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Technology and apparatus for preparing cyclohexanol, cyclohexanone and adipic acid by cyclohexane

A technology for air oxidation and cyclohexane, which is applied in the field of cyclohexanol prepared by air oxidation of cyclohexanone, adipic acid and cyclohexane, which can solve the problem of unsatisfactory metalloporphyrin catalytic effect, cyclohexane conversion rate and reaction selectivity And low yield of oxidation products, lower reaction temperature and pressure, etc., to achieve the effect of reducing the formation of deep oxidation products, inhibiting a series of side reactions, and improving the reaction conversion rate

Inactive Publication Date: 2006-10-25
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN 02113940.7 discloses a method of using cobalt double metal porphyrin to catalyze air oxidation of cyclohexane in a laminar flow reactor, and CN 200310110458.4 discloses a kind of iron tetraphenylporphyrin and cobalt tetraphenylporphyrin in three A method for catalytic air oxidation of cyclohexane in a stirred tank reactor in series, a bubbling single-pot reactor, a tube-and-tube single reactor, and a laminar flow single reactor. These methods can reduce the reaction temperature and pressure, but the reaction still remains There is a backmixing phenomenon that is unfavorable to the oxidation of hydrocarbons, the catalytic effect of metalloporphyrins is still unsatisfactory, and the conversion rate of cyclohexane, reaction selectivity and yield of oxidation products are still low

Method used

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  • Technology and apparatus for preparing cyclohexanol, cyclohexanone and adipic acid by cyclohexane
  • Technology and apparatus for preparing cyclohexanol, cyclohexanone and adipic acid by cyclohexane
  • Technology and apparatus for preparing cyclohexanol, cyclohexanone and adipic acid by cyclohexane

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Experimental program
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Effect test

Embodiment 1

[0011] The reaction equipment includes two bubble column reactors with external circulation and a tubular reactor connected in series. Production process: at 150°C, the metalloporphyrin dissolved in 10PPM structural formula (I) is introduced, R 1 = H, R 2 = R 3 =CH 3 , M=Mn cyclohexane, 0.4MPa air through the gas distributor is passed into the bottom of the first bubble column reactor, and the reaction liquid overflows from the upper part of the first bubble column reactor into the second bubble column At the bottom of the tower reactor, the catalyst-containing cyclohexane and the reaction liquid overflowing from the upper part of the second bubble column reactor are mixed with air by the Venturi mixer and then enter the tubular reactor, and the flow rate of the cyclohexane is controlled to make the residence The time is 90 minutes. The oxidized liquid from the tubular reactor is cooled and separated to obtain adipic acid crystals, the filtrate is decomposed after flash ev...

Embodiment 2

[0013] The reaction equipment includes 6 tank reactors with agitator connected in series. Production process: the catalyst is a metalloporphyrin with structural formula (II), R 1 = R 2 =OCH 3 , R 3 =Cl,M 1 = M 2 =Fe, the oxidant is 0.8MPa air. The cyclohexane containing 2PPM catalyst and the air through the gas distributor are passed into the bottom of the first reactor, and the reaction liquid overflows from the upper part of the first reactor to the bottom of the second reactor, and the reaction temperature is 145 ° C. The reaction pressure is 0.9MPa, and the reaction liquid overflowing from the upper part of the second reactor enters the third reactor, and then passes through the fourth, fifth and sixth reactors in sequence. Control the cyclohexane flow rate to make the residence time 45 minutes, and control the air flow rate to make the tail oxygen content not exceed 5%. The oxidized liquid is decomposed after being flashed, and the cyclohexane is recovered through ...

Embodiment 3

[0015] The reaction equipment includes two tank reactors with agitator and a tubular reactor connected in series. Production process flow: the catalyst is a metalloporphyrin with structural formula (I), R 1 = R 2 =C 2 h 5 , R 3 =Br, M=Fe, the oxidant is 0.6MPa air containing 25% oxygen. The cyclohexane containing 20PPM catalyst is passed into the bottom of the first tank reactor through the air of the gas distributor, and the reaction liquid overflows from the upper part of the first tank reactor into the bottom of the second tank reactor, and the reaction The temperature was 160°C. The reaction solution overflowed from the upper part of the second tank reactor was mixed with air by a Venturi mixer and then entered the tubular reactor, and the flow rate of toluene was controlled so that the residence time was 90 minutes. The oxidized liquid coming out of the tubular reactor is cooled and separated to obtain benzoic acid crystals, the filtrate is decomposed after being fl...

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Abstract

This invention discloses cyclohexane air dioxide prepare cyclohexanol, cyclohexanone and adipic acid technique and equipment. Its technique is that in series connecting reaction system in a 4-8 grade kettle reactor that contains agitator, or series connecting reaction system in a 3-7 bubbling column reactor that contains outer cycle, or series connecting reaction system in 2-6 different type reactor, cyclohexane that added catalyst of 1-100PPM metalloporphyrin and 0.1-2.0 PPM air, or oxygen or oxygen enriched air or oxygen denubed air is let in. temperature is 120-160 degree centigrade, reaction for 45-120 minutes. Corresponding equipment is also included in this invention. This invention can restrain train side reaction and reduce generating of depthoxide, so cyclohexane conversion, reaction selectivity and oxidation products yield can be improved.

Description

technical field [0001] The invention relates to a process and equipment for preparing cyclohexanol, cyclohexanone and adipic acid by air oxidation of cyclohexane, in particular to a method for preparing cyclohexanol, cyclohexanol and cyclohexane by air oxidation of cyclohexane using metalloporphyrin as a catalyst. Process and equipment for ketone and adipic acid. Background technique [0002] Air oxidation of cyclohexane is an important method for the preparation of cyclohexanone. At present, the method for industrially producing cyclohexanone by the oxidation of cyclohexane is a non-catalyzed oxidation method invented by Stamica in the Netherlands. The reaction is carried out under high temperature and high pressure conditions, the reaction yield is low, and the product selectivity poor. The method for producing cyclohexanone by oxidation of cyclohexane under the catalysis of metalloporphyrin, the reaction yield and product selectivity are ...

Claims

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Application Information

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IPC IPC(8): C07C27/12B01J31/12C07C31/135C07C49/11C07C55/14
CPCC07C45/33B01J2231/70B01J2531/025C07C29/50C07C51/313C07C2601/14
Inventor 郭灿城郭栋才罗伟平邓伟刘强江国防
Owner HUNAN UNIV
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