Technique for using methylbenzene to prepare benzaldehyde and benzene methanol by multistage oxidation and equipment

A technology for oxidizing toluene and benzaldehyde, which is applied in the preparation of oxidation reaction, the preparation of oxygenated compounds by oxidation of hydrocarbons, and the preparation of carbon-based compounds. It can solve complex operations, poor product purity, and unsatisfactory conversion rates of toluene and substituted toluene. problem, to achieve the effect of increasing conversion rate and improving selectivity

Inactive Publication Date: 2009-12-23
HUNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this reaction is carried out in an oxidation reactor, because the liquid phase reaction mixture contains toluene, water, benzaldehyde, benzyl alcohol, benzoic acid and other by-products, and the primary oxidation product benzaldehyde, benzyl alcohol may also occur Further oxidation; the purity of the product is not very good, and the conversion rate of toluene and substituted toluene is still unsatisfactory; in addition, in order to obtain high-purity benzaldehyde and benzyl alcohol, other equipment must be used to refine and purify it, and the operation is more complicated

Method used

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  • Technique for using methylbenzene to prepare benzaldehyde and benzene methanol by multistage oxidation and equipment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The reaction equipment consists of 6 reactors with stirring and air distributors and 2 fractionation towers connected in series.

[0020] The production process is as follows: at 190°C, the metalloporphyrin dissolved with 5ppm structural formula (III) is introduced, R 1 = Cl, R 2 = R 3 =H, M=Fe's toluene, 10atm air is passed into the bottom of the first stirred reactor through the gas distributor, and the reaction liquid overflowed from the upper part of the first stirred reactor is mixed with air and then passed into the second The bottom of the stirred reactor, the reaction solution overflowed from the upper part of the second stirred reactor is mixed with air and passed through the third stirred reactor, and so on. Control the toluene flow rate so that the average residence time is 73 minutes, and control the air flow rate so that the tail oxygen content does not exceed 5%. The reaction mixture overflowed from the sixth stirred reactor enters the fractionation col...

Embodiment 2

[0022] The reaction equipment consists of 3 reactors with stirring and air distributors and 3 fractionation towers connected in series.

[0023] The production process is: pass into the metalloporphyrin that dissolves 20ppm structural formula (II), R 1 =CH 3 , R 2 = R 3 =H, the toluene of M=Cr, 11atm air is passed into the bottom of the first stirred reactor through the gas distributor, and the reaction liquid overflowed from the upper part of the first stirred reactor is mixed with air and then passed into the second The bottom of the stirring reactor is stirred, and the reaction liquid overflowed from the upper part of the second stirred reactor is mixed with air and passed through the third stirred reactor. Control the temperature of the three reactors to be 190°C, 185°C, and 180°C respectively, control the toluene flow rate so that the average residence time is 73 minutes, and control the air flow rate so that the tail oxygen content does not exceed 5%. The reaction mi...

Embodiment 3

[0025] The reaction equipment consists of a reactor with stirring and air distributor and two fractionation towers.

[0026] The production process is: pass into the metalloporphyrin that dissolves 10ppm structural formula (III), R 1 =OCH 3 , R 2 = R 3 =H, the toluene of the N-hydroxyphthalimide of M=Ni and 120ppm, 5atm oxygen-containing 23% gas is passed into the bottom of the stirred reactor through a gas distributor, and the temperature of the controlled reactor is 90°C, and the toluene The flow rate makes the average residence time 180 minutes, and the air flow rate is controlled so that the tail oxygen content does not exceed 5%. The reaction mixture overflowed from the stirred reactor enters the fractionation column system. Pure products of toluene, benzaldehyde, benzyl alcohol and benzoic acid were obtained after separation. The recovered toluene is mixed with the toluene containing the metal porphyrin catalyst and passed into the stirred reactor for secondary oxid...

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Abstract

The invention discloses a technique for using methylbenzene to prepare benzaldehyde and benzene methanol by air oxidation and equipment. In a reaction separating system consisting of a multistage oxidation reactor as well as a gas-liquid separator, a lateral line fractionating column or a fractionating column system, 0.1 to 50ppm of monometallic porphyrin or u-oxygen bimetallic porphyrin is separately used as a catalyst, or metallic porphyrin and phthalimide (or salt) are used as a mixed catalyst according to the weight ratio of 1:20 to 100; when the reaction temperature is 80 to 200 DEG C, the methylbenzene is maintained in a multistage oxidizer for 60 to 180 minutes and prepared into the benzaldehyde and benzene methanol by catalytic oxidation; and the gas-liquid separation and purification are carried out. Compared with the prior art, the technique and equipment can obviously improve the conversion rate of the methylbenzene, and the conversion rate of the methylbenzene can reach to be more than 95% by experiments; in addition, the technique and equipment also can improve the selection of the benzaldehyde and benzene methanol, and the selection of the benzaldehyde and benzene methanol can reach to be more than 50%.

Description

technical field [0001] The invention relates to a process and equipment for preparing benzaldehyde and benzyl alcohol by multistage oxidation of toluene. Background technique [0002] 03118066.3 discloses the method for the selective catalytic air oxidation of toluene and the substitution of toluene into aldehydes and alcohols that I applied for. It is under the condition of feeding 2-10atm air, controlling the reaction temperature to 140-160°C, and the reaction pressure to 0.1-1MPa. One or more of μ-oxygen double metalloporphyrins and single metalloporphyrins similar in structure to biological enzymes, or the immobilized metalloporphyrins formed by the above metalloporphyrins and inorganic and organic polymers by physical or chemical methods As a catalyst, the catalyst concentration is 1-40ppm, catalytic air oxidation of toluene into benzaldehyde and benzyl alcohol; the conversion rate of substituted toluene varies between 10-50%, and the yield of substituted benzaldehyde a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C27/12C07C27/28C07C33/20C07C29/50C07C47/54C07C45/36B01J31/22
CPCC07C45/36C07C29/50B01J2531/025B01J31/1815B01J2231/70B01J2531/0216
Inventor 郭灿城罗伟平刘连冲刘强邓伟
Owner HUNAN UNIV
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