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A kind of dopo derivative flame retardant containing silicon and fluorine and preparation method thereof

A technology of derivatives and flame retardants, which is applied in the field of DOPO derivative flame retardants containing silicon and fluorine and its preparation, can solve the problems of unfavorable material performance and influence, and achieve excellent thermal stability, good chemical stability, Good surface migration effect

Active Publication Date: 2019-04-09
中山苏特宝新材料有限公司
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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 dopo derivative flame retardant containing silicon and fluorine and preparation method thereof
  • A kind of dopo derivative flame retardant containing silicon and fluorine and preparation method thereof
  • A kind of dopo derivative flame retardant containing silicon and fluorine and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The synthesis steps of a nitrogen-phosphorus-containing silicone flame retardant are:

[0030] (1) Heat 11.1 g of tris(4-aminophenyl) phosphate and 22.2 g of Zirosilicone in 166.3 g of ethanol at 75° C. for 5 hours. After the reaction is completed, a reaction system containing intermediate product I is obtained;

[0031] (2) Add 19.5 g of DOPO to the reaction system containing intermediate product I obtained in step (1) and heat it at 75° C. for 5 hours. After the reaction, wash and dry to obtain a silicon and fluorine-containing DOPO derivative barrier. Burning agent, the yield is 86.4%.

[0032] The infrared test results are as follows:

[0033] FTIR (KBr): N-H stretching vibration peak 3410cm -1 , C-H stretching vibration peak 3070cm -1 , C-N characteristic peak 1288cm -1 , C-F characteristic peak 1105cm -1 , C-Si characteristic peak 1255cm -1 , P-O-C characteristic peak 1032cm -1 , P-O-Ph characteristic peak 1231cm -1 , P-Ph characteristic peak 1595cm -1 , P=O characteristi...

Embodiment 2

[0037] The synthesis steps of a nitrogen-phosphorus-containing silicone flame retardant are:

[0038] (1) Heat 18.6g of tris(4-aminophenyl) phosphate and 37g of Zirosilicone in 388.8g of DMF at 75°C for 7h, after the reaction is over, a reaction system containing intermediate product I is obtained;

[0039] (2) Add 32.4g of DOPO to the reaction system containing intermediate product I obtained in step (1) and heat it at 75°C for 7 hours. After the reaction, wash and dry to obtain silicon and fluorine-containing DOPO derivatives. Burning agent, the yield is 86.2%.

[0040] The infrared test results are as follows:

[0041] FTIR (KBr): N-H stretching vibration peak 3410cm -1 , C-H stretching vibration peak 3075cm -1 , C-N characteristic peak 1287cm -1 , C-F characteristic peak 1105cm -1 , C-Si characteristic peak 1255cm -1 , P-O-C characteristic peak 1033cm -1 , P-O-Ph characteristic peak 1232cm -1 , P-Ph characteristic peak 1595cm -1 , P=O characteristic peak 1212cm -1 , The out-of-pla...

Embodiment 3

[0043] The synthesis steps of a nitrogen-phosphorus-containing silicone flame retardant are:

[0044] (1) Heat 37.1 g of tris(4-aminophenyl) phosphate and 73.9 g of zirosilicone in 999 g of DMSO at 75° C. for 10 hours. After the reaction is completed, a reaction system containing intermediate product I is obtained;

[0045] (2) 64.9g of DOPO was added to the reaction system containing intermediate product I obtained in step (1) and heated at 75°C for 9 hours. After the reaction, it was washed and dried to obtain silicon and fluorine-containing DOPO derivative barriers. Burning agent, the yield is 86.6%.

[0046] The infrared test results are as follows:

[0047] FTIR (KBr): N-H stretching vibration peak 3415cm -1 , C-H stretching vibration peak 3085cm -1 , C-N characteristic peak 1287cm -1 , C-F characteristic peak 1105cm -1 , C-Si characteristic peak 1254cm -1 , P-O-C characteristic peak 1033cm -1 , P-O-Ph characteristic peak 1232cm -1 , P-Ph characteristic peak 1595cm -1 , P=O chara...

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Abstract

The invention relates to the technical field of flame retardants and in particular relates to a DOPO (9,10-bihydro-9-oxa-10-phosphaphenanthrene-10-oxide) derivative flame retardant containing silicon and fluorine. A structural formula of the DOPO derivative flame retardant is shown in the description. A preparation method of the DOPO derivative flame retardant containing silicon and fluorine comprises the following steps: (1) heating tri(4-aminophenyl) phosphate and zifrosilone in a solvent, and reacting to obtain a reaction system containing an intermediate product I; (2) adding DOPO into the reaction system containing the intermediate product I, which is obtained by the step (1), and heating, and after reacting, washing and drying to obtain the DOPO derivative flame retardant containing silicon and fluorine. According to the derivative flame retardant containing silicon and fluorine and the preparation method thereof, the flame retarding property of cured products is increased along the increasing of the content of phosphorus in the cured products; and when the content of the flame retardant reaches 5 percent to 10 percent, the cured products 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 DOPO derivative flame retardant containing silicon and fluorine and a preparation method thereof. Background technique [0002] Halogen flame retardant is a type of flame retardant that contains halogen elements and uses halogen elements to play a flame retardant effect. The four halogen elements fluorine (F), chlorine (Cl), bromine (Br), and iodine (I) all have flame retardancy, and the flame retardant effect is enhanced in the order of F, Cl, Br, I. Iodine-based flame retardants are the strongest. In production, only chlorine and bromine flame retardants are used in large quantities. Fluorine and iodine flame retardants are rarely used. This is because the CF bond in fluorine-containing flame retardants is too strong to effectively capture free radicals. The CI bond of the I-containing flame retardant is too weak and easy to be destroyed. It affects the polymer performa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/544C08L25/06
CPCC07F9/657172C08K5/544C08L2201/02C08L25/06
Inventor 徐再徐惠凤徐靖丁磊赵琴芬卢路平
Owner 中山苏特宝新材料有限公司
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