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Zirconium-based alkylation catalyst and preparation method and application thereof

A technology of alkylation reagent and zirconium alkane, which is applied in the direction of catalyst activation/preparation, carbon compound catalyst, physical/chemical process catalyst, etc., can solve the problem of double-substituted alkyl anthracene easy to generate anthracene conversion rate, etc., and achieve easy recovery and recycling, high selectivity, and high catalytic activity

Active Publication Date: 2021-06-18
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, for the way of catalyzing the direct alkylation of anthracene to 2-alkylanthracene, different alkylating reagents have corresponding requirements on the acidity and pore channels of molecular sieve catalysts, so there are greater challenges. For example, disubstituted alkylanthracene is easy to form or low conversion rate of anthracene, it is necessary to further study and modify the catalyst
[0004] The invention provides a molecular sieve as carrier, ZrO 2 As the active component, organic acid is used as a highly dispersed solid acid catalyst as a modifier, and it is used for the reaction of anthracene and tert-amyl alcohol to prepare 2-tert-amylanthracene. There is no similar report before

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  • Zirconium-based alkylation catalyst and preparation method and application thereof

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Embodiment approach

[0025] According to a preferred embodiment of the present invention, the catalyst is composed of MOR carrier and highly dispersed zirconium obtained by complex modification with citric acid.

[0026] The second aspect of the present invention provides a method for preparing a highly dispersed zirconium-based catalyst, the method comprising:

[0027] (1) Disperse the zirconium salt and the modifying agent in water, stir, then add the carrier, and continue to stir under the magnetic force at room temperature, then evaporate the turbid liquid to remove excess water, and obtain the composite modified precursor after drying the obtained solid;

[0028] (2) Grinding, calcining and annealing the composite modified precursor to obtain a zirconium-based alkylation catalyst.

[0029] In the described composite modified precursor, relative to the carrier of 100 parts by weight, the total content of zirconium is 10-40 parts by weight, preferably 15-25 parts by weight, in terms of oxides; ...

Embodiment 1

[0042] The first step of catalyst preparation: 3.1g of zirconium nitrate pentahydrate and 1.65g 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 2 hours, and then the water was evaporated at 80°C, dried at 100°C for 24 hours, ground, and calcined at 500°C for 10 hours to prepare a citric acid-modified 18wt% Zr-MOR molecular sieve catalyst.

[0043] The second step of catalytic alkylation reaction: take the Zr-MOR molecular sieve catalyst (50wt%, 1.0g) and anthracene (2.0g) obtained in the first step, add 12mL3,4-dichlorobenzotrifluoride as a solvent, and then add tert-amyl Alcohol (1.1eq, 1.1g) was used as an alkylating agent. Stir at room temperature to fully mix and activate. The initial pressure was 2.0MPa, and then the temperature was programmed to rise to 170°C. The total reaction time was 4h. According to gas phase analysis, the selectivity of 2-tert-amylanthracen...

Embodiment 2

[0051] 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. Continue to stir for 2h, then evaporate the water at 80°C, dry at 100°C for 24h, grind, and calcine at 500°C for 10h to prepare a 22wt% Zr-MOR molecular sieve catalyst modified by citric acid. The X-ray single crystal diffraction pattern is shown in figure 1 .

[0052] The second step of catalytic alkylation reaction: take the Zr-MOR molecular sieve catalyst (30wt%, 0.6g) and anthracene (2.0g) obtained in the first step, add 12mL3,4-dichlorobenzotrifluoride as a solvent, and then add tert-amyl Alcohol (1.1eq, 1.1g) was used as an alkylating agent. Stir at room temperature to fully mix and activate. The initial pressure was 2.0MPa, and then the temperature was programmed to rise to 170°C. The total reaction time was 4h. According to gas phase analysis, ...

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Abstract

The invention discloses a zirconium-based alkylation catalyst and a preparation method and application thereof, and the preparation method of the catalyst comprises the following steps: (1) dispersing zirconium salt and a modifier in water, stirring, then adding a carrier, stirring under room-temperature magnetic force, evaporating to remove excessive moisture, and drying to obtain a compound modified precursor; and (2) grinding, calcining and annealing the compound modified precursor prepared in the step (1) to obtain the compound modified zirconium-based alkylation catalyst. The zirconium-based catalyst is high in activity, has relatively high selectivity on the target product 2-tert-amyl anthracene, is stable in catalytic performance, also has relatively excellent cyclic regeneration performance, and is suitable for popularization in industrial production.

Description

technical field [0001] The invention relates to the field of alkylanthracene compounds, in particular to a method for preparing an organic acid-modified highly dispersed zirconium-based catalyst and its application in anthracene alkylation to synthesize 2-tert-amylanthracene. Background technique [0002] 2-Alkyl anthracene, such as 2-methyl anthracene, 2-ethyl anthracene, 2-pentyl anthracene, 2-tert-amyl anthracene and 2-tert-butyl anthracene, is an important organic chemical raw material, and its oxidation product 2 -Alkyl anthraquinone is an important fine chemical. At present, most companies use 2-ethylanthraquinone as the carrier for the production of hydrogen peroxide, and the oxidation product of 2-tert-amylanthracene, 2-tert-amylanthraquinone, has greater solubility in the working fluid, which can reduce the production cost of hydrogen peroxide. Thereby having more obvious advantage. However, in the direct alkylation of anthracene, it is easy to generate polysubsti...

Claims

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Application Information

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IPC IPC(8): B01J31/04B01J29/70B01J37/00B01J37/08C07C2/70C07C2/86C07C15/28
CPCB01J31/04B01J29/7049B01J29/7057B01J37/0036B01J37/08C07C2/70C07C2/864C07C2531/04C07C2529/70C07C2603/24B01J2229/186B01J2229/16B01J2229/37B01J2231/4205C07C15/28
Inventor 戴立言蔡梦露王晓钟陈英奇
Owner ZHEJIANG UNIV
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