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DOPO-based silicon-phosphorus synergistic flame retardant as well as preparation method and application thereof

A synergistic flame retardant and silicon-based technology, applied in the field of flame retardants, can solve the problems of low limiting oxygen index, affecting material performance, and low flame retardant level

Pending Publication Date: 2020-10-20
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the smoke toxicity and environmental problems caused by halogen flame retardants, they are being restricted by many industries. Environmentally friendly halogen-free flame retardant products are becoming the development trend of the industry. The remaining flame retardants have low flame retardant levels when used alone , low limiting oxygen index, large amount of addition, etc., too large amount of addition will often affect the performance of the material

Method used

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  • DOPO-based silicon-phosphorus synergistic flame retardant as well as preparation method and application thereof
  • DOPO-based silicon-phosphorus synergistic flame retardant as well as preparation method and application thereof
  • DOPO-based silicon-phosphorus synergistic flame retardant as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] A preparation method of a DOPO-based silicon-phosphorus synergistic flame retardant, comprising the following steps:

[0052](1) Add 2.0g DOPO, 2.5g KH570 and 50.0g absolute ethanol into a three-necked flask filled with inert gas and mix to obtain solution A;

[0053] Dissolve 0.135g of azobisisobutyronitrile in 10.0g of absolute ethanol to obtain solution B;

[0054] Add solution B dropwise to solution A for 30 minutes, then react in an oil bath at 75°C for 12 hours to obtain a crude product, remove the solvent by rotary evaporation, and then dry it for 24 hours to obtain a flame retardant intermediate;

[0055] (2) Add 57.0 g of methanol and 3.0 g of deionized water to the flame retardant intermediate, add 0.14 g of acetic acid to adjust the pH to 4.0, and ultrasonically hydrolyze for 2 hours to obtain solution C;

[0056] (3) Transfer solution C into a three-necked flask with an inert gas, add 50.0 g of absolute ethanol and 2.0 g of kaolin, reflux at 75°C for 8 hour...

Embodiment 2

[0064] A preparation method of a DOPO-based silicon-phosphorus synergistic flame retardant, comprising the following steps:

[0065] (1) Add 2.0g DOPO, 3.0g KH570 and 50.0g toluene into a three-necked flask filled with inert gas and mix to obtain solution A;

[0066] Dissolve 0.15g of azobisisobutyronitrile in 10.0g of toluene to obtain solution B;

[0067] Add solution B dropwise to solution A for 30 minutes, then react in an oil bath at 120°C for 12 hours to obtain a crude product, remove the solvent by rotary evaporation, and then dry it for 24 hours to obtain a flame-retardant intermediate;

[0068] (2) Add 57.0 g of methanol and 3.0 g of deionized water to the flame retardant intermediate, add 0.14 g of acetic acid to adjust the pH to 4.0, and ultrasonically hydrolyze for 2 hours to obtain solution C;

[0069] (3) Transfer solution C into a three-necked flask with inert gas, add 50.0g toluene and 1.5g diatomaceous earth, reflux at 120°C for 8h, wash with ethanol three ti...

Embodiment 3

[0071] A preparation method of a DOPO-based silicon-phosphorus synergistic flame retardant, comprising the following steps:

[0072] (1) Add 1.5g DOPO, 2.0g KH570 and 50.0g toluene into a three-necked flask filled with inert gas and mix to obtain solution A;

[0073] Dissolve 0.105g of azobisisobutyronitrile in 10.0g of toluene to obtain solution B;

[0074] Add solution B dropwise to solution A for 30 minutes, then react in an oil bath at 120°C for 12 hours to obtain a crude product, remove the solvent by rotary evaporation, and then dry it for 24 hours to obtain a flame retardant intermediate;

[0075] (2) Add 76.0 g of methanol and 4.0 g of deionized water to the flame retardant intermediate, add 0.2 g of acetic acid to adjust the pH to 4.0, and ultrasonically hydrolyze for 2 hours to obtain solution C;

[0076] (3) Transfer the solution C into a three-necked flask with an inert gas, add 50.0 g of toluene and 3.0 g of kaolin, reflux at 75 ° C for 8 h, wash with ethanol thr...

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Abstract

The invention belongs to the technical field of flame retardants, and particularly discloses a DOPO-based silicon-phosphorus synergistic flame retardant. The raw materials comprise the following components: 1.0 to 3.0 parts of DOPO; 1.5 to 3.0 parts of a silane coupling agent, 0.075 to 0.180 part of a catalyst, 100.0 to 200.0 parts of a solvent, 1.0 to 3.0 parts of inorganic clay, 0.1 to 0.2 partof a pH regulator, 3.0 to 4.0 parts of deionized water, 57.0 to 76.0 parts of an alcohol compound and 1.0 to 2.0 parts of an auxiliary flame retardant. The preparation method comprises the following steps: carrying out free radical addition reaction on DOPO and a silane coupling agent to obtain a flame-retardant intermediate, and adding a catalyst to accelerate the reaction; then hydrolyzing to obtain a silanol group, carrying out dehydration combination on the silanol group and hydroxyl on inorganic clay, and supplementing with an auxiliary flame retardant to obtain the DOPO-based silicon-phosphorus synergistic flame retardant. The invention also discloses an application of the DOPO-based silicon-phosphorus synergistic flame retardant in preparation of flame-retardant modified epoxy resin.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, in particular to a DOPO-based silicon-phosphorus synergistic flame retardant and its preparation method and application. Background technique [0002] With the development of science and technology, polymer materials are widely used in aerospace, electronic appliances and many other fields because of their excellent mechanical properties, easy processing, corrosion resistance, and electrical insulation properties. However, most polymer materials are mainly composed of hydrocarbons and other elements, which are flammable and combustible materials with poor thermal stability. Among them, epoxy resin has good mechanical properties, adhesion, insulation, etc., and has been widely used in coatings, adhesives, and electronic and electrical products. Ordinary epoxy resin has poor flame retardancy, and there is a serious fire hazard. Therefore, it is of great significance to improve the flame ...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08K5/5419C08L63/00C08L63/02
CPCC07F9/657172C08K5/5419C08L63/00C08L2201/02C08L2201/08
Inventor 来水利陈功杨欣李晨辉
Owner SHAANXI UNIV OF SCI & TECH
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