Synthetic method and refining for tribromoneoamyl alcohol

A technique for the synthesis of tribromoneopentyl alcohol, which is applied in the field of synthesis of tribromoneopentyl alcohol, can solve problems such as hydrogen bromide escape, quality change, and product melting point reduction, and achieve superior performance, complete and thorough reaction, and high product quality. Good results

Inactive Publication Date: 2007-08-15
宜兴市中正化工有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The deficiencies that exist are: in the reaction process, because hydrogen bromide is excessive, normal pressure insulation can cause hydrogen bromide to escape, reduce the concentration of reactant, cause yield low; Normal pressure ester decomposition makes reaction incomplete, product The melting point is lowered and the quality is poor; especially fo

Method used

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  • Synthetic method and refining for tribromoneoamyl alcohol
  • Synthetic method and refining for tribromoneoamyl alcohol
  • Synthetic method and refining for tribromoneoamyl alcohol

Examples

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Embodiment 1

[0015] Embodiment 1, the synthetic method of tribromoneopentyl alcohol, under the acetic acid medium that concentration is more than 98%, pass into pentaerythritol and carry out substitution reaction with hydrogen bromide, the addition weight of acetic acid medium is 1.2 times of pentaerythritol weight, bromination The weight of the hydrogen introduced is twice the weight of pentaerythritol, the time for the introduction is 10 hours, and the temperature of the substitution reaction is 120°C; after the substitution reaction, it is kept at 120°C and a constant pressure of 0.6Mpa for 16 hours; after the heat preservation, it is separated Tribromoneopentyl alcohol esterification, add methanol and sulfuric acid to the tribromoneopentyl alcohol esterification and carry out constant pressure ester decomposition under the pressure of 0.5Mpa, the amount of methanol is 1.5 times of the weight of pentaerythritol, and the amount of sulfuric acid is 3% of the weight of pentaerythritol , con...

Embodiment 2

[0016] Embodiment 2, the synthetic method of tribromoneopentyl alcohol, under the acetic acid medium that concentration is more than 98%, pass into pentaerythritol and carry out substitution reaction with hydrogen bromide, the addition weight of acetic acid medium is 1.4 times of pentaerythritol weight, bromination The weight of hydrogen introduced is 2.3 times the weight of pentaerythritol, the time for passing in is 9 hours, and the temperature of the substitution reaction is 118°C; after the substitution reaction, it is kept at 118°C and a constant pressure of 0.7Mpa for 15 hours; Tribromoneopentyl alcohol esterification, adding methanol and hydrochloric acid to the tribromoneopentyl alcohol esterification and carrying out constant pressure ester decomposition under the pressure of 0.4Mpa, the amount of methanol is 1.3 times of the weight of pentaerythritol, and the amount of hydrochloric acid is 5% of the weight of pentaerythritol , constant pressure ester decomposition tem...

Embodiment 3

[0017] Embodiment 3, the synthetic method of tribromoneopentyl alcohol, under the acetic acid medium that concentration is more than 98%, pass into pentaerythritol and carry out substitution reaction with hydrogen bromide, the addition weight of acetic acid medium is 1.5 times of pentaerythritol weight, bromination The weight of hydrogen introduced is 1.8 times the weight of pentaerythritol, the time of introduction is 9.5 hours, and the temperature of the substitution reaction is 115°C; after the substitution reaction, it is kept at 125°C and a constant pressure of 0.8Mpa for 14 hours; after the heat preservation, it is separated Tribromoneopentyl alcohol esterification, adding methanol and hydrobromic acid to the tribromoneopentyl alcohol esterification under the pressure of 0.6Mpa to carry out constant pressure ester decomposition, the amount of methanol is 1.4 times the weight of pentaerythritol, and the amount of hydrobromic acid is pentaerythritol 4% by weight, the consta...

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Abstract

The invention discloses a synthesizing method of tribromo-neoamyl alcohol, which comprises the following steps: aerating hydrogen bromide into pentaerythrite to substitute; insulating; separating tribromo-neoamyl alcohol ester; adding carbinol and inorganic acid into tribromo-neoamyl alcohol to do ester decomposition under 0.4-0.6Mpa; insulating under 0.6-0.8Mpa after substituting; making the mass react completely; improving product property obviously.

Description

technical field [0001] The invention relates to a synthesis method and a refining method of tribromoneopentyl alcohol. Background technique [0002] Due to pollution reasons, the use of pentabromodiphenyl ether in flame retardants used in plastics, electronic products, home appliances, coatings and other industries will be completely stopped globally, while tribromoneopentyl alcohol contains about 73% fatty bromine and has high bromine content and special stability, heat resistance, hydrolysis resistance and light stability are particularly outstanding. As a reaction intermediate of high molecular weight flame retardants, tribromoneopentyl alcohol is the best substitute for pentabromodiphenyl ether. The existing preparation method of tribromoneopentyl alcohol is to dissolve pentaerythritol in acetic acid, then raise the temperature and feed quantitative hydrogen bromide, heat preservation reaction under normal pressure, carry out ester decomposition under normal pressure aft...

Claims

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Application Information

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IPC IPC(8): C07C29/62C07C31/42C07C31/36
Inventor 柯建君田青芝
Owner 宜兴市中正化工有限公司
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