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Preparation method for hexabromocyclododecane with high gamma isomer content

A technology of hexabromocyclododecane and water content, which is applied in the preparation of hexabromocyclododecane and the field of hexabromocyclododecane products, can solve the serious side reactions between alcohol solvents and brominating agents and reduce bromination Solvent utilization rate and other issues, to achieve the effect of simplifying the solvent refining process, facilitating dispersion, and low bulk density

Active Publication Date: 2013-05-08
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

In addition, the side reaction between alcohol solvent and brominating agent is more serious, which reduces the utilization rate of brominating agent

Method used

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  • Preparation method for hexabromocyclododecane with high gamma isomer content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A mixed solvent with a water content of 2.0wtwt% was prepared, consisting of a mixed solvent composed of 100g of isobutanol, 100g of chloroform, and 4.1g of water.

[0030] In a 500ml four-necked flask, put the mixed solvent prepared above (water content 2.0wt%), turn on the stirrer, and add sodium bromide to a supersaturated state (there is a small amount of sodium bromide that is not completely dissolved). Two 100ml dropping funnels were used to charge 40g (0.25mol) cyclododecatriene and 123.2g (0.77mol) bromine respectively, and part of bromine (3g) was pre-added to the cyclododecatriene before starting to add in the reaction flask. The speed of adding cyclododecatriene and bromine was adjusted so that both were completely added to the reaction flask almost simultaneously. The addition time of cyclododecatriene and bromine is about 150 minutes, and the temperature of the reaction material is controlled at 10-15°C by using an ice-water bath during the entire addition...

Embodiment 2

[0034] As described in Example 1, the difference is that the mixed solvent is composed of 50g chloroform and 150g isobutanol, and the water content in the mixed solvent is 5.0wt%.

[0035] The yield of HBCD is 92.5%, the melting point is 180.5-190.5°C, and the composition of each isomer in the product is 11.8wt%α, 10.1wt%β, 77.8%γ.

Embodiment 3

[0037] As described in Example 1, the difference is that the mixed solvent is composed of 80 g of 1,2-dichloroethane and 100 g of 2-ethylhexanol, and the water content in the mixed solvent is 3.0 wt%.

[0038] The yield of HBCD is 93.2%, the melting point is 182.0-190.5°C, and the composition of each isomer in the product is 10.2wt%α, 8.8wt%β, 80.3wt%γ.

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Abstract

The invention relates to a method for preparing hexabromocyclododecane. A water-containing mixed solvent is used as a reaction medium, wherein the mixed solvent comprises hydrochloric ether and low molecular fatty alcohol with carbon number smaller than 10; inorganic acid salt or organic acid salt is added to the water-containing mixed solvent, so that the water-containing mixed solvent achieves a dissolved saturation condition; the permissible moisture content in the mixed solvent can be increased to 10wt%. The selectivity and the product yield of the hexabromocyclododecane gamma isomer are improved by utilizing the preparation method disclosed by the invention; and moreover, the product grain size is small and the bulk density is low, so that the dispersion in the polymer is facilitated.

Description

Technical field [0001] The present invention is a chemical technology field, involving a preparation method of hexarium bromine duolane. The method of the present invention can produce high γ -hexide dulate products.Essence Background technique [0002] Hexide Twolane (1,2,5,6,9,10-hexaracromide dulate, hereinafter referred to as HBCD) is an excellent additive flame retardant, which can be used as a variety of thermoplastics.Food retardant.HBCD is usually composed of three heterosexuals called α, β and γ.In the three isomers, the alpha heterogeneous melting point was 179-181 ° C, the β heterogeneous melting point 170 ~ 172 ℃, and the melted point of the γ heterogeneous 207 ~ 209 ℃.The γ isomer is the highest melting point.The existence of the three heterogeneous products in commercial products makes the melting point of HBCD wide. It is generally believed that increasing the content of γ is the initial melting point of the product. [0003] In existing technologies, in order to o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C23/02C07C17/02
Inventor 李明晶杨树仁王美芹张绰王金宝段生芹丁瑞林李建业
Owner 山东旭锐新材股份有限公司
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