System and method for continuously synthesizing high-purity 3-chloro-1,2-propylene glycol

A high-purity, propylene glycol technology, applied in chemical instruments and methods, the preparation of organic compounds, the preparation of hydroxyl compounds, etc., can solve the problem that the molar ratio of deionized water to epichlorohydrin is too large, and the quality of different batches of products cannot be guaranteed. In order to avoid problems such as high reliability and increased operation time by distillation, the effects of low labor intensity, improved production environment and short reaction time are achieved.

Inactive Publication Date: 2016-01-13
TAISHAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the above-mentioned patents and traditional synthesis processes adopt intermittent production, and the reaction time is long. During the hydrolysis reaction, the control of temperature, pressure, heat and mass transfer, etc. is difficult to achieve stability, so that the quality stability of different batches of products cannot be guaranteed. , and the quality index varies greatly between different batches; the molar ratio of deionized water to epichlorohydrin is too large, that is, the amount of deionized water is

Method used

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  • System and method for continuously synthesizing high-purity 3-chloro-1,2-propylene glycol

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Experimental program
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Effect test

Embodiment 1

[0037] Such as figure 1 As shown, a system for continuously synthesizing high-purity 3-chloro-1,2-propanediol, the system includes a static mixer 5, a pipeline reactor 6, a hydrolyzate intermediate tank 7, a still 8, Distillation tower 13 and condenser 9, the first receiving tank 10, the second receiving tank 11 and the finished product receiving tank 12 are respectively connected on the outlet pipeline of described condenser 9;

[0038] The epichlorohydrin head tank 1 and the demineralized water head tank 2 are respectively connected with the input pipeline of the static mixer 5 through the epichlorohydrin metering pump 3 and the demineralized water metering pump 4;

[0039] A hydrolyzate feeding pump 16 is connected between the hydrolyzate intermediate tank 7 and the still 8;

[0040] The first receiving tank 10, the second receiving tank 11 and the finished product receiving tank 12 are simultaneously connected with a hydraulic jet vacuum pump 15 and a Roots-oil ring vacuu...

Embodiment 2

[0051] The system structure of this embodiment is the same as the system structure of Embodiment 1.

[0052] The method steps for the continuous synthesis of high-purity 3-chloro-1,2-propanediol are the same as in Example 1, except that:

[0053] In step (2), the speed of epichlorohydrin is 100kg / h, and the outlet pressure of demineralized water and epichlorohydrin is all adjusted to 2.3-2.4MPa respectively; In step (3), control pipeline reactor 6 top reaction temperature 79 -82° C.; in step (4), the rear fraction in the second receiving tank 11 is also added to the distillation still 8 .

[0054] The index of the prepared product: the product yield is 98.63%, and the purity (GC) is 99.74%.

Embodiment 3

[0056] The system structure of this embodiment is the same as the system structure of Embodiment 1.

[0057] The method steps for the continuous synthesis of high-purity 3-chloro-1,2-propanediol are the same as in Example 1, except that:

[0058] In step (2), the speed of epichlorohydrin is 105kg / h, and the outlet pressure of demineralized water and epichlorohydrin is all adjusted to 2.5-2.6MPa respectively; In step (3), control pipeline reactor 6 top reaction temperature 83 -86° C.; in step (4), the rear fraction in the second receiving tank 11 is also added to the distillation still 8 .

[0059] The index of the prepared product: the product yield is 98.93%, and the purity (GC) is 99.86%.

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Abstract

The invention discloses a system and a method for continuously synthesizing high-purity 3-chloro-1,2-propylene glycol. The system includes, in a successively connection manner through pipelines, an overhead tank, a static mixer, a tubular reactor, a hydrolysate intermediate tank, a distillation kettle, a distillation column and a condenser. An output pipeline on the condenser is respectively connected to a first receiving pot, a second receiving pot and a finish product receiving pot. The receiving pots are connected to a hydraulic jet vacuum pump and a Roots-oil ring vacuum machine set at the same time. The method includes the steps of pre-heating epoxy chloropropane and softened water, mixing the epoxy chloropropane and the softened water in the static mixer according to ratio, feeding the mixture into the tubular reactor, controlling the vacuum degree and temperature of the reaction liquid in the distillation kettle to produce different fractions, and finally producing the fraction at specified vacuum degree and temperature as a finish product.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a system and method for continuously synthesizing high-purity 3-chloro-1,2-propanediol. Background technique [0002] 3-Chloro-1,2-propanediol (also known as chlorinated glycerol in the industry) is one of the important chlorinated products of glycerol, used as an intermediate in organic synthesis for the preparation of plasticizers, surfactants, dyes, drugs and glycerol Derivatives, etc.; As a solvent, it is used in the production of cellulose acetate, etc., and is widely used in chemical, pharmaceutical, coating and other industries. [0003] Chinese patent (application number 201410174437.7) proposes a method for preparing chlorinated glycerin by hydrolyzing epichlorohydrin. When hydrolyzing, sulfuric acid is used as a catalyst, the molar ratio of epichlorohydrin and water is 1:4.25~4.5, the temperature is 95~98°C, the reaction time is 1~3 hours, cooled to 60~70°C, ...

Claims

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Application Information

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IPC IPC(8): C07C29/10C07C31/42
CPCC07C29/103C07C31/42
Inventor 杨荣华张恭孝王和欣郭学阳陈玉新高飞翔冯涛
Owner TAISHAN MEDICAL UNIV
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