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Intercalation preparation method of nylon 6/quaternary phosphonium salt modified montmorillonite nano composite material

A technology of nanocomposite material and quaternary phosphonium salt, which is applied in the field of intercalation preparation, can solve the problems of low thermal decomposition temperature of quaternary ammonium salt, difficult to manifest nanometer effect, and release of intercalation agent, achieves high thermal stability, and solves nylon 6 The effect of resin discoloration and chemical stability

Active Publication Date: 2013-03-27
GUANGDONG XINHUI MEIDA NYLON
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006]1. Commonly used intercalation modifiers are long-chain alkyl quaternary ammonium salts, but the thermal decomposition temperature of quaternary ammonium salts is low. When desoiling and engineering plastics are melt blended and intercalated, engineering plastics will be discolored due to the decomposition of quaternary ammonium salts, which restricts the application of organic montmorillonite in engineering plastics
[0007]2. The modification method of montmorillonite is that the organic small molecule intercalation agent enters the interlayer of montmorillonite through ion exchange, and the intercalation agent and montmorillonite sheet The bonding force between the layers is relatively weak. During the intercalation process of melt blending with nylon 6, a part of the intercalation agent between the layers will come out due to strong shearing, so that the polymer macromolecules cannot enter the montmorillonite layer to form a real nanostructured composites
Montmorillonite will re-aggregate into massive large particles, which is difficult to fully and effectively disperse uniformly, making the performance of nylon 6 / montmorillonite nanocomposites far lower than the theoretical expected value, and it is difficult to reflect the nano effect

Method used

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  • Intercalation preparation method of nylon 6/quaternary phosphonium salt modified montmorillonite nano composite material
  • Intercalation preparation method of nylon 6/quaternary phosphonium salt modified montmorillonite nano composite material

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preparation example Construction

[0021] A kind of intercalation preparation method of nylon 6 / quaternary phosphonium salt modified montmorillonite nanocomposite material, comprises the following steps:

[0022] 1) Add quaternary phosphonium salt and sodium montmorillonite into water at a mass ratio of 1:3-5, and stir at 60-100°C for 4-8 hours;

[0023] 2) Filtrating the solution in step 1), washing the obtained solid, drying, grinding, and sieving to obtain a quaternary phosphonium salt intercalation-modified montmorillonite;

[0024] 3) Take the quaternary phosphonium salt intercalation-modified montmorillonite and caprolactam in step 2), add them into the reaction kettle, stir evenly at room temperature, add water, benzoic acid, and isophthalic acid into the reaction kettle, and carry out the reaction under the protection of inert gas. Hydrolysis polymerization reaction, the reaction temperature is 250-260°C, the reaction time is 6-8h, after the reaction, pelletize to obtain slices of nylon 6 / montmorillonit...

Embodiment 1

[0029] A kind of intercalation preparation method of nylon 6 / quaternary phosphonium salt modified montmorillonite nanocomposite material, comprises the following steps:

[0030] 1) Weigh 200g of sodium montmorillonite powder and 60g of octadecyltributylphosphonium bromide, add them to 1L of distilled water, stir the above solution at 80°C for 360min, and carry out organic intercalation of montmorillonite Reactive modification;

[0031] 2) vacuum filter the above solution, wash the obtained solid with deionized water, vacuum dry, grind, and pass through a 300-mesh sieve, and the obtained solid is quaternary phosphonium salt intercalation modified montmorillonite;

[0032] 3) Weigh 150g of the above-mentioned quaternary phosphonium salt modified montmorillonite and 3000g of caprolactam, add them into the reaction kettle, stir evenly at room temperature, add water, benzoic acid and isophthalic acid into the reaction kettle, the quality of the added water is 6% of caprolactam, th...

Embodiment 2

[0036] A kind of intercalation preparation method of nylon 6 / quaternary phosphonium salt modified montmorillonite nanocomposite material, comprises the following steps:

[0037] 1) Weigh 180g of sodium montmorillonite powder and 60g of octadecyltributylphosphonium bromide, add them to 1L of distilled water, stir the above solution at 60°C for 4h, and carry out organic intercalation of montmorillonite Reactive modification;

[0038] 2) vacuum filter the above solution, wash the obtained solid with deionized water, vacuum dry, grind, and pass through a 300-mesh sieve, and the obtained solid is quaternary phosphonium salt intercalation modified montmorillonite;

[0039] 3) Weigh 150g of the above-mentioned quaternary phosphonium salt modified montmorillonite and 2700g of caprolactam, add them into the reaction kettle, stir evenly at room temperature, add water, benzoic acid and isophthalic acid into the reaction kettle, the quality of the added water is The mass of caprolactam i...

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Abstract

The invention discloses an intercalation preparation method of a nylon 6 / quaternary phosphonium salt modified montmorillonite nano composite material. The method comprises the following steps: 1) adding quaternary phosphonium salt and sodium-based montmorillonite into water in a mass ratio of 1:(3-5), and stirring for 4-8 hours at the temperature of 60-100 DEG C; 2) filtering a solution obtained in the step 1) so as to obtain a solid, washing, drying, grinding, and sieving so as to obtain quaternary phosphonium salt intercalation modified montmorillonite; 3) evenly stirring the quaternary phosphonium salt intercalation modified montmorillonite obtained in the step 2) with caprolactam at room temperature, adding water and an auxiliary for carrying out hydrolysis polymerization reaction on caprolactam, and pelletizing after reaction so as to obtain a nylon 6 / montmorillonite nano composite material slice, wherein the mass ratio of quaternary phosphonium salt intercalation modified intercalation modified montmorillonite to caprolactam is 1: (18-22); and 4) extracting the slice obtained in the step 3) with water. The product obtained by the method in the invention has good mechanical property and color is not easily to change.

Description

technical field [0001] The invention relates to an intercalation preparation method of nylon 6 / quaternary phosphonium salt modified montmorillonite nano composite material. Background technique [0002] Intercalation composite method is an important method to prepare high-performance polymer-based nanocomposites, and it is also one of the current research hotspots in the field of materials science. It is to insert the monomer between the montmorillonite sheets for in-situ polymerization, or the polymer is directly inserted between the montmorillonite sheets, thereby destroying the sheet structure of the montmorillonite to form a polymer nanocomposite material. The composite of the polymer and the montmorillonite at the nanometer level greatly increases the interfacial interaction between the polymer and the montmorillonite, so that the composite material has excellent mechanical properties. [0003] Polymer / montmorillonite nanocomposites have the advantages of excellent com...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/16C08K9/04C08K3/34
Inventor 梁伟东毛新华戈明亮宋明简锦炽陈欣谌继宗
Owner GUANGDONG XINHUI MEIDA NYLON