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Process for refining aqueous hexanolactam solution by hydrogenation

A caprolactam and hydrogenation refining technology, applied in the separation/purification of lactam, chemical instruments and methods, etc., can solve the problems of large volume of hydrogenation reactor, large investment in magnetic field coils, difficult uniformity of magnetic field, etc., and achieve small volume, Effect of low magnetic field strength and small diameter

Active Publication Date: 2004-12-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Although the above-mentioned hydrofining method using a magnetically stabilized bed has many advantages over a fixed bed, such as: small catalyst particle size, good mass transfer effect, and convenient catalyst replacement, it is only applicable to low-concentration caprolactam aqueous solutions, resulting in a large amount of liquid treatment , The volume of the hydrogenation reactor is large, and when the diameter of the magnetically stabilized bed reactor is large, the investment of the magnetic field coil is large, and the magnetic field is not easy to be uniform

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] This example illustrates the preparation of the amorphous alloy catalyst with nickel as the main active component used in the present invention.

[0028] Add 48g of nickel, 48g of aluminum, 1.5g of iron, and 2.5g of chromium into the quartz tube, heat it in a high-frequency furnace to above 1300°C to melt it, and make it alloy, and then use inert gas to transfer the alloy liquid from the quartz tube The lower nozzle is sprayed onto a copper roller with a rotating speed of 800rpm. Cooling water is passed through the copper roller. After rapid cooling, the alloy liquid is thrown out along the tangent of the copper roller to form scale-like strips. The scale-like strips are ground to the particle diameter 70 μm or less, a master alloy was obtained. The master alloy is heat-treated in a hydrogen environment, the temperature of the heat treatment is 600° C., and the constant temperature time is 3 hours. The heat-treated master alloy was slowly added into a three-neck flask ...

Embodiment 2

[0030] This example illustrates the preparation of the amorphous alloy catalyst with nickel as the main active component used in the present invention.

[0031] Add 80g of nickel, 50g of aluminum and 2g of iron into the quartz tube, heat it in a high-frequency furnace to above 1450°C to melt, and make it alloyed, and then use 0.08MPa inert gas to pour the alloy liquid out of the quartz tube The nozzle is sprayed onto a copper roller with a rotating speed of 1000rpm. Cooling water is passed through the copper roller. After rapid cooling, the alloy liquid is thrown out along the tangent of the copper roller to form scale-like strips. The scale-like strips are ground to a particle diameter of Below 70 μm, a master alloy is obtained. Take 50g of the master alloy powder, slowly add it to an aqueous solution prepared by 50g NaOH and 250g water, let it stand at room temperature for 1 hour, then raise the temperature to 80°C and stir at constant temperature for 2 hours. After stoppin...

Embodiment 3

[0033] This example illustrates the Raney nickel catalyst used in the present invention. The catalyst is Raney nickel conventionally used in the prior art produced and sold by Yangzhou Catalyst Factory in Jiangsu Province, which is stored in alkaline water with a pH value of 13 for subsequent use. This catalyst is designated Catalyst-3.

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PUM

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Abstract

A process for hydrorefining the aqueous solution of caprolactam includes such steps as gas-liquid-solid hydrorefining reacting between the raw aqueous solution of caprolactam, H2 and ferromagnetic catalyst while dissolving H2 in said aqueous solution, and liquid-solid hydrorefining reacting between said aqueous solution and catalyst in magnetically stabilized-bed reaction. Said catalyst can be reused. Its advantages are high reaction efficiency and less consumption of catalyst.

Description

technical field [0001] The invention relates to a method for hydrofining caprolactam. More specifically, the present invention relates to a method for hydrofinishing high-concentration caprolactam aqueous solution using a ferromagnetic catalyst. technical background [0002] Caprolactam is the starting material for nylon-6. The production of caprolactam includes processes such as hydrogenation of benzene to cyclohexane, cyclohexane oxidation to cyclohexanone, cyclohexanone oximation to cyclohexanone oxime, and cyclohexanone oxime transposition to caprolactam. In these production processes, some unsaturated by-products are formed in addition to caprolactam. The physical and chemical properties of these unsaturated by-products are very close to those of caprolactam, and it is difficult to remove them directly through extraction and distillation processes. The existence of these impurities will affect the caprolactam polymerization process, which is directly related to the q...

Claims

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Application Information

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IPC IPC(8): C07D201/16
Inventor 孟祥堃慕旭宏宗保宁张晓昕吴佳闵恩泽
Owner CHINA PETROLEUM & CHEM CORP
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