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Flame-retardant silane crosslinking agent and preparation method thereof

A technology of flame retardant silane and silane coupling agent, which is applied in the field of flame retardant silane crosslinking agent and its preparation, can solve the problems of heat resistance and other performance degradation of materials, achieve improved compatibility, controllable and adjustable reaction process, Preparation of the effect of mild reaction conditions

Inactive Publication Date: 2012-11-14
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at present, in order to obtain a certain flame retardant effect, it mainly depends on increasing the amount of a single flame retardant element, which leads to the introduction of too many chemical weak bonds, resulting in a significant decline in heat resistance and other properties of the material.

Method used

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  • Flame-retardant silane crosslinking agent and preparation method thereof
  • Flame-retardant silane crosslinking agent and preparation method thereof
  • Flame-retardant silane crosslinking agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation steps of flame retardant silane crosslinking agent: Add 21.5g DPPA and 100ml xylene into a 500ml flask equipped with a condenser, mechanical stirring, constant pressure dropping funnel and nitrogen protection, raise the temperature to 90°C, and wait until DPPA is completely dissolved at 0.5 Add 30g of vinyltrimethoxysilane and 10ml of xylene solution containing 0.5g of azobisisobutyronitrile dropwise within 1 hour, continue to react for 2 hours, then filter the reaction mixture, wash with ethanol, and dry in vacuum at 60°C for 12h, finally Obtain flame retardant silane crosslinking agent (CH 3 O) 3 Si-CH 2 -CH 2 -DPPA-CH 2 -CH 2 -Si(OCH 3 ) 3 (labeled FR-1) 49.1 g, 95.3% yield. The mass percentage content of each element in the organic halogen-free flame retardant is: C51.46%, H7.02%, O21.83%, P6.04%, N2.73%, Si10.92%; nuclear magnetic spectrum data for: 1 H NMR (DMSO-d6): 7.00-7.91ppm (8H, Ph-H), 2.00-2.13ppm (4H, P-CH 2 -, N-CH 2 -), 0.71-0.92pp...

Embodiment 2

[0033] Add 21.5g DAPO and 120ml ethyl acetate / isopropanol (volume ratio 1 / 1) into a 500ml flask equipped with a condenser, mechanical stirring, constant pressure dropping funnel and nitrogen protection, raise the temperature to 50°C, and wait until DAPO is completely dissolved After that, 38.5g vinyltriethoxysilane and 10ml of ethyl acetate solution containing 0.3g azobisisoheptanonitrile were added dropwise within 2 hours, and the reaction was continued for 12 hours, then the reaction mixture was subjected to rotary evaporation, ethanol washing, and 60 After vacuum drying at ℃ for 12 hours, 55.8 g of a flame-retardant silane crosslinking agent (marked as FR-2) was finally obtained, with a yield of 93.0%. The effect of flame retardant FR-2 on the thermal stability of polymer materials and the flame retardant effect are shown in Table 1.

Embodiment 3

[0035] Add 21.5g DPPA and 250ml methanol / toluene (volume ratio 1 / 2) into a 500ml flask equipped with a condenser, mechanical stirring, constant pressure dropping funnel and nitrogen protection, raise the temperature to 65°C, and wait for 0.5 hours after DPPA is completely dissolved 56g of vinyl tris(2-methoxyethoxy)silane and 10ml of toluene solution containing 0.15g of azobicyclohexylcarbonitrile were added dropwise, and the reaction was continued for 16 hours, then the reaction mixture was subjected to rotary evaporation, ethanol washing, After vacuum drying at 60°C for 12 hours, 71.2 g of a flame-retardant silane crosslinking agent (marked as FR-3) was finally obtained, with a yield of 91.9%. The effect of flame retardant FR-3 on the thermal stability of polymer materials and the flame retardant effect are shown in Table 1.

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Abstract

The invention discloses a flame-retardant silane crosslinking agent and a preparation method thereof. The flame-retardant silane crosslinking agent has one or more of the following structures: X3Si-R1-DPPA-R2-SiX3 and X3Si-R3-DAPO-R4-SiX3. The preparation method comprises the following steps of: 1) under the protection of inert gas, dissolving phosphorous azacyclo reactant into an organic solvent, adding a silane coupling agent and the corresponding catalyst, and stirring and reacting at the temperature of 25 to 150 DEG C for 0.5 to 24 hours to obtain reaction liquid, wherein the phosphorous azacyclo reactant is DPPA and / or DAPO; and 2) filtering or rotationally evaporating the reaction liquid, washing and drying to obtain the target product. The flame-retardant silane crosslinking agent can take part in reactions such as crosslinking and polycondensation through a silane active group and form one part of a polymer molecular structure, so that the polymer has an intrinsic flame-retardant function or can improve the flame resistance and can also be used for improving the compatibility of some inorganic fillers or additive flame retardant and high molecular materials. The method has the advantages of mild reaction condition, controllable and adjustable reaction process, high yield and the like.

Description

technical field [0001] The invention relates to the field of flame retardant processing aids, in particular to a flame retardant silane crosslinking agent and a preparation method thereof. Background technique [0002] Polymer materials have the characteristics of light weight, high strength, corrosion resistance, insulation, heat resistance, good elasticity, radiation resistance, transparency, and easy processing. Important materials essential to everyday life. However, most polymer materials are flammable and continue to burn after leaving the fire, which is easy to cause fire. This shortcoming makes it a great safety hazard in the application process, which seriously threatens the lives and property safety of the people. Therefore, improving the flame retardancy of polymer materials is one of the strategic measures to prevent and reduce fire accidents, which has important theoretical and practical significance. [0003] In view of the fact that the use of additive inorg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/544C08L63/00C08L23/06C08L67/06C08L75/04C07F9/6584
CPCY02P20/52
Inventor 袁彦超赵建青刘述梅朱亚明刘运春
Owner SOUTH CHINA UNIV OF TECH
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