Macromolecule coupling agent containing active cyano group and preparing method thereof

The technology of macromolecular coupling agent and cyano group is applied in the field of macromolecular coupling agent containing active cyano group and its preparation, which can solve the problems of unfavorable industrial production, high requirement of raw material purity, long reaction time and the like

Inactive Publication Date: 2008-01-16
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Free radical polymerization is commonly used in the preparation of macromolecular coupling agents. Most of the reported macromolecular silane coupling agents use atom transfer polymerization. Although the coupling agent prepared by this polymerization method has the characteristics of controllable molecular structure, the The preparation process is complex, the reaction time is long, and the purity requirements of raw materials are high, which is not conducive to industrial production

Method used

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  • Macromolecule coupling agent containing active cyano group and preparing method thereof
  • Macromolecule coupling agent containing active cyano group and preparing method thereof
  • Macromolecule coupling agent containing active cyano group and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Place the equipment used in the reaction process in an oven to fully dry, and then add 70ml xylene, 40.0ml styrene, 10.3ml vinyltrimethoxysilane, 0.54g BPO to the three-necked flask, stir and pour nitrogen into it. Slowly heat to 110°C. After 3.5 hours of reaction, the temperature is raised to 120°C, and after 1.5 hours of reaction at this temperature, the heating is stopped. After cooling to 70°C, 9.2ml of acrylonitrile was added to the three-necked flask, heated and kept at 75-80°C for 3.5h, and then distilled under reduced pressure. Finally, it was dissolved in tetrahydrofuran and precipitated in 200ml methanol. Finally, it was vacuum dried at 65°C for 4h to obtain a white solid powder. . The number average molecular weight of the synthesized terpolymer macromolecular coupling agent was determined by gel permeation chromatography (GPC) to be 11,600, and the molecular weight distribution width was 1.73.

Embodiment 2

[0035] Place the equipment used in the reaction process in an oven and fully dry it, then add 70ml xylene, 40.0ml styrene, 10.3ml vinyltrimethoxysilane, 0.27gBPO to the three-necked flask, stir and pour nitrogen into it. Slowly heat to 110°C. After 3.5 hours of reaction, the temperature is raised to 120°C, and after 1.5 hours of reaction at this temperature, the heating is stopped. After cooling to 70°C, 9.2ml of acrylonitrile was added to the three-necked flask, heated and kept at 75-80°C for 3.5h, and then distilled under reduced pressure. Finally, it was dissolved in tetrahydrofuran and precipitated in 200ml methanol. Finally, it was vacuum dried at 65°C for 4h to obtain a white solid powder. The number average molecular weight of the synthesized terpolymer macromolecular coupling agent was determined by gel permeation chromatography (GPC) to be 25,300, and the molecular weight distribution width was 2.82.

Embodiment 3

[0037] Place the equipment used in the reaction process in an oven and fully dry, add 70ml xylene, 40ml styrene, 20.6ml vinyl trimethoxysilane, 0.54g BPO to the three-necked flask, stir and blow in nitrogen slowly. After heating to 110°C and reacting for 3.5 hours, the temperature is raised to 120°C, and after reacting at this temperature for 1.5 hours, the heating is stopped. After cooling to 70°C, 9.2ml of acrylonitrile was added to the three-necked flask, heated and kept at 75-80°C for 3.5h, and then distilled under reduced pressure. Finally, it was dissolved in tetrahydrofuran and precipitated in 200ml methanol. Finally, it was vacuum dried at 65°C for 4h to obtain a white solid powder. The number average molecular weight of the synthesized terpolymer macromolecular coupling agent was determined by gel permeation chromatography (GPC) to be 14,700, and the molecular weight distribution width was 1.86.

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Abstract

The invention relates to a macromolecular coupling agent containing active cayno and a preparation method of the macromolecular coupling agent containing active cayno. The technology of the invention is characterized in that a ternary random copolymer is synthesized by means of free radical polymerization reaction with styrene, acrylonitrile and vinyl trimethoxy silane as monomers, dibenzoyl peroxide and azobisisobutyronitrile as an initiator, and one of xylene, toluene, benzene or dimethylformamide as a solvent. The preparation steps are as follow: the solvent, the monomers and the initiator are put into a three-mouth flask sequentially and mixed, nitrogen is input, and then the flask is heated slowly until thermal insulation, the heating is stopped after the reaction. A quantity of the acrylonitrile is put into the three-mouth flask after the flask is cooled, then the solution is vacuum distilled after being heated and thermal insulated. At last, the ternary copolymer macromolecular coupling agent is obtained with the solution being dissolved with tetrahydrofuran, precipitated in methanol and dried in vacuum. The coupling agent is suitable for the composite material system with cyanate ester resin as matrix, glass fiber or inorganic particles as reinforcing material with simple preparation process and short reaction time, which lays a foundation for industrialized production.

Description

Technical field [0001] The invention relates to an active cyano group-containing macromolecular coupling agent and a preparation method thereof, and belongs to the field of polymer materials. Background technique [0002] The improvement of material interface performance can optimize various properties of composite materials. At present, the most commonly used method is to use a coupling agent. The coupling agent can not only improve the compatibility between the organic phase and the inorganic phase, but also improve the mechanical properties, electrical properties, and wear resistance of the composite material. This is because the structural state of the interface layer is changed, chemical bonding is introduced, and the bonding strength and stress transfer of the interface layer are improved. There are many kinds of existing coupling agents, and there are more than one hundred kinds of silane coupling agents with known structures. However, most varieties are small molecule cou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/10C08F230/08C08F4/04C08F4/34C08L75/00C08K7/14
Inventor 颜红侠梁国正马晓燕
Owner NORTHWESTERN POLYTECHNICAL UNIV
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