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BPS product and method for preparing BPS product by virtue of bromine chloride method

A bromine chloride method and bromine chloride technology, applied in the field of fine chemicals, can solve the problems of unstable bromination reaction rate, low bromination reaction substitution efficiency, easy yellowing of products during use, and achieve fast reaction rate and Stable, shortened chlorination time, high bromine content effect

Active Publication Date: 2019-03-19
山东旭锐新材股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Based on the above patents, the existing BPS product preparation methods still have the above defects: (1) The main chain of the existing BPS product is easily replaced by bromine, which leads to the yellowing of the product during use and reduces the thermal stability of the product ;
[0005] 2) The existing BPS product preparation method has a long reaction cycle and low production efficiency;
[0006] 3) In the existing BPS product preparation method, the reaction rate of the bromination reaction is unstable and difficult to control, and the substitution efficiency of the bromination reaction is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1: the preparation method of the bromine chloride method of a kind of BPS product

[0043] The preparation method of the bromine chloride method of a kind of BPS product of the present embodiment, comprises the following steps:

[0044] Step 1. Raw material preparation:

[0045] (1) Preparation of anhydrous dichloromethane: put 360g of dichloromethane in a four-necked flask, add 1.5g of phosphorus pentoxide, stir for 5-6 hours, and check that the water content is less than 0.03%;

[0046] (2) Vaporization of liquid chlorine: After the liquid chlorine in the steel cylinder is vaporized by the vaporization pool, it is stored in the buffer tank for future use.

[0047] Step 2, synthetic bromine chloride:

[0048] Add 75g of dichloromethane and 50g of bromine into the four-necked bottle, lower the temperature to -10~-13°C, and then slowly inject 23g of chlorine gas into the four-necked bottle. After the chlorine gas is added, keep the low temperature for 10 min...

Embodiment 2

[0054] Embodiment 2: the preparation method of the bromine chloride method of a kind of BPS product

[0055] Step 1. Raw material preparation:

[0056] (1) Preparation of anhydrous dichloromethane: put 360g of dichloromethane in a four-necked flask, add 1.5g of phosphorus pentoxide, stir for 5-6 hours, and check that the water content is less than 0.03%;

[0057] (2) Vaporization of liquid chlorine: After the liquid chlorine in the steel cylinder is vaporized by the vaporization pool, it is stored in the buffer tank for future use.

[0058] Step 2, synthetic bromine chloride dispersion:

[0059](1) Add 75g of dichloromethane and 50g of bromine into the four-necked bottle, cool down to -10~-13°C, then slowly inject 23g of chlorine gas into the four-necked bottle, after the chlorine gas is added, keep the low temperature and keep warm for 10 minutes , then transferred to the constant pressure dropping funnel with jacket insulation to obtain bromine chloride solution;

[0060]...

Embodiment 3

[0071] Embodiment 3: a kind of BPS product

[0072] The BPS product of Example 2 of the present invention and antimony trioxide are made into a composite flame retardant according to a certain ratio according to a conventional method, and the composite flame retardant is added to engineering plastics, which has good compatibility, is not easy to yellow, and is flame retardant The effect is good. After adding, the flame retardant level reaches the V-0 level standard, and has little effect on the mechanical properties of plastics. details as follows:

[0073] (1) 22% composite flame retardant is added to Pbt, which can reach the UL94V-0 level addition standard;

[0074] (2) 16% compound flame retardant is added to the pet, which can reach the UL94V-0 level addition standard;

[0075] (3) 23% composite flame retardant is added to PA6, which can meet the UL94V-0 standard;

[0076] (4) 14% compound flame retardant is added to PA66, which can reach the UL94V-0 level addition stan...

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Abstract

The invention discloses a method for preparing a BPS product by virtue of a bromine chloride method. The method comprises the following steps: raw material preparation, synthesis of bromine chloride,bromination reaction and after-treatment, wherein the synthesis of bromine chloride comprises the steps of mixing dichloromethane with bromine, cooling to (-10)-(-13) DEG C, slowly introducing chlorine, and maintaining the temperature at a low temperature for 10 minutes. The invention further provides the BPS product. The BPS product has a white or faint yellow appearance, the bromine contents arehigher than or equal to 66% at 1%TGA@350DEG C and 5%TGA@350DEG C, and the thermal decomposition temperature is higher than or equal to 270 DEG C. According to the method, chlorine is replaced with liquid chlorine, so that the chlorination time can be greatly shortened, and the energy consumption can be saved; and by utilizing tin tetrabromide as a free radical quenching agent, the number of halogen atoms of a main chain is reduced, the thermal stability of the product is improved, the reaction period is shortened, the production efficiency is improved, and the method has great economic and social benefits.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a BPS product and a preparation method thereof by a bromine chloride method. Background technique [0002] Brominated polystyrene (BPS) is an internationally recognized brominated organic flame retardant, does not contain polybrominated diphenyl ethers and polybrominated biphenyls, and complies with ROHS standards. It has the advantages of good compatibility with materials, no precipitation, no frost, good electrical properties, little impact on the mechanical properties of materials, and low price. [0003] The Chinese patent with the patent publication number CN101701046.A discloses a method of synthesizing brominated polystyrene using antimony trichloride as a catalyst for the reaction of polystyrene and bromine chloride, and simultaneously adopting an emulsifying homogenizer for centrifugal separation; patent application Chinese patent No. 200910118032.0 discloses a m...

Claims

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Application Information

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IPC IPC(8): C08F8/20C08F112/08
CPCC08F8/20C08F112/08
Inventor 陶书伟李金忠王良民杨凯王强王慧段升芹
Owner 山东旭锐新材股份有限公司
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