Method for producing caprolactam by methylbenzene

A technology of caprolactam and toluene, which is applied in the field of caprolactam production, can solve problems such as huge investment costs, huge operating costs, troublesome separation of products and catalysts, astonishing catalyst consumption, etc., to extend the operation period, reduce the consumption of precious metal catalysts, and reduce equipment construction and operation The effect of fees

Active Publication Date: 2011-05-18
中科化物(大连)科技实业有限公司
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology describes an improved method for producing lactic esters that have fewer impurities than traditional methods like naphtha cracked with ethanol. Instead, it involves changing certain chemical components during manufacturing instead of replacing them altogether. These changes help prevent damage caused by these compounds while still maintain their effectiveness over longer periods of time. Additionally, this new design allows for more efficient utilization of expensive metals compared to current designs without sacrifices. Overall, this innovative approach helps produce higher quality lactic acids efficiently and effectively.

Problems solved by technology

The current methods involve multiple steps involved including different starting materials like tetrahydronaphthalene, dimethylcyclohexanone, acrylonitrile, formalin, and adiponcyclodimide. These techniques have drawbacks such as long cycle times during manufacturing due to their complexity, excessive waste streams generated, and difficulties in recovering and operating cost reduction.

Method used

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  • Method for producing caprolactam by methylbenzene
  • Method for producing caprolactam by methylbenzene
  • Method for producing caprolactam by methylbenzene

Examples

Experimental program
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Embodiment 1

[0055] Example 1. Oxidation reaction

[0056] 300 grams of toluene, 700 grams of methyl benzoate returned from the distillation process, 2 grams of catalyzer, oxidized with air in an oxidation kettle, at 160 ° C, under 1Mpa conditions, oxidized toluene to prepare benzoic acid, and cooled the reactant after 2 hours of reaction , Reaction result and the reaction comparison result that does not add methyl benzoate see the table below.

[0057] Table 1. Toluene Oxidation Reaction

[0058]

Embodiment 2

[0059] Embodiment 2. Esterification reaction

[0060] 6350g of toluene oxidation product enters from the upper part of the esterification tower, and 120g of methanol steam 7 is introduced from the bottom of the esterification tower. The temperature of the tower bottom is kept at 190°C, and the pressure inside the tower is kept at 3.4Mpa. The benzoic acid completely generates methyl benzoate in the tower. About 30 grams of unreacted methyl alcohol are discharged from the tower top condenser 9, 40 g of heavy by-products generated in the oxidation reaction process and catalysts are discharged from the tower kettle 8, and 400 g of methyl benzoate 10 generated by the esterification reaction are discharged from the top tower of the esterification tower Plate mining, wherein 50g of methyl benzoate is circulated back to the oxidation reactor 11, and 350g of methyl benzoate enters the hydrogenation reaction section 12.

Embodiment 3

[0061] Embodiment 3. hydrogenation reaction

[0062] 350g of methyl benzoate 12 and hydrogen 13 from the circulating compressor, at 160°C and 2.5Mpa hydrogen pressure, the hydrogen flow rate is 300L / h, after 1.5 hours of reaction, methyl benzoate is converted into methyl cyclohexyl formate, The hydrogenation product enters the gas-liquid separator, the hydrogenation tail gas 15 is recycled and compressed back to the hydrogenation reactor after removing CO, and 360 g of methyl cyclohexyl carboxylate 16 enters the amidation reactor.

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PUM

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Abstract

The invention relates to a method for producing caprolactam by methylbenzene, which comprises the following processes of oxidation, esterification, hydrogenation, distillation, amidation, hydrolyzing and refining, wherein in the oxidation process, the methylbenzene is completely converted into benzoic acid by adopting an ester solvent; in the esterification process, the benzoic acid dissolved in ester reacts with alcohol to form corresponding benzoate; in the hydrogenation reaction, a benzene ring of the benzoate is hydrogenated till saturation to form cyclohexanecarboxylate in a fixed bed reactor, and the cyclohexanecarboxylate enters the amidation process; and in the amidation process, the cyclohexanecarboxylate reacts with nitrosyl sulfuric acid, the reaction product is subjected to hydrolyzing rearrangement in the sulfuric acid to form the caprolactam by refining. In the method, the conventional rectification of the benzoic acid is changed into the rectification of the benzoate, a granular catalyst replaces the original powder palladium-carbon catalyst, the processes of catalyst sedimentation, centrifugal separation and the like are reduced, the generation of ammonium sulfate is reduced, and dimethyl sulfate serving as a by-product is produced simultaneously.

Description

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Claims

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Application Information

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Owner 中科化物(大连)科技实业有限公司
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