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Ruthenium-zirconium composite alkylation catalyst and preparation method thereof

A technology of compound alkyl and catalyst, applied in the field of alkyl anthracene compounds, can solve the problems of large proportion of di-substituted alkyl anthracene, low selectivity of 2-alkyl anthracene, serious equipment corrosion, etc., and achieve stable catalytic performance, alkyl anthracene The effect of high catalytic activity and selectivity, and overall acidity improvement

Pending Publication Date: 2021-10-01
QUZHOU RES INST OF ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to propose a ruthenium-zirconium composite alkylation catalyst in order to overcome the problems of low selectivity of 2-alkylanthracene, high specificity of double-substituted alkylanthracene and serious equipment corrosion in the anthracene alkylation process existing in the prior art. The preparation method and application of this method are simple, and the ruthenium-zirconium composite alkylation catalyst has the advantages of stable catalytic performance, high dispersion of active components, and high catalytic selectivity, so it can be used as a new choice for highly selective alkylation catalysts

Method used

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  • Ruthenium-zirconium composite alkylation catalyst and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0030] The first step of catalyst preparation: 4.12g of zirconium nitrate pentahydrate and 2.22g of citric acid were added to 60mL of deionized water at room temperature, stirred, and then 4g of MOR molecular sieves were added. Stirring was continued for 2h, and then the water was evaporated at 80°C, dried at 100°C for 24h, ground, and calcined at 500°C for 10h to prepare a citric acid-modified Zr-MOR (S1-0) molecular sieve catalyst. Add 113mg ruthenium trichloride hydrate and 115mg citric acid into 30mL deionized water at room temperature, stir, then add 2g (S1-0), continue stirring for 2h, then evaporate the water at 80°C, and dry at 100°C for 24h. Grinding and calcining at 500° C. for 10 h to prepare a ruthenium-zirconium composite alkylation catalyst (S1).

[0031] The second step of catalytic alkylation reaction: Take the S1 molecular sieve catalyst (30wt%, 300mg) and anthracene (1.0g) obtained in the first step, add 8mL of mesitylene as a solvent, and then add tert-amyl ...

Embodiment 2

[0039] The first step of catalyst preparation: add 1.03g of zirconium nitrate pentahydrate and 0.36g of tartaric acid into 30mL of deionized water at room temperature, stir, and then add 2g of all-silicon β molecular sieve. Stirring was continued for 2 hours, and then the water was evaporated at 80°C, dried at 100°C for 12 hours, ground, and calcined at 500°C for 10 hours to prepare a tartaric acid-modified 12wt% Zr-all-silicon β(S2-0) catalyst. Add 113mg ruthenium trichloride hydrate and 75mg tartaric acid into 30mL deionized water at room temperature, stir, then add 2g (S1-0), continue stirring for 2h, then evaporate the water at 80°C, dry at 100°C for 24h, grind , Calcined at 500° C. for 10 h to prepare a ruthenium-zirconium composite alkylation catalyst (S2).

[0040] The second step catalytic alkylation reaction: get S2 catalyst (30wt%, 300mg) and anthracene (1.0g) obtained in the first step, add 8mL mesitylene as solvent, then add tert-amyl alcohol (1.1eq, 0.55g) as For...

Embodiment 3

[0042] The first step of catalyst preparation: 4.12g of zirconium nitrate pentahydrate and 2.22g of citric acid were added to 60mL of deionized water at room temperature, stirred, and then 4g of MOR molecular sieves were added. Stirring was continued for 2h, and then the water was evaporated at 80°C, dried at 100°C for 24h, ground, and calcined at 500°C for 10h to prepare a citric acid-modified Zr-MOR (S1-0) molecular sieve catalyst. Add 225 mg of ruthenium trichloride hydrate and 230 mg of citric acid into 30 mL of deionized water at room temperature, stir, then add 2 g of (S1-0), continue stirring for 2 h, then evaporate the water to dryness at 80 ° C, and dry at 100 ° C for 24 h. Grinding and calcining at 500° C. for 10 h to prepare a ruthenium-zirconium composite alkylation catalyst (S3).

[0043] The second step of catalytic alkylation reaction: take the S3 molecular sieve catalyst obtained in the first step (30wt%, 300mg) and anthracene (1.0g), add 8mL of mesitylene as a...

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Abstract

The invention relates to the field of alkyl anthracene compounds, and concretely relates to a ruthenium-zirconium composite alkylation catalyst and a preparation method thereof. The catalyst comprises a carrier and a metal element loaded on the carrier, the metal element is subjected to compound modification through a modifier in advance, and the metal element is obtained by loading metal ruthenium on a zirconium alkylation catalyst; and the metal elements comprise ruthenium and zirconium, and the weight ratio of ruthenium to zirconium is (0.12-0.25): 1 in terms of oxide. The ruthenium-zirconium composite alkylation catalyst provided by the invention is a heterogeneous catalyst, the preparation method is simple and convenient, the catalyst is easy to recover and recycle, the overall acidity is improved due to modification of metal elements, and in addition, the alkylation catalytic activity and selectivity are high and the catalytic performance is more stable due to high-dispersion active components.

Description

technical field [0001] The invention relates to the field of alkylanthracene compounds, in particular to a ruthenium-zirconium composite alkylation catalyst and a preparation method thereof. Background technique [0002] 2-Alkyl anthracene is an important organic chemical intermediate. At present, the main method for producing pentanthrone is the phthalic anhydride method. There are a lot of aluminum chloride and oleum used, which seriously pollutes the environment. Anthracene and corresponding alkylating reagents are first alkylated and then oxidized to obtain 2-alkylanthracene, which is considered to be a more economical 2-alkylanthraquinone production route. It is very necessary to explore the catalyst, but the process currently has the problem of low alkylation conversion and selectivity, which seriously affects the subsequent oxidation process and then affects the quality of 2-alkylanthraquinone. [0003] For the alkylation reaction, the conversion / selectivity is close...

Claims

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Application Information

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IPC IPC(8): B01J29/22B01J29/03B01J29/74B01J31/04C07C2/86C07C15/28
CPCB01J29/22B01J29/0325B01J29/7476B01J31/04C07C2/864B01J2229/186C07C2603/24C07C15/28Y02P20/52
Inventor 戴立言蔡梦露王晓钟陈英奇
Owner QUZHOU RES INST OF ZHEJIANG UNIV
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