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A kind of sulfonic acid modified carrier supported solid acid catalyst and its preparation method and application

A solid acid catalyst, carrier-supported technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of long residence time, increased difficulty in cleaning equipment, and increased energy consumption for separation

Active Publication Date: 2022-04-26
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The incompletely reacted mixed acid stays at the bottom of the tower for too long, which may lead to the formation of high polymers and increase the difficulty of cleaning equipment
In addition, the unreacted mixed acid needs to be separated from the dibasic acid dimethyl ester in the rectification tower, which increases the energy consumption of the separation

Method used

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  • A kind of sulfonic acid modified carrier supported solid acid catalyst and its preparation method and application
  • A kind of sulfonic acid modified carrier supported solid acid catalyst and its preparation method and application
  • A kind of sulfonic acid modified carrier supported solid acid catalyst and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Preparation of sulfonic acid modified carrier loaded solid acid catalyst, the steps are:

[0064] (1) Dissolve 10g of fuming sulfuric acid in 990g of water, stir well and add 300g of activated carbon carrier (specific surface area is 1360m 2 / g, the average pore diameter is 2nm), stirred at 80°C for 3h, cooled to room temperature, and suction-filtered under a negative pressure of 30KPa to obtain a sulfonic acid-modified carrier.

[0065] (2) Dissolve 15g of zinc nitrate in 29.1g of methanol, stir well to dissolve, add 300g of sulfonic acid modified carrier to it, continue to stir until the system becomes a uniform suspension, soak at 30°C for 4h, filter, 80°C The catalyst precursor was obtained after drying for 6 h.

[0066] (3) Put the catalyst precursor into a low-temperature plasma discharger in a nitrogen environment, and discharge for 2 hours with a discharge power of 40W. Then, it was put into a microwave emitter, purged with nitrogen for 30 minutes, and then su...

Embodiment 2

[0070] Preparation of sulfonic acid modified carrier loaded solid acid catalyst, the steps are:

[0071] (1) Dissolve 37.5g chlorosulfonic acid in 713g water, stir well and add 300g porous alumina carrier (specific surface area is 300m 2 / g, the average pore diameter is 8.0nm), stirred at 90°C for 2h. After cooling down to room temperature, the sulfonic acid modified carrier was obtained by suction filtration under a negative pressure of 40KPa.

[0072] (2) Dissolve 30g of aluminum chloride in 170g of ethanol, stir well to dissolve, add 300g of sulfonic acid modified carrier to it, continue to stir until the system becomes a uniform suspension, soak at 45°C for 6h, filter, 90°C After drying for 8 hours, the catalyst precursor was obtained.

[0073] (3) Put the catalyst precursor into a low-temperature plasma discharger in a nitrogen environment, and discharge for 3 hours with a discharge power of 80W. Then, it was put into a microwave emitter, purged with argon gas for 40 m...

Embodiment 3

[0077] Preparation of sulfonic acid modified carrier loaded solid acid catalyst, the steps are:

[0078] (1) Dissolve 120g of sulfamic acid in 480g of water, stir well and add 300g of cerium-zirconium oxide carrier (specific surface area is 150m 2 / g, the average pore size is 6.6nm), stirred at 100°C for 1h. After cooling down to room temperature, the sulfonic acid-modified carrier was obtained by suction filtration under a negative pressure of 50KPa.

[0079] (2) Dissolve 90g of manganese nitrate in 270g of butanol, stir well to dissolve, add 300g of sulfonic acid modified carrier, continue to stir until the system becomes a uniform suspension, soak at 50°C for 12h, filter, 120°C After drying for 8 hours, the catalyst precursor was obtained.

[0080] (3) Put the catalyst precursor into a low-temperature plasma discharger in a nitrogen environment, and discharge for 5 hours with a discharge power of 120W. Then, it was put into a microwave emitter, purged with nitrogen for 3...

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Abstract

The invention discloses a sulfonic acid modified carrier-loaded solid acid catalyst and its preparation method and application. The preparation process is simple and easy for industrial scale-up production. The steps include (1) adding a porous material carrier into a soluble sulfur-containing liquid acid aqueous solution, Stir evenly, then perform heat treatment, cool down and filter to obtain a sulfonic acid modified carrier; (2) dissolve the soluble acidic metal salt in an organic solvent, then add a sulfonic acid modified carrier therein, stir evenly, then impregnate After filtration and drying, the catalyst precursor is obtained; (3) the catalyst precursor is treated with low-temperature plasma, and then subjected to microwave pyrolysis treatment to obtain the catalyst precursor; (4) the metal salt additive is dissolved in an organic solvent, and then added The catalyst precursor is uniformly stirred, impregnated, and then filtered and dried to obtain a solid acid catalyst loaded on a sulfonic acid modified carrier. The catalyst is used to prepare dibasic acid ester, and has the advantages of high reactivity, high selectivity and the like.

Description

technical field [0001] The invention belongs to the technical field of catalytic esterification, and in particular relates to a solid acid catalyst loaded on a sulfonic acid modified carrier and its preparation method and application. Background technique [0002] In the production process of adipic acid, after cyclohexanol and cyclohexanone are oxidized with nitric acid, while the main product adipic acid is produced, succinic acid and glutaric acid are also produced as by-products. Due to the good solubility of dibasic acids in water, the waste liquid produced by the adipic acid process has a high content of adipic acid, glutaric acid and succinic acid. It is commonly known as mixed dibasic acid waste liquid in the industry, and its color is green or green. tan. For every ton of adipic acid produced, there will be 60-70 kg of mixed dibasic acid by-products. Because the impurity and water content in these mixed dibasic acids are all very much, it is difficult to recycle. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/02C07C67/08C07C69/40C07C69/42C07C69/44
CPCB01J27/02C07C67/08C07C69/40C07C69/42C07C69/44
Inventor 靳少华刘运海蒋玉鑫赵欣丁可王磊杨洋宋延方陈永黎源
Owner WANHUA CHEM GRP CO LTD
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