Macromolecule coupling agent containing active cyano group and preparing method thereof

A technology of macromolecular coupling agent and cyano group, applied in the field of active cyano group-containing macromolecular coupling agent and its preparation, can solve the problems of unfavorable industrial production, complicated preparation process, and high purity requirements of raw materials

Inactive Publication Date: 2009-11-18
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] After the instruments to be used in the reaction process were placed in an oven and fully dried, 70ml of xylene, 40.0ml of styrene, 10.3ml of vinyltrimethoxysilane, and 0.54g of BPO were successively added to the three-necked flask, stirred and nitrogen gas was introduced. Slowly heated to 110°C, after 3.5 hours of reaction, the temperature was raised to 120°C, and after 1.5 hours of reaction at this temperature, the heating was stopped. After cooling down to 70°C, add 9.2ml of acrylonitrile into the three-necked flask, heat and keep it at 75-80°C for 3.5h, then distill under reduced pressure. Finally, it was dissolved in tetrahydrofuran, precipitated in 200ml of methanol, and finally vacuum-dried at 65°C for 4 hours to obtain a white solid powder. . The number-average molecular weight of the synthesized terpolymer macromolecular coupling agent was determined to be 11,600 by gel permeation chromatography (GPC), and the molecular weight distribution width was 1.73.

Embodiment 2

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

Embodiment 3

[0037] After placing the instruments used in the reaction process in an oven and fully drying them, add 70ml of xylene, 40ml of styrene, 20.6ml of vinyltrimethoxysilane, and 0.54g of BPO into the three-necked flask in sequence, stir and introduce nitrogen gas, slowly Heat to 110°C, react for 3.5 hours, then raise the temperature to 120°C, and react at this temperature for 1.5 hours, then stop heating. After cooling down to 70°C, add 9.2ml of acrylonitrile into the three-necked flask, heat and keep it at 75-80°C for 3.5h, then distill under reduced pressure. Finally, it was dissolved in tetrahydrofuran, precipitated in 200ml of methanol, and finally vacuum-dried at 65°C for 4 hours to obtain a white solid powder. The number-average molecular weight of the synthesized terpolymer macromolecular coupling agent was determined to be 14,700 by gel permeation chromatography (GPC), and the molecular weight distribution width was 1.86.

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Abstract

The invention relates to a macromolecular coupling agent containing active cyano groups and a preparation method thereof. Azodiisobutyronitrile is used as an initiator, and one of xylene, toluene, benzene or dimethylformamide is used as a solvent to synthesize a ternary random copolymer by free radical polymerization. Preparation steps: Add solvent, monomer and initiator to a three-necked flask in sequence, stir and feed nitrogen, slowly heat to keep warm, and stop heating after reaction. After cooling down, add a certain amount of acrylonitrile into the three-necked flask, heat and keep warm, and distill under reduced pressure. Finally, it was dissolved in tetrahydrofuran, precipitated in methanol, and dried in vacuum to obtain a terpolymer macromolecular coupling agent. The coupling agent is suitable for a composite material system with cyanate resin as the matrix and glass fiber or inorganic particles as the reinforcing material. The preparation process is simple and the reaction time is short, which lays the foundation for industrial production.

Description

technical field [0001] The invention relates to a macromolecular coupling agent containing active cyano groups and a preparation method thereof, belonging to the field of polymer materials. Background technique [0002] The improvement of material interface properties can optimize the 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 due to the change of the structure state of the interface layer, the introduction of chemical bonding, and the improvement of the bond strength and stress transfer of the interface layer. 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 m...

Claims

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Application Information

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Patent Type & Authority Patents(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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