Preparation method of nanometer organic modified zirconium phosphate/MC nylon composite material

A technology of nylon composite materials and organic zirconium phosphate, which is applied in the field of MC nylon composite materials, can solve undiscovered problems and achieve the effects of reducing flocculation, large layer spacing, and improving moisture resistance performance

Active Publication Date: 2017-09-15
HUNAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Research on this type of material has only focused on improving the interaction between inorganic nanofillers and polymer matrices by adding unmodified montmorillonite, surface-modified organic montmorillonite, or graphene oxide. Research reports and invention patents related to the modification of zirconium phosphate nanoparticles by doping during the preparation of MC nylon

Method used

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  • Preparation method of nanometer organic modified zirconium phosphate/MC nylon composite material
  • Preparation method of nanometer organic modified zirconium phosphate/MC nylon composite material
  • Preparation method of nanometer organic modified zirconium phosphate/MC nylon composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Preparation of zirconium organophosphate:

[0034] S1. Add 10g ZrOCl in the reaction flask 2 ·8H 2 O, 10g NaF and 100mL distilled water, after stirring and dissolving, add 50mL of 85wt% H 3 PO 4 , exhaust the air in the reaction bottle and then introduce N 2 , Electromagnetic stirring at 25°C continued the reaction for 196h, high-speed centrifugation to separate the precipitate, repeated washing with distilled water until the pH value was neutral, vacuum drying at 60°C and grinding to obtain α-zirconium phosphate powder, and its CEC (cation exchange capacity) was measured It is 195mmol / 100g, and the interlayer distance is 0.76nm.

[0035] S2. Weigh 4.0g of the α-zirconium phosphate powder prepared in step S1, disperse it in 100mL of deionized water, then add 0.1CEC of n-butylamine dropwise for pre-strut, stir and react in a constant temperature water bath at 40°C for 6h, and then continue to drop Add 0.9CEC of ethylene bis(dodecyldimethylammonium chloride) to c...

Embodiment 2

[0041] (1) Preparation of zirconium organophosphate:

[0042] S1. is the same as embodiment 1;

[0043] S2. Weigh 10g of the α-zirconium phosphate powder prepared in step S1, disperse it in 250mL of deionized water, and then add 0.2CEC of n-butylamine dropwise for pre-strutting, stir and react in a constant temperature water bath at 40°C for 6h, and then continue to add dropwise 0.8CEC of ethylene bis(tetradecyldimethylammonium chloride) was chemically modified, and the reaction was continued for 24h under the condition of stirring in a constant temperature water bath at 50°C. The precipitate was separated by high-speed centrifugation, washed by centrifugation with 50% (v / v) ethanol solution and deionized water respectively, vacuum-dried at 60° C., and ground to obtain an organic zirconium phosphate sample. The interlayer distance of modified zirconium phosphate is 3.30nm calculated by XRD detection and Bragg formula.

[0044] (2) Preparation of zirconium organophosphate / MC ...

Embodiment 3

[0049] (1) Preparation of zirconium organophosphate:

[0050] S1. is the same as embodiment 1;

[0051] S2. Weigh 100g of the α-zirconium phosphate powder prepared in step S1, disperse it in 2500mL of deionized water, then add 0.3CEC of n-butylamine dropwise for pre-strut, stir and react in a constant temperature water bath at 40°C for 6h, and then continue to add dropwise 0.7CEC of ethylene bis(hexadecyldimethylammonium chloride) was chemically modified, and the reaction was continued for 24 hours under the condition of stirring in a constant temperature water bath at 50°C. The precipitate was separated by high-speed centrifugation, washed by centrifugation with 50% (v / v) ethanol solution and deionized water respectively, vacuum-dried at 60° C., and ground to obtain an organic zirconium phosphate sample. The interlayer distance of modified zirconium phosphate is 2.90nm calculated by XRD detection and Bragg formula.

[0052] (2) Preparation of zirconium organophosphate / MC ny...

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Abstract

The invention provides a preparation method of a nanometer organic modified zirconium phosphate / MC nylon composite material, wherein organic zirconium phosphate, a caprolactam monomer, a catalyst, an initiator and a silane coupling agent are subjected to a reaction to obtain the nanometer organic modified zirconium phosphate / MC nylon composite material. According to the preparation method, alpha-zirconium phosphate is modified with n-butylamine and a Gemini surfactant, and then a co-precipitation method is performed to obtain the organic zirconium phosphate; the organic zirconium phosphate is subjected to high speed dispersion with the caprolactam monomer; the silane coupling agent and the catalyst are added; operations such as heating, high speed stirring and thermal insulation are performed, the obtained material is mixed with the caprolactam monomer added with the initiator after the melting, the obtained mixture is transferred into a mold, the mold is placed into an oven, the temperature is adjusted, and a thermal insulation reaction is performed; and cooling demolding is performed to obtain the nanometer organic modified zirconium phosphate / MC nylon composite material.

Description

technical field [0001] The invention relates to the technical field of MC nylon composite materials, in particular to a preparation method of nanometer organically modified zirconium phosphate / MC nylon composite materials. Background technique [0002] Because of its good physical stability, chemical corrosion resistance and high wear resistance, MC nylon products can replace steel, copper, aluminum and other metal materials within a certain range, and are suitable for chemical, mechanical, textile, petroleum, electrical, etc. and other application fields. However, pure MC nylon products have defects such as poor dimensional stability, thermal stability and low-temperature toughness, which limit its application to a certain extent. At present, the modification of MC nylon and the preparation of composite materials have been carried out in many aspects in China, and the inorganic modification and organic modification are more concentrated. Among them, the main method of ino...

Claims

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Application Information

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IPC IPC(8): C08G69/16C08G69/14C08K9/04C08K7/00C08K3/32C08K5/544C08K5/5435C08K5/5425
CPCC08G69/14C08G69/16C08K3/32C08K5/5425C08K5/5435C08K5/544C08K7/00C08K9/04C08K2003/328C08K2201/003C08K2201/011
Inventor 刘小超李知函刘跃军杨军
Owner HUNAN UNIV OF TECH
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