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A kind of preparation method and application of fly ash immobilized copper p-toluenesulfonate catalyst

A technology of copper p-toluenesulfonate and fly ash, applied in the field of fine chemical industry, can solve the problems of difficult separation of catalyst and product, high price of ionic liquid, narrow source surface, etc., and achieves good reuse performance, good industrialization prospects, and production simple craftsmanship

Active Publication Date: 2020-11-17
NANJING POLYTECHNIC INSITUTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is a large difference between coastal and inland areas. The utilization rate of fly ash in coastal areas such as Shanghai and Nanjing exceeds 100%, but the utilization rate of fly ash in inland areas such as Shanxi and Inner Mongolia is still less than 5%.
Due to the high price and narrow sources of ionic liquids, there is still a long way to go before large-scale industrialization; heteropolyacids, p-toluenesulfonic acid and their salts have the advantages of high activity and high selectivity, but they have their own As a liquid, it is difficult to separate the catalyst and product after the reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Preparation of fly ash immobilized copper p-toluene sulfonate catalyst Weigh dry fly ash 100g, prepare sodium hydroxide solution 0.1M, its ratio to dry weight of fly ash is 0.5:3.0, 90 ℃ and continue to fully stir for 0.5h, put The temperature drops to 30°C, and CO is continuously injected 2 And keep stirring until the pH value is controlled to 7.0, remove impurities by centrifugal filtration, wash with deionized water until neutral to obtain filter cake material; impregnation: add 5 times of deionized water (based on the weight of the above filter cake), add p-toluenesulfonate Acid copper (the amount is 5% of the above-mentioned dry filter cake), stirred until completely dissolved, added the above-mentioned wet filter cake and beating until no solid agglomerates exist, then sprayed into fine particles, controlled spray inlet temperature 350 ° C, outlet temperature 160°C, the obtained solid particles are the activated fly ash immobilized copper p-toluenesulfonate cataly...

Embodiment 2

[0025] Preparation of fly ash immobilized copper p-toluenesulfonate catalyst Weigh dry fly ash 100g, prepare sodium hydroxide solution 1.0M, its ratio to fly ash dry weight: 0.5:1.0, 40 ℃ continue to fully stir for 5.0h, put Lower the temperature to 30°C, continue to pour in hydrochloric acid and keep stirring, the acid solution concentration: 0.5M, until the pH value is controlled to 9.0, the dropping time: 1.0h, remove impurities by centrifugal filtration, wash with deionized water until 0.1N silver nitrate No detectable Cl in the solution - That is, the filter cake material; impregnation: add 10 times of deionized water (based on the weight of the above-mentioned filter cake), add copper p-toluenesulfonate (the amount is 30% of the above-mentioned dry filter cake), stir until completely dissolved, add the above-mentioned Wet the filter cake and beat until there is no solid agglomerate, and then use spray to form fine particles, control the spray inlet temperature to 300°C, ...

Embodiment 3

[0028] Preparation of fly ash immobilized copper p-toluenesulfonate catalyst Weigh dry fly ash 100g, prepare potassium hydroxide solution 0.5M, its ratio to fly ash dry weight: 0.5:1.5, continue to fully stir at 50°C for 2.0h, and The temperature will be 60°C, continue to pour sulfuric acid and keep stirring, the concentration of acid solution: 1.0M, until the pH value is controlled to 8.0, the time of dropping: 0.5h, centrifugal filtration to remove impurities, wash with deionized water until it is chlorinated with 0.1N Barium solution does not detect and obtains sulfate radical ion and obtains filter cake material; Impregnation: add 6 times of deionized water (based on the above-mentioned filter cake weight), add copper p-toluenesulfonate (its amount is 20% of the above-mentioned dry filter cake) ), stir until completely dissolved, add the above wet filter cake and beat until there is no solid agglomerate, then spray it into fine particles, control the spray inlet temperature...

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PUM

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Abstract

The invention provides a preparation method of a flyash-immobilized copper p-toluene sulfonate catalyst. The preparation method is characterized by comprising: activating flyash and immobilizing copper p-toluene sulfonate. The activating step of flyash includes: dissolving with a base, filtering to remove impurity, neutralizing, washing, and filtering to obtain filter cake. The immobilizing step of copper p-toluene sulfonate includes the steps, such as impregnating, spray-drying and activating, to obtain high-performance solid, the copper p-toluene sulfonate catalyst. The catalyst prepared bythe preparation method is equivalent to concentrated sulfuric acid catalysts in catalytic performance, while the catalyst has the advantages that, for instance, the reaction product is colorless, thecatalyst is simple to separate and well reusable, the production process is simple, and production investment is low.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and in particular relates to a preparation method of a fly ash immobilized copper p-toluenesulfonate catalyst and its application in the synthesis of tributyl citrate. Background technique [0002] Copper p-toluenesulfonate is a catalyst that can replace sulfuric acid, and it is widely used. In recent years, there are many research reports. It not only has high reactivity, good selectivity, and the product color is light or even colorless, and it is close to neutral. Equipment, pipeline valves, etc. are almost non-corrosive, which can greatly reduce the investment in equipment and so on; but because it is soluble in water, etc., there are problems such as difficult separation of catalyst and product. In order to facilitate the separation of the catalyst and the product after the reaction, facilitate the recovery and reuse of the catalyst, and reduce the amount of the active phase of the cata...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J37/02C07C67/08C07C69/704
CPCB01J31/0225B01J37/0063B01J37/0207B01J2231/49C07C67/08C07C69/704
Inventor 吴永忠展海风鹿康薛瑞陈蕾钱宇缪领珍张萍
Owner NANJING POLYTECHNIC INSITUTE
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