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Continuous synthesis process of epoxy chloropropane by hydrogen peroxide method

A technology for the synthesis of epichlorohydrin, applied in the direction of organic chemistry, etc., can solve the problems of short catalyst service time, high energy consumption of methanol recovery, complicated process, etc., achieve stable oxidant conversion rate, long service life, and simple process equipment Effect

Pending Publication Date: 2020-11-24
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN101124044A discloses a production process for epichlorohydrin, using titanium-silicon molecular sieve as a catalyst, methanol as a solvent, and direct epoxidation of chloropropene to prepare epichlorohydrin. Titanium-silicon molecular sieves are packed into a fixed bed, and chloropropene, methanol It is configured into a homogeneous phase with hydrogen peroxide. At a certain temperature, it is pumped into a fixed bed for reaction. This reaction requires the feed to be configured into a homogeneous phase, so a large amount of methanol is required, and the recovery of methanol consumes a lot of energy
The use time of the catalyst in this process is short, the catalyst needs to be regenerated for each reaction, the process is complex, and the energy consumption is high

Method used

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  • Continuous synthesis process of epoxy chloropropane by hydrogen peroxide method
  • Continuous synthesis process of epoxy chloropropane by hydrogen peroxide method
  • Continuous synthesis process of epoxy chloropropane by hydrogen peroxide method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) press figure 1 Fill the reactor with TS-1 catalyst, fill sections I-III, and install the reactor, pump in deionized water to fill the entire loop reactor, turn on the circulating water bath, the water temperature is 0°C, and turn on the forced circulation pump. Continue to inject deionized water into the system through the metering pump for 4 hours to wash and wet the catalyst, and drain the deionized water; continue to inject methanol into the system through the metering pump for 4 hours to wet and activate the catalyst, and drain the methanol.

[0027] (2) Allyl chloride and methanol are mixed uniformly according to the molar ratio of 1:1;

[0028] (3) Simultaneously turn on metering pumps A and B to feed materials to the mixer, control the molar ratio of chloropropene and hydrogen peroxide to 1:1, and the solubility of hydrogen peroxide is 50 wt%. The residence time of the control material in the loop reactor is 2h;

[0029] (4) Measure the hydrogen peroxide an...

Embodiment 2

[0032] (1) press figure 1 Fill the reactor with TS-1 catalyst, fill the first section, and install the reactor, pump in deionized water to fill the entire loop reactor, turn on the circulating water bath, the water temperature is 10°C, and turn on the forced circulation pump. Continue to inject deionized water into the system for 6 hours to wash and wet the catalyst through the metering pump, and drain the deionized water; continue to inject methanol into the system through the metering pump for 8 hours to moisten and activate the catalyst, and drain the methanol.

[0033] (2) allyl chloride and methanol are mixed evenly according to the molar ratio of 2:1;

[0034] (3) Simultaneously turn on metering pumps A and B to feed materials to the mixer, control the molar ratio of chloropropene and hydrogen peroxide to 1:1, and the solubility of hydrogen peroxide to 10wt%. The residence time of the control material in the loop reactor is 1h;

[0035] (4) with embodiment 1.

[0036]...

Embodiment 3

[0038] (1) press figure 1 Fill the reactor with TS-1 catalyst, fill sections I-IV, and install the reactor, pump in deionized water to fill the entire loop reactor, turn on the circulating water bath, the water temperature is 30°C, and turn on the forced circulation pump. Continue to inject deionized water into the system for 8 hours to wash and wet the catalyst through the metering pump, and drain the deionized water; continue to inject methanol into the system for 6 hours to wet the activated catalyst through the metering pump, and drain the methanol.

[0039] (2) Allyl chloride and methanol are mixed uniformly according to the molar ratio of 1:1;

[0040] (3) Simultaneously turn on the metering pumps A and B to feed the mixer, control the molar ratio of chloropropene and hydrogen peroxide to 3:1, and the solubility of hydrogen peroxide is 70wt%. The residence time of the control material in the loop reactor is 0.1h;

[0041] (4) with embodiment 1.

[0042] (5) with embod...

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Abstract

The invention provides a continuous synthesis process of epoxy chloropropane by hydrogen peroxide method. The continuous synthesis process comprises the following steps of adding hydrogen peroxide, methanol, chloropropene and a catalyst into a reactor for epoxidation reaction, wherein the reactor is a ring reactor, and the catalyst is pre-loaded into the ring reactor; enabling the chloropropene and the methanol to form a chloropropene and methanol mixed solution in a mixing tank, pumping chloropropene and methanol mixed solution into the ring reactor by a metering pump A, and pumping hydrogenperoxide into the ring reactor by a metering pump B. The synthesis process provided by the invention has the advantages of low methanol consumption, long service life of the catalyst, simple process device, realization of continuous operation, and realization of stable hydrogen peroxide conversion rate and high epichlorohydrin selectivity in a long-term continuous operation process.

Description

technical field [0001] The invention belongs to the field of catalytic synthesis, and relates to a method for synthesizing epichlorohydrin. More specifically, the invention relates to a continuous synthesis process of epichlorohydrin by hydrogen peroxide method. Background technique [0002] Epichlorohydrin is an important organic chemical raw material and fine chemical product. Because its molecule contains active epoxy groups and chlorine atoms, its chemical properties are quite active, and it has become an important basic organic chemical raw material and intermediate. Widely used in the synthesis of epoxy resin, glycerin, alcohol rubber, medicine, pesticides, surfactants, glass fiber reinforced plastics, ion exchange resins, coatings and plasticizers. [0003] At present, research at home and abroad is mainly focused on the process of preparing epichlorohydrin by direct epoxidation of chloropropene using hydrogen peroxide as the oxygen source. small. CN101124044A discl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/12C07D303/08
CPCC07D301/12C07D303/08
Inventor 徐林黄杰军丁克鸿徐志斌李明胡钦黄文嵘刘洋李幸霏徐文轩钱赟邓生才胡金良
Owner JIANGSU YANGNONG CHEM GROUP
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