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Reactive flame retardant with carboxylic acid or anhydride groups as well as preparation method and application of reactive flame retardant

A reactive flame retardant and acid anhydride technology, applied in the field of flame retardants, can solve the problems of expensive raw materials, narrow application range, and inability to be widely used, and achieve the effect of simple and easy preparation method

Inactive Publication Date: 2021-03-05
GUANGDONG GUANGSHAN NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] CN104072759A discloses a P-N series expansion reactive flame retardant and a preparation method thereof, the reactive flame retardant is p-(carboxyphenyl-amino)-(carboxyphenyl-amidoethyl)phenylphosphine oxide, The preparation method is as follows: (a) adding p-aminobenzoic acid solution to glacial acetic acid; (b) adding triethylamine and the mixed solution obtained in step a to the 2-carboxyethylphenylphosphinic acid solution, stirring at high speed for 2 hours, Raise the temperature to 80°C, react for 4 hours, then cool, hydrolyze, suction filter, wash with water, and dry to obtain a white powder that is a P-N series expansion reaction flame retardant. PA66 with intrinsic flame retardancy can be prepared, although it has a good Flame retardant effect, but the application range is too narrow, it can only be applied to polyamide, and the raw materials are expensive, so it cannot be widely used

Method used

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  • Reactive flame retardant with carboxylic acid or anhydride groups as well as preparation method and application of reactive flame retardant
  • Reactive flame retardant with carboxylic acid or anhydride groups as well as preparation method and application of reactive flame retardant
  • Reactive flame retardant with carboxylic acid or anhydride groups as well as preparation method and application of reactive flame retardant

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0029] A reactive flame retardant with a carboxyl group, the structure is as follows:

[0030]

[0031] The preparation method is as follows:

[0032] Add 1mol of DOPO, 1mol of glutaconedic acid, and 50mL of glacial acetic acid into a three-necked flask equipped with magnetic stirring and a thermometer. Add the glacial acetic acid solution containing 1mmol of Pb catalyst dropwise at 50°C under stirring. In the reaction system, the reaction was carried out for 12 hours, and the product was separated to obtain the reactive flame retardant with the above structure.

[0033] 1 H NMR (CDCl 3 ,400MHz,TMS):δ=6.94-7.64(m,8H,ph-H),2.60-2.64(d,4H,COOH-C H 2 -CH-C H 2 -COOH),1.90-1.94(m,1H,-CH-).

preparation example 2

[0035] A reactive flame retardant with an anhydride group, the structure is as follows:

[0036]

[0037] The preparation method is as follows:

[0038] Under a nitrogen atmosphere, put 50mL of glacial acetic acid, 0.5mol dimethyl phosphite and 0.5mol maleic anhydride into a three-port 200mL glass reactor with a stirring device and stir. At a stirring temperature of 60°C, 0.5mmol of Pb In 20mL of glacial acetic acid, then added dropwise to the reaction system, reacted for 12h, and then separated the product to obtain the phosphorus-containing flame retardant with the above structure.

[0039] 1 H NMR (CDCl 3 ,400MHz,TMS):δ=4.12-4.16(t,1H,-CH-),3.73-3.76(d,6H,-P-O-CH 3 ),3.38-3.42(d,2H,-CH 2 -).

preparation example 3

[0041] A reactive flame retardant with a carboxyl group, the structure is as follows:

[0042]

[0043] The preparation method is as follows:

[0044] Add 1 mol of dimethyl phosphite, 1 mol of glutaconedic acid, and 50 mL of glacial acetic acid into a three-necked flask equipped with magnetic stirring and a thermometer. At a stirring speed of 50 ° C, the glacial acetic acid solution containing 1 mmol of Pb catalyst is Add it dropwise into the reaction system, react for 12 hours, and separate the product to obtain the reactive flame retardant with the above structure.

[0045] 1 H NMR (400MHz, DMSO-d6): δ=10.62-10.64(s,2H,-COOH),3.73-3.76(d,6H,-P-O-CH 3 ),2.32-2.50(m,5H,COOH-C H 2 -C H -C H 2 -COOH).

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Abstract

The invention provides a reactive flame retardant with carboxylic acid or anhydride groups as well as a preparation method and application of the reactive flame retardant. The reactive flame retardantis obtained by carrying out addition reaction on a compound with a PH reaction group and a compound with at least one carboxyl or anhydride group and at least one unsaturated bond. The flame retardant provided by the invention stably exists in the form of molecular chain segments, has no emigration phenomenon, has no dissolving phenomenon along with water washing, and can truly achieve safety, environmental protection and flame retardance.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and relates to a reactive flame retardant with carboxylic acid or acid anhydride groups and its preparation method and application. Background technique [0002] With the advancement of science and technology, polymer materials such as synthetic fibers, rubber, and plastics are increasingly used in various fields, especially engineering plastics play a more important role in the national economy and people's lives. However, plastics are easily Combustible or combustible polymer materials are prone to fire and other accidents. In order to solve the problems of engineering plastics such as heat resistance and smoke suppression, the most effective method is to introduce flame retardants to convert flammable or combustible polymer materials into flame-retardant or non-flammable materials. Combustible materials, reduce the burning rate, delay the spread of flames, and control the occurrence o...

Claims

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Application Information

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IPC IPC(8): C07F9/40C07F9/655C07F9/6574C08L67/00C08L67/02C08K5/00C08K5/5333C08K5/5313C08L77/06C08K7/14C08K5/5425C08G69/42C08G59/42
CPCC07F9/657172C07F9/65515C07F9/4006C07F9/65517C07F9/4056C08L67/00C08L77/06C08G69/42C08G59/423C08G59/4238C08L2205/025C08L2205/02C08L2201/02
Inventor 潘庆崇
Owner GUANGDONG GUANGSHAN NEW MATERIALS CO LTD
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