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A kind of flame retardant with high phosphorus content and preparation method thereof

A flame retardant and solvent technology, applied in the field of high phosphorus content flame retardant and its preparation, can solve the problems of influence and unfavorable material properties, and achieve the effects of simple process, low cost and little influence

Active Publication Date: 2018-11-16
广州银塑阻燃新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although it has good flame retardant properties, as the amount added increases, it will have some adverse effects on the properties of the material itself

Method used

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  • A kind of flame retardant with high phosphorus content and preparation method thereof
  • A kind of flame retardant with high phosphorus content and preparation method thereof
  • A kind of flame retardant with high phosphorus content and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A kind of synthetic steps of high phosphorus content flame retardant is:

[0031] (1) Heat 15.0 g of biphenyl phosphoramidate and 6.2 g of 2,3,5,6-tetrafluoro-p-benzaldehyde in 126.9 g of ethanol at 75° C. for 6 hours. After the reaction, the intermediate product I reaction system;

[0032] (2) Add 13.0 g of DOPO to the reaction system containing intermediate product I obtained in step (1) and heat at 75° C. for 3 h. After the reaction is finished, wash and dry to obtain a flame retardant with a high phosphorus content. The rate is 85.8%.

[0033] The infrared test results are as follows:

[0034] FTIR (KBr): N-H stretching vibration peak 3410cm -1 , C-H stretching vibration peak 3080cm -1 , C-N characteristic peak 1288cm -1 , C-F characteristic peak 1100cm -1 , P-O-C characteristic peak 1030cm -1 , P-O-Ph characteristic peak 1231cm -1 , P-Ph characteristic peak 1595cm -1 , P=O characteristic peak 1215cm -1 , the out-of-plane bending vibration peak of the arom...

Embodiment 2

[0038] A kind of synthetic steps of high phosphorus content flame retardant is:

[0039] (1) Heat 24.9 g of biphenyl phosphoramidate and 10.3 g of 2,3,5,6-tetrafluoro-p-benzaldehyde in 317 g of DMF at 75°C for 8 hours. After the reaction, a reaction containing intermediate product I is obtained. system;

[0040] (2) Add 21.6g of DOPO to the reaction system containing the intermediate product I obtained in step (1) and heat it for 4.5h at 75°C. After the reaction is over, wash and dry to obtain a flame retardant with a high phosphorus content. Yield 86.1%.

[0041] The infrared test results are as follows:

[0042] FTIR (KBr): N-H stretching vibration peak 3415cm -1 , C-H stretching vibration peak 3065cm -1 , C-N characteristic peak 1288cm -1 , C-F characteristic peak 1105cm -1 , P-O-C characteristic peak 1030cm -1 , P-O-Ph characteristic peak 1231cm -1 , P-Ph characteristic peak 1590cm -1 , P=O characteristic peak 1215cm -1 , the out-of-plane bending vibration peak o...

Embodiment 3

[0044] A kind of synthetic steps of high phosphorus content flame retardant is:

[0045] (1) Heat 49.8g of biphenyl phosphoramidate and 20.6g of 2,3,5,6-tetrafluoro-p-benzaldehyde in 845g of DMSO at 75°C for 10h. After the reaction, a reaction containing intermediate product I is obtained. system;

[0046] (2) 21.6g of DOPO is added to the reaction system containing intermediate product I obtained in step (1) and heated at 75°C for 6h. After the reaction is finished, it is washed and dried to obtain a high phosphorus content flame retardant, which produces The rate is 86.6%.

[0047] The infrared test results are as follows:

[0048] FTIR (KBr): N-H stretching vibration peak 3410cm -1 , C-H stretching vibration peak 3070cm -1 , C-N characteristic peak 1287cm -1 , C-F characteristic peak 1100cm -1 , P-O-C characteristic peak 1035cm -1 , P-O-Ph characteristic peak 1230cm -1 , P-Ph characteristic peak 1590cm -1 , P=O characteristic peak 1215cm -1 , the out-of-plane bend...

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Abstract

The invention relates to the technical field of flame retardants, particularly a high-phosphorus-content flame retardant of which the structural formula is disclosed in the specification. The preparation method of the high-phosphorus-content flame retardant comprises the following steps: heating biphenyl phosphoramidate and 2,3,5,6-tetrafluoro-p-dibenzaldehyde in a solvent, and carrying out reaction to obtain a reaction system containing an intermediate product I; and (2) adding DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) into the reaction system containing the intermediate product I in the step (1), and heating to react; and after the reaction finishes, washing and drying to obtain the high-phosphorus-content flame retardant. As the phosphorus content in the condensate increases, the flame retardancy of the condensate increases. When the flame retardant content reaches 5-10%, the condensate can reach UL-94 Grade V-0.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a flame retardant with high phosphorus content and a preparation method thereof. Background technique [0002] Halogenated flame retardants are a class of flame retardants that contain halogen elements and use halogen elements as a flame retardant. The four halogen elements of the halogen series, fluorine (F), chlorine (Cl), bromine (Br), and iodine (I), all have flame retardancy, and the flame retardancy effect is enhanced in the order of F, Cl, Br, and I. Iodine-based flame retardants are the strongest. In production, only chlorine and bromine flame retardants are widely used. Fluorine and iodine flame retardants are rarely used because the C-F bond in fluorine-containing flame retardants is too strong to effectively capture free radicals. And The C-I bond of the I-containing flame retardant is too weak and easy to be destroyed. It affects the properties of the polym...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5399C08L25/06C07F9/6574
CPCC07F9/657172C08K5/5399C08L25/06
Inventor 徐再徐惠凤徐靖丁磊赵琴芬卢路平
Owner 广州银塑阻燃新材料股份有限公司
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