High-temperature-resistant solid acid catalyst based on direct coal liquefaction heavy organic component and preparation method and application of catalyst

A solid acid catalyst, coal direct liquefaction technology, applied in the direction of preparation of organic compounds, organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, etc., can solve the problem of poor high temperature resistance and heavy coal liquefaction Solve the problems of difficult utilization of organic fractions, and achieve the effects of good thermal stability, high mechanical strength and low cost

Active Publication Date: 2016-08-24
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems of poor high temperature resistance of traditional solid acid catalysts and difficult utilization of heavy organic fractions in coal liquefaction, the purpose of the present invention is to provide a high temperature resistant solid acid catalyst based on direct coal liquefaction of heavy organic fractions and its preparation method and application

Method used

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  • High-temperature-resistant solid acid catalyst based on direct coal liquefaction heavy organic component and preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Mechanically mix 10g of ground coal direct liquefaction heavy organic matter with 3g of p-phenylenedimethanol, and mechanically stir it under an inert atmosphere at 120°C to obtain a molten viscous mixture, then add 0.5g of p-toluenesulfonic acid , After reacting for 3 hours, the temperature was raised to 160°C and kept for 4 hours to obtain product A. A certain amount of product A was weighed and placed in a muffle furnace, and kept at 500° C. for 6 h under a flowing helium atmosphere (100 ml / min) to obtain product B. Weigh 1 g of product B in a reactor, and add 20 g of 50% fuming sulfuric acid. Under the argon gas flow rate of 100ml / min, the temperature was raised to 80°C, and the mixture was continuously stirred. After reacting for 2 hours, stop the reaction, suction filter and wash the obtained product until the filtrate is neutral, until no sulfate ions are detected in the filtrate with barium chloride aqueous solution, and then dry the filter cake to obtain a hig...

Embodiment 2

[0027] Mix 10g of the ground coal direct liquefaction heavy organic matter with 4g of benzaldehyde evenly, and under an inert atmosphere at 140°C, mechanically stir to obtain a molten viscous mixture, then add 0.1g of 98% sulfuric acid solution, and react for 3 hours , and then raise the temperature to 160° C., and keep the temperature for 4 hours to obtain the product A. A certain amount of product A was weighed and placed in a muffle furnace, and the temperature was raised to 600° C. under a flowing argon atmosphere (100 ml / min), and kept for 3 hours to obtain product B. Weigh 1 g of product B into a reactor, and add 20 g of chlorosulfonic acid. Under the nitrogen flow rate of 300ml / min, the temperature was raised to 60°C, and the mixture was stirred continuously. After reacting for 24 hours, stop the reaction, suction filter and wash the obtained product until the filtrate is neutral, until no sulfate ions are detected in the filtrate with barium chloride aqueous solution,...

Embodiment 3

[0028] Mechanically mix 10g of ground coal directly liquefied heavy organic matter with 3g of paraformaldehyde, and mechanically stir under an inert atmosphere at 120°C to obtain a molten viscous mixture, then add 0.5g of 50% sulfuric acid solution, and react After 4 hours, the temperature was raised to 160° C. and kept for 4 hours to obtain product A. A certain amount of product A was weighed and placed in a muffle furnace, and kept at 180° C. for 12 h under a flowing air atmosphere (500 ml / min) to obtain product B. Take by weighing product B1g in reactor, add 30 grams of fuming sulfuric acid (15wt% SO 3 ). Under the nitrogen flow rate of 250ml / min, the ice bath was cooled to 0°C, and the stirring was continued. After reacting for 48 hours, stop the reaction, suction filter and wash the obtained product until the filtrate is neutral, until no sulfate ions are detected in the filtrate with barium chloride aqueous solution, and then dry the filter cake to obtain a high temper...

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Abstract

The invention discloses a high-temperature-resistant solid acid catalyst based on a direct coal liquefaction heavy organic component and a preparation method and application of the catalyst. The method comprises the following steps that 1, the direct coal liquefaction heavy organic component reacts with a curing agent to obtain a product A, and the product A or the direct coal liquefaction heavy organic component is placed in air or an inert atmosphere for thermal treatment to obtain a thermal stabilization product B; 2, sulfonation is conducted, wherein the product B and a sulfonating agent are mixed and then placed in a closed reactor to react under an inert atmosphere, a generated reaction mixture is filtered, washed and dried, and then the high-temperature-resistant solid acid catalyst is obtained. Accordingly, the utilization mode of the direct coal liquefaction heavy organic component is widened, and the additional value of the direct coal liquefaction heavy organic component is increased. The high-temperature-resistant solid acid catalyst has the advantages of being high in acid content, good in thermal stability, low in cost, capable of being used repeatedly and the like and can be used for ester synthesis reactions such as synthesis of polyol ester, polybasicester and the like under the high temperature condition.

Description

technical field [0001] The invention relates to a high-temperature-resistant solid acid catalyst based on coal direct liquefaction of heavy organic matter, a preparation method and application thereof, and belongs to the technical field of fine chemicals. Background technique [0002] Compared with currently used liquid acid catalysts (such as sulfuric acid, phosphoric acid or hydrofluoric acid), solid acid catalysts have the advantages of easy separation, high recycling rate and environmental friendliness. Among many solid acid catalysts, ion exchange resin not only has the advantages of other solid acid catalysts, but also has the characteristics of adjustable catalytic activity, mild reaction conditions, good selectivity and low corrosion, and is widely used in esterification reactions, Condensation reaction and dehydration reaction and other fields. [0003] In recent years, the preparation of solid acid catalysts by low-temperature partial carbonization and sulfonation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/10C07C69/58C07C67/08B01J39/18
CPCB01J31/10B01J39/18C07C67/08C07C69/58
Inventor 周颖侯雨辰曹伟然邱介山王春雷肖南杨阳李玉龙刘瑞峰马冬菊万鹏
Owner DALIAN UNIV OF TECH
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