Method for synthesizing dichloropropanol by catalyzing glycerol for chlorination under existence of dicarboxylic acid-rare earth chloride

A rare earth chloride, dichloropropanol technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, chemical/physical process, etc., can solve the large loss of hydrogen chloride and increase the separation device , low utilization rate of equipment, etc., to achieve the effect of high activity, high reaction efficiency, and high utilization rate of hydrogen chloride

Active Publication Date: 2010-05-12
SHANDONG TIANCHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the use of a large amount of organic solvents in this method, there are disadvantages such as low utilization rate of equipment, large loss of hydrogen chloride and additional separation devices.

Method used

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  • Method for synthesizing dichloropropanol by catalyzing glycerol for chlorination under existence of dicarboxylic acid-rare earth chloride
  • Method for synthesizing dichloropropanol by catalyzing glycerol for chlorination under existence of dicarboxylic acid-rare earth chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0029]Add 650Kg glycerin (99.5%, W / W), 66Kg adipic acid (99%, W / W) and 0.65Kg cerium trichloride respectively in volume 1000L reactor R-1, R-2 and R-3, When the content of R-1 is heated to 100°C, hydrogen chloride gas is introduced under stirring, and at 100-120°C for 15 hours, a total of 1300Kg is introduced. After V-1 is received, hydrogen chloride tail gas is passed into R-2. After the chlorination reaction of R-1 is completed, dichloropropanol is distilled off under reduced pressure, and hydrogen chloride gas is passed into R-2 at the same time, and the generated water and part of dichloropropanol are Chloropropanol is stripped and distilled by hydrogen chloride. V-2 is received, and the hydrogen chloride tail gas of R-2 is passed into R-3. After R-1 dichloropropanol is evaporated under reduced pressure, add 500Kg glycerin and continue at 100-120°C Chlorination, start depressurizing to distill out the dichloropropanol of R-2 at this moment, feed hydrogen chloride gas to R-...

Embodiment 2

[0032] Equipment and method of operation are the same as in Example 1. 685Kg glycerol (95%, W / W), 66Kg adipic acid (99%, W / W) and 0.65Kg cerium trichloride were added. After ten cycles of production, the yield of dichloropropanol is 93% (calculated by the amount of glycerol).

Embodiment 3

[0034] Equipment and method of operation are the same as in Example 1. 650Kg glycerol (99.5%, W / W), 66Kg adipic acid (99%, W / W) and 0.65Kg lanthanum trichloride (99%, W / W) were added.

[0035] After ten cycles of production, the yield of dichloropropanol is 92% (calculated by the amount of glycerol).

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Abstract

The invention relates to a method for synthesizing dichloropropanol by catalyzing glycerol for chlorination under the existence of dicarboxylic acid-rare earth chloride, which comprises the following steps of: mixing glycerol and a dicarboxylic acid-rare earth chloride composite catalyst in a chloridizing reactor R-1, and then introducing chlorine hydride gas, constantly evaporating out water and partial dichloropropanol generated in the reactor; introducing chlorine hydride as a tail gas into a chloridizing reactor R-2 filled with the glycerol and the catalyst; after the chlorination of the reactor R-1 is ended, evaporating dichloropropanol by decompression and then adding the glycerol for further chlorination; during the distillation of the chloridizing reactor R-1, starting to introduce chlorine hydride into the chloridizing reactor R-2, and the chlorine hydride as the tail gas into a chloridizing reactor R-3, wherein the glycerol and the catalyst added into the chloridizing reactors R-1, R-2 and R-3 have the same dosage; after the chlorination of the chloridizing reactor R-2 is ended, repeating the procedures of distillation, feeding and chlorination in the chloridizing reactor R-1; connecting the chloridizing reactors R-1,R-2 and R-3 from head to tail, and introducing the chlorine hydride as the tail gas into the chloridizing reactor R-1 while introducing the chlorine hydride into the chloridizing reactor R-3; transferring a mixed liquor of the dichloropropanol, water and the chlorine hydride to a distillation still, and adding an organic solvent to remove water by azeotropy. The method has the advantages of high reaction speed, high utilization ratio of the chlorine hydride and high yield.

Description

1. Technical field [0001] The invention relates to a method and a reaction device for synthesizing dichloropropanol from glycerin. 2. Background technology [0002] Dichloropropanol is the precursor for the synthesis of epichlorohydrin. Epichlorohydrin is an important organic chemical raw material, which can be used in the synthesis of surfactants, medicines, pesticides, ion exchange resins, plasticizers, chlorohydrin rubber and many other products, and has a wide range of uses. The epoxy resin prepared from it has the characteristics of strong adhesion, chemical medium corrosion resistance and excellent dielectric properties. It is widely used in coatings, adhesives, reinforcing materials, wind turbine blades and other industries, and the consumption is huge. . my country is the largest producer and important consumer of epoxy resin in the world, and epichlorohydrin is mainly used in the production of epoxy resin. [0003] At present, there are mainly two industrial prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/36C07C29/62C07C29/80B01J31/26
Inventor 朱年德李保国
Owner SHANDONG TIANCHENG CHEM CO LTD
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