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Preparation method of organic silicon resin with alternating structure

A technology of alternating structure and organosilicon, applied in the field of synthesis of polyhydroxy organosilicon hybrid polymers, can solve the problems of equipment and environmental hazards, difficult control of molecular structure of hydroxyl-containing silicone resin, etc., to achieve no by-products and clear structure. Controllable, high reaction rate effect

Active Publication Date: 2015-08-05
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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  • Preparation method of organic silicon resin with alternating structure
  • Preparation method of organic silicon resin with alternating structure
  • Preparation method of organic silicon 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, 6.80mmol), and the photosensitive free radical initiator 2-hydroxymethylphenylpropan-1-one (0.41g, 1.0mmol) 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 an alternating structure. According to the method, under the protection of nitrogen or argon, mercapto-vinyl polymerization reaction of a dithiol compound and an organosilicon compound containing a divinyl group is initiated by a thermo-sensitive free radical initiator under a heating condition or by a photosensitive free radical initiator under an ultraviolet irradiation condition to obtain polyhydroxyl organosilicone hybrid resin with an alternating structure. The method has the advantages of no need of hydrolysis, drying and protection-deprotection processes, high reaction speed, clear and controllable structure of a product, easiness in adjustment of content of a hydroxyl group, no side product, low requirement on equipment material and the like. Meanwhile, the molecular structure contains a large amount of sulfur atoms, so the refractive index of the material can be obviously improved; besides, the molecular structure contains a large number of thioether bonds, the glass transition temperature of the product is low (smaller than 20 DEG C below zero), the texture is soft, and the product is also extremely suitable for making a fabric treating agent and a high-performance corrosion-resistant coating or wear-resistant layer.

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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IPC IPC(8): C08G75/04
Inventor 郑耀臣高正国薛清泉
Owner 烟台优尼泰电子科技有限公司