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A kind of brominated SBS product with low molecular weight and high thermal stability and preparation method thereof

A technology with high thermal stability and low molecular weight, applied in the field of fine chemicals, can solve the problems of low product purity, dark product color, low conversion rate, etc., and achieve the effect of high purity, stable raw material properties, and not easy to curl

Active Publication Date: 2021-07-30
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

Although this invention can obtain lower oligomers, and the bromine content can reach 65-70%, the purity of its product is not high, the product color is darker, the conversion rate in the reaction process is low, and the production capacity is low, so it cannot practical application in practice

Method used

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  • A kind of brominated SBS product with low molecular weight and high thermal stability and preparation method thereof
  • A kind of brominated SBS product with low molecular weight and high thermal stability and preparation method thereof
  • A kind of brominated SBS product with low molecular weight and high thermal stability and preparation method thereof

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Effect test

Embodiment 1

[0039] Embodiment 1: A kind of brominated SBS product of low molecular weight and high thermal stability and preparation method thereof

[0040] 1. Dissolution of TBAB: Add 12.82g of TBAB and 100g of DCM into a 250ml Erlenmeyer flask, observe the temperature and phenomenon; form material ①, wine red tetrabutylammonium tribromide;

[0041]

[0042] 2. Dissolution of SBS: Add SBS 5g+DCM 100g (determined according to the solubility of Br-SBS) into a 500ml four-necked bottle, and dissolve at room temperature;

[0043] 3. One-step mixing reaction: After the SBS is dissolved, add equimolar material ① dropwise at a temperature lower than 10°C, and the dropping rate is completed within one hour;

[0044] 4. End the reaction: After the dropwise addition is completed, keep warm for 1 hour. After the reaction is complete, add 10% sodium bisulfite solution to end the reaction;

[0045] 5. Decolorization and washing: Add 200.0g of 10% sodium bisulfite solution to decolorize and remove ...

Embodiment 2

[0053] Embodiment 2: A kind of brominated SBS product with low molecular weight and high thermal stability and preparation method thereof

[0054] 1. Add TBAB12.82g and DCM100g into a 250ml Erlenmeyer flask, observe the temperature and phenomenon, and form material ①, namely wine red tetrabutylammonium tribromide;

[0055] 2. Preparation of SBS miniemulsion:

[0056] 1) Add 0.25g co-stabilizer to 5g of commercially available SBS, place it under a magnetic stirrer and stir, add 0.1g calcium carbonate powder, disperse and grind until D90≤0.75um, and conduct ultrasonic-ultraviolet synergistic treatment under nitrogen flow for 65min, the ultrasonic frequency is 55KHz, the power is 425W, the wavelength of ultraviolet light is 385nm, the flow rate of nitrogen flow is 21ml / min;

[0057] In the present embodiment, described commercially available SBS, molecular formula is (C 6 h 5 C 2 h 3 )m(C 4 h 6 )n, where m:n=3:7;

[0058] The co-stabilizer is a mixture of styrene and 1,3-...

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Abstract

The invention provides a brominated SBS product with low molecular weight and high thermal stability and a preparation method thereof, comprising the following steps: dissolving TBAB, dissolving SBS, one-step mixing reaction, decolorization and washing, preparation of bromine solution, and two-step mixing reaction In the one-step mixed reaction, the temperature of the dissolved SBS is lowered to below 10°C, and an equimolar material ① is added dropwise; in the two-step mixed reaction: the temperature of the material obtained after decolorization and washing is lowered to lower than 10°C, and the dropwise added Equimolar material 2.; the method of the present invention obtains brominated SBS product, and 1% thermogravity loss temperature is 230 ℃, 5% thermogravity loss 245 ℃, 10% thermogravity loss 255 ℃, 50% thermogravity loss 280 ℃, bromine content is 66 %, the product has low molecular weight, high purity, good thermal stability, brominated SBS block is not easy to curl and entangle, low viscosity, simple process, and the conversion rate of the reaction is improved, which is conducive to popularization and application.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a brominated SBS product with low molecular weight and high thermal stability and a preparation method thereof. Background technique [0002] Brominated flame retardants have good flame retardant effects, light stability and antistatic properties, and are widely used in various plastics such as polyolefins, polyamides and polystyrene, fibers and synthetic rubber materials such as silicone rubber. Among them, the content of bromine element in the flame retardant system is an important parameter to evaluate the flame retardant performance of brominated flame retardants, and its size directly affects the quality of the product and the flame retardant effect. [0003] Brominated SBS, brominated styrene-butadiene block copolymer, as a new environmentally friendly brominated flame retardant, has been widely used in waterproof membranes and various types of plastic sheets. [00...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F297/04C08F8/20
Inventor 杨凯王强王良民李金忠张荣华杨清波
Owner 山东旭锐新材股份有限公司