polysiloxane resin and maleopimaric acid, which is applied in the field of maleopimaric acid modified polysiloxane resin and its preparation, can solve problems such as poor adhesion and low mechanical strength, and achieve improved water resistance and reduced The effect of simple production cost and production process

Active Publication Date: 2014-09-17
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

Existing silicone resins have disadvantages such as low mechanical strength and poor adhesion, and so far there is no public report on the introduction of maleopimaric acid into polysiloxane molecular chains

Method used

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  • Maleopimaric acid modified polysiloxane resin and preparation method thereof
  • Maleopimaric acid modified polysiloxane resin and preparation method thereof
  • Maleopimaric acid modified polysiloxane resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 100g octamethylcyclotetrasiloxane, 20g tetramethyltetravinylcyclotetrasiloxane, 34g aminopropylmethyldiethoxysilane, 10g hexamethyldisiloxane and 0.2 g potassium hydroxide, stirred and reacted at 100°C for 8 hours, then gradually warmed up to 180°C, vacuumized to remove low boilers; cooled to 120°C, added 72g maleopimaric acid (purity is 98%), stirred and reacted for 4 hours Afterwards, heat up to 180°C and vacuumize to remove low boilers; collect the maleopimaric acid-modified silicone resin while it is hot under the protection of nitrogen.

Embodiment 2

[0039] Add 206g of octamethylcyclotetrasiloxane, 20g of tetramethyltetravinylcyclotetrasiloxane, 10g of hexamethyldisiloxane and 0.2g of potassium hydroxide in the reaction kettle, and stir the reaction at 100°C for 8 Hours, then gradually raise the temperature to 180°C, vacuumize to remove low boilers; collect the silicone resin while it is hot under the protection of nitrogen.

[0040] Depend on figure 2 As can be seen, by the organosilicon resin prepared by example 2 1 The HNMR spectrogram peaks are relatively simple, within the range of 0.5-3.0ppm is the absorption peak of the proton on Si-CH3, and above 5.5ppm appears as the absorption peak of the proton on the vinyl Si-CH=CH2, the resulting product structural formula is:

[0041]

[0042] Among them, m 1 =44,m 2 =4.

[0043] Depend on figure 1 It can be seen that, in addition to the Si-CH of ordinary vinyl silicone resin 3 (0.5~3.0ppm) and Si-CH=CH 2 (5.7 ~ 6.2ppm) chemical shift peaks, maleopimaric acid modifie...

Embodiment 3

[0052] Modified 100 parts of methyl vinyl silicone rubber raw rubber (the molar content of vinyl units is 0.11%, and the molar mass is 800,000 g / mol), 4 parts of hydroxyl silicone oil (viscosity 100 Pa·S), 6 parts of maleopimaric acid Silicone resin (gained in embodiment 1) and 25 parts of fumed white carbon black Knead evenly in a kneader; after the rubber material is cooled to room temperature, add 1 part of vulcanizing agent 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane into the open mill to make the rubber The material is mixed evenly.

[0053] Put the above-mentioned rubber into the mold, pressurize and vulcanize on a flat vulcanizer for 30 minutes, and the vulcanization temperature is 170±2°C; remove the pressure and take out the sample; keep warm in an aging oven at 200°C for 4 hours; naturally cool to room temperature, and obtain a mixture Mixing film 1.

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Abstract

The invention discloses maleopimaric acid modified polysiloxane resin and a preparation method thereof. The maleopimaric acid modified polysiloxane resin is characterized by having a structure represented by a formula shown in descriptions, wherein R1 is C2-8 straight-chain or branched-chain alkyl, R2 is C2-3 straight-chain alkyl, X is a sub organic group, m and n are natural numbers between 1 and 200, and the ratio of n and m meets the condition that n / m is not smaller than 0.01 and not greater than 10. According to the maleopimaric acid modified polysiloxane resin disclosed by the invention, a ternary phenanthrene ring and an imide heteroatomic ring which have certain rigidity and polarity are introduced into organosilicon resin, so that the rigidity and polarity of a molecular chain are improved, and meanwhile, the properties, such as water resistance, high-temperature resistance, electric insulation, adhesive power and the like, of the resin are improved; the prepared maleopimaric acid modified polysiloxane resin has excellent intermiscibility with organosilicon materials, and mechanical properties, such as hardness, tear strength, resilience and the like, of the organosilicon rubber can be remarkably improved.

Description

technical field [0001] The invention relates to a maleopimaric acid-modified polysiloxane resin and a preparation method thereof, belonging to the technical field of silicone resin and silicone resin preparation. Background technique [0002] Rosin is a natural resource with abundant sources. It has the advantages of anti-corrosion, moisture-proof, insulation, and adhesion. Since the 1940s, foreign countries have used the active groups in the molecular structure of rosin to chemically modify it, artificially endowing it with various new characteristics, and made a series of deep-processing products, and the deep-processing utilization rate has almost reached 100%. However, due to the relatively late research on deep processing utilization in China, the current utilization rate of deep processing is less than 40%, which is far behind developed countries. Since rosin contains active groups such as carboxyl groups and unsaturated double bonds, rosin has been used to modify phe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/388C08G77/26
Inventor 宋湛谦徐涛刘鹤商士斌
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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