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Preparation method of dichloropropanol

A dichloropropanol, a catalytic preparation technology, applied in the field of fine chemistry, can solve problems such as the inability to directly use salty crude glycerin, high catalyst dosage, and influence on reaction yield, and achieve excellent thermal stability, catalytic activity, and catalytic activity High, to avoid the effect of polycondensation reaction

Pending Publication Date: 2022-03-15
山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The amount of catalyst used in this method is as high as 43.8%, so the cost is high, and the catalyst is easy to generate esterification with glycerol
[0006] At present, the reaction of glycerin chlorination to synthesize dichloropropanol also has the following problems: (1) can not directly use salty crude glycerol as a raw material, and this type of glycerol is the most common in by-product glycerol, and the use of salty crude glycerin can greatly Reduce the cost of raw materials; (2) Catalysts with good comprehensive performance such as high activity, high selectivity, and easy recycling need to be further developed, especially catalysts that can selectively generate 1,3-dichloropropanol
(3) Effective utilization of hydrochloric acid wastewater generated by glycerin chlorination; (4) By-products such as polyglycerol are easily generated in the later stage of glycerin chlorination, which affects the reaction yield

Method used

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  • Preparation method of dichloropropanol
  • Preparation method of dichloropropanol
  • Preparation method of dichloropropanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The preparation of dichloropropanol is as follows:

[0036] (1) Catalyst preparation

[0037] Weigh 146.16g (1mol) of adipic acid, 39.92g (0.25mol) of iron oxide and 40.69g (0.5mol) of zinc oxide into the reactor, add 350g of water and heat to reflux for 3h, remove most of the water under reduced pressure and filter to obtain brown solid. The solid was vacuum-dried and ground to obtain a total of 196.5 g of composite catalysts.

[0038] (2) Take by weighing 9.21g (5%) of composite catalyst and 193.9g (2mol) of glycerol with a purity of 95%, add in reactor A equipped with stirring, temperature measuring, water separation device and reflux device, and take by weighing composite catalyst 9.21g and purity are 95% glycerin 193.9g (2mol), add in the reactor B that stirring, temperature measurement, reflux device and tail gas absorption device are equipped with;

[0039](3) Turn on the stirring, raise the temperature of both reactors A and B to 120°C, then feed hydrogen chl...

Embodiment 2

[0043] The preparation of dichloropropanol is as follows:

[0044] (1) Catalyst preparation

[0045] Weigh 146.17g (1mol) of adipic acid, 39.96g (0.25mol) of iron oxide, 20.37g (0.25mol) of zinc oxide and 12.80g (0.125mol) of aluminum oxide and place them in a reactor, add 350g of water and heat to reflux for 3h, After most of the water was removed under reduced pressure, a brown solid was obtained by filtration. The solid was vacuum-dried and ground to obtain a total of 191.9 g of composite catalysts.

[0046] (2) Take by weighing 5.53g (3%) of the composite catalyst and 193.9g (2mol) of glycerol with a purity of 95%, add in the reactor A equipped with stirring, temperature measuring, water separation device and reflux device, and take the composite catalyst in addition 5.53g and purity are 95% glycerin 193.9g (2mol), add in the reactor B that stirring, temperature measurement, reflux device and tail gas absorption device are equipped with;

[0047] (3) Turn on the stirrin...

Embodiment 3

[0051] The preparation of dichloropropanol is as follows:

[0052] (1) Catalyst preparation

[0053] Weigh 146.16g (1mol) of adipic acid, 39.96g (0.25mol) of iron oxide, 8.14g (0.10mol) of zinc oxide and 20.39g (0.20mol) of aluminum oxide and place them in a reactor, add 350g of water and heat to reflux for 3h, After most of the water was removed under reduced pressure, a brown solid was obtained by filtration. The solid was vacuum-dried and ground to obtain a total of 183.3 g of composite catalysts.

[0054] (2) Take by weighing 18.42g (10%) of composite catalyst and 204.6g (2mol) of glycerol with a purity of 90%, add in reactor A equipped with stirring, temperature measuring, water separation device and reflux device, and take composite catalyst 18.42g and purity are 204.6g (2mol) of glycerol of 90%, add in the reactor B that stirring, temperature measurement, reflux device and tail gas absorption device are equipped with;

[0055] (3) Turn on the stirring, raise the temp...

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Abstract

The invention relates to a preparation method of dichloropropanol, and belongs to the technical field of fine chemistry. According to the method, glycerol with the purity of 50%-99.5% is used as a raw material, hydrogen chloride or hydrochloric acid is used as a chlorinating agent, and 1, 3-dichloropropanol is prepared through catalysis under the catalysis of a composite catalyst; the composite catalyst is obtained by reacting binary acid with metal oxide. According to the invention, the composite catalyst of binary acid and metal oxide is used as the catalyst for synthesizing dichloropropanol for the first time. The multi-component composite catalyst has the advantages of cheap and easily available raw materials, simple preparation method, good stability in air, and convenient transportation and storage; the catalyst has the advantages of high catalytic activity and good selectivity, the conversion rate of glycerol is 100%, the highest yield of dichloropropanol can reach 98.5%, and the selectivity of 1, 3-dichloropropanol can reach 98.4%; the catalyst is good in thermal stability, and the catalytic activity is kept unchanged when the catalyst is continuously used at 130 DEG C for 120 hours.

Description

technical field [0001] The invention belongs to the technical field of fine chemistry, and in particular relates to a preparation method of dichloropropanol. Background technique [0002] Epichlorohydrin is an important organic chemical raw material and fine chemical product, which is widely used in the production of epoxy resin, chlorohydrin rubber, glycidyl ether, etc. With the continuous improvement of people's living standards, the demand for epichlorohydrin in various industries continues to expand. The traditional synthesis methods of epichlorohydrin mainly include propylene high-temperature chlorination method and propylene acetate method, both of which use propylene as raw material. With the soaring price of international oil, the traditional method of producing epichlorohydrin has been severely impacted. [0003] my country is a big oil user. According to incomplete statistics, my country produces about 10 million tons of waste oil every year. These waste oils ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/62C07C29/82C07C29/86B01J31/04B01J31/28B01J31/26
CPCC07C29/62C07C29/82C07C29/86B01J31/04B01J31/28B01J31/26C07C31/36Y02P20/584
Inventor 王良广唐计光郜婷婷徐伟伟尹超
Owner 山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心
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