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Preparation method of adsorbent for adsorbing impurities in cyclohexanone

An adsorbent, cyclohexanone technology, applied in the field of adsorbent preparation, can solve the problems of uncontinuous feeding, waste of resources, low energy consumption, etc., and achieve the effects of improving product quality, strong product competitiveness, and low impurity content

Active Publication Date: 2017-12-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese patent CN 102491889 A, a method for removing hexanal and 2-heptanone in cyclohexanone, using a solid adsorbent to remove hexanal and 2-heptanone impurities from solvent-type cyclohexanone, and controlling the impurities in cyclohexanone The sum of the two contents is below 40mg / kg, and the supercritical gas carbon dioxide is used to desorb the adsorbate, which is a method for continuous online operation of adsorption and desorption, which has the characteristics of low energy consumption and low material consumption, but does not remove 2 - Hexanone, and cannot be fed completely continuously
[0005] Huang Yan, He Yangjin, Wang Shi et al. Invented the article "Study on the Adsorption Performance of Molecular Sieves on Hexanal and 2-Heptanone in Cyclohexanone" (. Fine Chemical Intermediates, 2011, 41(6), 58~60.) , using molecular sieves to adsorb cyclohexanone containing hexanal and 2-heptanone, but the used molecular sieves cannot be recycled and reused, resulting in waste of resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 50mL of 20% nitric acid to 5g of powdered ZSM-5 molecular sieve with a silicon-aluminum ratio of 200, stir with a magnetic stirrer at a temperature of 5°C for 0.5h, wash with distilled water to reach neutrality, filter and dry. Add 100mL of 30% H 2 o 2 After stirring at 20°C for 2h, soaking for 20h, washing to neutrality, drying at 150°C, and roasting at 200°C for 6h, H 2 o 2 Modified ZSM-5 molecular sieve. Cyclohexanone (the content of 2-heptanone is 10ppm, the content of 2-hexanone is 0ppm, and the content of hexanal is 0ppm) is carried out with the prepared adsorbent, and the content of 2-heptanone after adsorption is 1ppm, and the content of 2-hexanone is 1ppm. The content is 0ppm, the hexanal content is 0ppm, and the total impurity content is less than 5ppm.

Embodiment 2

[0024] Add 10g of MCM-41 molecular sieve to 50mL of 10% hydrochloric acid, stir with a magnetic stirrer at a temperature of 95°C for 4h, wash with distilled water to reach neutrality, filter and dry. Add 100mL of 10% H 3 PO 4 After stirring at 50°C for 0.5h, soaking for 5h, washing to neutrality, drying at 100°C, and roasting at 600°C for 8h to obtain H 3 PO 4 Modified MCM-41 molecular sieve. Cyclohexanone (the content of 2-heptanone is 56ppm, the content of 2-hexanone is 93ppm, and the content of hexanal is 92ppm) is carried out adsorption treatment with the prepared adsorbent, after the adsorption, the content of 2-heptanone is 0ppm, and the content of 2-hexanone is 0ppm. The content of hexanal is 2ppm, the content of hexanal is 1ppm, and the total content of impurities is less than 5ppm.

Embodiment 3

[0026] Add 100mL of 20% nitric acid to 5g of strip ZSM-5 molecular sieve with a silicon-aluminum ratio of 100, stir with a magnetic stirrer at a temperature of 80°C for 8h, wash with distilled water to reach neutrality, filter and dry. Add 100mL of 30% NaOH, stir at 60°C for 6h, impregnate for 0.5h, wash until neutral, dry at 120°C, and roast at 500°C for 2h to obtain NaOH-modified ZSM-5 molecular sieve. Cyclohexanone (the content of 2-heptanone is 102ppm, the content of 2-hexanone is 43ppm, and the content of hexanal is 22ppm) is carried out with the prepared adsorbent. The content of 2-heptanone after adsorption is 2ppm, and the content of 2-hexanone is 2ppm. The content of hexanal is 2ppm, the content of hexanal is 0ppm, and the total content of impurities is less than 5ppm.

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Abstract

The invention discloses a preparation method of an adsorbent for adsorbing impurities in cyclohexanone. The preparation method comprises: carrying out acid washing to remove impurities and the like generated during the early-stage preparation of an adsorbent carrier, and changing the pore size of the adsorbent by using a modifier, such that the adsorbent can just adsorb the impurities in cyclohexanone while cannot adsorb the cyclohexanone. According to the present invention, the prepared adsorbent can effectively remove 2-heptanone, hexanal, 2-hexanone and other impurities in cyclohexanone, such that the total content of the target impurities is less than 5ppm so as to remove the impurities from cyclohexanone.

Description

technical field [0001] The invention belongs to the technical field of organic chemical purification, and in particular relates to a preparation method of an adsorbent for adsorbing impurities in cyclohexanone. Background technique [0002] Cyclohexanone is an important organic intermediate widely used in fiber, synthetic rubber, industrial coating, medicine, pesticide and other industries. At present, the supply of solvent grade cyclohexanone exceeds the demand in the market. Due to the rapid development of the polyamide industry, chemical fiber grade cyclohexanone has also been rapidly developed as a raw material for the production of caprolactam. Chemical fiber grade cyclohexanone requires the content of by-products 2-hexanone, hexanal and 2-heptanone to be less than 40ppm. Cyclohexanone contains these by-products, which are difficult to remove in a small amount, which is an urgent problem to be solved. At present, there are few reports on the removal methods of 2-hexan...

Claims

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Application Information

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IPC IPC(8): B01J20/20B01J20/18B01J20/30B01J20/28C07C45/79C07C49/603
CPCB01J20/186B01J20/20B01J20/28014B01J20/28016C07C45/79C07C49/603
Inventor 刘卓金汉强吴其建何育苗陈永平金玉存
Owner CHINA PETROLEUM & CHEM CORP
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