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Low-cost method for preparing tribromophenoxy triazine

A tribromophenoxytriazine and low-cost technology, which is applied in the field of low-cost preparation of tribromophenoxytriazine, can solve problems such as pollution, high manufacturing cost, and inability to recycle, so as to reduce environmental pollution and improve product quality. quality effect

Pending Publication Date: 2021-08-06
JIANGSU XINZHOU CHEM SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Brominated flame retardant is a new type of pollution-free fiber flame retardant. Compared with the conventional product polybrominated diphenyl ether, the addition of this flame retardant has no toxic dibenzodioxin when the polymer is thermally cracked or burned. Alkanes and polybrominated dibenzofurans, this kind of flame retardants are very popular in the new flame retardants introduced in the United States in the 1990s. Tribromophenoxytriazine is an additive flame retardant containing bromine , Nitrogen migration resistant flame retardant, good thermal stability, there is a synergistic effect of bromine and nitrogen, it has smoke suppression effect, has a small dosage, has little impact on the performance of the substrate, overcomes the shortcomings of raw materials that cannot be recycled, and is a new type of green Environmentally friendly flame retardant, which makes up for the poor light resistance and yellow color of decabromodiphenyl ether. It is an upgraded product of decabromodiphenyl ether. It also has good thermal stability, electrical properties and excellent light resistance. Tribromodiphenyl ether Phenoxytriazine is different from the previous halogen-containing flame retardants. It has a high initial decomposition temperature and does not contain free bromine, which can make processing equipment safer and product performance better. It is widely used in polyester, ABS, HIPS, PC , PC / ABS and other engineering plastics, therefore, there is an increasing demand for a low-cost method for preparing tribromophenoxytriazine. In industry, methylene chloride is often used as a solvent for the synthesis of tribromophenoxytriazine. The higher cost will also cause pollution to the environment; the quality of the product is worse than that of foreign countries. Therefore, a low-cost method for preparing tribromophenoxytriazine is proposed for the above problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The present invention provides a technical solution:

[0019] Method for preparing tribromobenzoxazine at low cost, including the following steps:

[0020] Step 1: Take 2, 4, 6-tribromol as a raw material, triethylamine as a catalyst, and add 2, 4, 6-tribromol and triethylamine to chlorobenzene in chlorobenzene, While adding the raw material, stirring the mixing equipment, stirring at a speed of 40 R / min for 20 min, so that the raw material is sufficiently mixed;

[0021] Step 2: Preheating the mixing device, then adding trimerocyananyanocyanide to the mixed solution and stirring, and added to the addition of a liquid base solution while adding trimerocyanide, adding a liquid base solution, and the mixing raw material occurs. The condensation reaction is subsequently sealed to sealed the mixed solution;

[0022] Step 3: Add the mixed solution after completion of the reaction to the crystal extract, and the azeotropic agent is added to the azeotrope crystal reaction, and t...

Embodiment 2

[0030] The present invention provides a technical solution:

[0031] Method for preparing tribromobenzoxazine at low cost, including the following steps:

[0032] Step 1: Take 2, 4, 6-tribromol as a raw material, triethylamine as a catalyst, and add 2, 4, 6-tribromol and triethylamine to chlorobenzene in chlorobenzene, While adding the raw material, stirring the mixing equipment, stirring at a rate of 40 r / min for 25 min, so that the raw material is sufficiently mixed;

[0033] Step 2: Preheating the mixing device, then adding trimerocyananyanocyanide to the mixed solution and stirring, and added to the addition of a liquid base solution while adding trimerocyanide, adding a liquid base solution, and the mixing raw material occurs. The condensation reaction is subsequently sealed to sealed the mixed solution;

[0034] Step 3: Add the mixed solution after completion of the reaction to the crystal extract, and the azeotropic agent is added to the azeotrope crystal reaction, and th...

Embodiment 3

[0042] The present invention provides a technical solution:

[0043] Method for preparing tribromobenzoxazine at low cost, including the following steps:

[0044] Step 1: Take 2, 4, 6-tribromol as a raw material, triethylamine as a catalyst, and add 2, 4, 6-tribromol and triethylamine to chlorobenzene in chlorobenzene, While adding the raw material, stirring the mixing equipment, stirring at a rate of 40 r / min for 25 min, so that the raw material is sufficiently mixed;

[0045] Step 2: Preheating the mixing device, then adding trimerocyananyanocyanide to the mixed solution and stirring, and added to the addition of a liquid base solution while adding trimerocyanide, adding a liquid base solution, and the mixing raw material occurs. The condensation reaction is subsequently sealed to sealed the mixed solution;

[0046]Step 3: Add the mixed solution after completion of the reaction to the crystal extract, and the azeotropic agent is added to the azeotrope crystal reaction, and the...

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PUM

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Abstract

The invention relates to the technical field of chemical synthesis, in particular to a low-cost method for preparing tribromophenoxy triazine, which comprises the following steps: taking 2,4,6-tribromophenol as a raw material, using triethylamine as a catalyst, adding 2,4,6-tribromophenol and triethylamine into chlorobenzene at a constant speed to carry out dissolution reaction, uniformly adding cyanuric chloride and liquid caustic soda into the mixed solution, conducting stirring to carry out condensation reaction, adding the reacted mixed solution into a crystallization kettle, adding an entrainer to carry out azeotropic crystallization reaction, and then carrying out alkali washing, water washing and drying to obtain tribromophenoxy triazine. According to the preparation method, 2,4,6-tribromophenol and cyanuric chloride are taken as raw materials, triethylamine is taken as a catalyst, tribromophenoxy triazine is obtained after reaction, crystallization, water washing and drying are carried out under the alkaline condition, and the product quality is effectively improved; and cyanuric chloride is added in batches, hydrolysis of cyanuric chloride can be effectively reduced by dropwise adding liquid caustic soda, raw material consumption is reduced, and environmental pollution is reduced.

Description

Technical field [0001] The present invention relates to the field of chemical synthesis, in particular a method of preparing tribromobenzoxyzine at low cost. Background technique [0002] The bromine flame retardant is a non-pollution-free new fiber flame retardant. The addition of the flame retardant is added to the polymer, and when the high polymer is cracked or burned, there is no toxic diphenne. The present flame retardant is popular in the new flame retardant in the 1990s in the 1990s, and tribromobenzoxide is a added flame retardant, bromine containing bromide. , Nitrogen-resistant resistance flame retardant, good thermal stability, has a bromine, nitrogen cohability effect, and inhibition effect, it has a small amount of amount, which has little effect on the performance of the substrate, and overcomes the disadvantage of the raw material, it is the disadvantage. The environmentally friendly flame retardant is made up for the poor nipphenyl ether, and the color of the col...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/34C07D251/26
CPCC07D251/34C07D251/26
Inventor 徐春清郑学军冯繁吴爽柏安鹏
Owner JIANGSU XINZHOU CHEM SCI & TECH CO LTD
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