Method for separating 2-alkyl anthracene from anthracene through reaction and preparing 2-alkyl anthraquinone through catalytic oxidation

An alkyl anthracene, separation technology, applied in the field of preparation of organic matter

Active Publication Date: 2020-10-27
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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  • Method for separating 2-alkyl anthracene from anthracene through reaction and preparing 2-alkyl anthraquinone through catalytic oxidation
  • Method for separating 2-alkyl anthracene from anthracene through reaction and preparing 2-alkyl anthraquinone through catalytic oxidation
  • Method for separating 2-alkyl anthracene from anthracene through reaction and preparing 2-alkyl anthraquinone through catalytic oxidation

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specific Embodiment approach

[0055] According to a specific embodiment of the present invention, in step (2-3), the method for described multi-step distillation comprises:

[0056] 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;

[0057] 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

[0112] (1) Alkylation reaction.

[0113] Alkylation of anthracene and isopentene to prepare 2-pentylanthracene, mesitylene as solvent and methanesulfonic acid as catalyst. At room temperature, 460 g of anthracene, 800 ml of mesitylene, and 42 g of methanesulfonic acid 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 conditions, and then the reaction was terminated. 10 batches were reacted under the same conditions. After the catalyst was separated, the alkylation reaction product was collected uniformly as the raw material for the separation of alkylanthracene.

[0114] (2) Separation.

[0115] The alkylation reaction product is sent to the atmospheric distilla...

Embodiment 2

[0125] 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 300°C, ...

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Abstract

The invention relates to the field of preparation of 2-alkyl anthraquinone, and particularly discloses a method for preparing 2-alkyl anthraquinone by performing reaction on anthracene, performing separating to obtain 2-alkyl anthracene and performing catalytic oxidation on the 2-alkyl anthracene. The preparation method comprises the following steps: (1) preparing a reaction product containing the2-alkyl anthracene from the anthracene; (2) separating the anthracene from the reaction product containing the alkyl anthracene through melt crystallization and performing distillation seperation toobtain the 2-alkyl anthracene; and (3) under an oxidation condition and in the presence of an oxidation reaction solvent and a catalyst, contacting the 2-alkyl anthracene with an oxidizing agent for an oxidation reaction, wherein the oxidizing agent is tert-butyl hydroperoxide, the catalyst contains a carrier and an active component loaded on the carrier, and the active component is selected fromone or more of VA group elements and transition metals. The method is a green preparation method of the 2-alkyl anthraquinone, the separation method can significantly reduce the separation operation difficulty, and the product yield and purity are high; the developed oxidation system is high in activity, the conversion rate is as high as 96.29%, and the selectivity is 98.67%.

Description

technical field [0001] The invention relates to a method for preparing organic matter, in particular to a method for separating 2-alkylanthracene from anthracene through reaction and then preparing 2-alkylanthraquinone through catalytic oxidation. 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-ethylanthraq...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C2/70C07C7/00C07C46/04C07C50/16C07C15/28
CPCC07C2/70C07C7/005C07C46/04C07C50/16C07C15/28
Inventor 郑博郄思远张月琴费建奇潘智勇朱振兴毛俊义宗保宁
Owner CHINA PETROLEUM & CHEM CORP
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