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Preparation method for co-production of 1,3-dichloropropanol and potassium formate

A technology of dichloropropanol and potassium formate, which is applied in the preparation of carboxylate, carboxylate, and organic compounds, and can solve the problems of no published patent documents, difficulty in realizing added value, and difficult separation of by-products. , to achieve the effects of weakening restrictions on raw material sources, high added value of products, and low cost

Inactive Publication Date: 2019-04-19
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are two main production methods of dichloropropanol in China: 1. Propylene is chlorinated at high temperature and chloropropene is hypochlorinated in series. This method has low yield, large equipment corrosion, and many by-products. The amount of sewage in the production process is large; 2. It is prepared by reacting glycerin with hydrogen chloride in the presence of glacial formic acid. Produce a large amount of 1,2-dichloropropanol, resulting in low yield, only about 60%, high cost and serious pollution
Moreover, the by-products are not easy to separate, and it is difficult to achieve the purpose of adding value
[0004] Through the search of published patent documents, no published patent documents identical to this patent application have been found

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A preparation method for the co-production of potassium formate by 1,3-dichloropropanol, characterized in that potassium chloride is dissolved in a potassium formate solution with a concentration of 0.002mol / L to prepare a saturated potassium chloride mixed solution; Then stir and mix the mixed solution of epichlorohydrin and saturated potassium chloride, and keep the temperature at 5°C; then slowly add formic acid to it for reaction within 4 hours, after the drop is completed, continue to stir under normal pressure React for 24 hours; after the reaction is completed, after standing and stratifying, collect the product potassium formate solution and 1,3-dichloropropanol solution distributed in the upper and lower layers.

Embodiment 2

[0022] A preparation method for the co-production of potassium formate by 1,3-dichloropropanol, characterized in that potassium chloride is dissolved in a potassium formate solution with a concentration of 0.014mol / L to prepare a saturated potassium chloride mixed solution; Then stir the mixed solution of epichlorohydrin and saturated potassium chloride, and keep the temperature at 50°C; then slowly add formic acid to it for reaction within 12 hours, after the dropwise addition, under the pressure of 1MPa, continue The reaction was stirred for 16 hours; after the reaction was completed, after standing and stratifying, the product potassium formate solution and 1,3-dichloropropanol solution distributed in the upper and lower layers were collected.

Embodiment 3

[0024] A preparation method for the co-production of potassium formate with 1,3-dichloropropanol, characterized in that potassium chloride is dissolved in a potassium formate solution with a concentration of 0.035mol / L to prepare a saturated potassium chloride mixed solution; Then stir the mixed solution of epichlorohydrin and saturated potassium chloride, and keep the temperature at 95°C; then slowly add formic acid to it for reaction within 18 hours, after the dropwise addition, under the pressure of 2MPa, continue Stir and react for 8 hours; after the reaction is completed, after standing and stratifying, collect the product potassium formate solution and 1,3-dichloropropanol solution distributed in the upper and lower layers.

[0025] Strictly speaking, the separated lower layer solution is a mixture of 1,3-dichloropropanol and 2,3-dichloropropanol, but since the content of 2,3-dichloropropanol is less than 1%, it can be ignored here .

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PUM

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Abstract

The invention relates to a preparation method for co-production of 1,3-dichloropropanol and potassium formate, the preparation method is characterized in that: mixing epoxy chloropropane with a saturated potassium chloride solution or a saturated potassium chloride mixed solution, and maintaining the mixture at a certain reaction temperature; then slowly dropwise adding formic acid to the mixturein specified time to carry out a reaction, and continuously reacting at a certain reaction pressure for a certain reaction time; after the reaction is finished, performing standing and layering, and respectively collecting products of a potassium formate solution and a 1,3-dichloropropanol solution which are distributed respectively on the upper layer and the lower layer. The method is scientificand reasonable in design, high in yield and high in purity, the corrosion of equipment is small, byproducts are few, the cost is low, the pollution is small, the additional value is high in, and the preparation method for co-production of the 1,3-dichloropropanol and the potassium formate is high in innovation.

Description

technical field [0001] The invention belongs to the field of methods for producing fine chemicals, and relates to a preparation method of 1,3-dichloropropanol, in particular to a preparation method of co-producing potassium formate from 1,3-dichloropropanol. Background technique [0002] 1,3-Dichloropropanol, also known as dichloroglycerin, is mainly used as a solvent and in organic synthesis. It is the synthetic antiviral drug "ganciclovir" (used to treat organ transplant virus infection, AIDS, etc.), histamine H2 receptor antagonist famotidine, antifungal drug fluconazole, 1,3-dichloroacetone, cross-linking agent, demulsifier, water treatment agent and other chemical products are also used in the manufacture of epoxy resin , ion exchange resin, etc. Potassium formate is mainly used to prepare water-bearing oil well injection fluid, etc. [0003] At present, there are two main production methods of dichloropropanol in China: 1. Propylene is chlorinated at high temperature...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/62C07C31/36C07C51/41C07C53/06
CPCC07C29/62C07C51/412C07C31/36C07C53/06
Inventor 鲁林平李俊秀张博阳郭帆
Owner TIANJIN UNIVERSITY OF TECHNOLOGY