Preparation method of composite material for inorganic modified melamine chlorinated isocyanurate flame-retardant nylon 6

A technology of melamine cyanurate and inorganic modification is applied in the preparation of composite materials and the field of preparation of inorganic modified melamine cyanurate flame retardant nylon 6 composite materials, which can solve the problem of color deterioration of composite materials and other problems of composite materials. Performance degradation, environmental pollution, etc.

Inactive Publication Date: 2013-05-01
HUNAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods have greatly improved the flame retardant performance of nylon 6 and expanded its application range; but these methods also have deficiencies in varying degrees, mainly in the following aspects: First, some flame retardants have energy consumption during the preparation process High and environmental pollution; second, some composite materials need to add a large amount of flame retardants to reach the UL 94 V-0 level; third, some flame re

Method used

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  • Preparation method of composite material for inorganic modified melamine chlorinated isocyanurate flame-retardant nylon 6
  • Preparation method of composite material for inorganic modified melamine chlorinated isocyanurate flame-retardant nylon 6
  • Preparation method of composite material for inorganic modified melamine chlorinated isocyanurate flame-retardant nylon 6

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Preparation of silica-modified melamine cyanurate flame-retardant nylon 6 composite material: add 2 kg of caprolactam to a 5-liter polymerization kettle, heat up to 70 ° C, add 65 g of melamine, 65 g of cyanuric acid and 15 ml of orthosilicic acid Ethyl ester, adjust the pH value to 2.0, react for 2 hours, replace the air in the kettle with high-purity nitrogen, raise the temperature to 180°C, pressurize to 1.0MPa, polymerize for 3 hours, then depressurize to -1.0MPa, polymerize for 13 hours, The material is discharged to obtain a silica-modified melamine cyanurate flame-retardant nylon 6 composite material, which is extracted with water and dried to obtain a finished product. The flame retardant performance and mechanical performance test of the product obtained by implementing Lee 1 are carried out, and the commercially available industrial nylon 6 sample is tested simultaneously. See Table 1 for the data.

[0017] Table I

[0018]

Embodiment 2

[0020] Preparation of silica-modified melamine cyanurate flame-retardant nylon 6 composite material: add 2 kg of caprolactam to a 5-liter stainless steel polymerization kettle, heat up to 100 ° C, add 50 g of melamine, 50 g of cyanuric acid and 15 ml of orthosilicone Ethyl acetate, adjust the pH value to 6.0, react for 2 hours, replace the air in the kettle with high-purity nitrogen, raise the temperature to 280°C for polymerization for 2 hours, then reduce the pressure to -1.0MPa, polymerize for 1 hour, and discharge the material to obtain two Silica-modified melamine cyanurate flame-retardant nylon 6 composite material, extracted with water and dried to obtain a finished product. The flame retardancy and mechanical properties of the product obtained in the implementation of Lee 2 were tested, and the commercially available industrial nylon 6 samples were tested at the same time. See Table 2 for the data.

[0021] Table II

[0022]

Embodiment 3

[0024] Preparation of graphene oxide modified melamine cyanurate flame retardant nylon 6 composite material: add 2 kg of caprolactam to a 5 liter stainless steel polymerization kettle, heat up to 95°C, add 80 g of melamine, 80 g of cyanuric acid and graphene oxide 120 ml of 0.8 grams of colloid, adjust the pH value to 10.0, react for 1.5 hours, replace the air in the kettle with high-purity nitrogen, heat up to 260 ° C for 4 hours, then reduce the pressure to -0.8MPa, polymerize for 1.5 hours, and discharge , the graphene oxide modified melamine cyanurate flame-retardant nylon 6 composite material was obtained, extracted with water, and dried to obtain a finished product. The flame retardant performance and mechanical performance test of the product obtained by implementing Lee 3 are carried out, and the commercially available industrial nylon 6 samples are tested at the same time. See Table 3 for the data.

[0025] Table three

[0026]

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Abstract

The invention discloses a preparation method of a composite material for inorganic modified melamine chlorinated isocyanurate flame-retardant nylon 6. The preparation method is characterized in that melted caprolactam is taken as a reaction medium; melamine and cyanuric acid react under the conditions of certain temperature and certain pH value; during the reaction process, water, an inorganic modified component and/or a precursor for generating the inorganic modified component, and other blending agents are added to prepare inorganic modified melamine chlorinated isocyanurate compound flame retardant; and then the composite material for the inorganic modified melamine chlorinated isocyanurate flame-retardant nylon 6 is prepared through in-situ polymerization under the conditions of certain temperature and certain pressure. During the whole preparation process, melted caprolactam not only serves as a resolvent for preparation of inorganic modified melamine chlorinated isocyanurate, but also serves as a polymerization monomer of the nylon 6; and synthesis and modification of modified melamine chlorinated isocyanurate and polymerization of the nylon 6 are accomplished at one step. The composite material for the flame-retardant nylon 6 has the characteristics of small additive amount of flame retardant, excellent overall performance of the composite material, and the like.

Description

technical field [0001] The invention relates to a preparation method of a composite material, in particular to a preparation method of an inorganic modified melamine cyanurate flame-retardant nylon 6 composite material, belonging to the field of new material synthesis. [0002] Background technique [0003] Due to its excellent comprehensive performance, nylon 6 has been widely used in the fields of automobiles, electronic appliances and machinery, and has become the most widely used engineering plastic. However, the limiting oxygen index of nylon 6 is not high, which is easy to cause fire, which limits its further application in many fields; especially in recent years, some brominated flame retardants have been banned by the EU RoSH directive due to the Dioxin problem, which has a negative impact on nylon 6 in my country. The export of products puts forward higher requirements, so it is of great significance to prepare halogen-free flame-retardant nylon 6 composite material...

Claims

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Application Information

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IPC IPC(8): C08G69/16C08K9/02C08K5/3492C08L77/02
Inventor 魏珊珊陈宪宏谢祥王乐宇
Owner HUNAN UNIV OF TECH
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