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In-situ polymerization PI modified nylon composite material

An in-situ polymerization and modified nylon technology, which is applied in the field of in-situ polymerization PI-modified nylon composite materials, can solve the problems of PI-modified PA's water absorption and mechanical properties are not good enough, and achieve the effect of effectively blocking moisture

Inactive Publication Date: 2008-07-30
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to overcome the disadvantages of insufficient water absorption and mechanical properties of PI modified PA produced by the prior art, the present invention proposes a method for preparing in-situ polymerized PI modified nylon composite materials. The composite materials produced by this method have both good The water absorption performance has excellent mechanical properties

Method used

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  • In-situ polymerization PI modified nylon composite material
  • In-situ polymerization PI modified nylon composite material
  • In-situ polymerization PI modified nylon composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Using rigid segments such as polyimide to modify nylon resin and prepare composite materials can improve its mechanical properties and take into account toughness and water resistance. The specific steps are as follows:

[0028]The first step: prepare polyimide (PI) prepolymer, the molar ratio of 1~1.6:1 can be 1:1, 1.2:1 or 1.6:1 will have the dianhydride / diamine of ether bond group The solid is dissolved in a polar solvent and stirred at room temperature, and reacted with nitrogen for 5 hours to obtain a polyamic acid polymer, and then add toluene or xylene solvent at 160°C to 180°C, which can be 160°C, 168°C or 180°C for reflux cyclization 3h, get the acid anhydride-terminated polyimide macromolecules, remove the water in the system, add isocyanate, the reaction temperature is controlled at 80°C to 90°C, it can be 80°C, 83°C or 90°C for 1h to 1.5h It is 1h, 1.3h or 1.5h, and then the temperature is raised to 120°C ~ 130°C, it can be 120°C, 126°C or 130°C for 3h ~ 5h,...

Embodiment 2

[0032] The steps are the same as in Example 1, wherein the molecular weight of the PI modifier is selected to be 4000, the weight percentage of the PI modifier to the monomer is 15%, 10%, and 5% respectively, and the viscosity of the system after being incorporated into the monomer is respectively 0.2Pa.s , 0.6Pa.s, 1Pa.s, the impregnated fiber is good. The NaOH content accounts for 0.1% and 0.2% of the monomer respectively. The main antioxidant (1098) was 0.1%, 0.25%, 0.5%, and the auxiliary antioxidant (168) was 0.1%, 0.25%, 0.5%, respectively. Wherein the dianhydrides with ether bond groups described in the first step are respectively bisphenol A ether dianhydrides, or select 3,3',4,4'-tetracarboxylic acid diphenyl ether dianhydrides. The diamines are 2,2-bis[4-(4-aminophenoxy)phenyl]propane or 3,3'-diaminodiphenyl ether and 3,4'-diaminodiphenyl ether respectively. The polar solvent in the first step can be N-methylpyrrolidone, dimethylformamide or dimethylacetamide. Usi...

Embodiment 3

[0034] The steps are the same as in Example 1, wherein the molecular weight of the PI modifier is selected to be 8000 or 13000 respectively, and the PI modifier accounts for 15%, 10%, and 5% by weight of the monomer respectively, and the viscosities of the systems after being respectively incorporated into the monomer are respectively 0.2Pa.s, 0.6Pa.s, 1Pa.s, impregnated fiber is good. The NaOH content accounts for 0.1% and 0.2% of the monomer respectively. The main antioxidant (1098) was 0.1%, 0.25%, 0.5%, and the auxiliary antioxidant (168) was 0.1%, 0.25%, 0.5%, respectively. Wherein the dianhydrides with ether bond groups described in the first step are respectively bisphenol A ether dianhydrides, or select 3,3',4,4'-tetracarboxylic acid diphenyl ether dianhydrides. The diamines are 2,2-bis[4-(4-aminophenoxy)phenyl]propane or 3,3'-diaminodiphenyl ether and 3,4'-diaminodiphenyl ether respectively. The polar solvent in the first step can be N-methylpyrrolidone, dimethylfor...

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Abstract

The invention discloses a preparation method of in-situ polymerization PI modified nylon composite material, which comprises the following steps: step one, polyimide prepolymer is prepared, a dianhydride / diamidogen monomer with ether linkage base group is dissolved in polar solvent according to the mol ratio of 1-1.6: 1 and then agitated to react, then, dissolvent is added to perform the backflow cyclization in order to remove water content in the system, carbimide is added to react to obtain PI large molecule which is end-capped with carbimide, caprolactam is added to close a carbimide base group, methanol is added to precipitate out PI, and then the PI is washed and dried for standby, the PI with mass occupying by 5-15 percent of the weight percentage of the caprolactam monomer is added into a caprolactam molten mass, and the system viscosity is maintained to 0.02-1 Pa.s; step two, according to the 50-85 percent of volume ratio, carbon fiber is laid in the die and preheated, NaOH, primary antioxidant and secondary antioxidant are mixed with the prepolymer manufactured in the step one are filled into the die under 90-120 DEG C to perform the in-situ polymerization reaction to obtain FRP sheet material.

Description

technical field [0001] The invention relates to the field of preparation of nylon modified materials, in particular to an in-situ polymerized PI modified nylon composite material. Background technique [0002] At present, there are many nylon modified alloys, and the method of adding reactive compatibilizers to the blend system is often used to increase the compatibility between polymers. [0003] There have been a small amount of research abroad on PI-modified nylon 6 resin systems, but there is no research report on fiber-reinforced in-situ polymerization of PI-modified PA composites. Hong Ding studied the synthesis and performance of nylon 6-P I-nylon 6 triblock copolymer, the route is as follows [0004] [0005] Adopt 3,3-dimethyl-4,4-diaminobiphenyl (OTOL), biphenyl dianhydride (BPDA), hexafluoro dianhydride (6FDA) reaction to obtain the polyamic acid oligomer of acid anhydride termination, add para Aminobenzoyl caprolactam is capped, and then pyridine and acetic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08K7/06C08K5/20C08K5/526C08J5/18C08G73/14B29C70/34B29C70/54
Inventor 钱春香赵洪凯
Owner SOUTHEAST UNIV