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Method for fast producing caprolactam by means of strengthening and mixing

A caprolactam, jet mixer technology, applied in chemical recovery, organic chemistry and other directions, can solve problems such as affecting the mixing effect and affecting the quality of rearranged products, and achieve the effect of ensuring the mass transfer effect.

Active Publication Date: 2013-09-25
HUBEI JINXIANGNING CHEM ENG TECHENOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The change of the flow rate of the two streams will affect the mixing effect, which will ultimately affect the quality of the rearrangement product
[0013] It can be seen that the Beckmann rearrangement process of the external circulation heat storage and heat transfer method has its matching hybrid technology and structural form, but for the rearrangement of the solvent vaporization heat transfer method, due to the difficulties of the above-mentioned engineering problems, there is no better one at present. solutions to ensure the matching of reaction and mass transfer

Method used

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  • Method for fast producing caprolactam by means of strengthening and mixing
  • Method for fast producing caprolactam by means of strengthening and mixing
  • Method for fast producing caprolactam by means of strengthening and mixing

Examples

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Effect test

Embodiment 1

[0067] Using oleum as an acid source, catalyzing the rearrangement of cyclohexanone oxime to produce caprolactam, the mass transfer and reaction are realized through a single jet mixer, and the reaction temperature is controlled by solvent vaporization and heat transfer. Cyclohexanone oxime is fully mixed with the flow rate of 12087.7kg / h and 68500.6kg / h of n-hexane to obtain a 15%wt cyclohexanone oxime-n-hexane solution with a concentration of cyclohexanone oxime, its mass flow rate and volume flow rate Respectively 80588.3kg / h and 120.55m 3 / h. The cyclohexanone oxime solution enters axially through the mixer, the inner diameter of the throat is 45mm, and the throat speed is about 21.0m / s.

[0068]A plurality of small holes are uniformly distributed on the circumference of the narrowest part of the throat of the mixer. Another raw material for the rearrangement reaction is SO 3 Fuming sulfuric acid with a content of 20.0% (mass fraction) enters the interior of the nozzle ...

Embodiment 2

[0071] Taking the nitrosation product of cyclohexyl formic acid as the acid source, its typical composition is: 23.1% (mass percentage, the same below) of cyclohexyl formic acid, 11.3% of sulfur trioxide, 28.2% of sulfuric acid, 18.3% of n-hexane, 16.0% of caprolactam, and the rest are by-product. Further catalyze the rearrangement of cyclohexanone oxime to produce caprolactam, so as to reduce the byproduct of ammonium sulfate per unit of caprolactam.

[0072] A double-jet mixer is adopted, and the axial feed is 15%wt cyclohexanone oxime solution, the mass flow rate is 80602kg / h, and the corresponding volume flow rate is 120.6m3 / h. The viscosity of the material fed into the throat is 0.873mPas, the temperature is 39.3°C, the inner diameter of the throat is 79mm, the diameter of the plug is 70mm, and the speed of the throat is about 16m / s.

[0073] There is an annular gap around the narrowest part of the throat of the mixer, and the nitrosation product of cyclohexyl formic aci...

Embodiment 3

[0076] With the nitrosation product of cyclohexyl formic acid as the acid source, the light phase n-hexane is first removed by centrifugation, and the heavy phase consists of: cyclohexyl formic acid 28.1% (mass percentage, the same below), sulfur trioxide 13.0%, sulfuric acid 34.6% , Caprolactam 19.8%, the rest is by-products. Further catalyze the rearrangement of cyclohexanone oxime to produce caprolactam, so as to reduce the byproduct of ammonium sulfate per unit of caprolactam.

[0077] Using a double-jet mixer, the axial feed of the nozzle is 12%wt cyclohexanone oxime solution, the mass flow rate is 100730kg / h, and the corresponding volume flow rate is 150.68m 3 / h. The inner diameter of the throat is 51mm, the diameter of the plug is 41mm, and the speed of the throat is about 29.0m / s.

[0078] The axial direction is a whole except for the plug, and 40 3 holes are opened in the radial direction at the narrowest part of the throat. Its mass flow rate is 46375kg / h, and th...

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Abstract

The invention discloses a method for fast producing caprolactam by means of strengthening and mixing. The method comprises the steps of: mixing solution of cyclohexane oxime-inert solvent with sulfuric acid and sulfur trioxide-containing strongly acid material which is radially added in the manner of dispersing through the axial direction of a specially-designed jet flow mixer in the manner of continuous phase, performing the Beckmann rearrangement reaction, and discharging reaction heat in a gas phase space of a stirring kettle by means of evaporating solvent. At higher linear velocity and lower reaction temperature, the rearrangement can achieve better mass transfer effect and reaction effect, the sulfuric acid consumption is reduced, and the product quality can be improved.

Description

technical field [0001] The present invention relates to a method for preparing caprolactam by Beckmann rearrangement of cyclohexanone oxime. It is further explained that in the presence of an inert solvent, cyclohexanone oxime is mixed with a substance containing sulfuric acid and sulfur trioxide through a special mixing method to achieve strengthening Mass transfer and fast reaction to ensure high yield and high product quality caprolactam preparation method. Background technique [0002] Caprolactam, as a monomer of polyamide 6, is an important petrochemical product widely used in the manufacture of nylon and engineering plastics. There are many preparation methods of caprolactam, but there are only a few industrial methods that can meet the requirements of polymerization and are economical and reasonable. At present, the production methods of caprolactam in industry mainly include cyclohexanone-hydroxylamine method, cyclohexane photonitrosation method and toluene method,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D223/10
CPCY02P20/582
Inventor 罗和安吴剑袁霞
Owner HUBEI JINXIANGNING CHEM ENG TECHENOLOGY CO LTD