Preparation method and application of flame retardant DDSP

A flame retardant and reaction technology, used in the field of preparing DDSP without acid binding agent, can solve the problems of explosion, danger to construction personnel and users, and achieve the effects of high reaction efficiency, stable properties and high phosphorus content

Pending Publication Date: 2022-07-01
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Chinese Patent Publication No. CN102186870B uses 3-picoline as an acid-binding agent and a reaction solvent to prepare a flame retardant intermediate. This invention provides a simple method for preparing a flame retardant, which does not require different solvents and will not There is the formation of by-product inorganic salts. The disadvantage is that 3-picoline will release toxic nitrogen oxide fumes when heated, and there is a danger of explosion, which will cause danger to construction workers and users.

Method used

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  • Preparation method and application of flame retardant DDSP
  • Preparation method and application of flame retardant DDSP
  • Preparation method and application of flame retardant DDSP

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A method for preparing DDSP, comprising the following experimental steps:

[0029] Weigh 20mg (0.2mmol) of neopentyl glycol in a 50ml double-neck flask, add 0.2ml of acetonitrile solvent, add 33mg (0.2mmol) of trichloride to the double-neck flask, and use an air pump with an exhaust volume of 30L / min Air was introduced into the double-necked flask, heated at 25°C under the condition of condensation and reflux to dissolve, mechanically stirred for 1 hour, after the reaction was completed, acetonitrile was removed under reduced pressure, washed with deionized water, filtered and dried to obtain the target compound 39 mg, 98% yield.

[0030]

Embodiment 2

[0032] A method for preparing DDSP, a gram-level experiment, comprises the following experimental steps:

[0033] Weigh 1.04g (10mmol) of neopentyl glycol into a 50ml double-neck flask, add 5ml of acetonitrile solvent, add 1.53g (10mmol) of phosphorous trichloride into the double-neck flask, and heat it at 25°C under the condition of condensation and reflux. Dissolve, use an air pump with a displacement of 30L / min to introduce air into the double-necked flask, stir mechanically for 1h, after the reaction is completed, remove acetonitrile under reduced pressure, and wash with deionized water, filter, and dry to obtain the target compound 1.85 g, 92.5% yield.

Embodiment 3

[0035] A method for preparing DDSP, the reaction under nitrogen gas is introduced, comprising the following experimental steps:

[0036] Weigh 1.04g (10mmol) of neopentyl glycol into a 50ml double-neck flask, add 5ml of acetonitrile solvent, add 1.53g (10mmol) of phosphorous trichloride into the double-neck flask, and heat it at 25°C under the condition of condensation and reflux. Dissolve, use a nitrogen bottle with an exhaust volume of 30L / min to introduce nitrogen into the double-necked bottle, stir mechanically for 1h, after the reaction is completed, remove acetonitrile under reduced pressure, and wash with deionized water, filter, and dry to obtain the target compound 1.81 g, 90.5% yield.

[0037]

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Abstract

The invention provides a preparation method and application of a flame retardant DDSP, a product is prepared from neopentyl glycol and thiophosphoryl chloride in the presence of acetonitrile as a solvent without using an acid-binding agent, and no by-product inorganic salt is generated in the process. The reaction needs to be carried out under the condition of introducing air or nitrogen so as to discharge hydrogen chloride gas generated in the reaction process. According to the reaction, the defects of environmental pressure generated by using a triethylamine or pyridine acid-binding agent due to relatively strong odor and harm to production operators due to relatively strong toxicity in the traditional process are avoided, the generation of inorganic salt is avoided, and the target compound is synthesized with relatively high yield by a relatively green and energy-saving method. The method has the advantages of short reaction time, simple operation steps, simple post-treatment and less pollution, and is easy for industrial production. According to the application, the compound can be used as a flame retardant intermediate to efficiently generate the flame retardant dithio pyrophosphate.

Description

technical field [0001] The invention belongs to the technical field of flame retardant, and particularly relates to a method for preparing DDSP without an acid binding agent and its application. Background technique [0002] Flame retardants are additives used to improve the flame resistance of materials, prevent materials from being ignited and inhibit the spread of flames. They are mainly used for flame retardant polymer materials. Currently available flame retardant elements are halogen, phosphorus, nitrogen, silicon, sulfur, boron and some metal elements such as antimony, magnesium, aluminum and so on. Most of the phosphorus-based flame retardants have the advantages of low smoke, non-toxicity, low halogen, and no halogen, which are in line with the development direction of flame retardants and have good development prospects. In particular, in 1986, a Swiss research institute discovered the dioxin problem of halogenated flame retardants, which prompted researchers to d...

Claims

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Application Information

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IPC IPC(8): C07F9/6574
CPCC07F9/65742
Inventor 王龙孙宏媛汤全阳青青胡为民
Owner CHINA THREE GORGES UNIV
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