Reaction-type halogen-free flame retardant bis-(p-aminocarboxyphenyl)phenylphosphine oxide and synthetic method thereof

A technology of aminocarboxyphenyl and phenylphosphine oxide, which is applied in the chemical field, can solve the problems of long cycle time, complex process, and environmental pollution, and achieve the effect of fewer production steps, simple process, and low cost

Inactive Publication Date: 2015-09-30
NANJING LIHAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention aims at the problems that the existing reactive halogen-free flame retardants have too many synthesis steps, long cycle, complex process and environmental pollution due to too many synthesis raw materials. The present invention provides a reactive halogen-free flame retardant bi-( -Aminocarboxyphenyl) phenylphosphine oxide and its synthesis method meet environmental protection requirements and solve the above-mentioned technical defects

Method used

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  • Reaction-type halogen-free flame retardant bis-(p-aminocarboxyphenyl)phenylphosphine oxide and synthetic method thereof
  • Reaction-type halogen-free flame retardant bis-(p-aminocarboxyphenyl)phenylphosphine oxide and synthetic method thereof
  • Reaction-type halogen-free flame retardant bis-(p-aminocarboxyphenyl)phenylphosphine oxide and synthetic method thereof

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Effect test

Embodiment 1

[0027] The synthetic method of reactive type halogen-free flame retardant bis-(p-aminocarboxyphenyl) phenyl phosphine oxide is carried out in the following steps:

[0028] Add 0.055mol of p-aminobenzoic acid and 30mL of glacial acetic acid into a dry three-necked flask with a capacity of 100mL equipped with a condenser tube, a thermometer and a stirrer, and then slowly add 0.025mol of benzene dropwise under the condition of a stirring speed of 500r / min. Phosphoryl dichloride was added dropwise within 20 minutes, heated to 90°C after addition, refluxed for 5 hours, then cooled to room temperature, then filtered, recovered solvent acetic acid, washed with acetic acid and distilled water in turn, and then used Recrystallize with distilled water, and finally dry at 105°C in a circulating blast drying oven to obtain a white powdery solid with a yield of 84%. The product confirmed by infrared spectroscopy is bis-(p-aminocarboxyphenyl)phenyl Phosphine oxide.

[0029] in figure 1 Th...

Embodiment 2

[0039] The synthetic method of reactive type halogen-free flame retardant bis-(p-aminocarboxyphenyl) phenyl phosphine oxide is carried out in the following steps:

[0040] Add 0.11mol of p-aminobenzoic acid and 60mL of glacial acetic acid into a dry three-neck flask with a capacity of 250mL equipped with a condenser tube, a thermometer and a stirrer, and then slowly add 0.05mol of benzene dropwise at a stirring speed of 500r / min. Phosphoryl dichloride, after the addition, heat up to 85°C, reflux for 6 hours, then cool to room temperature, then filter, recover the solvent acetic acid, then wash with acetic acid and distilled water in turn, and recrystallize with distilled water, after suction filtration Drying with circulating air at 110° C. gave a white powdery solid with a yield of 82%. It was confirmed by infrared spectrum analysis that the obtained product was bis-(p-aminocarboxyphenyl)phenylphosphine oxide. After the reaction product is salted with hexamethylenediamine, it...

Embodiment 3

[0042] The synthetic method of reactive type halogen-free flame retardant bis-(p-aminocarboxyphenyl) phenyl phosphine oxide is carried out in the following steps:

[0043] Add 0.24mol of p-aminobenzoic acid and 120mL of glacial acetic acid into a dry three-neck flask with a capacity of 250mL equipped with a condenser tube, a thermometer, and a stirrer, and then slowly add 0.1mol of benzene dropwise at a stirring speed of 500r / min. Phosphoryl dichloride, after the addition, heat up to 95°C, reflux for 4 hours, then cool to room temperature, then filter, recover the solvent acetic acid, then wash with acetic acid and distilled water in turn, then recrystallize with distilled water, and finally recycle Dried at 106° C. in a blast drying oven to obtain a white powdery solid with a yield of 80%, which was confirmed to be bis-(p-aminocarboxyphenyl)phenylphosphine oxide by infrared spectrum analysis. After the reaction product is salted with hexamethylenediamine, it is copolymerized ...

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Abstract

The invention relates to reaction-type halogen-free flame retardant bis-(p-aminocarboxyphenyl)phenylphosphine oxide and its synthetic method and application and belongs to the field of preparation of a flame retardant. The synthetic method comprises the following steps: using glacial acetic acid as a solvent, adding para amino benzoic acid into glacial acetic acid, slowly dropwise adding dichlorophenylphosphine oxide into an acetic acid solution of para aminobenzoic acid, continuously stirring and reacting at 85-95 DEG C for 4-6 h, and absorbing hydrogen chloride discharged by the reaction by the use of aqueous alkali; and cooling a reaction product after the end of the reaction, carrying out suction filtration, washing and drying to obtain white powdery bis-(p-aminocarboxyphenyl)phenylphosphine oxide. The bis-(p-aminocarboxyphenyl)phenylphosphine oxide flame retardant has advantages of low toxicity, low smoke, innocuousness, high efficiency and the like, is a reactive flame retardant integrating a carbon source, an acid source and a gas source, and is applied in inherent flame retarding of nylon or thermoplastic polyester copolymer.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a reactive halogen-free flame retardant bis-(p-aminocarboxyphenyl)phenylphosphine oxide and a synthesis method thereof Background technique [0002] As one of the five general-purpose engineering plastics, nylon is widely used in many fields of the national economy because of its excellent comprehensive performance and moderate price. It is very popular in the electronic and electrical industry. Although nylon is a flame retardant polymer that disappears immediately after fire, its flame retardancy is still insufficient as an electronic and electrical component. With the advancement of science and technology, the requirements for the flame retardancy of materials are getting higher and higher, and it is not uncommon to meet the requirements of UL94 V-0 or 5VA at a thickness of 0.4mm. The current measures to improve the flame retardancy of materials are mainly to add inorganic or organi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5399C07F9/44C08G69/48
Inventor 袁锦瑶张伟孙圳吴玉成曹玺曹凤根崔益华吕文晏张绪杰
Owner NANJING LIHAN CHEM CO LTD
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