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Production method of dichloropropanol

A technology of dichloropropanol and its production method, which is applied in the chemical industry and can solve the problems of increased investment in equipment, increased energy consumption, and ignorance of effective effects, etc.

Active Publication Date: 2010-08-18
NINGBO HUANYANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Higher pressure results in increased energy consumption and increased equipment investment
[0017] 3. The existing technology ignores the effective effect of "mechanical dispersion" of hydrogen chloride gas in the reaction liquid medium, so the conversion rate of hydrogen chloride is very low
However, due to the removal of water by evaporation, the pseudo-azeotropic composition of the reaction liquid will take away useful organic matter at the same time

Method used

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  • Production method of dichloropropanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0105] A tank reactor made of glass-lined carbon steel, with a volume of 11 liters and an inner diameter of 200 mm. The reactor is equipped with a steam heating or water cooling jacket, a magnetically driven stirrer, and the impeller is a six-bladed disc turbine. The blade end distance is 55mm, the motor input power is 22W, the reactor is equipped with a pressure gauge interface and a thermocouple temperature gauge interface, a microwave generator, an inlet for adding raw and auxiliary materials, an exhaust outlet on the top, a liquid outlet on the bottom, and a gaseous HCl nozzle . The raw material gaseous HCl is supplied by gasification of liquefied HCl with a purity of 99.8% in a high-pressure steel gas cylinder, and the supply of HCl is weighed by an electronic scale and measured by a cylinder reduction method.

[0106] 5000 g (54.29 moL) of glycerin and 325 g (2.22 moL) of adipic acid were added to Reactor 1. Under slow stirring and mixing, use industrial steam to pass t...

Embodiment 2

[0133] A low-boiler distillation column (15) with a heating kettle is connected in series with a dichloropropanol product rectification column (16), and the top of the rectification column is equipped with a condenser and a phase separator. , the aqueous phase is refluxed, and the organic phase is the product of dichloropropanol.

[0134] The reaction solution weighing after the reaction of embodiment 1 finishes, gets 9961.5g, and its main component quantity is shown in table 5

[0135] table 5

[0136] components

Weight (g)

The reaction solution

9961.5

3-Chloro-1.2-propanediol

2-Chloro-1.3-propanediol

1.3-Dichloro-2-propanol

2.3-Dichloro-1-propanol

Adipic acid

Adipate

water

hydrogen chloride

other

150.5

164.2

6346.6

157.3

211.3

171.5

1882.7

806.9

70.5

[0137] The reaction solution was continuously sent to the low boilers for distillation, distilled under normal pressu...

Embodiment 3

[0146] Take 2215.7 g of the still feed liquid of the product column (16) obtained in the embodiment of the present invention, and its composition is shown in Table 9.

[0147] Table 9

[0148] composition

[0149] 2215.7 g of the still feed liquid is added to the reactor described in Example 1 of the present invention, and 4000 g (43.44 mol) of glycerin and 24 g (0.164 mol) of adipic acid are added, and the pressure and temperature as described in Example 1 are carried out in three stages Reaction, the first section of reaction took 76 minutes, the second section of reaction took 70 minutes, and the third section of reaction took 64 minutes, the total reaction time was 210 minutes, and a total of 3773.5g (103.5mol) of hydrogen chloride was introduced.

[0150] At the end of the reaction, 10040.9 g of the reaction solution was obtained, and its composition is shown in Table 10.

[0151] Table 10

[0152] composition

[0153] The reaction solution was conti...

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Abstract

The invention relates to a production method of dichloropropanol, comprising the following reaction steps: glycerol reacts with gaseous HCl in the presence of organic carboxylic acid catalyst, reaction liquid reactant reacts with gaseous HCl in the presence of Lewis acid catalyst and then reacts with gaseous HCl again under the action of microwave and the stirring action; after passing through a low-boiling-point substance distillation tower and a rectifying tower, the mixture is prepared into the product of the invention. Compared with the prior art, HCl conversion rate is improved by about one time. When the combined catalysis technology of the invention is adopted, the dosage of the organic carboxylic acid catalyst is lowered by half, glycerol conversion rate is improved by 2%, and product yield is improved by 5%; and meanwhile, side reaction is reduced so as to avoid the defect that extra potentially toxic organic carboxylic acid side reaction generates a great quantity of waste, thus protecting environment.

Description

【Technical field】 [0001] The invention belongs to the technical field of chemical industry. More particularly, the present invention relates to a kind of production method of dichloropropanol. 【Background technique】 [0002] The invention relates to a production method for producing mainly 1,3-dichloro-2-propanol isomers through nucleophilic substitution reaction of renewable raw material glycerin and gaseous hydrogen chloride. Dichloropropanol is used to produce epichlorohydrin, and epichlorohydrin is the raw material for producing epoxy resin. Epoxy resin is mainly used in electronics, electrical industry, building materials, new materials, wind power equipment, epichlorohydrin is also used It is used in the production of surfactants and synthetic rubber, and is widely used in the fields of daily chemical and light industry technology. [0003] At present, traditional epichlorohydrin is prepared from dichloropropanol produced from propylene extracted from petroleum. [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/36C07C29/62
Inventor 施德龙车学兵沈作伟宋玉平符林健董平金敬燕周秋生高兵强
Owner NINGBO HUANYANG CHEM
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