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Method for preparing dichloropropanol by glycerol method

A technology of dichloropropanol and glycerin, applied in the direction of introduction of halogen preparation, organic chemistry, etc., can solve the problems of less large-scale production of epichlorohydrin, difficulty in industrial scale production, complex production process, etc., shorten the reaction time, improve The effect of the reaction rate and the simplicity of the reaction process

Active Publication Date: 2013-05-01
ZHUHAI CHANGXIAN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Among the various techniques for synthesizing dichloropropanol disclosed at present, most of the production processes are complicated, the reaction time is long, and it is difficult to carry out industrial scale production, which leads to the production of dichloropropanol by the real glycerol method, and then the synthesis of epichlorohydrin. Very little mass production

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  • Method for preparing dichloropropanol by glycerol method

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Embodiment 1

[0017] Embodiment 1: adopt batch reaction, at first, inject 300g glycerol solution that has dissolved 2g acetic acid in each reactor of microreactor integrated system, described microreactor is 3.0Mpa that can withstand pressure, internal diameter diameter is 30mm, long 600mm , a cylindrical reactor lined with PP and steel parts on the outside, one end is closed, and the other end is fixed with a screw-type inflatable switch valve with a pressure gauge, and then continuously injects hydrogen chloride gas to make hydrogen chloride excess and generate a pressure of 1.0Mpa , under the pressure of 1.0Mpa, seal it, put it in a water bath and heat it. When the temperature rises to 90°C, the pressure rises to 1.6Mpa and keeps for three hours. The pressure drops to 0.6Mpa to generate chlorinated glycerin; then, the chlorinated glycerol mixture reacted in each microreactor is collected in the reactor, and finally it is detected that the mass content of dichloropropanol is 68.3%. Remove...

Embodiment 2

[0018] Embodiment 2: adopt continuous reaction, continuous feeding: make a microreactor that can withstand pressure of 3.0Mpa, with a diameter of 50mm and a length of 1000mm, made in three sections, with two seals in the middle, and 6 openings in each seal The hole of ￠3mm is used to reduce the flow of glycerin liquid and make hydrogen chloride stay in the tube more. There is a switch at the outlet end to adjust the outflow (with a pressure gauge). There are two inlets at the feed end, one is for glycerin catalyst mixture, One is for pressing the hydrogen chloride in. At the beginning, first pass hydrogen chloride gas from the lower part, and after driving away the air inside, close the outlet end, continue to pass hydrogen chloride, so that the internal pressure is 8kg, and the glycerin catalyst mixture heated to 80°C is pumped into the tube, and the pressure is maintained. The glycerin solution can be slowly injected. When the amount of glycerin containing 3.0% adipic acid a...

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Abstract

The invention discloses a technique for synthesizing dichloropropanol by using glycerol and relates a method for preparing dichloropropanol by introducing glycerol and hydrogen chloride into a microreactor integrated system and quickly reacting. In the method, reaction is performed quickly under the conditions of excessive hydrogen chloride, pressure and a certain temperature; after the reaction in each microreactor, a dichloropropanol-based mixture is collected and rectified to separate out pure 1,3-dichloropropanol and 2,3-dichloropropanol; and the dichloropropanol can be used for synthesizing epoxy chloropropane through saponification and cyclization. The microreactors are used for performing reaction, so yield can be improved and reaction time can be shortened; and the cheapest materials are used for production, so the reaction process is simple and the reaction rate is increased.

Description

【Technical field】 [0001] The invention relates to a method for synthesizing dichloropropanol from glycerol, in particular to a method for feeding hydrogen chloride gas into a microreactor integrated system to react with glycerin to synthesize dichloropropanol. 【Background technique】 [0002] At present, there are two main production processes for epichlorohydrin and its precursor dichlorohydrin, propylene high temperature chlorination method, allyl alcohol method and glycerin chlorination method. The high-temperature chlorination of propylene is the main production method of epichlorohydrin and its precursor dichloropropanol in the world so far, and propylene is a petroleum reaction product. The process is to chlorinate propylene with chlorine gas at a high temperature of 500 degrees, and then hydrolyze Finally, low-concentration dichloropropanol is generated. The production process is flexible, the process is mature, and the operation is stable, but the method has the defec...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/36C07C29/62
Inventor 杨伟明
Owner ZHUHAI CHANGXIAN CHEM TECH