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Method for preparing 2-alkylanthraquinone by separating 2-alkylanthracene from anthracene by reaction and then catalyzing oxidation

A technology for catalytic oxidation of alkyl anthraquinones, used in the preparation of oxidized quinones, chemical instruments and methods, purification/separation of hydrocarbons, etc.

Active Publication Date: 2021-05-14
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 preparing 2-alkylanthraquinone by separating 2-alkylanthracene from anthracene by reaction and then catalyzing oxidation
  • Method for preparing 2-alkylanthraquinone by separating 2-alkylanthracene from anthracene by reaction and then catalyzing oxidation
  • Method for preparing 2-alkylanthraquinone by separating 2-alkylanthracene from anthracene by reaction and then catalyzing 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<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...

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 present invention relates to the field of preparation of 2-alkylanthraquinones, and specifically discloses a method for separating 2-alkylanthracenes from anthracene through reaction and then preparing 2-alkylanthraquinones through catalytic oxidation. The preparation method comprises: ( 1) prepare the reaction product containing alkyl anthracene by anthracene; (2) separate the reaction product containing alkyl anthracene by melt crystallization anthracene and distillation separation 2-alkyl anthracene; (3) under oxidation condition and in oxidation reaction solvent And under the presence of catalyst, 2-alkylanthracene is contacted with oxidizing agent to carry out oxidation reaction, and described oxidizing agent is tert-butyl hydroperoxide, and described catalyzer contains support and the active component that is loaded on the support, and described active component One or more selected from group VA elements and transition metals. The invention is a green preparation method of 2-alkylanthraquinone, wherein the separation method can significantly reduce the difficulty of separation operation, the product yield is high, and the purity is high; the developed oxidation system has high activity, the conversion rate is as high as 96.29%, and the selectivity is high. was 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 Patents(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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