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In-situ preparation method of ceramic whisker/nylon composite material

A technology for nylon composite materials and ceramic whiskers, which is applied in the field of preparing whisker/nylon composite materials by in-situ hydrolysis polymerization, which can solve the problem of reducing the reinforcement effect of whiskers, making it difficult to achieve uniform dispersion of whiskers, and difficult to achieve uniform dispersion of whiskers And other problems, to achieve the effect of high modulus, good impact toughness

Active Publication Date: 2010-07-07
HEFEI GENIUS NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The screw extrusion process is difficult to achieve uniform dispersion of whiskers, which will greatly reduce the reinforcing effect of whiskers
Another method is to use normal pressure in-situ polymerization, disperse the whiskers in the monomer, add the initiator and carry out polymerization under normal pressure. Similarly, it is difficult to achieve uniform dispersion of the whiskers in this method.

Method used

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  • In-situ preparation method of ceramic whisker/nylon composite material
  • In-situ preparation method of ceramic whisker/nylon composite material
  • In-situ preparation method of ceramic whisker/nylon composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Silicon nitride whisker / nylon 6 system

[0023] The monomer of the system is caprolactam, and the ceramic whiskers are silicon nitride whiskers. Mix 5 parts of silicon nitride whiskers with 100 parts of caprolactam, 50 parts of water, and 0.5 parts of benzoic acid, and then add them to the polymerization kettle. The temperature was raised to 240°C, the pressure was raised to 2.0Mpa, the pre-polymerization reaction time was 8 hours, and then the gas was slowly exhausted to reduce the pressure of the polymerization tank to normal pressure. After polymerization under normal pressure for 2 hours, carry out polymerization under reduced pressure at 250°C. The pressure of the polymerization tank is 2000 Pa. After the viscosity is constant, the reaction is completed. Extruded into strips, water-cooled and pelletized to obtain finished pellets.

[0024] In order to better illustrate the superiority of the present invention, a sample prepared by atmospheric pressure in-situ pol...

Embodiment 2

[0030] Silicon nitride whisker / nylon 66 system

[0031] The nylon monomer of this system is nylon 66 salt, 5 parts of silicon nitride whiskers, 100 parts of nylon 66 salt, 50 parts of water, 0.5 part of benzoic acid (molecular weight regulator), 0.1 part of antioxidant 168 are added to the polymerization kettle Pre-polymerize at 230°C and 2.6MPa for 4 hours, then raise the temperature to above 260°C and exhaust to normal pressure, after 1 hour of normal compression polymerization, reduce pressure and polymerize at 300°C and 1000Pa for 2 hours until the viscosity is constant Post-polymerization ends. Pure nylon 66 was prepared by the same method as a comparison sample without adding silicon nitride whiskers. The mechanical properties of nylon 66 and silicon nitride whisker / nylon 66 composite materials are compared in Table 2.

[0032] Table 2 The mechanical properties of pure nylon 66 and silicon nitride whisker / nylon 66 composites when the silicon nitride whisker content is 5...

Embodiment 3

[0036] Potassium titanate whisker / nylon 12 system

[0037] Mix 50 parts of potassium titanate whiskers with 100 parts of laurolactam, 225 parts of water, and 1 part of adipic acid, and then add them to the polymerization kettle. The temperature was raised to 260°C, the pressure was raised to 3.2Mpa, the pre-polymerization reaction time was 14 hours, and then the gas was slowly exhausted to reduce the pressure of the polymerization tank to normal pressure. After 4 hours of polymerization under normal pressure, polymerize under reduced pressure at 300°C. The pressure of the polymerization tank is 6000 Pa. After the viscosity is constant, the reaction is completed. Extruded into strips, water-cooled and pelletized to obtain finished pellets.

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Abstract

The invention relates to an in-situ preparation method of ceramic whisker / nylon composite material. The method includes that ceramic whiskers are mixed with water, polymer monomers and molecular weight regulator in a certain proportion and then put in a polymerization autoclave; the mixed substances are pre-polymerized for 1-14 hours under the conditions of 200-260 EDG C and 0.6-3.2 MPa in the polymerization autoclave, then polymerized for 0.5-4 hour(s) under constant pressure after vapor is discharged, and finally polymerized for 0.2-2 hour(s) under the conditions of 220-300 DEG C and 200-6000Pa after pressure is lowered; the nylon composite material enforced by ceramic whiskers is directly prepared. Compared with the traditional screw extrusion melt blending technology and the constant-pressure in-situ polymerization technology, the method of the invention realizes even dispersion of the whiskers in the composite material and great improvement of enforcing and toughing effect of the whiskers.

Description

technical field [0001] The invention relates to a method for preparing a ceramic whisker-reinforced polymer composite material, in particular to a method for preparing a whisker / nylon composite material by in-situ hydrolysis polymerization. Background technique [0002] Ceramic whiskers are single crystals with a large aspect ratio. Because of their extremely high degree of crystallization perfection and high orientation, the strength of the whiskers is very close to the theoretical strength. For example, the tensile strength and Young's modulus of silicon nitride whiskers are as high as 50-60GPa and 550-750GPa, respectively, while the tensile strength and modulus of ordinary glass fibers are only 3GPa and 60-90GPa, respectively. In addition, whiskers also have good toughness. Using ceramic whiskers to fill polymers to prepare composite materials can often not only significantly improve the strength and modulus of the material, but also significantly improve the impact toug...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L77/00C08K7/04C08G69/04
Inventor 李兰杰杨桂生
Owner HEFEI GENIUS NEW MATERIALS