Alkylation solid acid catalyst and process for preparing the same

A solid acid catalyst, alkylation technology, applied in physical/chemical process catalysts, chemical instruments and methods, organic chemistry, etc. Separation, high conversion rate and good regeneration performance

Inactive Publication Date: 2009-06-24
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A variety of solid acid catalysts for alkylation reactions such as molecular sieves, supported heteropolyacids, and solid superacids have been reported. Solid superacid catalysts mainly include SO 4 2- /M x o y (Metal oxide) type catalyst, but the catalyst has fatal defects such as easy deactivation and short life. Molecular sieve catalys

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 16.1 gZrOCl 2 ·8H 2 Dissolve O in 100mL deionized water, slowly add 28wt% ammonia water dropwise under stirring to hydrolyze and precipitate to pH 8.5, continue stirring for 0.5h, age at 20°C for 14h, filter with suction, and wash the precipitate repeatedly with deionized water Until the filtrate is tested with silver nitrate, there is no Cl - Until the existence of , the precipitate was dried at 120 ° C for 24 hours to obtain white powder ZrO 2 ·xH 2 O precipitate. The above ZrO 2 ·xH 2 O precipitate powder 6.0g with 18.1mL 10mmol / L of KNO 3 Immerse at 20°C for 24h, evaporate to dryness at 80°C, and dry at 120°C for 24h to obtain K-modified modified zirconia. The modified zirconia was impregnated with 20.0mL 17.4mmol / L phosphotungstic acid ethanol solution at 20°C for 24h, evaporated to dryness at 60°C, dried at 120°C for 24h, calcined at 700°C for 6h, and cooled to obtain an alkylated solid acid catalyst.

[0019] 50.0g of C9 mixed aromatics as the reaction ra...

Embodiment 2

[0021] 16.1g ZrOCl 2 ·8H 2 Dissolve O in 100mL deionized water, slowly add 30wt% ammonia water dropwise under stirring for hydrolysis and precipitation until the pH value is 10.0, continue to stir for 0.5h, age at 20°C for 14h, filter with suction, and wash the precipitate repeatedly with deionized water Until the filtrate is tested with silver nitrate, there is no Cl - Until the existence of , the precipitate was dried at 120 ° C for 24 hours to obtain white powder ZrO 2 ·xH 2 O precipitate. The above ZrO 2 ·xH 2 O precipitate powder 6.0g with 10.2mL 0.5mmol / L LaNO 3 Immerse at 20°C for 24h, evaporate to dryness at 80°C, and dry at 120°C for 24h to obtain La-modified modified zirconia. The modified zirconia was impregnated with 20.0mL 17.4mmol / L phosphotungstic acid ethanol solution at 20°C for 24h, evaporated to dryness at 60°C, dried at 120°C for 24h, calcined at 800°C for 6h, and cooled to obtain an alkylated solid acid catalyst.

[0022]50.0g of C9 mixed aromatics...

Embodiment 3

[0024] 16.1 gZrOCl 2 ·8H 2 Dissolve O in 100mL deionized water, slowly add 25wt% ammonia water dropwise under stirring to hydrolyze and precipitate to a pH value of 9.5, continue to stir for 0.5h, age at 20°C for 13h, filter with suction, and wash the precipitate repeatedly with deionized water Until the filtrate is tested with silver nitrate, there is no Cl - The precipitate was dried at 120°C for 24 hours to obtain white powder ZrO 2 ·xH 2 O precipitate. The above ZrO 2 ·xH 2 O precipitate powder 6.0g with 9.1mL 10mmol / L KNO 3 and 5.1mL of 0.5mmol / L LaNO 3 The mixed solution was impregnated at 25°C for 24h, evaporated to dryness at 80°C, and dried at 120°C for 24h to obtain K and La modified zirconia. The modified zirconia was impregnated with 20.0mL 17.4mmol / L phosphotungstic acid ethanol solution at 25°C for 24h, evaporated to dryness at 60°C, dried at 120°C for 24h, calcined at 800°C for 6h, and cooled to obtain an alkylated solid acid catalyst.

[0025] 50.0g of...

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PUM

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Abstract

The invention discloses an alkylated solid acid catalyst and a preparation method thereof, and relates to an alkylated solid acid catalyst for a process of preparing mesitylene by mixed C9 aromatic hydrocarbon through alkalation separation and a preparation method thereof. The catalyst has higher alkylation conversion rate of the mixed C9 aromatic hydrocarbon and yield of the mesitylene under high temperature and normal pressure conditions. The catalyst takes heteropoly acid as a main active constituent, modified zirconium oxide as a carrier and alkali metal or rare earth element metal as a modifying agent; and calculated as the weight of zirconium oxide, the adding amount of the alkali metal is between 0.01 and 10 weight percent, the adding amount of the rare earth element metal is between 0.01 and 10 weight percent, the loading capacity of the heteropoly acid is between 5 and 30 weight percent, and the balance being the carrier.

Description

technical field [0001] The invention relates to an alkylation solid acid catalyst used in the process of preparing mesitylene by alkylation and separation of C9 mixed aromatics and a preparation method thereof, belonging to the catalyst preparation technology in the technical field of industrial catalysis. Background technique [0002] Mesitylene (1,3,5-trimethylbenzene) is an important chemical raw material, and it can be used as a raw material to prepare dye intermediates, mesitidine, wheat field herbicides, and ultraviolet absorbers2,4,6 -Trimethylphenol, Antioxidant 330, etc. It is also the main raw material for the preparation of mesitylenesulfonic acid, trimesic acid, trimesic triacetic acid, etc. At present, its industrial production mainly adopts methods such as isomerization of trimethylbenzene and alkylation of C9 mixed aromatics, separation and purification, while the method of isomerization of trimethylbenzene needs to be carried out under high temperature and pr...

Claims

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Application Information

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IPC IPC(8): B01J27/19C07C15/02
Inventor 周钰明盛晓莉张黎莉朱菊芬赵宏海
Owner SOUTHEAST UNIV
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