Method for preparing brominated styrene-butadiene copolymer through heterogeneous oxidation

A technology of brominated styrene and heterogeneous oxidation, which is applied in the production of bulk chemicals, etc., can solve the problems of failing to meet the requirements of flame retardant properties of building materials products, poor flame retardant effect of halogen-free flame retardants, and halogen-free flame retardants. The problem of low flame retardant efficiency of the flame retardant, to achieve the effect of high bromine content, easy to control, and ensure the formation rate

Active Publication Date: 2019-06-28
TIANJIN BUILDING MATERIALS SCI RES INST
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of the above situation, the current international solution is to actively research halogen-free flame retardants. However, halogen-free flame retardants have low flame retardant efficiency, high dosage, high price, and high cost. They are generally used in toys, clothing, e

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  • Method for preparing brominated styrene-butadiene copolymer through heterogeneous oxidation
  • Method for preparing brominated styrene-butadiene copolymer through heterogeneous oxidation
  • Method for preparing brominated styrene-butadiene copolymer through heterogeneous oxidation

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[0034] Example 1

[0035] (1) dissolve 10g SBS with 70ml organic solvent chloroform, add 180g 45% tetraethylammonium bromide aqueous solution, be warming up to 25 ℃, add 0.3g tin tetrachloride, drip 4.8g 50% citric acid aqueous solution to make catalyst, 154g of ceric ammonium nitrate was added, and after the addition was completed, a constant temperature reaction was performed for 3-5 hours, and the layers were left to stand for stratification;

[0036] (2) Under the condition of constant temperature of 25°C, wash the organic phase of the lower layer with 50ml of 5% NaOH solution each time for 2-4 times, and each washing time is 0.5-1h to remove impurities, and then use 50ml of distilled water to remove impurities. The organic phase was washed several times with water, and the lower organic phase was dried with anhydrous calcium chloride solid;

[0037] (3) Add 1 g of Zr(OH) to the dried organic phase 4 and 0.2g phosphoric acid, at a temperature of 15°C-25°C, add 80ml dimet...

Example Embodiment

[0038] Example 2

[0039] (1) dissolve 10g SBS with 70ml organic solvent chloroform, add 180g 45% tetraethylammonium bromide aqueous solution, be warming up to 25 ℃, add 0.3g tin tetrachloride, add 154g cerium ammonium nitrate, after adding, constant temperature reaction 3- 5 hours, stand for stratification;

[0040] (2) Under the condition of constant temperature of 25°C, wash the organic phase of the lower layer with 50ml of 5% NaOH solution each time for 2-4 times, and each washing time is 0.5-1h to remove impurities, and then use 50ml of distilled water to remove impurities. The organic phase was washed several times with water, and the lower organic phase was dried with anhydrous calcium chloride solid;

[0041] (3) Add 1 g of Zr(OH) to the dried organic phase 4 and 0.2g phosphoric acid, at a temperature of 15°C-25°C, add 80ml dimethyl sulfoxide solution containing 10g NBS, heat up to 90-100°C and reflux for 1-2 hours, and neutralize the excess with sodium hydroxide aft...

Example Embodiment

[0042] Example 3

[0043] (1) dissolve 10g SBS with 70ml organic solvent chloroform, add 180g 45% tetraethylammonium bromide aqueous solution, be warming up to 25 ℃, add 0.3g tin tetrachloride, drip 4.8g 50% sodium carbonate aqueous solution to make catalyst, 154g of ceric ammonium nitrate was added, and after the addition was completed, a constant temperature reaction was performed for 3-5 hours, and the layers were left to stand for stratification;

[0044] (2) Under the condition of constant temperature of 25°C, wash the organic phase of the lower layer with 50ml of 5% NaOH solution each time for 2-4 times, and each washing time is 0.5-1h to remove impurities, and then use 50ml of distilled water to remove impurities. The organic phase was washed several times with water, and the lower organic phase was dried with anhydrous calcium chloride solid;

[0045] (3) Add 1 g of Zr(OH) to the dried organic phase 4 and 0.2g phosphoric acid, at a temperature of 15°C-25°C, add 80ml ...

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Abstract

The invention provides a method for preparing a brominated styrene-butadiene copolymer through heterogeneous oxidation. The method comprises the following main steps: (1) dissolving SBS by virtue of an organic solvent, adding organic ammonium bromide water solution and a methyl bromination inhibitor, dropwise adding a small amount of an acid catalyst so as to adjust the pH value, adding a metal oxidizing agent, carrying out constant-temperature reaction, and standing for layering; (2) washing and drying an organic solvent on a lower layer; and (3) adding a solid acid catalyst and an NBS-containing organic solution into the dried organic phase, heating to 90-100 DEG C, carrying out reflux for 1-2 hours, cooling, neutralizing free bromine by virtue of an alkaline substance, precipitating byvirtue of a precipitant, filtering, and drying, so as to obtain a brominated SBS product. The method provided by the invention has the beneficial effects that the production energy consumption is low,the discharging of three wastes is greatly reduced, the obtained product is high in bromine content and yield, good in stability and suitable for the flame prevention of foam rubber products such asfoamed polyethylene, polypropylene and polystyrene.

Description

technical field [0001] The invention belongs to the technical field of synthesis of brominated flame retardants, and in particular relates to a method for preparing brominated styrene-butadiene copolymers through heterogeneous oxidation. Background technique [0002] Brominated flame retardants have high flame retardant properties, good heat resistance, and can meet the flame retardant requirements of various polymer materials. In addition, the source of raw materials is sufficient, the price is cheap, and the physical and mechanical properties of the substrate do not deteriorate too much. It is unmatched by other flame retardants and has always been favored by people. It is currently one of the largest and most widely used flame retardants on the market. Among all flame retardants currently used in polystyrene (PS) materials, hexabromocyclododecane (HBCD) has better compatibility with PS resins, and can make PS materials It has good flame retardant properties and can maint...

Claims

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Application Information

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IPC IPC(8): C08F8/20C08F297/04C08L23/06C08L23/12C08L25/06C08L53/02
CPCY02P20/52
Inventor 杨倩刘彤张鹏宇滕藤李剑光
Owner TIANJIN BUILDING MATERIALS SCI RES INST
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