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Obtaining 2-alkylanthracene by anthracene alkylation and reacting to prepare 2-alkylanthraquinone

A technology of alkylation reaction and alkyl anthraquinone, which is applied in the field of preparation of organic matter, to achieve the effect of reducing operation difficulty, reasonable and feasible technical route, and low pollution

Active Publication Date: 2021-07-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In summary, there is no report on a complete set of technology for the preparation of 2-alkylanthraquinones from anthracene

Method used

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  • Obtaining 2-alkylanthracene by anthracene alkylation and reacting to prepare 2-alkylanthraquinone
  • Obtaining 2-alkylanthracene by anthracene alkylation and reacting to prepare 2-alkylanthraquinone
  • Obtaining 2-alkylanthracene by anthracene alkylation and reacting to prepare 2-alkylanthraquinone

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specific Embodiment approach

[0060] According to a specific embodiment of the present invention, in step (2-3), the method for described multi-step distillation comprises:

[0061] 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;

[0062] 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<j1<i+1, and the heavy component Cj2-anthracene is the total carbon number of the alkyl side chain j2 is i< The alkylanthracene product of t...

Embodiment 1

[0107] (1) Alkylation reaction.

[0108] 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 reactio...

Embodiment 2

[0118] 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-alkylanthraquinones, and specifically discloses a method for preparing 2-alkylanthraquinones by alkylation of anthracene and reacting them to prepare 2-alkylanthraquinones, the method comprising: (1) Under alkylation conditions and in the presence of an alkylation reaction solvent and a catalyst, anthracene is contacted with an alkylation agent to carry out an alkylation reaction to prepare a reaction product containing alkyl anthracene, and the alkylation reaction solvent is 20° C. A combination of solvent A with a dielectric constant of 1-10 and a solvent B with a dielectric constant of greater than 10 to less than or equal to 50 at 20°C; (2) melting and crystallizing the reaction product containing anthracene to separate anthracene and distillation Separating 2-alkylanthracene; (3) preparing 2-alkylanthraquinone from 2-alkylanthracene. The method provided by the invention opens up a new direction for the green preparation of 2-alkylanthraquinone.

Description

technical field [0001] The invention relates to a method for preparing organic matter, in particular to a method for obtaining 2-alkylanthracene by alkylation of anthracene and reacting to prepare 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....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C2/70C07C46/04C07C15/28C07C50/16
CPCC07C2/70C07C46/04C07C2529/08C07C15/28C07C50/16
Inventor 郑博潘智勇费建奇朱振兴毛俊义宗保宁
Owner CHINA PETROLEUM & CHEM CORP
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