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Pentabromobenzyl bromide production method

A kind of technology of pentabromobenzyl bromide and pentabromotoluene is applied in the field of production of pentabromobenzyl bromide, can solve the problems of high industrialization cost, expensive brominating agent NBS, etc., and achieves the advantages of short reaction time, simple operation and low reaction temperature. Effect

Active Publication Date: 2015-07-22
盐城创咏新能源投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The bromination agent NBS used in the former is more expensive, and the cost of industrialization is higher; while the ultraviolet light method required by the latter is only suitable for laboratory production due to its high equipment requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 97.4g of pentabromotoluene (0.2mol), 220ml of chlorobenzene, 38.4g of liquid bromine (0.24mol) and 33ml of deionized water into a 500ml three-necked flask with a condenser and mechanical stirring, and stir at a speed of 350r / min Lower the temperature to 45°C, add initiator: 0.974g each of AIBN and BPO, react at 45°C for 2h, then rapidly raise the temperature to 70°C for 2.5h; cool the reaction solution to room temperature and filter, and wash with chlorobenzene and water to The filtrate was colorless and pH=7; then vacuum-dried at 60°C for 12 hours to obtain the product pentabromobenzyl bromide as white crystals with a yield of 88.3%.

Embodiment 2

[0018] Add 97.4g of pentabromotoluene (0.2mol), 220ml of chlorobenzene, 44.8g of liquid bromine (0.28mol) and 33ml of deionized water into a 500ml three-necked flask with a condenser and mechanical stirring, and stir at a speed of 350r / min Lower the temperature to 45°C, add initiator: 0.974g each of AIBN and BPO, react at 45°C for 2h, then rapidly raise the temperature to 70°C for 2.5h; cool the reaction solution to room temperature and filter, and wash with chlorobenzene and water to The filtrate was colorless and pH=7; then vacuum-dried at 60°C for 12 hours to obtain the product pentabromobenzyl bromide as light yellow crystals with a yield of 90.2%. Because liquid bromine is easy to volatilize, so if the consumption of liquid bromine is a little excessive, but compare and draw by embodiment 1 and 2: when liquid bromine consumption is too much, the amount of polybrominated product may be increased, and product color turns yellow.

Embodiment 3

[0020] Add 97.4g of pentabromotoluene (0.2mol), 167ml of chlorobenzene, 38.4g of liquid bromine (0.24mol) and 33ml of deionized water into a 500ml three-necked flask with a condenser and mechanical stirring, and stir at a speed of 350r / min Lower the temperature to 45°C, add initiator: 0.974g each of AIBN and BPO, react at 45°C for 2h, then rapidly raise the temperature to 70°C for 2.5h; cool the reaction solution to room temperature and filter, and wash with chlorobenzene and water to The filtrate was colorless and pH=7; then vacuum-dried at 60°C for 12 hours to obtain the product pentabromobenzyl bromide as white crystals with a yield of 92.6%.

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Abstract

The invention discloses a pentabromobenzyl bromide production method and relates to the technical field of flame retardant. The method includes: sequentially adding pentabromotoluene, halohydrocarbon, liquid bromine and deionized water; by means of a gradual heating reaction method, adding unite initiator at 40-50 DEG C for reacting for 2h, heating to 70-75 DEG C, continuing reacting for 2-2.5h, and keeping the stirring speed at about 350r / min; cooling and filtering reaction liquid, and respectively using halohydrocarbon and water for washing until filtrate is colorless and pH=7; and performing vacuum drying for 12h at 60 DEG C to obtain the pentabromobenzyl bromide. By using the unit initiator, the pentabromobenzyl bromide production method is short in reaction time, low in reaction temperature, low in energy consumption and high in yield. The prepared pentabromobenzyl bromide is up to 84% in bromine content, has excellent flame retardant performance, can be used as an additive flame retardant for direct use, and can be also use as an important chemical material to be reacted with various carboxylic acids to generate a series of derivatives.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular designing a method for producing pentabromobenzyl bromide. Background technique [0002] Brominated flame retardants are the most widely used flame retardants. In recent years, due to environmental pressure and "dioxin" problems, some brominated flame retardants such as polybrominated diphenyl ethers have been phased out, but brominated flame retardants Flame retardant has excellent cost performance, and it is still the most practical choice for some fields with strict flame retardant standards and some materials that are difficult to flame retardant. [0003] Pentabromobenzyl bromide has a bromine content of 84.8%, which has excellent flame retardant properties and can be used directly as an additive flame retardant; at the same time, the bromine on the benzyl group in its molecule has high reactivity and can be used with a variety of Carboxylic acid or acid anhydride rea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C25/02C07C17/14
Inventor 王标兵王留阳王玉龙
Owner 盐城创咏新能源投资有限公司
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