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A kind of nitrogen phosphorus-containing surface migration flame retardant and preparation method thereof

A technology of surface migration and flame retardant, which is applied in the field of flame retardants, can solve the problems of unfavorable material performance and impact, and achieve the effect of low cost, simple process and easy access to raw materials

Active Publication Date: 2019-01-15
宁波华腾首研新材料有限公司
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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 nitrogen phosphorus-containing surface migration flame retardant and preparation method thereof
  • A kind of nitrogen phosphorus-containing surface migration flame retardant and preparation method thereof
  • A kind of nitrogen phosphorus-containing surface migration flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The synthesis steps of a nitrogen-phosphorus-containing surface migration flame retardant are:

[0031] (1) Heat 11.1 g of tris(4-aminophenyl) phosphate and 12.9 g of 3,5-difluoropyridine-4-carbaldehyde in 144 g of ethanol at 70°C for 7 hours. After the reaction, an intermediate product containing The reaction system of I;

[0032] (2) Add 19.5g of DOPO to the reaction system containing the intermediate product I obtained in step (1) and heat at 70°C for 4h. After the reaction, wash and dry to obtain a nitrogen-phosphorus-containing surface migration flame-retardant agent, the yield was 84.9%.

[0033] The infrared test results are as follows:

[0034] FTIR (KBr): N-H stretching vibration peak 3410cm -1 , C-H stretching vibration peak 3075cm -1 , C-N characteristic peak 1289cm -1 , C-F characteristic peak 1100cm -1 , P-O-C characteristic peak 1032cm -1 , P-O-Ph characteristic peak 1231cm -1 , P-Ph characteristic peak 1595cm -1 , P=O characteristic peak 1212cm ...

Embodiment 2

[0038] The synthesis steps of a nitrogen-phosphorus-containing surface migration flame retardant are:

[0039] (1) Heat 18.6g of tris(4-aminophenyl)phosphate and 21.5g of 3,5-difluoropyridine-4-carbaldehyde in 401g of DMF at 70°C for 10h. After the reaction, an intermediate product containing The reaction system of I;

[0040] (2) Add 32.4g of DOPO to the reaction system containing intermediate product I obtained in step (1) and heat at 70°C for 6h. After the reaction is completed, wash and dry to obtain a nitrogen-phosphorus-containing surface migration flame-retardant agent, yield 84.8%.

[0041] The infrared test results are as follows:

[0042] FTIR (KBr): N-H stretching vibration peak 3415cm -1 , C-H stretching vibration peak 3075cm -1 , C-N characteristic peak 1289cm -1 , C-F characteristic peak 1100cm -1 , P-O-C characteristic peak 1033cm -1 , P-O-Ph characteristic peak 1231cm -1 , P-Ph characteristic peak 1590cm -1 , P=O characteristic peak 1212cm -1 , the ou...

Embodiment 3

[0044] The synthesis steps of a nitrogen-phosphorus-containing surface migration flame retardant are:

[0045] (1) Heat 37.1g of tris(4-aminophenyl) phosphate and 42.9g of 3,5-difluoropyridine-4-carbaldehyde in 960g of DMSO at 70°C for 12h. After the reaction, an intermediate product containing The reaction system of I;

[0046] (2) Add 64.9g of DOPO to the reaction system containing intermediate product I obtained in step (1) and heat at 70°C for 8 hours. After the reaction is completed, wash and dry to obtain a nitrogen-phosphorus-containing surface migration flame-retardant agent, yield 84.6%.

[0047] The infrared test results are as follows:

[0048] FTIR (KBr): N-H stretching vibration peak 3420cm -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 1033cm -1 , P-O-Ph characteristic peak 1231cm -1 , P-Ph characteristic peak 1590cm -1 , P=O characteristic peak 1212cm -1 ,...

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Abstract

The invention relates to the technical field of flame retardants, in particular to a surface migration flame retardant containing nitrogen and phosphorus and a preparation method of the surface migration flame retardant. The surface migration flame retardant has the structural formula shown in the specification. The preparation method of the surface migration flame retardant containing nitrogen and phosphorus comprises steps as follows: (1) tris(4-aminophenyl) phosphate and 3,5-difluoropyridine-4-formaldehyde are heated in a solvent, and a reaction system containing an intermediate product I is obtained after the reaction ends; (2) DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) is added to the reaction system containing the intermediate product I in the step (1) to be heated, washing and drying are performed after the reaction ends, and the surface migration flame retardant containing nitrogen and phosphorus is obtained. According to the surface migration flame retardant containing nitrogen and phosphorus and the preparation method of the surface migration flame retardant, with increase of phosphorus in a cured product, the flame retardancy of the cured product is increased; when the content of the flame retardant reaches 5%-10%, the cured product can reach the UL-94, V-0 level.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a nitrogen-phosphorus-containing surface-migrating flame retardant 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 pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/5313C08L25/06
CPCC07F9/657172C08K5/5313C08L2201/02C08L2201/08C08L25/06
Inventor 徐再徐惠凤徐靖丁磊赵琴芬卢路平
Owner 宁波华腾首研新材料有限公司
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