Method for preparing dichloropropanol by glycerol

A technology of dichloropropanol and glycerin, which is applied in the introduction of halogen preparation, organic chemistry, etc., can solve the problems of low equipment utilization, high process energy consumption, and low reaction rate, and achieve increased reaction rate, high content, and glycerin conversion high rate effect

Inactive Publication Date: 2008-05-21
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The gas-liquid reactants flow in reverse, the utilization rate of HCl is improved, and the water in the reaction system is taken away by the reaction gas itself, and the non-volatile catalyst is preferred, the catalyst consumption is small, but the process energy consumption is still high and the equipment utiliza

Method used

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  • Method for preparing dichloropropanol by glycerol
  • Method for preparing dichloropropanol by glycerol
  • Method for preparing dichloropropanol by glycerol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In the jet reactor, add 986g of industrial glycerol (91.9% by weight, 9.84mol) and 98g of adipic acid, the amount of catalyst is 9.9%, heat to 110°C, feed HCl gas to react, first pass 7.7mol HCl / h 2.05h, and then 3.18h at 3.3molHCl / h, a total of 24.4molHCl was introduced, and the molar ratio of glycerol to HCl gas was 1:2.5. During the reaction, the temperature was controlled at 115°C. The aeration time of hydrogen chloride was 5.23h, and 764g of chlorinated liquid was obtained, and 1134g of distillate was obtained by cooling during the reaction. The composition of the reaction product is:

[0032] Material name

Embodiment 2

[0034] Then embodiment 1 repeats test continuously 3 times, and condition is all the same with the condition of embodiment 1, does not emit at the bottom of the still, just adds industrial glycerin (91.9% by weight), and adds adipic acid and hydrogen chloride gas. The amount added is shown in the table below:

[0035] times

Industrial glycerin (g)

Adipic acid (g)

Hydrogen chloride (g)

the first time

1412

20

1445

the second time

845

0

770

the third time

1010

20

925

[0036] The composition of the reaction product is:

[0037] times

Embodiment 3

[0039] In the jet reactor, add 1200g industrial glycerin (91.9% by weight, 12.0mol) and 57.5ml (60.4g) of acetic acid, the amount of catalyst is 5.5%, heat to 110 ℃, pass into HCl gas to react, first with 3.3mol HCl / h was fed for 3 h, and then 1.7 mol HCl / h was fed for 5.9 h, a total of 19.8 mol of HCl gas was fed, and the molar ratio of glycerol to HCl gas was 1:1.6. During the reaction, the temperature was controlled at 115°C. The aeration time of hydrogen chloride was 8.9h, and 882g of chlorinated liquid was obtained, and 1102g of distillate was obtained by cooling during the reaction.

[0040] The composition of the reaction product is:

[0041] Material name

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Abstract

A method of preparing for dichloropropanol from glycerol is that the glycerol and catalyst are added into a spraying type reactor; a liquid circulating pump is used to pump the glycerol and the catalyst our from the spraying type reactor, then the glycerol and the catalyst are sent into the spraying type reactor from the top of the spraying type reactor by the manner of spraying; HCl gas which is absorbed from the lateral part of the spraying type reactor is mixed completely and react with the materials of the glycerol and the catalyst inside the spraying type reactor; at the same time the negative pressure produced by spraying brings a resultant inside the spraying type reactor in the form of an azeotropic matter of water, the dichloropropanol and the HCl; the water and the dichloropropanol in the azeotropic matter are condensed down by a condenser, and the unreacted HCl gas and the complementary HCl gas are sent into the spraying type reactor together for cyclic reaction. The invention has the advantages of the improvement of the reaction velocity and high glycerol transformation rate.

Description

technical field [0001] The invention belongs to a method for preparing dichloropropanol, in particular to a method for preparing dichloropropanol from glycerin. Background technique [0002] The main method of producing dichloropropanol at present is the propylene high-temperature chlorination method developed by U.S. Shell Company in 1948. The reaction principle is as follows: [0003] CH 2 =CH-CH 3 +Cl 2 →CH 2 =CH-CH 2 Cl+HCl [0004] CH 2 =CH-CH 2 Cl+Cl 2 +H 2 O→CH 2 Cl-CHOH-CH 2 Cl+CH 2 Cl-CHCl-CH 2 Oh [0005] The method is characterized by flexible production process, mature process, stable operation, and the production of various organic intermediates, but has disadvantages such as low conversion rate, many by-products, high energy consumption, serious equipment corrosion, and many waste water and waste residues. [0006] Another less-applied process is the propylene acetate method, and the reaction principle is as follows: [0007] [0008] [0...

Claims

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Application Information

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IPC IPC(8): C07C31/36C07C29/62
Inventor 康保安王勒孙晋源武华萍
Owner CHINA RES INST OF DAILY CHEM IND
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