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Method for catalytic hydrocracking of phenol-containing tar to recycle diphenol and catalyst

A technology for catalytic hydrogenation and phenol tar, which is used in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical recovery, etc. Process economy, effect of reducing disposal costs

Active Publication Date: 2019-04-19
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is relatively simple and effective to realize the reuse of tar, but due to the strong dyeing property of tar, the application range is greatly limited

Method used

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  • Method for catalytic hydrocracking of phenol-containing tar to recycle diphenol and catalyst
  • Method for catalytic hydrocracking of phenol-containing tar to recycle diphenol and catalyst

Examples

Experimental program
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Effect test

Embodiment example 1

[0037] Weigh 10g of titanium dioxide and dissolve it in 10ml of aqueous solution in a round-bottomed flask, add 0.1g of palladium nitrate dihydrate solid, 0.1g of silver nitrate solid, and 0.01g of cesium carbonate solid under constant stirring, and continue stirring for 10 hours, then turn off the stirring. After standing still for 8 hours, the excess aqueous solution was removed by rotary evaporation, dried overnight, calcined at 300°C for 8 hours, and finally reduced at 300°C for 6 hours under a hydrogen atmosphere to obtain a catalyst supporting palladium and silver on titanium dioxide, wherein palladium is 0.45 wt%, silver It is 0.62wt%, and cesium oxide is 0.08wt%. Take 0.1g of the titanium dioxide-supported catalyst prepared above, 10ml of water, and 5g of tar into the reaction kettle, replace the air in the reaction kettle with hydrogen 5 times, react at a temperature of 80°C, a pressure of 1MPa, and a stirring speed of 600rpm for 5 hours, and cool to room temperature ...

Embodiment example 2

[0039]Weigh 10g of titanium dioxide and dissolve it in 80ml of aqueous solution in a round-bottomed flask, add 0.5g of palladium nitrate dihydrate solid, 0.5g of silver nitrate solid, and 0.03g of cesium carbonate solid under constant stirring, and continue stirring for 12 hours, then turn off the stirring. After resting for 10 hours, the excess aqueous solution was removed by rotary evaporation, dried overnight, calcined at 400°C for 5 hours, and finally reduced at 300°C for 5 hours under a hydrogen atmosphere to obtain palladium and silver catalysts supported on titanium dioxide. Among them, 2.17wt% of palladium, 2.99wt% of silver, and 0.23wt% of cesium oxide. Take 0.2g of the titanium dioxide-supported catalyst prepared above, 50ml of water, and 5g of tar into the reaction kettle, replace the air in the reaction kettle with hydrogen for 5 times, react at a temperature of 100°C, a pressure of 2MPa, and a stirring speed of 800rpm for 2 hours, and then cool to room temperature ...

Embodiment example 3

[0041] Weigh 10g of titanium dioxide and dissolve it in 100ml of aqueous solution in a round-bottomed flask, add 2g of palladium nitrate dihydrate solid, 2g of silver nitrate solid, and 0.1g of cesium carbonate solid under constant stirring, and continue stirring for 16 hours, then turn off the stirring and stand still for 12 After one hour, the excess aqueous solution was removed by rotary evaporation, dried overnight, calcined at 500°C for 5 hours, and finally reduced at 350°C for 4 hours under a hydrogen atmosphere to obtain a catalyst of palladium and silver supported on titanium dioxide. Wherein, palladium is 7.42wt%, silver is 10.2wt%, and cesium oxide is 0.65wt%. Get the titania-supported catalyst 1g prepared above, water 100ml, and tar 5g and join in the reactor, and hydrogen replaces the air in the reactor for 5 times. , at a temperature of 120° C., a pressure of 3 MPa, a stirring speed of 900 rpm, and react for 1 h. After cooling to room temperature, the reaction solu...

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Abstract

The invention relates to a method for the catalytic hydrocracking of phenol-containing tar to recycle diphenol, and a catalyst used for the method. The method takes cesium salt modified titanium dioxide supported with palladium and silver as the catalyst, and takes phenol-containing tar as a reaction raw material to perform direct catalytic hydrogenation to directly synthetize catechol/hydroquinone in an ethanol solvent. The method is simple in operation, green and environmentally friendly; the method can perform recycling on hydroquinone products remained in the phenol-containing tar, and canperform re-hydrocracking on the tar generated by phenol dimerization and deep oxidation so that diphenol products with high added values can be obtained, and therefore, treatment costs of solid wastecan be reduced, and the yield of the diphenol products can be significantly enhanced.

Description

technical field [0001] The invention belongs to the technical field of catalytic hydrogenation, and in particular relates to a method for recovering diphenol by catalytic hydrocracking of phenol-containing tar and a catalyst used in the method. Background technique [0002] Catechol and hydroquinone are important fine chemical products with a wide range of uses. The method of producing o- and hydroquinone by hydroxylation of phenol with hydrogen peroxide as an oxidant is a production process widely used in the world. At present, the international development of hydrogen peroxide phenol hydroxylation synthetic quinone process routes include Rhone-Poulenc method, keto-acid method, Brichima method, Enichem method, etc. Currently, the commonly used methods in industry are Rhone-Poulenc method and Enichem method. Regardless of the process, a certain amount of phenol-containing tar is produced as a by-product during the phenol hydroxylation reaction. [0003] craft ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/58B01J37/08B01J37/18C07C37/055C07C39/08
CPCC07C37/055B01J23/58B01J37/082B01J37/18C07C39/08Y02P20/584Y02P20/52
Inventor 付松李俊平吴训锟丁大康林建东王锐黎源
Owner WANHUA CHEM GRP CO LTD
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