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

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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 o

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

Example Embodiment

[0050] Example 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 to the three-necked flask filled with inert gas and mix to obtain solution A;

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

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

[0055] (2) adding 57.0g methanol and 3.0g deionized water to the flame retardant intermediate, adding 0.14g acetic acid to adjust pH to 4.0, and ultrasonically hydrolyzing for 2h to obtain solution C;

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

Example Embodiment

[0063] Example 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 in the three-necked flask filled with inert gas and mix to obtain solution A;

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

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

[0068] (2) adding 57.0g methanol and 3.0g deionized water to the flame retardant intermediate, adding 0.14g acetic acid to adjust pH to 4.0, and ultrasonically hydrolyzing for 2h to obtain solution C;

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

Example Embodiment

[0070] Example 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 in the three-necked flask filled with inert gas and mix to obtain solution A;

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

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

[0075] (2) adding 76.0g methanol and 4.0g deionized water to the flame retardant intermediate, adding 0.2g acetic acid to adjust the pH to 4.0, and ultrasonically hydrolyzing for 2h to obtain solution C;

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

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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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