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Method for continuously preparing epichlorohydrin by glycerine reaction fractional distillation

An epichlorohydrin, reactive distillation technology, applied in chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, organic chemistry, etc. The effect of mild reaction conditions and high water content

Inactive Publication Date: 2009-01-07
JIANGSU POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The optimal concentration of the homogeneous acetic acid catalyst is about 1-2% by weight; at higher concentrations, unwanted by-products will be formed to a greater extent, which will reduce the yield

Method used

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  • Method for continuously preparing epichlorohydrin by glycerine reaction fractional distillation
  • Method for continuously preparing epichlorohydrin by glycerine reaction fractional distillation
  • Method for continuously preparing epichlorohydrin by glycerine reaction fractional distillation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] 300g glycerol, 3g oxalic acid and 1.5g ZnCl 2 , 0.75gFeCl 2 , 0.75g CuCl, 0.3g benzoyl peroxide, and 0.3g hydroquinone are added intermittently or continuously from the top of the chlorination reaction tower, and 450g of dried hydrogen chloride is introduced from the bottom of the tower to control the reaction temperature at 105°C. The chlorinated mixed liquid is sent to the degassing tower to release hydrogen chloride, rectified under reduced pressure, and tracked and detected by gas chromatography. The fraction collected at 68~75°C (1.87KPa) is 1,3-dichloro-2-propanol and 2,3 -The mixture of dichloro-1-propanol, and then carry out saponification and cyclization with 450g NaOH solution of 10% mass concentration in the saponification reaction tower to obtain 216g of epichlorohydrin product. The basic parameters and results described are shown in the table below:

[0068]

Embodiment 2

[0070] 300g glycerin, 4.5g malonic acid and 2g ZnCl 2 , 0.5gFeCl 3 , 0.5gTiCl 4, 0.45g of benzoyl peroxide, and 0.45g of hydroquinone are added intermittently or continuously from the top of the chlorination reaction tower, and 462g of dried hydrogen chloride is introduced from the bottom of the tower, and the reaction temperature is controlled at 108°C. The liquid is sent to the degassing tower to release hydrogen chloride, rectified under reduced pressure, tracked and detected by gas chromatography, and the fraction collected at 68~75°C (1.87KPa) is 1,3-dichloro-2-propanol and 2,3-dichloro - the mixture of 1-propanol, and then carry out saponification and cyclization with 430g NaOH solution of 15% mass concentration in the saponification reaction tower to obtain 220g of epichlorohydrin product. The basic parameters and results described are shown in the table below:

[0071]

Embodiment 3

[0073] 500g glycerol, 10g succinic acid and 5gZnCl 2 , 1.25gFeCl 2 , 1.25gKCl, 0.75g benzoyl peroxide, and 0.75g hydroquinone are added intermittently or continuously from the top of the chlorination reaction tower, and 450g of dried hydrogen chloride is introduced from the bottom of the tower to control the reaction temperature at 105°C. The chlorinated mixed liquid is sent to the degassing tower to release hydrogen chloride, rectified under reduced pressure, and tracked and detected by gas chromatography. The fraction collected at 68~75°C (1.87KPa) is 1,3-dichloro-2-propanol and 2,3 -The mixture of dichloro-1-propanol, then carry out saponification and cyclization with 550g NaOH solution of 20% mass concentration in the saponification reaction tower to obtain 360g of epichlorohydrin product. The basic parameters and results described are shown in the table below:

[0074]

[0075]

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Abstract

The invention relates to a method for preparing epoxy chloropropane which is obtained through successive reaction and distillation coupling technology after glycerine that is the by-product of biological diesel oil reacts with chlorine hydride through substitution reaction under homogeneous multielement catalysis and further performs saponification cyclization reaction. The method comprises the following steps: (1) chlorine hydride is pumped in glycerine that is the by-product of biological diesel oil for reaction under homogeneous multielement catalysis, and the mixture composed of 1, 3-dichloro-2-propanol and 2, 3-dichloro-1-propanol is prepared through the technologies of continuous feeding, continuous catalyzed chlorination and continuous rectification; (2) the isomeride mixture solution of 1, 3-dichloro-2-propanol and 2, 3-dichloro-1-propanol performs the saponification cyclization to generate a product of epoxy chloropropane in alkaline solution. The method has the advantages of mild reaction condition is mild, high catalyst activity, dedicated catalytic performance, high product selectivity, process 'cleaning', easy separation, continuous operation, environment-friendliness, etc.

Description

technical field [0001] The invention relates to a production process of epichlorohydrin, in particular to a method for preparing epichlorohydrin from biodiesel by-product glycerin through continuous catalytic chlorination, reactive distillation and saponification. Background technique [0002] As a "petroleum plant" with great potential for green and clean alternative fuels in the 21st century, biodiesel has shown a strong development trend in the field of fossil fuel substitutes due to its renewability and good environmental friendliness. widespread attention. At present, with the rise of a new round of biodiesel technology using renewable biomass as raw material, the sustainable development of its downstream industries has gradually become a research hotspot, and the research on deep processing technology of biodiesel by-product glycerol is in the ascendant all over the world. [0003] During the production of biodiesel, a large amount of glycerin is produced by-product, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/24C07D303/08B01J31/04
CPCY02P20/52
Inventor 张跃严生虎刘建武
Owner JIANGSU POLYTECHNIC UNIVERSITY
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