Method for improving recovery rate of epoxidation catalyst

A technology of catalyst and recovery rate, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., to improve recovery rate, improve safety, and reduce the risk of thermal decomposition Effect

Pending Publication Date: 2020-02-25
JIANGSU YANGNONG CHEM GROUP +3
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, in the actual reaction process, it is found that the heteropolyacid catalyst cannot completely become solid and precipitate after the reaction, and a small amount of catalyst will combine with residual hydrogen peroxide to form a peroxide intermediate, which is dissolved in the oil phase and the water phase.

Method used

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  • Method for improving recovery rate of epoxidation catalyst

Examples

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Effect test

Embodiment 1

[0013] In a 1L four-necked glass flask, there is 200g of epoxidation reaction solution (10g of catalyst on a dry basis for reaction), and the hydrogen peroxide content of the aqueous layer is 0.6%. Add 0.05g of sodium hypophosphite thereinto, heat up to 45°C, stir and keep warm for 1h, measure The content of hydrogen peroxide in the aqueous phase was 0.03%, and 9.93 g of the catalyst was obtained on a dry basis after separation.

Embodiment 2

[0015] In a 1L four-necked glass flask, there is 300g of epoxidation reaction solution (12g of catalyst on a dry basis for reaction), and the hydrogen peroxide content in the aqueous layer is 0.9%. Add 0.4g of hypophosphorous acid thereinto, heat up to 35°C, stir and keep warm for 1.5h, measure The content of hydrogen peroxide in the aqueous phase was 0.05%, and 11.9 g of the catalyst was obtained on a dry basis after separation.

Embodiment 3

[0017] In the 1L four-necked glass flask, 400g of epoxidation reaction solution (11g of catalyst dry basis) is arranged, and the hydrogen peroxide content of the aqueous layer is 1.1%. Add 2.0g mass concentration 0.5% sodium pyrophosphate aqueous solution and 1.0g mass concentration 2 % pyrophosphoric acid, the temperature was raised to 40°C, stirred and kept for 2 hours, the hydrogen peroxide content in the water phase was measured to be 0.05%, and 10.92g of the catalyst was obtained on a dry basis after separation.

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Abstract

The invention provides a method for improving the recovery rate of a heteropolyacid catalyst for hydrogen peroxide method epoxy chloropropane. A tiny amount of a P-containing assistant into a reactionsolution, a stirring heat-insulation reaction is performed at a certain temperature, the hydrogen peroxide content of a water layer obtained after the reaction is finished is lower than 0.05%, and the recovery rate of the catalyst obtained by separation is higher than 99%. The P-containing assistant is one or more of hypophosphorous acid, sodium (or potassium, calcium and the like) hypophosphite,phosphorous acid, sodium (or potassium, calcium and the like) phosphite, sodium (or potassium, calcium and the like) pyrophosphate and the like. The purpose of separating the dissolved catalyst is achieved by destroying residual hydrogen peroxide in the system and supplementing a P source to maintain the catalyst structure, so the catalyst recovery rate is increased.

Description

technical field [0001] The invention relates to a method for improving the recovery rate of a heteropolyacid catalyst used in hydrogen peroxide method epichlorohydrin. 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 epichlorohydrin salty wastewater, which seriously pollutes the environment. At present, the new domestic production capacity comes from the glycerin method, but this process is limited by the supply of glycerin, and it is difficult to continue to increase production capacity, which cannot meet the growing demand. [0003] In this context, researchers began to pay attention to the hydrogen peroxide method. From the perspective of green che...

Claims

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Application Information

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IPC IPC(8): B01J31/34B01J27/188C07D301/12C07D303/08
CPCB01J31/34B01J27/188C07D301/12C07D303/08
Inventor 孙诚徐林丁克鸿李明吕丽邓小伟胡钦李幸霏刘越
Owner JIANGSU YANGNONG CHEM GROUP
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