Method for preparing dichloropropanol with chemical reaction-pervaporation coupling method

A technology of pervaporation and dichloropropanol, which is applied in organic chemistry, the introduction of halogen preparation, the separation/purification of hydroxyl compounds, etc., can solve the problems of inability to maximize the efficiency of chlorination reaction, energy loss, waste of resources, etc. Achieve low cost, reduce heat load, and save energy

Inactive Publication Date: 2013-01-23
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] In a word, the existing dichloropropanol production process is very difficult in how to remove the water generated by the reaction while recycling hydrogen chloride, or how to reduce the loss of the catalyst in the reaction and save the energy waste caused by the excessive stream in the condensation process. It is difficult to find a good solution, or cause waste of resources, or consume a lot of energy, and cannot maximize the efficiency of the chlorination reaction

Method used

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  • Method for preparing dichloropropanol with chemical reaction-pervaporation coupling method
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  • Method for preparing dichloropropanol with chemical reaction-pervaporation coupling method

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Embodiment 1

[0039] Example 1: A stirred tank reactor (produced by Jiangsu Gongtang Chemical Equipment Co., Ltd., K-type VN50, with a volume of 350L), glycerin was preheated and added to the reactor at a feed rate of 1.05kmol / h, and the reactor 9.2Kg catalyst (Rohm and Haas series Amberlyst 15 wet type, produced by Dow Chemical Company, treated with soaking water) was pre-loaded inside, and hydrogen chloride gas was fed from the bottom of the reactor at a feed rate of 2.5 kmol / h. The reaction is operated under normal pressure, and the reaction temperature is controlled at 110°C. After the steam at the top of the reactor is condensed, the liquid stream enters the inlet of the pervaporation device at a flow rate of 2.25 kmol / h, and the water vapor preferentially permeated on the downstream side of the pervaporation membrane is circulated. After the ethylene glycol is condensed, it flows out at 1.95 kmol / h, and the impermeable liquid on the upstream side of the membrane returns to the reactor ...

Embodiment 2

[0041] Example 2: Stirred tank reactor with a volume of 500 L, produced by Foshan Tesai Chemical Equipment Co., Ltd., model DJ35, glycerol is added to the reactor at a feed rate of 1.05 kmol / h after preheating, and the reactor is preheated. Load 6.5Kg catalyst (Rohm and Haas series Amberlyst 36 wet type, produced by Dow Chemical Company, treated by immersion water), and hydrogen chloride gas is added from the bottom of the reactor at a feed rate of 3.5 kmol / h. The operating pressure of the reaction is 3atm, the reaction temperature is controlled at 120°C, and the flow rate at the bottom of the reactor enters the inlet of the pervaporation device at a flow rate of 4.55 kmol / h. 2.02kmol / h flows out, and the impermeable liquid on the upstream side of the membrane returns to the reactor at a flow rate of 1.01kmol / h, and the other part is withdrawn as a product at a flow rate of 1.02kmol / h. The pervaporation membrane material is polyvinyl alcohol, and the membrane material is made ...

Embodiment 3

[0043] Embodiment 3: Stirred tank reactor, volume is 300L, produced by Foshan Tesai Chemical Equipment Co., Ltd., model DJ55, adds the glycerin and catalyst mixture after preheating (catalyst is acetic acid, Produced by Xuguang Chemical Co., Ltd., the amount used is 5% of the total amount of glycerin), and hydrogen chloride gas is fed from the bottom of the reactor at a feed rate of 1.5 kmol / h. The operating pressure of the reaction is 4atm, the reaction temperature is controlled at 140°C, and the flow rate at the bottom of the reactor enters the inlet of the pervaporation device at a flow rate of 1.95 kmol / h. A flow rate of 1.10 kmol / h flows out, a part of the impermeable liquid on the upstream side returns to the reactor at a flow rate of 0.35 kmol / h, and another part is withdrawn at a flow rate of 0.50 kmol / h. The pervaporation membrane material is polyvinyl alcohol, and the membrane material is made of polyvinyl alcohol GM-17s from Nippon Synthetic Chemical Industry Co., L...

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Abstract

The invention discloses a method for preparing dichloropropanol with a chemical reaction-pervaporation coupling method, wherein the method provided by the invention comprises the following steps of: directly adding glycerol and a liquid catalyst into a chemical reactor (if a solid catalyst is used, putting the solid catalyst into the reactor in advance) after pre-heating, simutaneously feeding a hydrogen chloride gas into the reactor, chlorinating the glycerol with the hydrogen chloride in the reactor, instantly introducing the reaction product into a pervaporation device, wherein a permeable film in the device preferably permeates and removes water generated in the reaction to accelerate chlorination reaction efficiently, thereby finally obtaining the dichloropropanol with high concentration. The method provided by the invention couples the pervaporation device with the chemical reactor to instantly remove the water generated in the reaction, thereby improving the efficiency of the chlorination reaction, reducing the hot load in the subsequent dehydration process of a dichloropropanol rectifying column, and improving the utilization efficiency of hydrogen chloride.

Description

technical field [0001] The invention relates to a method for preparing dichloropropanol, in particular to a method for preparing dichloropropanol by using a chemical reaction-permeation vaporization coupling method. [0002] Background technique [0003] Epichlorohydrin is an important organic chemical raw material and fine chemical product, mainly used in the production of epoxy resin, nitroglycerin explosives, glass fiber reinforced plastics, electrical insulation products, (glycidin) derivatives, chlorohydrin rubber and other products , at the same time it can also be used to synthesize surfactants, medicines, pesticides, coatings, rubber, ion exchange resins and other products, widely used in the production of chemical stabilizers, chemical dyes and water treatment, in addition, it can also be used directly As a solvent for cellulose esters, resins, and cellulose ethers. As we all know, at present, the production methods of epichlorohydrin mainly include the high-tempe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/36C07C29/62C07C29/76
Inventor 李磊吕权殷海燕武法文
Owner NANJING UNIV
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