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Method for preparing epoxy chloropropane by micro-channel reactor

A technology of microchannel reactor and epichlorohydrin, which is applied in the direction of organic chemistry, can solve the problem of excessive waste water, and achieve the effects of simplified process, good environmental protection and safety, and easy scale-up

Inactive Publication Date: 2012-03-14
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0017] Patents CN10046282.8 and CN10138861.8 respectively introduced the process of using extractant for anhydrous cyclization, which overcomes the disadvantage of more waste water in the cyclization process
However, considering the constraints of factors such as production cost, environmental protection and safety, the defects of the above two methods are also very obvious.

Method used

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  • Method for preparing epoxy chloropropane by micro-channel reactor
  • Method for preparing epoxy chloropropane by micro-channel reactor
  • Method for preparing epoxy chloropropane by micro-channel reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0037] A microchannel reactor with an inner diameter of 0.2mm and a length of 15m was selected, and a NaOH solution with a mass fraction of 25% was selected for the cyclization reaction. Set the reaction temperature at 35°C, the residence time is 60s, and the feed molar ratio N[DCH]:N[NaOH]=1:1.4. Calculate the flow of the two materials according to the above molar ratio and residence time, and use a metering pump to first Dichloropropanol and NaOH are pumped into their respective preheaters for preheating through their respective pumps, and then the raw materials enter the micro-mixer for mixing, and finally the mixed material liquid reacts in the micro-channel, and the temperature of the constant temperature water tank is maintained at 35°C. After the reaction solution flows out, use 35% H 2 SO 4 The solution neutralizes it. The neutralized liquid is subjected to oil-water separation, and the oil phase is subjected to normal-pressure rectification to obtain refined epichl...

Embodiment 2

[0040] A microchannel reactor with an inner diameter of 0.4mm and a length of 10m was selected, and a NaOH solution with a mass fraction of 25% was selected for the cyclization reaction. Set the reaction temperature at 50°C, the residence time is 45s, the feed molar ratio N[DCH]:N[NaOH]=1:1.3, calculate the flow rate of the two materials according to the above molar ratio and residence time, and use the metering pump to first Dichloropropanol and NaOH are pumped into their respective preheaters for preheating through their respective pumps, and then the raw materials enter the micro-mixer for mixing, and finally the mixed material liquid reacts in the micro-channel, and the temperature of the constant temperature water tank is maintained at 50°C. After the reaction solution flows out, use 35% H 2 SO 4 The solution neutralizes it. The neutralized liquid is subjected to oil-water separation, and the oil phase is subjected to normal-pressure rectification to obtain refined epi...

Embodiment 3

[0043]A microchannel reactor with an inner diameter of 0.6mm and a length of 10m was selected, and a NaOH solution with a mass fraction of 25% was selected for the cyclization reaction. Set the reaction temperature at 65°C, the residence time is 30s, and the feed molar ratio N[DCH]:N[NaOH]=1:1.2. Calculate the flow rate of the two materials according to the above molar ratio and residence time, and use a metering pump to first Dichloropropanol and NaOH solution are pumped into their respective preheaters for preheating through their respective pumps, and then the raw materials enter the micro-mixer for mixing, and finally the mixed material liquid reacts in the micro-channel, and the temperature of the constant temperature water tank is maintained at 65°C. After the reaction solution flows out, use 35% H 2 SO 4 The solution neutralizes it. The neutralized liquid is subjected to oil-water separation, and the oil phase is subjected to normal-pressure rectification to obtain r...

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Abstract

The invention discloses a method for preparing epoxy chloropropane by a micro-channel reactor, which belongs to the technical field of chemical products. Dichloropropanol and alkali liquor are mixed through a micro-mixer and are then fed into the micro-channel reactor for carrying out cyclization reaction. Products obtained through reaction carry out oil-water separation after being neutralized by acid solution, then, oil phases are rectified at the ordinary pressure, and final products of epoxy chloropropane are obtained. The inner diameter of a micro channel is 0.2 to 1.0mm, the length is 5 to 15m, the reaction is carried out at the ordinary pressure and at the temperature being 30 to 90 DEG C, the retention time is 15 to 60s, the alkali liquor is NaOH or Ca(OH)2 solution, the mole ratio of NaOH to dichloropropanol is 1 to 1.5, the mole ratio of Ca(OH)2 to the dichloropropanol is 0.5 to 1, the acid solution is H2SO4 or HCl solution, and the yield of the epoxy chloropropane is about 97 percent. The method has the advantages that the energy consumption is low, the wastewater discharge quantity is small, the selectivity is high, the production cost is low, the process magnification is simple and convenient, and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical products, and more specifically relates to a process for preparing epichlorohydrin. Background technique [0002] At present, the main industrialization route of epichlorohydrin is: 1. The high-temperature chlorination method of propylene represented by Shell Company (hereinafter referred to as the chloropropene method), the intermediate product is 3-chloropropene, and finally epichlorohydrin is obtained. At present, more than 95% of epichlorohydrin production in the world adopts this method. ② The allyl acetate-allyl alcohol method developed by Showa Denko in the mid-1980s (hereinafter referred to as the allyl alcohol method), the intermediate product is allyl alcohol. [0003] The high-temperature chlorination of propylene is the most commonly used method for the industrial production of epichlorohydrin. In 1948, Shell Corporation of the United States successfully developed a production device...

Claims

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Application Information

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IPC IPC(8): C07D303/08C07D301/26
Inventor 张跃李津石严生虎刘建武沈介发
Owner CHANGZHOU UNIV
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