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Causticization method for acidamide oil

A technology for amide oil and amide oil extraction, which is applied in the field of causticization of amide oil, can solve the problems of increasing the chemical oxygen consumption of waste liquid, having no application value, and good solubility of ammonium salt, so as to reduce the chemical oxygen consumption of waste liquid, Improve product quality and improve product quality

Inactive Publication Date: 2009-07-15
TSINGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One is the weak alkalinity of ammonia water, which cannot convert the sulfonic acid by-products into salts that are easy to remove during the extraction process. The sulfonic acid by-products and the sulfur element in them will remain in the system for subsequent purification and wastewater treatment Bring trouble; the 2nd, the cost of ammonia water is higher, and the solubility of ammonium salt is good, and the ammonia nitrogen introduced by causticizing ammonia water all enters waste liquid eventually, has increased the chemical oxygen demand (COD) of waste liquid, and has no application value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A kind of amide oil causticizing method, the slurry prepared with calcium hydroxide and water is used as causticizing agent, and the method steps are as follows,

[0016] (1) prepare causticizing agent, take calcium hydroxide and water as the slurry of raw material preparation as causticizing agent, wherein, the weight percentage of calcium hydroxide is 30%, all the other are water, prepare 20mL of slurry altogether;

[0017] (2) According to the volume ratio of causticizing agent: amide oil = 1:7, take 140mL amide oil, add the causticizing agent and amide oil into the kettle-type causticizing reactor, mix, stir, and react for 30 minutes to obtain a pH value of 9.0 product slurry;

[0018] (3) Filtrate the product slurry with a suction filtration device, separate solid and liquid, obtain causticized amide oil, and perform extraction and separation operations.

[0019] After causticizing, the sulfur content in amide oil decreased by 63% compared with that before caustic...

Embodiment 2

[0021] A kind of amide oil causticizing method, the slurry prepared with calcium hydroxide and water is used as causticizing agent, and the method steps are as follows,

[0022] (1) prepare causticizing agent, take calcium hydroxide and water as the slurry of raw material preparation as causticizing agent, wherein, the weight percentage of calcium hydroxide is 10%, all the other are water, prepare slurry 60mL altogether;

[0023] (2) According to the volume ratio of causticizing agent: amide oil = 1:2, take 120mL amide oil, add the causticizing agent and amide oil into the kettle-type causticizing reactor, mix, stir, and react for 1min to obtain a pH value of 11.0 product slurry;

[0024] (3) Carry out solid-liquid separation to the reaction product slurry with a centrifuge to obtain causticized amide oil, and perform extraction and separation operations.

[0025] After causticizing, the sulfur content in amide oil decreased by 95% compared with that before causticizing.

Embodiment 3

[0027] A kind of amide oil causticizing method, the slurry prepared with calcium hydroxide and water is used as causticizing agent, and the method steps are as follows,

[0028] (1) prepare causticizing agent, take calcium hydroxide and water as the slurry of raw material preparation as causticizing agent, wherein, the weight percentage of calcium hydroxide is 60%, all the other are water, prepare slurry 20mL altogether;

[0029] (2) According to the volume ratio of causticizing agent: amide oil = 1:20, take 400mL of amide oil, add the causticizing agent and amide oil into the kettle-type causticizing reactor, mix, stir, and react for 60 minutes to obtain a pH value of 8.0 product slurry;

[0030] (3) Carry out solid-liquid separation to the product slurry with a hydrocyclone separation device to obtain causticized amide oil, and perform extraction and separation operations.

[0031] After causticizing, the sulfur content in amide oil decreased by 24% compared with that befor...

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Abstract

The invention discloses a causticization method of amide oil which belongs to the technical field of chemical separation. Slurry prepared from calcium hydroxide and water is taken as a causticizer. The method comprises the following steps: preparing the causticizer, taking the slurry prepared by the calcium hydroxide and the water as the causticizer, wherein, weight percentage of the calcium hydroxide is 10-60%, the rest is water; taking the amide oil according to (1-10):20 volume ratio of the causticizer and the amide oil, adding the causticizer and the amide oil to a causticization reactor, mixing, stirring and reacting for 1-60min to obtain product slurry with pH value of 8.0-11.0; directly performing extraction and separation operation on the product slurry, or performing extraction and separation operation on the causticized amide oil which is obtained by solid-liquid separation. Compared with causticization by ammonia, cheaper causticizer is used in the method. The method is expected to achieve the excellent effects of reduced ammonia consumption, improved caprolactam product quality, reduced chemical oxygen consumption of waste liquor, and reduced sulfur emission.

Description

technical field [0001] The invention belongs to the technical field of chemical separation, and in particular relates to a method for causticizing amide oil. Background technique [0002] Amide oil is an intermediate product in the production of nylon 6 monomer caprolactam. The amide oil contains 55-75wt% of caprolactam, 20-25wt% of water, and the rest is ammonium sulfate, sulfonic acid by-products, etc., and is generally weakly acidic. The amide oil undergoes a series of purification steps such as extraction and rectification to obtain caprolactam products. Since the extraction of caprolactam is suitable to be carried out in a neutral or slightly alkaline environment, it is necessary to causticize the amide oil before extraction and separation. At present, the industry generally uses ammonia water causticization to adjust the pH value. There are two deficiencies in this method. One is the weak alkalinity of ammonia water, which cannot convert the sulfonic acid by-produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/10C07D201/16
Inventor 吕阳成骆广生赵承军王仲霞
Owner TSINGHUA UNIV
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