Method for obtaining 2-alkyl anthracene through anthracene alkylation and preparing 2-alkyl anthraquinone through catalytic oxidation

A technology for catalytic oxidation and alkyl anthraquinone, applied in the direction of oxidized quinone preparation, carbon compound catalysts, chemical instruments and methods, etc.

Active Publication Date: 2020-10-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In summary, there is no report on a complete set of techno

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  • Method for obtaining 2-alkyl anthracene through anthracene alkylation and preparing 2-alkyl anthraquinone through catalytic oxidation
  • Method for obtaining 2-alkyl anthracene through anthracene alkylation and preparing 2-alkyl anthraquinone through catalytic oxidation
  • Method for obtaining 2-alkyl anthracene through anthracene alkylation and preparing 2-alkyl anthraquinone through catalytic oxidation

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specific Embodiment approach

[0063] According to a specific embodiment of the present invention, in step (2-3), the method for described multi-step distillation comprises:

[0064] Method 1: if figure 2 As shown, the feed liquid of a series of alkylanthracene products containing 2-alkylanthracene is subjected to the first distillation, and the distillate containing the light component Cj1-anthracene and the bottom product containing the heavy component Cj2-anthracene are separated; The distillate containing the light component C1j-anthracene is subjected to a second distillation to obtain a distillate containing the light component Cj3-anthracene, and a bottom product containing the target product Ci-anthracene;

[0065] Among them, the light component Cj1-anthracene is an alkyl anthracene product whose total carbon number j1 of the alkyl side chain is an integer of 1

Embodiment 1

[0118] (1) Alkylation reaction.

[0119]Alkylation of anthracene and isopentene to prepare 2-pentylanthracene, mesitylene and N,N-dimethylformamide as a combined solvent, the catalyst is a spherical catalyst containing active Y-type molecular sieve, and alumina is used as a binder , based on the total weight of the catalyst, the content of the active Y molecular sieve is 82% by weight, the content of the binder is 18% by weight, and the average particle diameter of the catalyst particles is 100 μm. At room temperature, 460 g of anthracene, 640 ml of mesitylene, 160 ml of N,N-dimethylformamide, and 205 g of catalyst were added to a 2L stirred tank. After sealing, the temperature is raised to 165° C. at a rotational speed of 1000 rpm, and the pressure is 0.3 MPa. 151 g of isoamylene was added to the kettle through a plunger pump, and the feed rate was 6.6 g / min. After the feeding of isopentene was completed, the reaction was continued for 270 min while maintaining the reaction...

Embodiment 2

[0130] Prepare 2-alkylanthraquinones according to the method of Example 1, the difference is that in step (2), the cooling rate is 5.0°C / h, the crystallization temperature is 190°C, and the amount of seed crystal anthracene added accounts for 4% of the mass of the molten mixture. % by weight, the crystal growth time is controlled at 4h. After the crystallization process is over, the uncrystallized feed liquid is discharged and sent to the vacuum distillation system. Slowly heat up and sweat the crystal in the crystallizer, the heating rate is 4°C / h, the sweating end temperature is 195°C, the sweating amount is 10% by weight of the crystal mass, the sweating liquid circulates and contacts the material entering the melting crystallizer After that, the crystallization operation is carried out together. The uncrystallized alkylanthracene mixture is sent to the vacuum distillation system for the first vacuum distillation. The top pressure is 1KPa, the bottom temperature is 259°C, ...

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Abstract

The invention relates to the field of preparation of 2-alkyl anthraquinone. The invention specifically discloses a method for obtaining 2-alkyl anthracene through anthracene alkylation and preparing 2-alkyl anthraquinone through catalytic oxidation. The method comprises the following steps: anthracene makes contact with an alkylation reagent for an alkylation reaction, a reaction product containing alkyl anthracene is prepared, and an alkylation reaction solvent is a combination of a solvent A with the dielectric constant being 1-10 at the temperature of 20 DEG C and a solvent B with the dielectric constant being larger than 10 and smaller than or equal to 50 at the temperature of 20 DEG C; the anthracene is separated from the reaction product containing the alkyl anthracene through melt crystallization, and the 2-alkyl anthracene is separated through distillation; the 2-alkyl anthracene is contacted with an oxidizing agent for oxidation reaction. The alkylation combined solvent and the catalyst are adopted, so that the selectivity of the 2-alkyl anthracene is high; the adopted separation method can significantly reduce the separation operation difficulty, and the product purity ishigh; the adopted oxidation system is simple and efficient, and the catalyst is low in cost and easy to recycle.

Description

technical field [0001] The invention relates to a method for preparing organic matter, in particular to a method for preparing 2-alkylanthracene by catalyzing and oxidizing anthracene to obtain 2-alkylanthraquinone. Background technique [0002] Hydrogen peroxide is an important green basic chemical with a high degree of industrial relevance. Since 2008, my country has become the largest country in the production of hydrogen peroxide, and its consumption in 2015 has exceeded 10 million t / a ( at 27.5%). At present, the process technology for producing hydrogen peroxide at home and abroad is mainly the anthraquinone method. The 2-alkylanthraquinone in this process is used as the "carrier" of the process, which directly affects the quality and output of hydrogen peroxide. The phthalic anhydride method is the main method to produce 2-alkylanthraquinones, but there are serious pollution problems in this process. To produce 1 ton of 2-ethylanthraquinone, it needs to invest 1.76 ...

Claims

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Application Information

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IPC IPC(8): C07C46/04C07C50/18
CPCC07C2/02C07C7/005C07C7/04C07C7/14C07C46/04C07C2521/06C07C2523/10C07C2523/28C07C2523/745C07C2529/70C07C2603/24C07C50/18C07C15/28
Inventor 郑博费建奇潘智勇朱振兴毛俊义宗保宁
Owner CHINA PETROLEUM & CHEM CORP
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