Prepn of phosphotungstic anion intercalated strontium aluminate hydrotalcite-solid acid alkylation catalyst

A technology of solid acid catalyst and anion intercalation, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc. It can solve the problems of reducing the yield of mesitylene, limiting the scope of product application, and requiring high production equipment. problems, to achieve the effects of no catalyst residue, stable reaction activity, and reduced production costs

Inactive Publication Date: 2006-05-17
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the main problem that this method exists at present is: the alkylation catalyst adopts anhydrous AlCl 3 , while anhydrous AlCl 3 The activity is too high, and part of mesitylene also participates in the alkylation reaction, which reduces the yield of mesitylene; while AlCl 3 It has strong water absorption and corrosiveness, and has high requirements for production equipment; anhydrous AlC...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 15.05g Al(NO 3 ) 3 9H 2 O and 18.76g Sr(NO 3 ) 2 Dissolve in 200mL deionized water, vigorously mix and stir, heat to 90°C, slowly add 0.1mol / L NaOH dropwise until the pH is 8.5. After stirring for 4 hours, cool down to 60°C and crystallize for 24 hours to obtain a white precipitate, filter it while it is hot, and disperse the precursor in deionized water to form a suspension with a solid content of 7%. Take 5g of phosphotungstic acid Dissolve in 200mL precursor suspension, ion-exchange in an ultrasonic oscillator for 2h, filter and exchange again in this way, adjust the pH to 6.0 with NaOH, filter with suction, and dry in an oven at 60°C to obtain a white solid. Sieve after crushing, and take 60-80 mesh particles as the catalyst.

[0022] Butene / C9(n / n)

0

0.3

0.6

0.9

n-Propylbenzene%

Cumene%

m-p-methylethylbenzene%

o-methyl ethyl benzene%

Trimethylbenzene%

Mesitylene%

other%

Mesitylene / C9

...

Embodiment 2

[0028] 18.76g Al(NO 3 ) 3 9H 2 O and 21.163g Sr(NO 3 ) 2 Dissolve in 200mL deionized water, vigorously mix and stir, heat to 95°C, slowly add 0.1mol / L NaOH dropwise until the pH is around 8.5. After stirring for 4 hours, cool down to 80°C and crystallize for 24 hours to obtain a white precipitate, filter it while it is hot, and obtain the precursor; disperse the precursor in deionized water to form a suspension with a solid content of 8%, take 7g of phosphotungstic acid Dissolve in 200mL precursor suspension, ion-exchange in an ultrasonic oscillator for 2 hours, filter and exchange again in this way, adjust the pH to 6.0-6.5 with NaOH, filter with suction, and dry in an oven at 70°C to obtain a white solid . Sieve after crushing, and take 60-80 mesh particles as the catalyst.

[0029] Butene / C9(n / n)

0

0.3

0.6

0.9

n-Propylbenzene%

Cumene%

m-p-methylethylbenzene%

o-methyl ethyl benzene%

Trimethylbenzene%

Mesi...

Embodiment 3

[0035] 20.05g Al(NO 3 ) 3 9H 2 O and 24.18g Sr(NO 3 ) 2Dissolve in 200mL deionized water, vigorously mix and stir, heat to 98°C, slowly add 0.1mol / L NaOH dropwise until the pH is 9.1. After stirring for 2 hours, lower the temperature to 80°C and crystallize for 12 hours to obtain a white precipitate, filter it while it is hot, and obtain the precursor; disperse the precursor in deionized water to form a suspension with a solid content of 10%, take 10g of phosphotungstic acid to dissolve In the suspension of 200mL precursor, ion exchange in ultrasonic oscillator for 2h, filter and exchange again according to this method, adjust pH to 6.5 with NaOH, filter with suction, dry in oven at 80°C to obtain white solid. Sieve after crushing, and take 60-80 mesh particles as the catalyst.

[0036] The product composition (liquid phase reaction) when the mixed C9 aromatic hydrocarbons containing 38.43% mesitylene is fed with different amounts of 1-butene:

[0037] Butene / C9...

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PUM

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Abstract

The present invention is the preparation process of phosphotungstic anion intercalated strontium aluminate hydrotalcite as one kind of solid acid catalyst for C9 arene alkylation to separate and prepare trimethylbenzene. The preparation process includes the following steps: dissolving Al(NO3)3.9H2O in 15-21 weight portions and Sr(NO3)2 in 18-25 weight portions separately in deionized water of 100 weight portions and mixing via stirring; dropping 0.1 mol/L concentration NaOH or CsOH solution slowly while heating to reach pH 8.2-9.1; dispersing the precursor in deionized water to form suspension with solid content 7-10 %, dissolving phosphotungstic acid in 3-5 wt% in the suspension, and ion exchanging and filtering in a ultrasonic vibrator; adding NaOH or CsOH solution to regulate pH value to 6.0-6.5, suction filtering and stoving at 60-100 deg.c in an oven.

Description

technical field [0001] The invention relates to a preparation method of a phosphotungstic acid anion intercalation aluminum strontium hydrotalcite alkylation solid acid catalyst used in the process of preparing mesitylene by alkylation and separation of mixed C9 aromatic hydrocarbons. 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, mesitylene, wheat field herbicides, and ultraviolet absorbers 2,4,6-trimethylbenzene Methyl phenol, antioxidant 330, etc. It is also the main raw material for the preparation of mesitylenesulfonic acid, trimesic acid, trimesic triacetic acid, etc. Its industrial production methods mainly include isomerization and alkylation separation and purification methods. The isomerization method uses mesitylene as a raw material to carry out an isomerization reaction to generate mesitylene, but due to technical reasons, it is difficult...

Claims

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Application Information

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IPC IPC(8): B01J37/00B01J27/188B01J37/30C07C7/00C07C15/02
Inventor 周钰明陈伴生
Owner SOUTHEAST UNIV
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