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a co 2 Method for preparing aromatic acid by direct carboxylation method

An aromatic acid and carboxylation technology, which is applied in the field of preparing aromatic acids by CO2 direct carboxylation, can solve the problems of harsh operating conditions, strong Lewis corrosion to equipment, and high catalyst cost, and achieves improved reaction selectivity, excellent solubility, The effect of shortening the reaction time

Active Publication Date: 2021-04-27
SHAANXI COAL & CHEM TECH INST
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Problems solved by technology

However, these catalysts still have disadvantages such as large dosage, low efficiency, poor substrate adaptability, high cost and poor safety, making CO 2 Direct carboxylation method is difficult to industrialize
[0004] In 2002, Olah et al. (J.Am.Chem.Soc., 2002,124:11379-11391) reported that AlCl 3 / The Al system can realize the highly selective synthesis of a variety of aromatic acids under relatively mild conditions. This method has the advantages of mild reaction conditions, high yield and good selectivity, and is expected to be used in CO 2 The industrialization of the preparation of aromatic acids by direct carboxylation method, but the system still has the disadvantages of large amount of catalyst, severe corrosion of equipment by strong Lewis, and potential explosion hazard of Al in contact with water, which needs to be further optimized
However, chloroaluminate ionic liquids usually need to be operated under vacuum conditions, and there are problems such as complicated preparation process, harsh operating conditions, and high cost, which restrict its industrialization.
[0006] Therefore, how to overcome the existing CO 2 The disadvantages of high catalyst cost, harsh operating conditions, and poor safety in the preparation of aromatic acids by direct carboxylation are still a challenging work, and the development of new CO 2 The preparation of aromatic acids by direct carboxylation can not only realize the transformation and upgrading of the aromatic acid industry, but also enrich CO 2 The content of chemical utilization, and at the same time of obtaining important chemicals, realizes the chemical cycle of carbon, making it a powerful supplement to the natural carbon cycle, and improving the deteriorating global greenhouse effect

Method used

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  • a co <sub>2</sub> Method for preparing aromatic acid by direct carboxylation method
  • a co <sub>2</sub> Method for preparing aromatic acid by direct carboxylation method
  • a co <sub>2</sub> Method for preparing aromatic acid by direct carboxylation method

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preparation example Construction

[0039] In the preparation method of the present invention: aromatic hydrocarbon is benzene, alkyl substituted benzene (alkyl substituted benzene is toluene, 1,2-xylene, 1,3-xylene, 1,4-xylene, 1,3,5- trimethylbenzene, ethylbenzene, propylbenzene or tert-butylbenzene), halogenated benzene, naphthalene or alkyl-substituted naphthalene;

[0040] Lewis acid is AlCl 3 , AlBr 3 , FeCl 3 , FeBr 3 , BF 3 , SbF 5 , NbCl 5 and La(CF 3 SO 3 ) 3 One of, preferably AlCl 3 , less preferably AlBr 3 , FeCl 3 or FeBr 3 ;

[0041] Organic bases include alkylamines (alkylamines are primary amines R-NH 2 , secondary amine R 1 R 2 -NH or tertiary amine R 1 R 2 R 3 -N, where R 1 , R 2 and R 3 Both are C 1 ~C 18 Alkyl, allyl and various secondary or tertiary alkyl groups), imidazole / N-alkyl substituted imidazole (in imidazole / N-alkyl substituted imidazole, the alkyl is C 1 ~C 18 Alkyl, allyl and various secondary or tertiary alkyl groups), pyridine / alkyl substituted pyridin...

Embodiment 1

[0043] Under argon atmosphere, quickly add 40mL dry 1,3,5-trimethylbenzene, 2.5g anhydrous AlCl 3 , 1.76g of dry N-methyldicyclohexylamine, and the reaction kettle was sealed after the feeding was completed. Then CO 2 The cylinder is connected to the autoclave through the pipeline, and the valve is opened to control the CO 2 The pressure was 6MPa, and at the same time, the stirring was started at a stirring rate of 1000 rpm, and finally heating was started and kept at 40°C for 30h. After the reaction was completed, 150 mL of water was added to the reaction system, and the reaction was carried out for 30 min under stirring conditions, and then extracted three times with 50 mL of ether, and the extracts were combined and concentrated to dryness to obtain 2.72 g of off-white solid. Dissolve the above-mentioned off-white solid in 20mL of 10%wt sodium hydroxide solution, filter the insoluble matter to obtain the filtrate, then adjust the pH value of the filtrate to 1 with 1mol / L ...

Embodiment 2

[0045] Under argon atmosphere, quickly add 40mL dry 1,3,5-trimethylbenzene, 2.5g anhydrous AlCl 3 , 0.54g of dry 1-allylimidazole, and the reaction kettle was sealed after the feeding was completed. Then CO 2 The cylinder is connected to the autoclave through the pipeline, and the valve is opened to control the CO 2 The pressure was 6MPa, and at the same time, the stirring was started at a stirring rate of 1000rpm, and finally heating was started and kept at 40°C for 24h. After the reaction was completed, 150 mL of water was added to the reaction system, and the mixture was reacted for 30 min under stirring, and then extracted three times with 50 mL of ether. The extracts were combined, concentrated and dried to obtain 2.85 g of off-white solid. Dissolve the above-mentioned off-white solid in 20mL of 10%wt sodium hydroxide solution, filter the insoluble matter to obtain the filtrate, then adjust the pH value of the filtrate to 1 with 1mol / L HCl, stand at room temperature for...

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Abstract

The invention discloses a CO 2 The method for preparing aromatic acid by direct carboxylation comprises the following steps: step 1), aromatic hydrocarbon, organic base and Lewis acid are added in the autoclave in an inert gas atmosphere, and then CO is passed into the autoclave in the autoclave 2 The gas is reacted, and after the reaction is completed, a reaction solution that generates an aromatic acid is obtained; step 2), adding water to the reaction solution obtained in step 1), and then extracting the aromatic acid in the reaction solution with an extractant, and the reaction solution in the reaction solution The aromatic acid enters the extraction phase, and then the extraction phase is separated from the raffinate phase, and the extraction phase is concentrated to obtain the aromatic acid. The present invention not only avoids the complex preparation process of ionic liquid, but also the organic base neutralizes the hydrogen halide generated by the reaction in time, which is beneficial to shifting the balance to the right. After the reaction, the organic base can also be recycled by alkali treatment. The process has the advantages of simple operation, With the advantages of mild conditions, green process and low cost, it is expected to be used in industrial production.

Description

technical field [0001] The invention belongs to the field of fine chemical technology, in particular to a CO 2 A method for preparing aromatic acids by direct carboxylation. Background technique [0002] Aromatic acids are an important class of chemical products with a wide range of uses, and are widely used in the production of medicines, food additives, dyes, photosensitizers, plasticizers, spices and cosmetics. At present, the vast majority of aromatic acids are obtained through oxidation reactions and multi-step organic synthesis reactions, which have disadvantages such as low atom economy, complicated operations, harsh reaction conditions, many by-products, and serious environmental pollution. [0003] Compared with traditional methods, CO 2 The preparation of aromatic acids by direct carboxylation has the advantages of high atom economy, short reaction process, simple operation, low raw material cost, green and high efficiency, etc. But due to CO 2 It has strong th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C63/04C07C63/06C07C51/15C07C63/08C07C51/41C07C51/02
CPCC07C51/02C07C51/15C07C51/412C07C63/04C07C63/06C07C63/08Y02P20/141
Inventor 王文涛田士东戚文博薛其才张生军郑化安殷海龙
Owner SHAANXI COAL & CHEM TECH INST
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