Method for separating 2-alkylanthracene from products containing alkylanthracene and catalytic oxidation to prepare 2-alkylanthraquinone

A technology for catalytic oxidation and alkyl anthraquinone, which is applied in the preparation of oxidized quinone, organic chemistry, crystallization purification/separation, etc., to achieve the effect of improving purity and total yield, simple and efficient catalytic oxidation system, and low difficulty in separation and recovery

Active Publication Date: 2021-10-08
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-alkylanthracene from products containing alkylanthracene and catalytic oxidation to prepare 2-alkylanthraquinone
  • Method for separating 2-alkylanthracene from products containing alkylanthracene and catalytic oxidation to prepare 2-alkylanthraquinone
  • Method for separating 2-alkylanthracene from products containing alkylanthracene and catalytic oxidation to prepare 2-alkylanthraquinone

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specific Embodiment approach

[0056] According to a specific embodiment of the present invention, in step (2-3), the method for described multi-step distillation comprises:

[0057] 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;

[0058] 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

[0110] (1) Alkylation reaction.

[0111] 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.

[0112] (2) Separation.

[0113] The alkylation reaction product is sent to the atmospheric distilla...

Embodiment 2

[0122] 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-alkylanthraquinones, and specifically discloses a method for separating 2-alkylanthracenes from products containing alkylanthracenes and catalytic oxidation to prepare 2-alkylanthraquinones. The preparation method includes (1) prepare the reaction product containing alkyl anthracene by anthracene; (2) separate the reaction product containing alkyl anthracene, the separation method comprises: melt crystallization separation anthracene and distillation separation 2-alkyl anthracene; (3 ) Under oxidation conditions and in the presence of an oxidation reaction solvent and a catalyst, the 2-alkylanthracene is contacted with an oxidant to carry out an oxidation reaction, the oxidant is hydrogen peroxide, and the catalyst is selected from the oxides of alkaline earth metals and / or One or more of hydroxides, oxygen-containing compounds of transition metals, and oxygen-containing compounds of lanthanide metals. In the method of the present invention, the operation difficulty of the separation process is low and the separation efficiency is high; the oxidation reaction system is simple and efficient, and the catalyst cost is low.

Description

technical field [0001] The invention relates to a method for preparing organic matter, in particular to a method for separating 2-alkylanthracene from a product containing alkylanthracene and catalyzing and oxidizing it 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-ethylan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C46/04C07C50/16
CPCC07C7/14C07C46/04C07C50/16C07C13/573
Inventor 郑博费建奇潘智勇宗保宁朱振兴毛俊义
Owner CHINA PETROLEUM & CHEM CORP
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