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Method for purifying cyclohexanone through distillation adsorption

A cyclohexanone and adsorbent technology, applied in chemical instruments and methods, other chemical processes, separation/purification of carbonyl compounds, etc. value, the effect of reducing the content

Active Publication Date: 2014-08-27
沧州旭阳化工有限公司 +1
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the traditional production process of chemical fiber grade cyclohexanone, the method of secondary saponification is generally used, which can remove hexanal and 2-heptanone better, but this method has the disadvantages of large energy consumption, high loss rate, waste liquid Many disadvantages

Method used

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  • Method for purifying cyclohexanone through distillation adsorption
  • Method for purifying cyclohexanone through distillation adsorption
  • Method for purifying cyclohexanone through distillation adsorption

Examples

Experimental program
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Effect test

preparation Embodiment 1

[0039] Preparation Example 1: Treatment of Adsorbent

[0040] Treat the sorbent as follows:

[0041] a) Modification of 4A molecular sieve: add conventional 4A molecular sieve to excess sodium hydroxide solution with a concentration of 0.02mol / L, heat and stir in an oil bath at 85°C for 5h, filter with suction, and rinse with deionized water until neutral , place the obtained sample in a 90°C oven to dry;

[0042] Then the dried 4A molecular sieve was used with 0.02mol / L NH 4 NO 3 The solution was soaked with a solid-to-liquid ratio of 1:15, that is, 15 mL of ammonium nitrate solution per 1 g of 4A molecular sieve, stirred for 5 h under heating in an oil bath at 85 ° C, and then suction filtered and washed. This process was repeated three times;

[0043] After the finally obtained 4A molecular sieve was placed in an oven at 90°C for 5h, it was roasted in a muffle furnace at 550°C for 6h, and after cooling, the 4A molecular sieve used in the above step 2) was obtained;

[0...

Embodiment 1

[0050] In the four adsorption columns (each adsorption column specification: column height 200mm, internal diameter 50mm, volume 0.39L) are respectively filled with 299.48g of activated alumina with an outer diameter of 2 to 3mm prepared in Preparation Example 1; 297.28g of 4A molecular sieve with a diameter of ~3mm; 264.38g of silica gel with an outer diameter of 3~5mm; According to distillation temperature 230℃, adsorption temperature 50℃, adsorption pressure 0.7MPa, liquid space velocity 2.0hr -1 Under the technological conditions of the present invention, the cyclohexanone raw material (the content of hexanal is 371mg / kg, and the content of 2-heptanone is 71mg / kg) before the secondary saponification is first passed through the distiller, and then passed through the adsorption column. The content of the impurity (hexanal and 2-heptanone) of cyclohexanone before and after treatment is shown in Table 2.

[0051] Table 2.

[0052]

[0053]

[0054] Note: "─" indicates ...

Embodiment 2

[0063] In four adsorption columns (each adsorption column specification: column height 200mm, inner diameter 50mm, volume 0.39L), fill successively according to the activated alumina 297.32g of outer diameter 2-3mm prepared in the preparation example 1; 295.58g of 3mm 4A molecular sieve; 270.38g of silica gel with an outer diameter of 3-5mm and 293.64g of bar-shaped 4A molecular sieve, a total of 1156.9g of four kinds of adsorbents. According to distillation temperature 230°C, adsorption temperature 50°C, adsorption pressure 0.7MPa, liquid space velocity 2.5hr -1 Under the technological conditions of the present invention, the cyclohexanone raw material (hexanal content is 290mg / kg, 2-heptanone content is 69mg / kg) before the secondary saponification is first passed through the distiller, and then passed through the adsorption column. The content of the impurity (hexanal and 2-heptanone) of cyclohexanone before and after treatment is shown in Table 4.

[0064] Table 4.

[006...

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Abstract

The invention relates to a method for purifying cyclohexanone through distillation adsorption. The method is characterized in that impurities (hexanal and 2-heptanone) are removed out of cyclohexanone through distillation adsorption. By adsorption columns in a specific order, hexanal and 2-heptanone in the cyclohexanone can be removed by using the distillation adsorption. A secondary saponification method with high cost is not used, the contents of hexanal and 2-heptanone can be fast reduced, a large quantity of solvent type cyclohexanone is converted into chemical fiber cyclohexanone so as to greatly improve the additional value of the cyclohexanone product, and therefore the method has strategic importance to the cyclohexanone production.

Description

technical field [0001] The invention relates to a method for purifying cyclohexanone through distillation and adsorption. The method mainly uses distillation and adsorption to remove the impurities hexanal and 2-heptanone in the cyclohexanone. Background technique [0002] Cyclohexanone is an important organic chemical raw material and industrial solvent, and is also the main intermediate for the preparation of caprolactam and adipic acid. At present, 70% of cyclohexanone in the Chinese market is used to produce caprolactam. The impurities hexanal and 2-heptanone in cyclohexanone are important factors affecting the quality of caprolactam. Therefore improving the purity of cyclohexanone is crucial to improving and improving the quality of caprolactam. At the same time, the total content of hexanal and 2-heptanone is an important factor to distinguish the quality of cyclohexanone. When the sum of the two is lower than 40mg / kg, it is chemical fiber grade cyclohexanone, and whe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/403C07C45/78C07C45/79B01J20/18B01J20/30
CPCB01J20/186B01J20/30C07C45/78C07C45/79C07C45/82C07C2601/14C07C49/403
Inventor 张英伟石峰陈西波王鹏慧闫晶红孙长江
Owner 沧州旭阳化工有限公司
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