CN109809982B - Long-chain dicarboxylic acid industrialized refining system and refining process - Google Patents
Long-chain dicarboxylic acid industrialized refining system and refining process Download PDFInfo
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Abstract
The invention discloses a long-chain dicarboxylic acid industrialized refining system and a refining process, wherein the long-chain dicarboxylic acid industrialized refining system comprises: the device comprises a dibasic acid fermentation liquid tank, a crude product filtering unit, a dissolving and extracting unit, an active carbon decoloring unit, an active carbon filtering unit, a crystallizing unit, a vacuum filtering unit, a vacuum drying unit, a packaging unit, a dibasic acid recovering unit and a solvent recovering unit, and also comprises a waste residue processing unit, a waste water processing unit and a waste gas processing unit. By adopting the long-chain dibasic acid industrialized refining system and the refining process, the yield of the dibasic acid reaches over 90 percent, the total acid content in a dibasic acid finished product is over 99 percent, the three wastes are discharged after reaching the standard, and the annual output of the dibasic acid can reach kiloton grade.
Description
Technical Field
The invention relates to the technical field of long carbon chain dibasic acid preparation, in particular to an industrial refining system and a refining process for long carbon chain dibasic acid.
Background
The long carbon chain dibasic acid refers to aliphatic dicarboxylic acid (DCn for short) with more than 10 carbon atoms in the carbon chain, comprises saturated and unsaturated dicarboxylic acid, is a fine chemical product with important and wide industrial application, and is an important raw material for synthesizing high-grade spices, high-performance engineering plastics, high-temperature dielectric media, high-grade hot melt adhesives, cold-resistant plasticizers, high-grade lubricating oil, high-grade paint, coating and the like in the chemical industry.
The existing methods related to refining long-chain dicarboxylic acid have many reports, and are basically divided into a water phase method and a solvent method.
The aqueous phase method means that the refining and extraction process of the long-chain dibasic acid is completely finished in the aqueous phase. For example, patent application No. 201420265115.9 discloses a refining and purifying device for long-chain dibasic acid produced by a biological fermentation method by an aqueous phase method, which comprises a dissolving tank, a first filter, a decoloring tank, a filter, an acidification tank, a first centrifugal separator, a high-temperature and high-pressure water washing tank, a second centrifugal separator, an auger, a flash evaporation dryer and other devices, wherein the device uses sodium hydroxide solution to precipitate impurities, uses activated carbon to decolor, and dissolves, crystallizes, crushes and dries the long-chain dibasic acid after the long-chain dibasic acid is separated out by acid liquor. And for another example, in patent application No. 201110269422.5, the crude dibasic acid produced by biological fermentation is added into a dissolving tank, activated carbon or resin is added into the dissolving tank, deionized water is added, stirring is started, the temperature is raised, the temperature is kept for 30min, the material is pressed into a filter for filtration, and the clear liquid is cooled, crystallized and centrifugally dried to obtain the refined dibasic acid.
The solvent method means that the purification of the long-chain dibasic acid is completed in an organic solvent. At present, alcohols, ethers, esters and the like are mainly used as organic solvents. For example, in patent application No. 201410354804.1, the biological fermentation broth is heated to demulsify, filtered by a ceramic membrane and an ultrafiltration membrane to obtain an ultrafiltrate, the ultrafiltrate is mixed with isoamyl alcohol, heated and preserved, concentrated sulfuric acid is added to adjust the pH of the material, the mixture is stirred, mixed and then kept stand, an extract phase is taken, cooled, crystallized, filtered and dried to obtain binary acid crystals. Also, for example, patent application No. 201310391257.X provides a continuous crystallization method of long-chain dibasic acid, which comprises the steps of firstly obtaining an organic solution containing dibasic acid by microbial fermentation or chemical synthesis, then cooling and crystallizing the organic solution, wherein the continuous crystallization is divided into three-stage crystallization, the retention time of each stage of crystallization is more than or equal to 1 hour, the three-stage crystallization devices are connected in series, each stage of crystallization equipment is provided with a cooling device, the crystallization temperature of the first-stage crystallization is 1-10 ℃ lower than the precipitation temperature of the dibasic acid in an organic solvent, the crystallization temperature of the second-stage crystallization is 5-15 ℃ lower than the crystallization temperature of the first-stage crystallization, the crystallization temperature of the third-stage crystallization is 5-70 ℃ lower than the crystallization temperature of the second-stage crystallization, and finally drying the crystallization liquid to obtain the dibasic acid.
The operation conditions of the prior art water phase method patent application No. 201420265115.9 and the prior art water phase method patent application No. 201110269422.5 are high temperature and high pressure, and have certain dangerousness; meanwhile, the aqueous phase method uses acid and alkali solution, so that the requirement on equipment is high, the waste acid and alkali solution pollute the environment to a certain extent, and long-chain dibasic acid products prepared by the aqueous phase method are low in purity and poor in appearance, color and crystal form. The solvent process patent application No. 201410354804.1 uses batch operation, is a laboratory scale preparation method only, and cannot be directly applied to industrial production. The device report of refining dibasic acid by a solvent method in the patent application number 201310391257.X is only concentrated on a crystallization section, is not comprehensive enough, and cannot be directly applied to industrial production.
Disclosure of Invention
The invention provides an industrial refining system and a refining process for long-chain dibasic acid, which aim to solve the problems in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the first aspect of the invention provides a long-chain dibasic acid industrialized refining system, which comprises a dibasic acid fermentation liquid tank, a crude product filtering unit, a dissolving and extracting unit, an active carbon decoloring unit, an active carbon filtering unit, a crystallizing unit, a vacuum filtering unit, a vacuum drying unit and a packaging unit which are connected in sequence, and further comprises:
the liquid inlet of the dibasic acid recovery unit is connected with the dissolving and extracting unit through a pipeline, and the liquid outlet of the dibasic acid recovery unit is connected with the crude product filtering unit through a pipeline and is used for receiving the water phase extracted by the dissolving and extracting unit, recovering the dibasic acid from the water phase and conveying the recovered dibasic acid to the crude product filtering unit; and
and a liquid inlet of the solvent recovery unit is respectively connected with the vacuum filtration unit and the vacuum drying unit through pipelines, and a liquid outlet of the solvent recovery unit is connected with the dissolving and extracting unit through pipelines and is used for receiving the solvent filtered by the vacuum filtration unit and the solvent dried by the vacuum drying unit and conveying the solvent to the dissolving and extracting unit for recycling.
Further, the industrialized refining system for the long-chain dibasic acid further comprises:
and the waste residue treatment unit is connected with the activated carbon filtering unit and is used for receiving and treating the activated carbon filter cake used by the activated carbon filtering unit.
Further, the industrialized refining system for the long-chain dibasic acid further comprises:
and the wastewater treatment unit is connected with the crude product filtering unit and the solvent recovery unit through pipelines respectively and is used for receiving and treating wastewater discharged by the crude product filtering unit and the solvent recovery unit.
Further, the industrialized refining system for the long-chain dibasic acid further comprises:
and the waste gas treatment unit is respectively connected with the crude product filtering unit, the dissolving and extracting unit, the activated carbon decoloring unit, the activated carbon filtering unit, the crystallizing unit, the vacuum filtering unit, the vacuum drying unit, the dibasic acid recovering unit and the solvent recovering unit through pipelines and is used for receiving and treating waste gas generated in the crude product filtering unit, the dissolving and extracting unit, the activated carbon decoloring unit, the activated carbon filtering unit, the crystallizing unit, the vacuum filtering unit, the vacuum drying unit, the dibasic acid recovering unit and the solvent recovering unit.
Further, the long-chain dicarboxylic acid industrial refining system is characterized in that the packaging unit is connected with the vacuum drying unit and used for receiving and packaging the long-chain dicarboxylic acid finished product dried by the vacuum drying unit.
The second aspect of the invention provides an industrial refining process of long-chain dibasic acid by adopting the refining system, which comprises the following steps:
step 1, conveying a dibasic acid crude product in a dibasic acid fermentation liquid tank to a crude product filtering unit for filter pressing, conveying a dibasic acid filter cake to a dissolving and extracting unit, and conveying a filtrate to a wastewater treatment unit for treatment;
step 2, dissolving the dibasic acid filter cake in the dissolving and extracting unit by a solvent, carrying out water washing extraction and layering, sending an oil phase into the activated carbon decoloring unit, and sending a water phase into the dibasic acid recovery unit for recovery treatment;
step 3, carrying out activated carbon decoloration treatment on the oil phase in the activated carbon decoloration unit, feeding the decolored solution into the activated carbon filtration unit for filtration, feeding the filtered decolored solution into the crystallization unit for crystallization, and feeding the filtered activated carbon filter cake into a waste residue treatment unit;
step 4, sending the crystallized liquid into the vacuum filtration unit for vacuum filtration, and sending the solvent subjected to vacuum filtration and vacuum drying into the solvent recovery unit for refining treatment and recycling; and sending the filter cake into the vacuum drying unit for vacuum drying to obtain a long-chain dicarboxylic acid finished product, and sending the long-chain dicarboxylic acid finished product to a packaging unit.
Further, in the industrial refining process of the long-chain dibasic acid, acid-containing waste gas generated by the crude product filtering unit and the dibasic acid recovering unit is conveyed to the waste gas treatment unit through a pipeline, and is discharged after being subjected to alkali washing treatment; and solvent-containing waste gas generated in the dissolving extraction unit, the activated carbon decoloring unit, the activated carbon filtering unit, the crystallizing unit, the vacuum filtering unit, the vacuum drying unit and the solvent recovery unit is conveyed to the waste gas treatment unit through a pipeline and is discharged after condensation and activated carbon adsorption treatment.
Further, in the industrial refining process of the long-chain dibasic acid, the crude product of the dibasic acid in the step 1 is dibasic acid fermentation liquor obtained by biological fermentation; in the step 2, the solvent is alcohol or ether, and the alcohol or ether is selected from one or more of isoamylalcohol, 1-pentanol, 1-hexanol, ethylene glycol, butyl ether, amyl ether, anisole and phenetole.
Further, in the industrial refining process of the long-chain dicarboxylic acid, the moisture content of the dicarboxylic acid filter cake in the step 2 is 25-75%, the extraction operation temperature is 50-170 ℃, and the operation pressure is 0.0-0.5 MPaG.
Further, in the long-chain dicarboxylic acid industrial refining process, the operating temperature for decoloring the activated carbon in the step 3 is 50-170 ℃, the operating pressure is 0.0-0.5 MPaG, and the adding amount of the activated carbon is 1-15%; the operation temperature of the crystallization is 0-140 ℃, and the operation pressure is 0.0-0.5 MPaG.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the long-chain dibasic acid industrialized refining system provided by the invention integrates dibasic acid refining, dibasic acid recovery and solvent recycling, a dibasic acid fermentation liquid obtained by biological fermentation is adopted as a dibasic acid crude product, alcohol and ether are adopted as an extraction solvent, and based on the refining system and the refining process, the yield of dibasic acid reaches over 90 percent, the total acid content in a dibasic acid finished product is over 99 percent, the three wastes are discharged up to the standard, and the annual output of the dibasic acid can reach the kiloton level.
Drawings
FIG. 1 is a schematic structural diagram of an industrial refining system for long-chain dicarboxylic acid according to the present invention.
Detailed Description
The present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
Example 1
As shown in fig. 1, an embodiment of the present invention provides an industrial refining system for long-chain dibasic acid, which includes a dibasic acid fermentation tank, a crude product filtering unit, a dissolving and extracting unit, an activated carbon decoloring unit, an activated carbon filtering unit, a crystallizing unit, a vacuum filtering unit, and a vacuum drying unit, which are connected in sequence, and further includes: the liquid inlet of the dibasic acid recovery unit is connected with the dissolving and extracting unit through a pipeline, and the liquid outlet of the dibasic acid recovery unit is connected with the crude product filtering unit through a pipeline and is used for receiving the water phase extracted by the dissolving and extracting unit, recovering the dibasic acid from the water phase and conveying the recovered dibasic acid to the crude product filtering unit; and the liquid inlet of the solvent recovery unit is respectively connected with the vacuum filtration unit and the vacuum drying unit through pipelines, and the liquid outlet of the solvent recovery unit is connected with the dissolving and extracting unit through pipelines and is used for receiving the solvent filtered by the vacuum filtration unit and the solvent dried by the vacuum drying unit and conveying the solvent to the dissolving and extracting unit for recycling.
As shown in fig. 1, in this embodiment, the system for industrially refining a long-chain dibasic acid further includes a waste residue treatment unit, which is connected to the activated carbon filtration unit and is configured to receive and treat an activated carbon filter cake used by the activated carbon filtration unit.
As shown in fig. 1, in this embodiment, the system for industrially refining a long-chain dibasic acid further comprises a wastewater treatment unit, which is respectively connected to the crude product filtration unit and the solvent recovery unit through pipelines, and is configured to receive and treat wastewater discharged from the crude product filtration unit and the solvent recovery unit.
As shown in fig. 1, in this embodiment, the long-chain dicarboxylic acid industrial refining system further includes an exhaust gas treatment unit, which is connected to the crude product filtering unit, the dissolution extraction unit, the activated carbon decoloring unit, the activated carbon filtering unit, the crystallization unit, the vacuum filtering unit, the vacuum drying unit, the dicarboxylic acid recovery unit and the solvent recovery unit through pipelines, respectively, and is configured to receive and treat the exhaust gas generated in the crude product filtering unit, the dissolution extraction unit, the activated carbon decoloring unit, the activated carbon filtering unit, the crystallization unit, the vacuum filtering unit, the vacuum drying unit, the dicarboxylic acid recovery unit and the solvent recovery unit.
In addition, as shown in fig. 1, the long-chain dicarboxylic acid industrial refining system further comprises a packaging unit, which is connected to the vacuum drying unit and is used for receiving and packaging the finished product dried by the vacuum drying unit.
In the embodiment, the crude product filtering unit is a known filtering machine; the dissolving and extracting unit is the existing known dissolving and extracting equipment; the activated carbon decoloring unit and the activated carbon filtering unit are both the existing known activated carbon decoloring equipment and an activated carbon filter; the crystallization unit is a crystallization tank which is known in the prior art; the vacuum filtering unit is a known control drum separator, and the vacuum drying unit is a vacuum belt dryer; the packaging unit is a packaging machine known in the art.
Example 2
The embodiment provides a refining process adopting the long-chain dicarboxylic acid industrialized refining system, which specifically comprises the following steps:
step 1, conveying a dibasic acid crude product in a dibasic acid fermentation liquid tank to a crude product filtering unit for filter pressing, conveying a dibasic acid filter cake to a dissolving and extracting unit, and conveying a filtrate to a wastewater treatment unit for treatment;
step 2, dissolving the dibasic acid filter cake in the dissolving and extracting unit by a solvent, carrying out water washing extraction and layering, sending an oil phase into the activated carbon decoloring unit, and sending a water phase into the dibasic acid recovery unit for recovery treatment;
step 3, carrying out activated carbon decoloration treatment on the oil phase in the activated carbon decoloration unit, feeding the decolored solution into the activated carbon filtration unit for filtration, feeding the filtered decolored solution into the crystallization unit for crystallization, and feeding the filtered activated carbon filter cake into a waste residue treatment unit;
step 4, sending the crystallized liquid into the vacuum filtration unit for vacuum filtration, and sending the solvent subjected to vacuum filtration and vacuum drying into the solvent recovery unit for refining treatment and recycling; and sending the filter cake into the vacuum drying unit for vacuum drying to obtain a long-chain dicarboxylic acid finished product, and sending the long-chain dicarboxylic acid finished product to a packaging unit.
In this embodiment, the acid-containing waste gas generated by the crude product filtering unit and the dibasic acid recovery unit is conveyed to the waste gas treatment unit through a pipeline, and is discharged after being subjected to alkali washing treatment; and solvent-containing waste gas generated in the dissolving extraction unit, the activated carbon decoloring unit, the activated carbon filtering unit, the crystallizing unit, the vacuum filtering unit, the vacuum drying unit and the solvent recovery unit is conveyed to the waste gas treatment unit through a pipeline and is discharged after condensation and activated carbon adsorption treatment.
In this embodiment, the crude diacid in step 1 is a diacid fermentation broth obtained by biological fermentation; in the step 2, the solvent is alcohol, and the alcohol is isoamylol.
In this example, the dibasic acid cake in step 2 had a moisture content of 50%.
In this example, the extraction in step 2 was carried out at 95 ℃ and at 0.1 MPaG.
In this example, the operating temperature for decolorizing the activated carbon in step 3 was 105 ℃, the operating pressure was 0.1MPaG, and the amount of activated carbon added was 8.5%.
In this example, the crystallization in step 3 was carried out at 60 ℃ and at 0.1 MPaG.
Example 3
The embodiment provides an application example based on the long-chain dicarboxylic acid industrial refining system and the refining process, wherein the production scale of a long-chain dicarboxylic acid device is 100 tons/year, and the method specifically comprises the following steps:
step 1, adding a 70 ℃ phenetole solvent into a dissolving and extracting unit, filtering a dibasic acid fermentation liquor in a dibasic acid fermentation liquor tank through a crude product filtering unit, and sending a filtrate to a wastewater treatment unit for treatment;
step 2, conveying the filter cake with the moisture content of 60% obtained after filtering to a dissolving and extracting unit, fully stirring, keeping the temperature in equipment at 90 ℃, and preserving the heat for a period of time to ensure that the dibasic acid is completely dissolved in the solvent; stopping stirring after the binary acid is completely dissolved, standing for a period of time, and dividing water; the separated water phase is sent to a dibasic acid recovery tank for storage; adding deionized water of 70 ℃ into a dissolving and extracting device, heating until the temperature in the dissolving and extracting device reaches 90 ℃, stirring for a period of time, stopping stirring, standing for a period of time, dividing water, and sending the separated water phase to a dibasic acid recovery tank for storage;
step 3, sending the oil phase extracted in the step 2 to an active carbon decoloring unit, adding 2.0% of active carbon, heating until the temperature of the active carbon decoloring unit reaches 95 ℃, stirring for a period of time, then conveying a decoloring solution to an active carbon filtering unit for active carbon filtering, simultaneously preheating a crystallization unit to 90 ℃, transferring a decoloring clear solution, and controlling a binary acid solution in a crystallization tank to slowly cool;
step 4, when the temperature in the crystallization equipment is lower than 40 ℃, conveying the crystallization liquid into a vacuum drum separator for solid-liquid separation, conveying the obtained filter cake to a vacuum belt dryer for drying to obtain a refined long-chain dicarboxylic acid finished product, and bagging the finished product in a packaging machine; and collecting the filtrate obtained by filtering by the filter and the solvent obtained by cooling the tail gas of the dryer in a solvent recovery device, and refining and recycling the solvent.
By adopting the long-chain dibasic acid industrialized refining system and the refining process, the yield of the dibasic acid reaches over 90.0 percent, the total acid content in a dibasic acid finished product is over 99.0 percent, and the three wastes are discharged after reaching the standard.
Example 4
The embodiment also provides an application example based on the long-chain dicarboxylic acid industrial refining system and the refining process, wherein only the production scale of a long-chain dicarboxylic acid device is enlarged to 5000 tons/year, the yield of the dicarboxylic acid reaches more than 91.0 percent, the total acid content in a finished product of the dicarboxylic acid reaches more than 99.2 percent, and the three wastes reach the standard and are discharged.
Example 5
In this example, like example 3, there is also provided an application example based on the above-mentioned long-chain dibasic acid industrial refining system and refining process, in which the production scale of only the long-chain dibasic acid apparatus is modified to 3000 tons/year, and the process operation conditions are as follows:
in this embodiment, the crude diacid in step 1 is a diacid fermentation broth obtained by biological fermentation; in the step 2, the solvent is alcohol, and the alcohol is 1-hexanol; the moisture content of the dibasic acid filter cake is 25 percent; the extraction temperature is 50 ℃, and the extraction pressure is 0.0 MPaG; in the step 3, the operating temperature for decoloring the activated carbon is 50 ℃, the operating pressure is 0.0MPaG, and the adding amount of the activated carbon is 1.0 percent; the crystallization was carried out at 0 ℃ and at 0.0 MPaG.
By adopting the long-chain dibasic acid industrialized refining system and the refining process, the yield of the dibasic acid reaches over 90.4 percent, the total acid content in a dibasic acid finished product is over 99.0 percent, and the three wastes are discharged after reaching the standard.
Example 6
In this example, like example 3, there is also provided an application example based on the above-mentioned long-chain dibasic acid industrial refining system and refining process, in which the production scale of only the long-chain dibasic acid apparatus is modified to 3000 tons/year, and the process operation conditions are as follows:
in this embodiment, the crude diacid in step 1 is a diacid fermentation broth obtained by biological fermentation; in the step 2, the solvent is ether, and the ether is amyl ether; the moisture content of the dibasic acid filter cake is 75 percent; the extraction temperature is 170 ℃, and the extraction pressure is 0.5 MPaG; in the step 3, the operating temperature for decoloring the activated carbon is 170 ℃, the operating pressure is 0.5MPaG, and the adding amount of the activated carbon is 15.0 percent; the crystallization was carried out at 140 ℃ and at an operating pressure of 0.5 MPaG.
By adopting the long-chain dibasic acid industrialized refining system and the refining process, the yield of the dibasic acid reaches over 90.2 percent, the total acid content in a dibasic acid finished product is over 99.1 percent, and the three wastes are discharged after reaching the standard.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (7)
1. The utility model provides a long chain binary acid industrialization refining system which characterized in that, includes binary acid fermentation fluid reservoir, crude filter unit, the extraction unit that dissolves, active carbon decoloration unit, active carbon filter unit, crystallization unit, vacuum filter unit, vacuum drying unit and the packing unit that connects gradually to and still include:
the binary acid recovery unit is connected with the dissolving and extracting unit through a pipeline, and connected with the crude product filtering unit through a pipeline, and is used for receiving the water phase extracted by the dissolving and extracting unit and the water phase extracted and layered by water washing, recovering the binary acid from the water phase, and conveying the recovered binary acid to the crude product filtering unit; and
a liquid inlet of the solvent recovery unit is respectively connected with the vacuum filtration unit and the vacuum drying unit through pipelines, and a liquid outlet of the solvent recovery unit is connected with the dissolving and extracting unit through a pipeline and is used for receiving the solvent filtered by the vacuum filtration unit and the solvent dried by the vacuum drying unit and conveying the solvent to the dissolving and extracting unit for recycling;
the wastewater treatment unit is connected with the crude product filtering unit and the solvent recovery unit through pipelines respectively and is used for receiving and treating wastewater discharged by the crude product filtering unit and the solvent recovery unit;
and the waste residue treatment unit is connected with the activated carbon filtering unit and is used for receiving and treating the activated carbon filter cake used by the activated carbon filtering unit.
2. The system for industrially refining the long-chain dibasic acid according to claim 1, further comprising:
and the waste gas treatment unit is respectively connected with the crude product filtering unit, the dissolving and extracting unit, the activated carbon decoloring unit, the activated carbon filtering unit, the crystallizing unit, the vacuum filtering unit, the vacuum drying unit, the dibasic acid recovering unit and the solvent recovering unit through pipelines and is used for receiving and treating waste gas generated in the crude product filtering unit, the dissolving and extracting unit, the activated carbon decoloring unit, the activated carbon filtering unit, the crystallizing unit, the vacuum filtering unit, the vacuum drying unit, the dibasic acid recovering unit and the solvent recovering unit.
3. An industrial refining process of long-chain dibasic acid by using the refining system of any one of claims 1 to 2, which is characterized by comprising the following steps:
step 1, conveying a dibasic acid crude product in a dibasic acid fermentation liquid tank to a crude product filtering unit for filter pressing, conveying a dibasic acid filter cake to a dissolving and extracting unit, and conveying a filtrate to a wastewater treatment unit for treatment;
step 2, dissolving the dibasic acid filter cake in the dissolving and extracting unit by a solvent, carrying out water washing extraction and layering, sending an oil phase into the activated carbon decoloring unit, and sending a water phase into the dibasic acid recovery unit for recovery treatment;
step 3, carrying out activated carbon decoloration treatment on the oil phase in the activated carbon decoloration unit, feeding the decolored solution into the activated carbon filtration unit for filtration, feeding the filtered decolored solution into the crystallization unit for crystallization, and feeding the filtered activated carbon filter cake into a waste residue treatment unit;
step 4, sending the crystallized liquid into the vacuum filtration unit for vacuum filtration, and sending the solvent subjected to vacuum filtration and vacuum drying into the solvent recovery unit for refining treatment and recycling; and sending the filter cake into the vacuum drying unit for vacuum drying to obtain a long-chain dicarboxylic acid finished product, and sending the long-chain dicarboxylic acid finished product to a packaging unit.
4. The industrial refining process of long-chain dibasic acid according to claim 3, wherein the acid-containing waste gas generated by the crude product filtering unit and the dibasic acid recovering unit is conveyed to the waste gas treatment unit through a pipeline, and is discharged after being subjected to alkali washing treatment; and solvent-containing waste gas generated in the dissolving extraction unit, the activated carbon decoloring unit, the activated carbon filtering unit, the crystallizing unit, the vacuum filtering unit, the vacuum drying unit and the solvent recovery unit is conveyed to the waste gas treatment unit through a pipeline and is discharged after condensation and activated carbon adsorption treatment.
5. The industrial refining process of long-chain dicarboxylic acid according to claim 3, wherein the crude dicarboxylic acid in step 1 is a fermentation broth of dicarboxylic acid obtained by biological fermentation; in the step 2, the solvent is alcohol or ether, and the alcohol or ether is selected from one or more of isoamylalcohol, 1-pentanol, 1-hexanol, ethylene glycol, butyl ether, amyl ether, anisole and phenetole.
6. The industrial refining process of long-chain dicarboxylic acid according to claim 3, wherein the moisture content of the dicarboxylic acid filter cake in step 2 is 25-75%, the extraction temperature is 50-170 ℃, and the extraction pressure is 0.0-0.5 MPaG.
7. The industrial refining process of long-chain dicarboxylic acid according to claim 3, wherein the operating temperature for decoloring the activated carbon in step 3 is 50-170 ℃, the operating pressure is 0.0-0.5 MPaG, and the adding amount of the activated carbon is 1-15%; the operation temperature of the crystallization is 0-140 ℃, and the operation pressure is 0.0-0.5 MPaG.
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| CN102911036A (en) * | 2011-08-01 | 2013-02-06 | 中国石油化工股份有限公司 | Method for obtaining high pure dicarboxylic acid |
| CN104591997A (en) * | 2013-11-03 | 2015-05-06 | 中国石油化工股份有限公司 | Extraction and refining method for long-chain dicarboxylic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102911036A (en) * | 2011-08-01 | 2013-02-06 | 中国石油化工股份有限公司 | Method for obtaining high pure dicarboxylic acid |
| CN104591997A (en) * | 2013-11-03 | 2015-05-06 | 中国石油化工股份有限公司 | Extraction and refining method for long-chain dicarboxylic acid |
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