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Method for continuous removal of impurities in cyclohexanone

A cyclohexanone and impurity technology, applied in the field of organic chemical purification, can solve the problems that molecular sieve cannot be recycled and reused, 2-hexanone is not removed, and cannot be continuously fed, so as to achieve continuous online adsorption and desorption and product competitiveness. Strong, improve the effect of product quality

Inactive Publication Date: 2017-04-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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
In the literature "Research on the Adsorption Performance of Molecular Sieves on Hexanal and 2-Heptanone in Cyclohexanone", molecular sieves are used to adsorb cyclohexanone containing hexanal and 2-heptanone, but the used molecular sieves cannot be recycled and reused. cause waste of resources

Method used

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  • Method for continuous removal of impurities in cyclohexanone
  • Method for continuous removal of impurities in cyclohexanone
  • Method for continuous removal of impurities in cyclohexanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 2 parts of 80g MCM-41 bar-shaped molecular sieve, put them in adsorber 1 and adsorber 2 respectively, the temperature of cyclohexanone is 25°C, check all valves to make them in the closed state, and open the inlet and outlet valves 7 and 7 of adsorber 1. 8, 15, control the flow rate of the flowmeter to 5mL / min, and take the cyclohexanone flowing out from the adsorber 1 as 0h, and analyze the sample at the outlet of the adsorber 1. The analysis data is as follows:

[0024]

[0025] When 5h, the total impurity content is 30ppm, and the product does not meet the target requirements, close the inlet and outlet valves 8 and 15 of the adsorber 1, open the inlet and outlet valves 11 and 17 of the adsorber 2, and use the adsorber 2 to adsorb cyclohexanone . At the same time, the molecular sieve in the adsorber 1 is desorbed, the main intake valve 20 is opened, and the gas heater turns the N 2 Heating to 300°C, opening the valves 16 and 10 in turn, desorbing the adsor...

Embodiment 2

[0030] After the adsorbent in Example 1 is continuously adsorbed and desorbed 10 times, under the same conditions, continue to adsorb, the temperature of cyclohexanone is 25 ° C, check all valves to make it in a closed state, open the inlet and outlet valves 7, 8, 15, control the flow rate of the flowmeter to 5mL / min, and take the cyclohexanone flowing out from the adsorber 1 as 0h, and analyze the sample at the outlet of the adsorber 1. The analysis data is as follows:

[0031]

[0032] When 5h, the total impurity content is 30ppm, and the product does not meet the target requirements, close the inlet and outlet valves 8 and 15 of the adsorber 1, open the inlet and outlet valves 11 and 17 of the adsorber 2, and use the adsorber 2 to adsorb cyclohexanone , the effect is the same as that of the adsorber 1, and the total impurity content after adsorption is less than 30ppm. At the same time, the molecular sieve in the adsorber 1 is desorbed, the main intake valve 20 is opene...

Embodiment 3

[0034] Weigh 50g of ZSM-5 bar-shaped molecular sieve with a silicon-aluminum ratio of 100, and place them in two adsorbers respectively. The temperature of cyclohexanone is 30°C. Check all valves to keep them closed, and open the inlet and outlet of adsorber 1. Valves 7, 8, and 15 control the flow rate of the flowmeter to 5mL / min, and take cyclohexanone to flow out from the adsorber 1 as 0h, and analyze the sample at the outlet of the adsorber 1. The analysis data is as follows:

[0035]

[0036] When 5h, the total impurity content is 29ppm, close to 30ppm, and the product does not meet the target requirements. Close the inlet and outlet valves 8 and 15 of the adsorber 1, open the inlet and outlet valves 11 and 17 of the adsorber 2, and use the adsorber 2 to treat cyclohexanone Adsorption treatment is carried out, and the total content of impurities in the output is less than 30ppm. At the same time, the molecular sieve in the adsorber 1 is desorbed, the main intake valve ...

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Abstract

The invention discloses a method for continuous removal of impurities in cyclohexanone. According to the invention, two adsorbing devices are connected in series; an adsorbent is added into the adsorbing devices for continuous adsorption of impurities in cyclohexanone; and when the total content of impurities discharged by one of the adsorbing devices is greater than 30 ppm, the adsorbing device is subjected to desorption and the other adsorbing device is used for continuous adsorption of impurities in cyclohexanone at the same time. The method provided by the invention effectively removes impurities consisting of 2-heptanone, caproic aldehyde and 2-hexanone in cyclohexanone and allows the total content of the impurities to be less than 300 ppm, which meets requirements of chemical fiber-grade cyclohexanone; and the method can carry out continuous adsorption and desorption, so continuous controllable operation is realized.

Description

technical field [0001] The invention belongs to the technical field of organic chemical purification, in particular to a method for continuously removing 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-hexanone, hexanal and 2-heptanone...

Claims

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Application Information

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IPC IPC(8): C07C45/79C07C49/403
CPCC07C45/79C07C49/403
Inventor 刘卓金汉强吴其建何育苗金玉存陈永平
Owner CHINA PETROLEUM & CHEM CORP
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