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Synthetic method and refining for dibromoneopentyl glycol

A technology of dibromoneopentyl glycol and synthesis method, which is applied in the field of synthesis of dibromoneopentyl glycol, can solve problems such as low product yield, high reaction temperature, and difficult separation, and achieve high product yield and high reaction temperature. low effect

Inactive Publication Date: 2010-09-01
宜兴市中正化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production process of dibromoneopentyl glycol is to adopt pentaerythritol to react with liquid hydrobromic acid or pentaerythritol to directly react with gaseous hydrogen bromide. The former reaction temperature is high, and the content of dibromoneopentyl glycol in the crude product formed after About 67%, product yield is low, energy consumption is high, and tar is produced; A mixture of pentanols, the content of dibromoneopentyl glycol in the crude product is generally 73%, it is difficult to separate, and the yield is also low

Method used

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  • Synthetic method and refining for dibromoneopentyl glycol
  • Synthetic method and refining for dibromoneopentyl glycol
  • Synthetic method and refining for dibromoneopentyl glycol

Examples

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Effect test

Embodiment 1

[0013] Embodiment 1, the synthetic method of dibromoneopentyl glycol, pentaerythritol is carried out esterification reaction with the acetic acid of concentration above 98%, the addition weight of acetic acid is 1.1 times of pentaerythritol weight, reflux esterification reaction 5 hours; Esterification After the reaction, the esterified product is separated by dehydration and acid distillation, the time of dehydration and acid distillation is 3.5 hours, and the temperature is 115°C; then the esterified product is dissolved with acetic acid with a concentration of more than 98%. 0.9 times, hydrogen bromide gas was introduced to carry out the substitution reaction at 85 ° C, the amount of hydrogen bromide introduced was 1.2 times the weight of pentaerythritol, the aeration time was 4 hours, and then kept at 95 ° C under normal pressure for 3.5 hours; separated after heat preservation Go out the diester of dibromoneopentyl glycol, carry out constant pressure ester decomposition un...

Embodiment 2

[0014] Embodiment 2, the synthetic method of dibromoneopentyl glycol, pentaerythritol is carried out esterification reaction with the acetic acid of concentration above 98%, the addition weight of acetic acid is 1.2 times of pentaerythritol weight, reflux esterification reaction 4 hours; Esterification After the reaction, the esterified product is separated by dehydration and acid distillation, the time of dehydration and acid distillation is controlled at 2.5 hours, and the temperature is 125°C; then the separated ester product is dissolved with acetic acid with a concentration above 98%, and the amount of acetic acid added is 1.1 times the weight, hydrogen bromide gas was introduced to carry out the substitution reaction at 105°C, the amount of hydrogen bromide introduced was 1.1 times the weight of pentaerythritol, the ventilation time was 4.5 hours, and then kept at 100°C under normal pressure for 4.5 hours; Separate the diester compound of dibromoneopentyl glycol afterward...

Embodiment 3

[0015] Embodiment 3, the synthetic method of dibromoneopentyl glycol, pentaerythritol is carried out esterification reaction with the acetic acid of concentration above 98%, the addition weight of acetic acid is 1.3 times of pentaerythritol weight, reflux esterification reaction 6 hours; Esterification After the reaction, separate the esterified product by dehydrating and distilling acid, the time of dehydrating and distilling acid is controlled to 3 hours, and the temperature is 120°C; then dissolve the separated esterified product with acetic acid with a concentration of more than 98%, and the amount of acetic acid added is 0.7 times of the weight, hydrogen bromide gas was introduced to carry out the substitution reaction at 95°C, the amount of hydrogen bromide introduced was 1.25 times the weight of pentaerythritol, the ventilation time was 5 hours, and then kept at 90°C under normal pressure for 5.5 hours; heat preservation Separate the diester of dibromoneopentyl glycol af...

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Abstract

The invention discloses a synthesizing method of dibromide-neopentyl glycol, which comprises the following steps: esterifying pentaerythritol and acetic acid with density over 98%; dissolving and separating ester the acetic acid; aerating hydrogen bromide to substitute; insulating to separate diester of dibromide-neopentyl glycol; proceeding constant pressure decomposition through carbinol and inorganic acid under 0.4-0.6Mpa.

Description

technical field [0001] The invention relates to a method for synthesizing dibromoneopentyl glycol, and simultaneously provides a method for refining the crude product of dibromoneopentyl glycol obtained through synthesis. Background technique [0002] Dibromoneopentyl glycol is a new type of bromine-containing flame retardant. It can be used as one of the monomers in the reaction to prepare flame-retardant unsaturated polyester, polyurethane, etc., and can also be directly added to high molecular weight polyethylene, polyurethane, etc. In expanded polystyrene; as an additive flame retardant, due to its structural characteristics, the products made have excellent flame retardancy, significant light stability and excellent UV resistance, especially transparent flame retardant products that can be used outdoors for a long time The property of not fading under sunlight is unmatched by other flame retardants. At present, the production process of dibromoneopentyl glycol is to ad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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