Method for regenerating phosphorus molybdenum/tungsten heteropolyacid quaternary ammonium salt catalyst

A heteropolyacid quaternary ammonium salt and catalyst technology, which is applied in the direction of catalyst regeneration/reactivation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of low processing efficiency, cumbersome process, long regeneration cycle, etc., and achieve The regeneration process is simple and the process is stable

Active Publication Date: 2018-12-14
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has a long process flow, cumbersome process, long regeneration cycle, and low treatment efficiency, which still cannot meet the requirements of modern industrial applications.

Method used

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  • Method for regenerating phosphorus molybdenum/tungsten heteropolyacid quaternary ammonium salt catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In the process of preparing epichlorohydrin by direct epoxidation of propylene chloride using aqueous hydrogen peroxide solution as the oxygen source and phosphomolybdenum / tungsten heteropoly acid quaternary ammonium salt as the catalyst, the catalyst will be deactivated or catalytically active as the catalyst is recycled for a certain period of time Reduce to a predetermined level (effective utilization rate of hydrogen peroxide 80.0%). Take 50g of the reduced activity catalyst (phosphomolybdenum / tungsten heteropoly acid quaternary ammonium salt), add 50g of deionized water, at 60℃, pass in the ozone concentration of 12mg / L at a rate of 2.5L / h for 2h; after oxidation Add 250g of water to the catalyst of, and perform stripping at a negative pressure of -0.05Mpa to a temperature of 80℃; add 20.0g of 5.0wt% quaternary ammonium salt aqueous solution to the rest of the reactor, stir and wash at 20℃ to regenerate for 12h, then separate the water after standing. Phase, the bot...

Embodiment 2

[0024] Take 50g of the catalyst with reduced activity and add 50g of deionized water. At 20°C, pass the ozone concentration of 12mg / L at a rate of 2.5L / h to oxidize for 3h; add 500g of water to the oxidized catalyst, and the negative pressure is- Stripping is carried out at 0.07Mpa to a kettle temperature of 70°C; adding 40.0g of a 1.0wt% quaternary ammonium salt aqueous solution to the rest of the kettle, stirring and washing at 30°C for 10h regeneration, after standing still, the water phase is separated, and the bottom solid is the regenerated catalyst.

Embodiment 3

[0026] Take 50g of the catalyst with reduced activity, add 50g of deionized water, and at 70℃, pass the ozone concentration of 12mg / L at a rate of 2.5L / h to oxidize for 5h; add 750g of water to the oxidized catalyst, and the negative pressure is- Stripping is carried out at 0.03Mpa to a kettle temperature of 90°C; 10.0g of a 10.0wt% quaternary ammonium salt aqueous solution is added to the remainder of the kettle, stirred and washed at 50°C for 16h regeneration, after standing still, the water phase is separated, and the bottom solid is the regenerated catalyst.

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Abstract

The invention discloses a method for regenerating a phosphorus molybdenum / tungsten heteropolyacid quaternary ammonium salt catalyst. The method comprises the following steps: (1) adding equivalent deionized water into a phosphorus molybdenum / tungsten heteropolyacid quaternary ammonium salt catalyst with activity decrease, and oxidizing in an ozone atmosphere; (2) adding water into the oxidized phosphorus molybdenum / tungsten heteropolyacid quaternary ammonium salt catalyst, and stripping under a negative pressure; (3) adding a quaternary ammonium salt aqueous solution into the kettle, stirring,washing and regenerating. The method has the main advantages that (1) the catalyst regeneration process is simple, and the process is stable; (2) the regenerated catalyst and the novel catalyst havebasically consistent activity. The requirements on modern industrial application are met.

Description

Technical field [0001] The invention relates to a method for regenerating a heteropolyacid catalyst, in particular to a method for regenerating a heteropolyacid catalyst used for the catalytic preparation of epoxy chloropropane, a key intermediate of epoxy resin, and more specifically to a phosphomolybdenum / The regeneration method of tungsten heteropoly acid quaternary ammonium salt catalyst. Background technique [0002] Epichlorohydrin is an important organic chemical raw material and fine chemical product, 75% of the total consumption is used to produce epoxy resin. At present, the industrial synthesis methods of epichlorohydrin mainly include propylene acetate method, propylene high-temperature chlorination method and glycerin method; these processes will cause a large number of "three wastes" pollution problems, and they are increasingly unsuitable for the development of green chemistry. . With the advancement of the sustainable development strategy, the current research ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J38/04B01J38/48B01J31/40
CPCB01J31/40B01J38/04B01J38/48
Inventor 徐林黄杰军丁克鸿徐志斌徐文轩王玉霜钱赟
Owner JIANGSU YANGNONG CHEM GROUP
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