Synthesis method for 2,3-dibromo-1,4-butylene glycol

A technology of butene diol and synthesis method, which is applied in the separation/purification of hydroxyl compounds, organic chemistry, and the preparation of halogens, which can solve the problems of reduced yield, product process loss, low temperature and difficult suction filtration, etc., and achieve reduction The loss of solvent, beneficial to recycling, the effect of simple and easy method

Inactive Publication Date: 2019-06-14
SHANDONG RUNKE CHEM
View PDF4 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In addition, at present, the domestic production of 2,3-dibromo-1,4-butenediol production process, due to the addition reaction will produce a large number of exothermic reactions, generally rely on freezing and cooling for a cycle of 24 hours, and the temperature in the middle is difficult to control. High cost, poor appearance, low main content
The commonly used production process is to use 1,4 butynediol and bromine addition reaction conditions, the temperature is about 15 ℃, water is used as the solvent, and the reaction time is about 24 hours. Due to the high temperature of the reaction process, the temperature is difficult to control. Bromine It belongs to the amplification of tail gas emission, the crude product is not reused after dehydration, serious environmental pollution, low production efficiency, high cost and poor product performance
Moreover, most of the

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A method for synthesizing 2,3-dibromo-1,4-butenediol, comprising the following steps:

[0029] 1) Preparation of brominating agent tetraethylammonium bromide complex bromide:

[0030] In a four-necked flask equipped with an electric stirrer and a thermometer, add 150ml of dichloromethane, add 110g of tetraethylammonium bromide, add 82.4g of liquid bromine dropwise while stirring, and react for 1 hour until the reaction is complete. Brominating agent tetraethylammonium bromide complex bromide;

[0031] 2) Preparation of crude 2,3-dibromo-1,4-butenediol:

[0032] In the dichloromethane solvent, add butynediol and the brominating agent tetraethylammonium bromide complex bromide prepared in step 1) to undergo electrophilic addition reaction to generate 2,3-dibromo-1,4 -butenediol; wash with water, lower the temperature to crystallize 2,3-dibromo-1,4-butenediol, and filter to obtain 2,3-dibromo-1,4-butenediol Crude product: the mol ratio of the butynediol added in the ste...

Embodiment 2

[0036] 3) Purification of crude 2,3-dibromo-1,4-butenediol:

[0037] In a four-neck flask equipped with a condenser tube, an electric stirrer, and a thermometer, add the crude 2,3-dibromo-1,4-butenediol obtained in step 2) and 250 g of water, start stirring, and raise the temperature to control the temperature Stir at 80-90°C to dissolve the material completely, add 6g of sodium sulfite to remove residual bromine, add 5g of activated carbon for decolorization treatment: the decolorization process is 80-90°C and heat preservation reaction for 1.5 hours, heat suction filtration, and cool the filtrate to 0-5 °C, recrystallize the purified 2,3-dibromo-1,4-butenediol, filter it with suction, and dry the filter cake under vacuum at room temperature to obtain pure white 2,3-dibromo-1,4- Butenediol; bromine content 64.97%, yield 80%, purity 99.4%.

Embodiment 3

[0039] Mother liquor all reclaims and applies mechanically the method for synthesizing 2,3-dibromo-1,4-butenediol, comprises the following steps:

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a synthesis method for 2,3-dibromo-1,4-butylene glycol. The invention aims to solve the technical problems of the prior art that the synthesis method for 2,3-dibromo-1,4-butylene glycol is complex, reaction conditions are harsh and unsafe, parameters are difficult to be controlled, production cost is high, product quality is low and use is limited. The synthesis method for2,3-dibromo-1,4-butylene glycol disclosed by the invention comprises the following steps: 1) adding a catalyst tetraethyl ammonium bromide into a dichloromethane solvent, and then dropwise adding liquid bromine while stirring, thereby acquiring a brominating agent tetraethyl ammonium bromide complex bromide; 2) adding butynediol into the dichloromethane solvent, triggering electrophilic addition reaction with the brominating agent tetraethyl ammonium bromide complex bromide prepared in the step 1), thereby generating 2,3-dibromo-1,4-butylene glycol; adding water for washing, cooling, separating 2,3-dibromo-1,4-butylene glycol crystal, and performing suction filtration, thereby acquiring a crude product of 2,3-dibromo-1,4-butylene glycol; 3) purifying the crude product of 2,3-dibromo-1,4-butylene glycol. The synthesis method provided by the invention can be widely applied to the technical field of chemical synthesis.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis method of 2,3-dibromo-1,4-butenediol. Background technique [0002] Polymer materials have been widely used in various fields of the national economy and in all aspects of people's lives. However, most polymer materials are combustible or combustible materials, and major fires are mainly caused by the ignition of polymer materials. Therefore, the research and development of high-quality, high-performance flame retardants has received increasing attention. [0003] 2,3-dibromo-1,4-butenediol is widely used in organic synthesis, pharmaceutical intermediates, used as a surfactant in the production of flux and solder paste, with high resistance and strong activity. Bright spots and full soldering have a certain effect; it is the best surface-active additive among all fluxes, and is widely used in high-precision electronic components as high-end env...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C33/42C07C29/62C07C29/76C07C29/78
Inventor 王东全吴多坤秦善宝张君营孙盛元
Owner SHANDONG RUNKE CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap