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Brominated styrene/butadiene copolymer fire retardant and bromination method thereof

A technology for brominating styrene and butadiene, applied in the field of brominated copolymer flame retardants and their bromination, can solve the problems of hydrogen bromide vapor hazards, toxic and harmful fumes, etc. The effect of flammability

Inactive Publication Date: 2015-02-04
青岛方泰克新材料有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The harm of hydrogen bromide vapor will be more significant, and it will produce toxic and harmful fumes when used as a flame retardant; therefore, hexabromocyclododecane will be banned in a certain range

Method used

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  • Brominated styrene/butadiene copolymer fire retardant and bromination method thereof
  • Brominated styrene/butadiene copolymer fire retardant and bromination method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment A

[0023] Add 20g of SBS (D1101, 30% styrene content) and 200g of isobutanol, 12g of sodium bromide and 50g of water into a 250mL chlorination reactor equipped with a condenser. into a dilute alkali solution, the temperature of the reaction solution was gradually raised to 45°C, then 2g of ferric chloride was added, the temperature was raised to 80°C and stirred for 1 hour. The temperature was purged with nitrogen, filtered and washed to obtain 28 g of the target product as a white solid, namely brominated styrene / butadiene copolymer (abbreviated as Br-SBS).

Embodiment B

[0025] Add 20g of SBS (MD6459, 75% styrene content) and 200g of isobutanol, 6g of sodium bromide into a 250mL chlorination reactor equipped with a condenser, and then inject chlorine gas from the bottom of the reactor after heating and dissolving , the tail gas is passed into the dilute alkali solution, after three hours, 2g of ferric chloride is added and the temperature is raised to 80°C, stirred for one hour, after the reaction is completed, the temperature is purged with nitrogen to cool down, the reaction liquid is filtered in a closed filter, and the obtained light yellow solid Pour it into 100mL of methanol and heat up to 60°C for recrystallization. After filtering and washing with water, a white solid was obtained, which was Br-SBS.

Embodiment C

[0027] Bromination reaction of tri-block SBS, synthesis of SBS: The synthesis of SBS adopts three-step feeding method. Firstly, 100g of 30% styrene-cyclohexane solution is added to the polymerization bottle, and after impurities are removed by chemical purification, 0.3g is added. Initiate polymerization with n-butyllithium to obtain the active polymer solution of polystyrene in the first stage, add 100g of 30% butadiene-cyclohexane solution and tetrahydrofuran corresponding to the required 1,2-structure content in another polymerization bottle After the residual impurities are removed by chemical purification, the first stage of active polystyrene solution that has been polymerized is immediately pressed with high-purity nitrogen, and the active polystyrene gradually triggers the second stage of butadiene monomer to continue to grow; the second stage After the stage of polymerization is completed, the third stage of styrene-cyclohexane solution that has been purified by chemic...

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Abstract

The invention provides a brominated styrene / butadiene copolymer fire retardant and a bromination method thereof. The copolymer of the fire retardant is formed by polymerizing a brominated styrene monomer and a butadiene monomer. In the brominated styrene / butadiene copolymer, the brominated aryl of styrene comprises 2-bromostyrene, 4-bromostyrene and 2,4-dibromostyrene. A preparation method comprises the following steps: (1) selecting the following raw materials: a styrene / butadiene copolymer (shortened as SBS), sodium bromide of which the content is 98%-99%, chlorine gas of which the content is higher than 99% and isobutyl alcohol of which the content is higher than 99%; (2) adding the SBS in an enamel reactor and dissolving the SBS in a heating manner by using isobutyl alcohol; (3) adding a sodium bromide solution, introducing an oxidant, stirring during a reaction process, and absorbing unreacted oxidant by using lime milk at the tail part of the reactor; (4) afterwards cooling to room temperature, adding a catalyst and continuing to stir and heat; (5) filtering after cooling to room temperature to obtain a target product brominated styrene / butadiene polymer.

Description

technical field [0001] The invention relates to the field of plastic additives in the chemical industry, in particular to a brominated copolymer flame retardant and a brominated method thereof. Background technique [0002] Brominated styrene / butadiene polymers are considered to be new flame retardants that can replace hexabromocyclododecane flame retardants in expanded polystyrene and extruded polystyrene foam sheets. Hexabromocyclodecane products commonly used in the market are additive flame retardants, mainly used as polystyrene (addition amount is 2%), polypropylene, ABS, polycarbonate, unsaturated polyester, etc., it is regarded as It is a flame retardant that is bioaccumulative and harmful to aquatic organisms or the environment. It is highly toxic. In addition, the dehydrobromination of hexabromocyclododecane becomes severe above 190 °C. The harm of hydrogen bromide vapor will be more significant, and it will produce toxic and harmful fumes when used as a flame reta...

Claims

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Application Information

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IPC IPC(8): C08F236/10C08F212/08C08F297/04C08F8/20C08L25/06C08L25/10C08L47/00C08L53/02
Inventor 王添琪石昌玉
Owner 青岛方泰克新材料有限公司
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