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Method for preparing benzoic acid by means of catalytic oxidation of Anderson type polyacid

A multi-acid catalysis and benzoic acid technology, which is applied in the preparation of carboxylate, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of many by-products, environmental pollution, and chlorine consumption, and achieve easy operation and cost reduction , the effect of reducing environmental pressure

Inactive Publication Date: 2018-08-10
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has many steps, many by-products and is difficult to separate. It needs to consume chlorine, and the discharged HCl aqueous solution etc. have serious environmental pollution. Therefore, this method is generally only a supplementary method for the recycling of benzaldehyde or benzyl alcohol by-products produced by chlorination and hydrolysis of toluene.

Method used

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  • Method for preparing benzoic acid by means of catalytic oxidation of Anderson type polyacid
  • Method for preparing benzoic acid by means of catalytic oxidation of Anderson type polyacid
  • Method for preparing benzoic acid by means of catalytic oxidation of Anderson type polyacid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] With the toluene of 0.9214g (0.01mol), the Fe‐Anderson type polyoxometalate catalyst ([NH 4 ] 3 [FeMo 6 o 18 (OH) 6 ]), 0.0040g (0.1equiv) of sodium hydroxide additive, and the solvent dimethyl succinate of 5mL are put into the dry reaction test tube, after being heated up to 80 ℃, react in the air, at a pressure (gauge pressure) of After heat preservation reaction at 1.0MPa for 24h, the reaction was stopped, and the reaction system was extracted 3 times with ethyl acetate. The obtained product was desolventized under reduced pressure, separated by column chromatography to obtain benzoic acid, and 0.9648g of the product was obtained, with a yield of 79%. image 3 It is the Anderson type polyoxometalate [NH that iron is metal center in embodiment 1 4 ] 3 [FeMo 6 o 18 (OH) 6 ] Infrared characterization chart after 6 cycles.

Embodiment 2

[0036] With the toluene of 0.9214g (0.01mol), the Fe-Anderson type polyoxometalate catalyst ([NH 4 ] 3 [FeMo 6 o 18 (OH) 6 ]), 0.0106 (0.1equiv) of sodium carbonate additive, and 3mL of solvent acetic acid are put into the hydrothermal reaction kettle lined with polytetrafluoroethylene. Attention, check whether the equipment is damaged before use, and pour into the hydrothermal reaction kettle container Add solvent and raw materials to the medium, stir and dissolve, blow nitrogen into the container for a period of time, make the system in an inert atmosphere, tighten the lid of the hydrothermal reaction kettle in use, then add the catalyst and place it in an oven, heat up to 120°C, Connect the oxygen tank so that the pressure (gauge pressure) is about 1.0MPa, and stop the reaction after the heat preservation reaction for 8 hours. After the kettle body was naturally cooled to room temperature, the lid was opened, and the reaction system was extracted 3 times with ethyl acet...

Embodiment 3

[0038] With the toluene of 0.9214g (0.01mol), the Fe-Anderson type polyoxometalate catalyst ([NH 4 ] 3 [FeMo 6 o 18 (OH) 6 ]), 0.0106g (0.1equiv) of sodium carbonate additive, 0.03mol of 30% hydrogen peroxide and 8mL of solvent acetic acid were put into a dry and clean pressure-resistant tube. ) after 12h of insulation reaction under 1.0MPa, stop reaction, with ethyl acetate, reaction system is extracted 3 times, the product obtained decompresses and removes solvent, and column chromatography separation obtains benzoic acid, obtains product 0.9769g, and yield is 80 %.

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Abstract

The invention discloses a method for preparing benzoic acid by means of catalytic oxidation of Anderson type polyacid. The method comprises the following steps: (1) enabling toluene to be subjected toan oxidation reaction in a solvent in action of a catalyst, an oxidizing agent and an additive, wherein the reaction temperature is 80-130 DEG C, the reaction gage pressure is 1.0-5.0MPa, the reaction time is 3-24h, and the catalyst is an Anderson type polyacid parent or polyacid modified parent; (2) after the oxidation reaction is completed, removing the catalyst by filtering, and then adding anextraction solvent and water to obtain an organic phase and an aqueous phase; drying, filtering and concentrating the organic phase, and carrying out purification treatment to obtain benzoic acid. The method adopts the highly reactive Anderson type polyacid as the catalyst, and the catalyst has high specific selectivity and can be recycled; hydrogen peroxide, air or oxygen is used as the oxidizing agent, so that the cost is lowered and the generation of three wastes can be reduced; the method is mild in reaction conditions, high in yield and simple and convenient to operate, thus being suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of catalytic chemistry, in particular to the field of catalysis of polyoxometalates, and in particular relates to a method for preparing benzoic acid by catalytic oxidation of Anderson-type polyacids. Background technique [0002] Benzoic acid, also known as benzoic acid, is a colorless, odorless flaky crystal. The melting point is 122.13°C, the boiling point is 249°C, and the relative density is 1.2659 (15 / 4°C). It sublimates rapidly at 100°C, and its vapor is highly irritating, which can easily cause coughing after inhalation. Slightly soluble in water, easily soluble in organic solvents such as ethanol and ether. Benzoic acid is a weak acid, stronger than fatty acids. Their chemical properties are similar, and they can form salts, esters, acid halides, amides, acid anhydrides, etc., and are not easily oxidized. Benzoic acid and its sodium salt can be used as a bacteriostatic agent for latex, toothpast...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/265C07C63/06B01J31/16B01J31/18B01J27/188
CPCY02P20/584C07C51/265B01J23/881B01J27/188B01J31/18B01J2231/70C07C63/06
Inventor 余焓王静静何慧红
Owner SHANGHAI INST OF TECH
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