Flame retardant containing phosphorus, nitrogen and sulfur and used for epoxy resin and preparation method of flame retardant

An epoxy resin and epoxy resin curing technology, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as excessive smoke, achieve good compatibility, improve Flame retardant performance, easy post-processing effect

Inactive Publication Date: 2016-10-12
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the introduction of halogen into the epoxy resin can effectively improve the self-extinguishing ability of the material during the combustion process, there are secondary hazards such as smoke, toxic or corrosive gas emission when the material is burned.

Method used

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  • Flame retardant containing phosphorus, nitrogen and sulfur and used for epoxy resin and preparation method of flame retardant
  • Flame retardant containing phosphorus, nitrogen and sulfur and used for epoxy resin and preparation method of flame retardant
  • Flame retardant containing phosphorus, nitrogen and sulfur and used for epoxy resin and preparation method of flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 11.9 g DOPO, 8.3 g 2-aminobenzothiazole, 7.6 ml triethylamine, and 100 ml methylene chloride were added to a reactor with a temperature control device and a stirring device, and an inert gas was introduced, under stirring and ice bath conditions Add 5.3 ml of carbon tetrachloride dropwise, and control the temperature not higher than 15°C, and return to room temperature for reaction after the dropwise addition is completed. After the reaction is completed, the reaction mixture is suction-filtered first, and the filtrate is suspended and evaporated to obtain a viscous liquid. Finally, the viscous liquid is washed with water and acetone for 3 to 4 times, and vacuum-dried to obtain the product DOPO-ABZ, with a yield of 82%. .

Embodiment 2

[0028] Add 11.9 g DOPO, 8.3 g 2-aminobenzothiazole, 15.2 ml triethylamine, and 30 ml acetone into a reactor with a temperature control device and a stirring device, feed inert gas, and drop Add 5.3 ml of carbon tetrachloride, and control the temperature not higher than 15 ° C, return to room temperature after the dropwise addition is complete. After the reaction was completed, it was filtered with suction, washed with water, and dried in vacuum to obtain the product DOPO-ABZ with a yield of 86%.

Embodiment 3

[0030] Add 11.9 g DOPO, 9.9 g 2-aminobenzothiazole, 8.4 ml triethylamine, and 150 ml acetone into a reactor with a temperature control device and a stirring device, feed inert gas, and drip under stirring and ice-bath conditions Add 10.6 ml of carbon tetrachloride, and control the temperature not higher than 15 ° C, return to room temperature after the dropwise addition is complete. After the reaction was completed, it was filtered with suction, washed with water, and dried in vacuum to obtain the product DOPO-ABZ with a yield of 86%.

[0031] The test and analysis results of flame retardant DOPO-ABZ are as follows:

[0032] 1 H NMR (400 MHz, DMSO-d 6 ), δ (ppm): 12.73 (s, N-H), 8.15-8.19 (m, 2H), 7.84 (dd, J=14Hz, 7.2 Hz, 1H), 7.71-7.77 (m, 2H), 7.56 (td, J=7.6 Hz, 3.2 Hz, 1H), 7.44 (t, J=7.6 Hz, 1H), 7.26-7.33 (m, 3H), 7.14-7.21 (m, 2H);

[0033] 31 P NMR (400 MHz, DMSO-d 6 ), δ (ppm): 12.00;

[0034] FTIR (KBr, cm -1 ), 3439.8 (N-H), 3064.6 (Ar-H), 1468.3 (P-Ph), 11...

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Abstract

The invention discloses a flame retardant containing phosphorus, nitrogen and sulfur and used for epoxy resin and a preparation method of the flame retardant. Firstly, DOPO and aminothiazole are taken as reaction raw materials and subjected to an Atherton-Todd reaction for preparation of the flame retardant containing phosphorus, nitrogen and sulfur. The process steps of the method are simple, the yield and the purity of the flame retardant are high, and the post-treatment process is simple and convenient. The flame retardant containing phosphorus, nitrogen and sulfur and prepared with the method is used for modifying cured epoxy resin and has good compatibility with epoxy resin, and the obtained cured flame-retardant epoxy resin has excellent flame retardancy; when the phosphorus content of the epoxy curing system reaches 0.43wt%-1.23wt%, the vertical burning grade can pass UL-94 V-0 level, and the limit oxygen index is as high as 36%.

Description

technical field [0001] The invention relates to a novel phosphorus-nitrogen-sulfur flame retardant, its preparation method and application. The phosphorus-nitrogen-sulfur flame retardant is added to epoxy resin, which can effectively improve the flame-retardant performance of epoxy resin cured product and keep epoxy resin mechanical properties. Background technique [0002] As a very important class of thermosetting resins, epoxy resins are widely used in coatings, adhesives, composite materials, and electronic and electrical equipment due to their excellent mechanical properties, insulation, thermal stability, and chemical corrosion resistance. Insulation materials and other fields. As epoxy resins are used more and more widely in these fields, the performance requirements for them are also getting higher and higher. However, epoxy resin is a very flammable material, which cannot meet some application fields that require the material to have a flame retardant grade. Ther...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5399C08L63/00C07F9/6574
CPCC07F9/65744C08K5/5399C08L63/00C08L2201/02
Inventor 简荣坤王盼段伟森翁家宝
Owner FUJIAN NORMAL UNIV
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