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Production method of brominated butadiene styrene rubber

A production method and technology of bromide, which are applied in the field of flame retardants, can solve the problems of insufficient substitution of hexabromocyclododecane, toxic environmental effects of aquatic plants, and lack of thermal stability to prevent application, and achieve environmental protection of production technology, The effect of high product yield and stable quality

Active Publication Date: 2015-07-08
SHANDONG RUNKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, HBCD has one or more types of bioaccumulation, toxicity to aquatic plants, and persistence of environmental impact, resulting in the need for a new environmentally friendly flame retardant to replace the application of this product
[0008] Brominated styrene-butadiene rubber has not been reported in China at present, and the related product mainly studied abroad is the synthesis of brominated butadiene homopolymer (Br~PBD), but the above-mentioned products have poor thermal stability and are not enough to replace six Bromocyclododecane
The lack of sufficient thermal stability prevents the application of the above products

Method used

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  • Production method of brominated butadiene styrene rubber
  • Production method of brominated butadiene styrene rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Put 555kg of dichloroethane into a 1000L reactor, turn on the mixer, add 48kg of styrene-butadiene rubber into the reactor under stirring, and stir at room temperature for 35 minutes to dissolve it completely.

[0042] Add 302.9 kg of tetrabutylammonium tribromide (dissolved in dichloroethane) dropwise to the reactor, and control the temperature at 40°C during the dropwise addition process, and the rate of addition can be controlled depending on the temperature.

[0043] The temperature was raised to 80°C, and the reaction was kept under reflux for 17 hours.

[0044] Alkali washing: transfer the material to the neutralization kettle, add 180kg of sodium bisulfite solution with a mass concentration of 20%, stir for 8 minutes, let stand to separate layers, and the pH value is >14.

[0045] Water washing: transfer the lower organic phase to a water washing kettle, add 180kg of water, stir for 20 minutes, wash with water, and let stand to separate layers.

[0046] Salt was...

Embodiment 2

[0051] Put 605kg of dichloroethane into a 1000L reactor, turn on the mixer, add 48kg of styrene-butadiene rubber into the reactor under stirring, stir at room temperature for 40 minutes, and dissolve it completely.

[0052] Add 350kg of bromosuccinimide (dissolved in dichloroethane) dropwise to the reaction kettle, and control the temperature at 50°C during the dropwise addition process, and the rate of addition can be controlled depending on the temperature.

[0053] The temperature was raised to 80°C, and the reaction was kept under reflux for 15 hours.

[0054] Alkali washing: transfer the material to the neutralization kettle, add 200kg of sodium bisulfite solution with a mass concentration of 20% (40kg of sodium bisulfite dissolved in 160kg of water), stir for 10 minutes, let stand to separate layers, and the pH value is > 14 .

[0055] Water washing: transfer the lower organic phase to a water washing kettle, add 200kg of water, stir for 20 minutes, wash with water, and...

Embodiment 3

[0061] Put 655kg of dichloroethane into a 1000L reactor, turn on the mixer, add 48kg of styrene-butadiene rubber into the reactor under stirring, stir at room temperature for 35 minutes, and dissolve it completely.

[0062] Add 305 kg tetrabromocyclone (dissolved in dichloroethane) dropwise to the reaction kettle, and control the temperature at 45°C during the dropwise addition process, and the rate of addition can be controlled depending on the temperature.

[0063] The temperature was raised to 80°C, and the reaction was kept under reflux for 20 hours.

[0064] Alkali washing: transfer the material to the neutralization kettle, add 220kg of sodium bisulfite solution with a mass concentration of 20%, stir for 12 minutes, let stand to separate layers, and the pH value is >14.

[0065] Water washing: transfer the lower organic phase to a water washing tank, add 220kg of water, stir for 20 minutes, wash with water, and let stand to separate layers.

[0066] Salt wash: transfer ...

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Abstract

The invention provides a production method of brominated butadiene styrene rubber. The production method comprises, by weight, the following steps: adding 555-655 parts of dichloroethane to a reaction still; adding 43-54 parts of butadiene styrene rubber in a stirring state, stirring and dissolving under normal temperature; adding 302.9-322.9 parts of brominating agent to halohydrocarbon, carrying out dissolving, adding brominating agent solution to the reaction still, rising the temperature to 75-85 DEG C to flowback to thermal response; alkali washing, enabling a potential of hydrogen (pH) value to be larger than 14, cleaning with water, cleaning with brine, standing and layering until an organic layer is layered out, adding emulgator and water, rising the temperature, distilling the dichloroethane, then carrying out water cleaning after carrying out suction filtering; and obtaining the product of the brominated butadiene styrene rubber by drying. The production method of the brominated butadiene styrene rubber has the advantages of being environment-friendly in production technology, low in energy consumption, high in yield of the product, stable and up to standard in quality, simple and safe in operation technology, and the like.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a production method of brominated styrene-butadiene rubber. Background technique [0002] At present, the total output of the world's six major general-purpose polymers has reached 180 million tons per year, of which 8-9%, or 14 million to 15 million tons per year, are added with flame retardants, and the proportion will continue to increase, especially It is plastics used in the electronics and electrical industries. Currently, about 18% of them are added with flame retardants, and it is expected to reach 23-25% in the next five years. [0003] In addition, the flame-retardant ratio of engineering plastics is higher than that of general-purpose plastics. From 2007 to 2008, the total output of engineering plastics in the world was 6 million tons per year, of which 35% were flame-retardant products, and they were used in projects in the electronics and electrical industri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L15/02C08F236/10C08F8/20
Inventor 宗先庆
Owner SHANDONG RUNKE CHEM
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