CN106905139B - Process for extracting high-purity adipic acid - Google Patents
Process for extracting high-purity adipic acid Download PDFInfo
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- CN106905139B CN106905139B CN201710091555.5A CN201710091555A CN106905139B CN 106905139 B CN106905139 B CN 106905139B CN 201710091555 A CN201710091555 A CN 201710091555A CN 106905139 B CN106905139 B CN 106905139B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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Abstract
The invention belongs to the technical field of chemical preparations, and relates to a high-purity adipic acid extraction process which comprises the steps of dissolving crude adipic acid in absolute ethyl alcohol, decoloring by using activated carbon, filtering, adding deionized water to evaporate part of an ethanol-water azeotrope, stirring for crystallization, centrifuging to dry, and drying in vacuum to obtain high-purity adipic acid. The process realizes the high-precision purification of the adipic acid and breaks the monopoly of imported adipic acid on high-tech markets.
Description
Technical Field
The invention relates to the technical field of chemical preparations, in particular to a high-purity adipic acid extraction process which is high in etching speed and stable and enables the surface of a substrate to be smooth and free of residues.
Background
Adipic acid (Adipic acid), also known as Adipic acid, is an important organic dibasic acid, can undergo salt formation reaction, esterification reaction, amidation reaction and the like, and can be polycondensed with diamine or dihydric alcohol to form a high-molecular polymer and the like. Adipic acid is a dicarboxylic acid with important industrial significance, plays an important role in chemical production, organic synthesis industry, medicine, lubricant manufacturing and other aspects, and the yield is the second place in all dicarboxylic acids.
Adipic acid is mainly used as a raw material for nylon 66 and engineering plastics, and also for producing various ester products, and also as a raw material for polyurethane elastomers, and an acidulant for various foods and beverages, which sometimes functions better than citric acid and tartaric acid. Adipic acid is also a raw material for medicines, yeast purification, insecticides, adhesives, synthetic leather, synthetic dyes and perfumes.
The domestic adipic acid market is in a saturated state at present, downstream requirements are not vigorous, and domestic enterprises begin to develop an international market for better ensuring enterprise profits. The capacity of China currently occupies the first position in the international market, secondly, the United states mainly has Inviada and Oldham, wherein shale gas is used in the device of the Inviada in the United states, the production cost is low, secondly, the European Union is the market, adipic acid discharge projects are completely forbidden in 2013, the living environment of adipic acid in the European Union is also restrained to a certain extent, Korea and Brazil are Soowei, and Japan is the formation of Asahi.
The demand of high-end adipic acid products is increased year by year, but the high-end adipic acid source in China mainly depends on import, and the research and development of the purification process of the high-quality adipic acid are particularly important in order to improve the product quality of the adipic acid and the market competitiveness of the product.
Disclosure of Invention
The invention mainly aims to provide a high-purity adipic acid extraction process which has high-speed and stable etching and enables the surface of a substrate to be smooth and have no residue.
The invention realizes the purpose through the following technical scheme:
a process for extracting high-purity adipic acid comprises the following steps:
dissolving and filtering: adding 1 part by mass of crude adipic acid into 1-1.5 parts by mass of absolute ethyl alcohol, heating to 50 ℃ until the crude adipic acid is completely dissolved, adding activated carbon for decolorization, stirring for 30-40 minutes, and filtering to obtain a filtrate.
② evaporative crystallization: adding the filtrate into a crystallization kettle, adding 2-3 parts by mass of deionized water, then distilling 1.5-2.25 parts by mass of ethanol-water azeotrope under vacuum reduced pressure at a controlled temperature of 40-45 ℃, continuing stirring for 2 hours, and fully crystallizing.
Centrifugal drying: and (3) putting the liquid in the crystallization kettle into a centrifugal machine for centrifuging until the liquid is dry, and then drying in a vacuum drier to obtain the high-purity adipic acid.
Specifically, the filtration in the first step is performed by using a ceramic membrane double-filtration device.
Specifically, the amount of the activated carbon is 0.001 parts by mass.
Specifically, the vacuum degree of the vacuum reduced pressure distillation in the step II is 0.08 MPa.
Specifically, the drying temperature is not more than 50 ℃.
By adopting the technical scheme, the technical scheme of the invention has the beneficial effects that:
the process realizes the high-precision purification of the adipic acid and breaks the monopoly of imported adipic acid on high-tech markets.
Detailed Description
A process for extracting high-purity adipic acid comprises the following steps:
dissolving and filtering: adding 1 part by mass of crude adipic acid into 1-1.5 parts by mass of absolute ethyl alcohol, heating to 50 ℃ until the crude adipic acid is completely dissolved, adding activated carbon for decolorization, stirring for 30-40 minutes, and filtering to obtain a filtrate.
② evaporative crystallization: adding the filtrate into a crystallization kettle, adding 2-3 parts by mass of deionized water, then distilling 1.5-2.25 parts by mass of ethanol-water azeotrope under vacuum reduced pressure at a controlled temperature of 40-45 ℃, continuing stirring for 2 hours, and fully crystallizing.
Centrifugal drying: and (3) putting the liquid in the crystallization kettle into a centrifugal machine for centrifuging until the liquid is dry, and then drying in a vacuum drier to obtain the high-purity adipic acid.
The present invention will be described in further detail with reference to specific examples.
Example 1:
dissolving and filtering
Adding 1000kg of 96% crude adipic acid into 1000kg of absolute ethyl alcohol, heating to 50 ℃ until the adipic acid is completely dissolved, adding 1kg of activated carbon for decolorization, stirring for 30 minutes, and pumping the solution into a ceramic membrane double-filtration device for filtration to a crystallization kettle.
② evaporative crystallization
2000kg of normal temperature deionized water is added to reduce the temperature of the liquid in the kettle to below 15 ℃, the temperature is controlled to be 45 ℃, the ethanol-water azeotrope is evaporated under vacuum pressure reduction under the vacuum degree of 0.08MPa for 1500L, white crystals are gradually generated in the crystallization kettle, and the mixture is stirred for 2 hours and fully crystallized.
③ centrifugal drying
And (3) putting the liquid in the crystallization kettle into a centrifuge for centrifuging until the liquid is dry, putting the solid into a vacuum drier for drying at the temperature of below 50 ℃, and weighing to calculate the yield and the purity.
Example 2:
dissolving and filtering
Adding 1000kg of 96% crude adipic acid into 1500kg of absolute ethyl alcohol, heating to 50 ℃ until the adipic acid is completely dissolved, adding 1kg of activated carbon for decolorization, stirring for 30 minutes, and pumping the solution into a ceramic membrane double-filtration device for filtration to a crystallization kettle.
② evaporative crystallization
3000kg of normal temperature deionized water is added to reduce the temperature of the liquid in the kettle to below 15 ℃, ethanol-water azeotrope 2250L is evaporated out under vacuum pressure reduction at 40 ℃ under the vacuum degree of 0.08MPa, white crystals are gradually generated in the crystallization kettle, and the mixture is stirred for 2 hours and fully crystallized.
③ centrifugal drying
And (3) putting the liquid in the crystallization kettle into a centrifuge for centrifuging until the liquid is dry, putting the solid into a vacuum drier for drying at the temperature of below 50 ℃, and weighing to calculate the yield and the purity.
Example 3:
dissolving and filtering
Adding 1000kg of 96% crude adipic acid into 1200kg of absolute ethyl alcohol, heating to 50 ℃ until the adipic acid is completely dissolved, adding 1kg of activated carbon for decolorization, stirring for 30 minutes, and pumping the solution into a ceramic membrane double-filtration device for filtration to a crystallization kettle.
② evaporative crystallization
2400kg of normal temperature deionized water is added to reduce the temperature of the liquid in the kettle to below 15 ℃, the temperature is controlled to be 43 ℃, the ethanol-water azeotrope is distilled out by vacuum decompression under the vacuum degree of 0.08MPa, 1800L of ethanol-water azeotrope is gradually generated in the crystallization kettle, white crystals are generated, and the mixture is stirred for 2 hours and fully crystallized.
③ centrifugal drying
And (3) putting the liquid in the crystallization kettle into a centrifuge for centrifuging until the liquid is dry, putting the solid into a vacuum drier for drying at the temperature of below 50 ℃, and weighing to calculate the yield and the purity.
In the method, the adipic acid is gradually separated out along with the evaporation of the ethanol, the crystals slowly grow, and the wall-bonding and caking phenomena caused by the concentrated separation of a large amount of solids are avoided, so that the peritectic phenomena are reduced to the maximum extent, the product purity is improved, and the subsequent drying is more convenient.
Comparative examples 1 to 3:
dissolving 1000kg of 96% crude adipic acid in 2000kg of deionized water, adding 1kg of activated carbon for decolorization, then carrying out evaporation crystallization in a crystallizer, carrying out centrifugal drying to obtain a product, and weighing to calculate the yield and the purity.
The above process was repeated twice and the yield and purity were calculated by weighing.
In the conventional process, water is used as a solvent and a special crystallizer is used for ensuring the separation of blocky crystals, the operation is complicated, seed crystals are required to be added for controlling crystallization, the subsequent centrifugal drying is difficult, and the quality is possibly unstable due to peritectic crystallization.
The data on the yield purity of the high purity adipic acid obtained in examples 1 to 3 were compared with the data on the yield purity of the adipic acid obtained in comparative examples 1 to 3 by crystallization with water only, as shown in Table 1.
Table 1:
as can be seen from Table 1, the higher purity oxalic acid was obtained without a significant decrease in yield in the examples, and the disappearance of the caking phenomenon is more indicative of the decrease in the impurity peritectic phenomenon. Therefore, the process realizes the high-precision purification of the adipic acid and breaks through the monopoly of imported adipic acid on high-tech markets.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (3)
1. A high-purity adipic acid extraction process is characterized by comprising the following steps:
dissolving and filtering: adding 1 part by mass of crude adipic acid into 1-1.5 parts by mass of absolute ethyl alcohol, heating to 50 ℃ until the crude adipic acid is completely dissolved, adding activated carbon for decolorization, stirring for 30-40 minutes, and filtering to obtain a filtrate;
② evaporative crystallization: adding the filtrate into a crystallization kettle, adding 2-3 parts by mass of deionized water, then evaporating 1.5-2.25 parts by mass of ethanol-water azeotrope under vacuum reduced pressure at the controlled temperature of 40-45 ℃, keeping the vacuum degree of vacuum reduced pressure distillation at 0.08MPa, continuing stirring for 2 hours, and fully crystallizing;
centrifugal drying: and (3) putting the liquid in the crystallization kettle into a centrifuge for centrifuging until the liquid is dry, and then drying in a vacuum drier at the drying temperature of not more than 50 ℃ to obtain the high-purity adipic acid.
2. The process for extracting high purity adipic acid according to claim 1, wherein: and (4) filtering in the step I by adopting a ceramic membrane double-filtering device.
3. The process for extracting high purity adipic acid according to claim 1, wherein: the amount of the active carbon is 0.001 part by mass.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710091555.5A CN106905139B (en) | 2017-02-20 | 2017-02-20 | Process for extracting high-purity adipic acid |
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| CN201710091555.5A CN106905139B (en) | 2017-02-20 | 2017-02-20 | Process for extracting high-purity adipic acid |
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| CN106905139A CN106905139A (en) | 2017-06-30 |
| CN106905139B true CN106905139B (en) | 2020-10-02 |
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| CN112441915A (en) * | 2019-09-04 | 2021-03-05 | 中国石油化工股份有限公司 | Method for treating crystallization mother liquor in adipic acid crystallization refining process |
| CN112441913B (en) * | 2019-09-04 | 2022-11-04 | 中国石油化工股份有限公司 | Method for purifying adipic acid |
| CN115010595B (en) * | 2022-07-27 | 2024-07-09 | 江苏道尔顿石化科技有限公司 | Method for forming sorbic acid coarse crystals |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1611477A (en) * | 2003-10-29 | 2005-05-04 | 宁波敏特尼龙工业有限公司 | Process for producing adipic acid and hexanediamine by depolymerization of nylon-66 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1611477A (en) * | 2003-10-29 | 2005-05-04 | 宁波敏特尼龙工业有限公司 | Process for producing adipic acid and hexanediamine by depolymerization of nylon-66 |
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