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A kind of method preparing dichloropropanol by glycerol

A technology of dichloropropanol and glycerol, applied in the introduction of halogen preparation, organic chemistry and other directions, can solve problems such as the utilization rate of equipment affecting the reaction rate, and achieve the improvement of the reaction rate and HCl utilization rate, the simplification of the reaction process, and the improvement of the rate and HCl. The effect of utilization

Inactive Publication Date: 2011-12-07
WANHUA CHEM GRP CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has improved in terms of reactor combination, but the reactor used still retains the bubbling tank, so it directly affects the reaction rate and the utilization rate of equipment per unit volume.

Method used

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  • A kind of method preparing dichloropropanol by glycerol
  • A kind of method preparing dichloropropanol by glycerol
  • A kind of method preparing dichloropropanol by glycerol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Such as figure 1 As shown, the mixture of glycerol (99% by mass industrial product) and acetic acid (wherein the acetic acid catalyst accounts for 4% of the total mass of glycerol) is first mixed uniformly in the mixer 1, and then the above-mentioned mixture is fed at a rate of 1mol / h The pump 9 feeds the material into the tank reactor 2, HCl gas is passed into the tank reactor 2 at 1.5 mol / h, and the reaction residence time of the above-mentioned materials in the tank reactor 2 is 3 h. Sampling by the sampling valve 18 for gas chromatographic analysis shows that the conversion rate of glycerin is 88.2%, the generation rate of monochloropropanediol is 79.3%, and the generation rate of dichloropropanol is 6.8%.

[0029]The reaction liquid from the tank reactor 2 is pumped to the preheater 13 through the discharge pump 10, heated to a specified temperature of 80° C. through the preheater 13, and then pumped through the pump (not shown in the figure) to the reactive rectif...

Embodiment 2

[0035] The mixture of glycerin (99% by mass) and acetic acid is first mixed uniformly in the mixer 1, and then fed to the tank reactor 2 through the feed pump 9 at 1mol / h, and HCl gas is fed into the tank reactor at 1.5mol / h. Reactor 2, the reaction residence time is 5h. Samples are taken through sampling valve 18 for gas chromatographic analysis. It can be seen that the conversion rate of glycerin is 93.2%, the production rate of monochloropropanediol is 87.3%, and the production rate of dichloropropanol is 7.9%. All the other operations are the same as in Example 1.

[0036] Within 3 hours of steady-state operation, 3 mol of glycerol and 7.5 mol of HCl were fed, and glycerol was almost completely converted. The condensate collected from the top of reactive distillation column 3 was 111.2 g, and the amount collected from the top of purification distillation column 4 was 342.7 g. Dichloropropanol yield is 82.1% (shown in Table 1).

Embodiment 3

[0038] The mixture of glycerol (99% by mass) and adipic acid (wherein the adipic acid catalyst accounts for 4% of the total mass of glycerol) is first mixed uniformly in mixer 1, and then fed to 1.5 mol / h through feed pump 9 to In the tank reactor 2, HCl gas is passed into the tank reactor 2 at 1.5mol / h, and the reaction residence time is 3h. Samples are taken through sampling valve 18 for gas chromatographic analysis. It can be seen that the conversion rate of glycerin is 92.4%, the production rate of monochloropropanediol is 82.7%, and the production rate of dichloropropanol is 7.4%. All the other operations are the same as in Example 1.

[0039] The condensate collected from the top of reactive distillation column 3 was 257.4 g, and the amount collected from the top of purification distillation column 4 was 506.1 g. Dichloropropanol yield is 89.9% (shown in Table 1).

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Abstract

A method for preparing dichloropropanol from glycerol, the method comprising the steps of: mixing glycerin with a carboxylic acid catalyst, and carrying out chlorination reaction of the obtained mixture with HCl in a chlorination reactor; sending the obtained reaction mixture to into the reactive distillation tower (3) to contact with HCl to continue the chlorination reaction; the water, hydrochloric acid and part of dichlorohydrin produced by the reaction are steamed from the top of the reactive distillation tower (3), and the product is recovered after condensation The still liquid of reactive distillation column (3) enters purifying distillation column (4) and carries out purification and separation. The method is easy to operate, can increase the reaction rate and the utilization rate of HCl, and the yield of dichloropropanol can reach more than 80%.

Description

technical field [0001] The invention relates to a method for preparing dichloropropanol from glycerin. Background technique [0002] In organic or pharmaceutical synthesis, epoxy compound is an important intermediate, and dichloropropanol is an important precursor for preparing epoxy compound. [0003] There are many methods for preparing dichloropropanol, for example, propylene high-temperature chlorination method (developed by SHELL Corporation of the United States in 1984), propylene acetate method and glycerin chlorination method (for the technology of Showa-Denko, referring to U.S. Patent No. 5,011,980, US Patent No. 5,227,541 or US Patent No. 4,634,784). Both the propylene high-temperature chlorination method and the propylene acetate method require the addition reaction of hypochlorous acid with chlorine gas, and a large amount of chlorine-containing by-products are obtained at the same time, which brings problems such as an increase in manufacturing costs and an out...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/42C07C31/36C07C29/62
Inventor 罗正鸿尤小姿华卫琦罗务习胡兵波张宏科廖增泰丁建生杨万宏
Owner WANHUA CHEM GRP CO LTD
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