Continuous synthesizing process of epichlorohydrin

A technology for the synthesis of epichlorohydrin, which is applied in chemical recovery, organic chemistry, etc., can solve the problems of catalyst separation loss engineering, the impact of catalyst stability and recycling, and the catalyst contains too much water, so as to reduce the loss probability and recovery rate High, the effect of improving the recovery rate

Active Publication Date: 2019-08-02
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, how to reduce the separation loss of the catalyst and how to realize the continuous separation operation are also the difficulties that plague the engineering
CN206232636, adopts the combined mode of screw pump+liquid-solid separator to realize the separation of catalyst, but the catalyst separated by screw pump contains much water (about 20% of water), and the catalys

Method used

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  • Continuous synthesizing process of epichlorohydrin
  • Continuous synthesizing process of epichlorohydrin
  • Continuous synthesizing process of epichlorohydrin

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0018] Example 1

[0019] The stainless steel reactor and the two-stage stainless steel loop reactor are connected in series. The reactor volume is 100L, the volume of each stage loop reactor is 100L, the total reactor volume is 300L, and the residence time is 3h. A centrifugal pump was used to pump 75L / h of 3-chloropropene and catalyst slurry into the reactor (the slurry was prepared according to the catalyst's weight of 5% of the chloropropene) and 50% hydrogen peroxide at 17.5L / h, and the reaction temperature was 47°C. The pressure is 0.2MPa, 50% hydrogen peroxide is pumped into the primary loop reactor 7.5L / h, the reaction temperature is 53℃, the pressure is 0.3MPa, the secondary loop reactor temperature is 52℃, the pressure is 0.3MPa, and 0.5kg / h 10% is added. For ammonium sulfate aqueous solution, a sufficient amount of nitrogen is introduced at the condenser inlet to ensure that the oxygen content in the tail gas is less than 5%.

[0020] The reaction materials are continuo...

Example Embodiment

[0021] Example 2

[0022] The stainless steel reactor and the two-stage stainless steel loop reactor are connected in series, the reactor volume is 100L, the volume of each stage loop reactor is 100L, the total reactor volume is 300L, and the residence time is 2.5h. A centrifugal pump was used to pump 96L / h of 3-chloropropene and catalyst into the reactor respectively (the slurry formed by the catalyst accounts for 4% of the chloropropene weight) and 48% hydrogen peroxide 16L / h, reaction temperature 49℃, pressure 0.3MPa, pump 48% hydrogen peroxide 8L / h into the primary loop reactor, reaction temperature 51℃, pressure 0.25MPa, secondary loop reactor temperature 52℃, pressure 0.3MPa, and add 0.8kg / h 10% diphosphoric acid For the aqueous solution of ammonium hydrogen, pass enough nitrogen into the condenser inlet to ensure that the oxygen content in the tail gas is less than 5%.

[0023] The reaction materials are continuously extracted from the secondary loop reactor, enter the scra...

Example Embodiment

[0024] Example 3

[0025] The stainless steel reactor and the two-stage stainless steel loop reactor are connected in series. The reactor volume is 100L, the volume of each stage loop reactor is 100L, the total reactor volume is 300L, and the residence time is 4h. A centrifugal pump was used to pump 42.5L / h of 3-chloropropene and catalyst slurry into the reactor (according to the catalyst accounted for 4% by weight of the chloropropene) and 60% hydrogen peroxide 18L / h, the reactor temperature was 45℃ , Pressure 0.15MPa, pump 60% hydrogen peroxide 14.5L / h into the primary loop reactor, reaction temperature 52℃, pressure 0.3MPa, secondary loop reactor temperature 50℃, pressure 0.2MPa, and add 0.8kg / h 10 % Potassium dihydrogen phosphate aqueous solution, a sufficient amount of nitrogen is passed through the condenser inlet to ensure that the oxygen content in the tail gas is less than 5%.

[0026] The reaction materials are continuously extracted from the secondary loop reactor, ente...

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Abstract

The invention relates to a continuous synthesizing process of epichlorohydrin. Specifically, a kettle type reactor and a circulation flow reactor are connected in series; different ratios of hydrogenperoxide are added in stages for reaction; different temperatures and times are controlled; a product directly enters a closed type scraper centrifugal machine to separate out a catalyst and a reaction liquid after the reaction is ended; the reaction liquid is layered to obtain an oil layer and a water layer; chloropropene and the separated catalyst are recycled and pulped to return to a reactionsystem; continuous catalytic operation of the catalyst is realized.

Description

technical field [0001] The invention relates to a continuous synthesis process of epichlorohydrin. Specifically, a tank reactor and a loop reactor are connected in series, and different proportions of hydrogen peroxide are added to react in stages to improve the utilization rate of hydrogen peroxide. After the reaction, the materials are directly Enter the closed scraper centrifuge to separate the solid catalyst and the reaction liquid, and the separated catalyst and allyl chloride are beaten into a slurry and returned to the reaction system to realize the continuous circulation of the catalyst. Background technique [0002] Epichlorohydrin is an important petrochemical product, mainly used in the production of epoxy resins. At present, there are two main production processes of epichlorohydrin: chlorohydrin method and glycerin method. 70% of domestic epichlorohydrin comes from the chlorohydrin method, and its biggest disadvantage is that it produces 50 tons / ton of epichlor...

Claims

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Application Information

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IPC IPC(8): C07D301/12C07D301/32C07D303/08
CPCC07D301/12C07D301/32C07D303/08Y02P20/584
Inventor 徐林孙诚丁克鸿王怡明曹亚丽李明吕丽
Owner JIANGSU YANGNONG CHEM GROUP
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