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A kind of preparation method of organosilicon resin with alternating structure

A technology of alternating structure and silicone, applied in the field of synthesis of polyhydroxy silicone hybrid polymers, can solve problems such as equipment and environmental hazards, difficult to control the molecular structure of hydroxyl silicone resin, etc., to achieve no by-products and clear structure The effect of controllability and low equipment material requirements

Active Publication Date: 2018-08-07
烟台优尼泰电子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, a large amount of acidic wastewater will be generated during the production process, which will cause great harm to equipment and the environment.
In addition, due to the very high reactivity of chlorosilanes, it is difficult to control the molecular structure of hydroxyl-containing silicone resins

Method used

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  • A kind of preparation method of organosilicon resin with alternating structure
  • A kind of preparation method of organosilicon resin with alternating structure
  • A kind of preparation method of organosilicon resin with alternating structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Under nitrogen or argon protection, add 2,3-dimercaptopropanol (0.68g, 5.51mmol) successively in the reactor, divinyltetramethylsilane (0.95g, 4.95mmol), add photosensitive radical initiator Benzoin dimethyl ether (0.041 g, 0.16 mmol) and 1.5 mmol N-methylpyrrolidone. Polymerization was carried out for 4.0 hours by ultraviolet light irradiation at room temperature. After precipitation, separation and drying, a polyhydroxy hybrid organosilicon polymer is obtained.

[0025] The NMR spectrum of the product ( 1 H NMR) see figure 1 , showing an obvious signal (2.6-2.9ppm) of the carbon-hydrogen protons linked to the thioether bond; the signal (5.7-6.0ppm) of the hydrogen protons on the vinyl group in divinyltetramethylsilane has disappeared, generating the same Signals for thioether-linked hydrocarbon protons appear at 0.8 ppm.

Embodiment 2

[0027] Under nitrogen or argon protection, 2,3-dimercaptopropanol (0.85g, 6.9mmol), divinyltetramethylsilane (0.73g, 3.8mmol), dimethyldivinyl Silicon (0.42 g, 3.79 mmol). The thermosensitive radical initiator azobisisobutyronitrile (0.033 g, 0.2 mmol) and 0.12 mmol 1,4-dioxane were added. Polymerization was carried out at 75°C for 24 hours. After precipitation, separation and drying, a polyhydroxy hybrid organosilicon polymer is obtained.

[0028] figure 2 It is the gel permeation chromatogram curve of the polymerization product of 2,3-dimercaptopropanol, divinyltetramethylsilane and dimethyldivinylsilane mixture in the present invention. The number average molecular weight of the polymerization product is 8840g·mol -1 , The molecular weight distribution coefficient is 1.31.

Embodiment 3

[0030] Under the protection of nitrogen or argon, propylene thiol (0.356g, 3.3mmol), 2,3-dimercaptopropanol (0.427g, 3.5mmol), divinyltetramethylsilane (1.30 g, 6.80 mmol), and the photosensitive free radical initiator 2-hydroxymethylphenylpropan-1-one (0.41 g, 1.0 mmol) was added. Polymerization was carried out for 1.5 hours by ultraviolet light irradiation at room temperature. After precipitation, separation and drying, a polyhydroxy hybrid organosilicon polymer is obtained.

[0031] image 3 It is the gel permeation chromatogram curve of the polymerization product of propanedithiol and 2,3-dimercaptopropanol mixture and divinyltetramethylsilane in the present invention. The number average molecular weight of the polymerization product is 7400g·mol -1 , The molecular weight distribution coefficient is 1.36.

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Abstract

The invention discloses a preparation method of organic silicon resin with alternating structure. The method is that under the protection of nitrogen or argon, the thermosensitive free radical initiator is under heating conditions or the photosensitive free radical initiator is under the condition of ultraviolet light irradiation, causing the dithiol compound and the divinyl organosilicon compound to undergo mercapto- Vinyl polymerization reaction to obtain a polyhydroxy silicone hybrid resin with an alternating structure. The invention does not need hydrolysis, drying, protection-deprotection process, high reaction rate, clear and controllable product structure, easy adjustment of hydroxyl content, no by-products, and low requirements on equipment materials. At the same time, its molecular structure contains a large number of sulfur atoms, which can significantly increase the refractive index of the material. In addition, the molecular structure contains a large number of sulfide bonds. The glass transition temperature of the product is low (less than ‑20 ° C), and the texture is soft and very Suitable for fabric treatment agent and high-performance corrosion-resistant coating or wear-resistant coating.

Description

technical field [0001] The invention relates to a preparation method of polyhydroxyl silicone resin with alternating structure, in particular to a synthesis method of polyhydroxyl silicone hybrid polymer containing thioether bonds. Background technique [0002] The traditional hydroxyl-containing silicone resin is synthesized by hydrolysis of one or more chlorosilanes. It has good high and low temperature resistance, corrosion resistance, aging resistance, low surface energy and other excellent properties, and is often used as polyurethane , Epoxy resin and other modified materials. At present, hydroxyl-containing organosilicon resin modified materials have been widely used in corrosion-resistant coatings, fabric treatment materials, and packaging materials for organic light-emitting diodes (OLEDs). [0003] Preparation of hydroxy silicone resin by chlorosilane hydrolysis requires the use of toxic solvents such as toluene, and auxiliary processes such as washing with water,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/045
Inventor 郑耀臣高正国薛清泉
Owner 烟台优尼泰电子科技有限公司