CN111807951A - Method for treating itaconic acid fermentation mother liquor by multistage extraction and steam stripping coupling - Google Patents
Method for treating itaconic acid fermentation mother liquor by multistage extraction and steam stripping coupling Download PDFInfo
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- CN111807951A CN111807951A CN202010756197.7A CN202010756197A CN111807951A CN 111807951 A CN111807951 A CN 111807951A CN 202010756197 A CN202010756197 A CN 202010756197A CN 111807951 A CN111807951 A CN 111807951A
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- 238000000605 extraction Methods 0.000 title claims abstract description 135
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 title claims abstract description 70
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000012452 mother liquor Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000000855 fermentation Methods 0.000 title claims abstract description 38
- 230000004151 fermentation Effects 0.000 title claims abstract description 38
- 230000008878 coupling Effects 0.000 title claims abstract description 8
- 238000010168 coupling process Methods 0.000 title claims abstract description 8
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000003860 storage Methods 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000000284 extract Substances 0.000 claims abstract description 12
- 238000011084 recovery Methods 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 239000011555 saturated liquid Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004064 recycling Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 125000004122 cyclic group Chemical group 0.000 abstract description 3
- 150000002148 esters Chemical class 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 7
- 239000012528 membrane Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- KSSNXJHPEFVKHY-UHFFFAOYSA-N phenol;hydrate Chemical compound O.OC1=CC=CC=C1 KSSNXJHPEFVKHY-UHFFFAOYSA-N 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000002921 fermentation waste Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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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
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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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
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for treating itaconic acid fermentation mother liquor by multi-stage extraction and steam stripping coupling and a device suitable for the method. According to the method, ethyl acetate is used as an extracting agent, itaconic acid fermentation mother liquor firstly enters an extraction kettle for extraction and separation, a part of mixture of the extracting agent and the itaconic acid fermentation mother liquor enters a next-stage extraction kettle for cyclic extraction and separation in sequence, an extract phase enters a stripping tower through an extract phase storage tank, a raffinate phase enters a raffinate phase ester recovery kettle through an extract phase storage tank, a top material flow enters the bottom of the stripping tower, a high-purity itaconic acid-containing saturated liquid is obtained at the bottom after stripping, the bottom material flow is recycled to the stripping tower, and the top material flow enters a delayer after being condensed by a condenser to obtain the extracting agent for cyclic use. The method has the advantages of low energy consumption, simple process, high purity of the separated itaconic acid and the like, the adopted extractant ethyl acetate is easy to recover, the chemical thermal stability is good, and the loss of the extractant is reduced.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of chemical separation and purification, particularly relates to a method for treating itaconic acid fermentation mother liquor by multistage extraction and stripping coupling, and further relates to a method for extracting and stripping purified itaconic acid fermentation mother liquor by using ethyl acetate as an extracting agent and adopting an extraction tower and a stripping tower.
[ background of the invention ]
Itaconic acid is also called itaconic acid, is a chemical intermediate with wide application prospect, and the annual total demand of itaconic acid is about 150 million tons in the world. At present, the industrial production method of itaconic acid comprises a chemical synthesis method and a fermentation method, and the fermentation method mainly adopts biomass energy sources such as straws and the like as raw materials, so that the use of fossil energy is avoided, the advantages of energy safety, environmental protection, economy and the like are combined, and the fermentation method is adopted to produce the itaconic acid internationally. In the fermentation method, a recrystallization method is generally adopted to separate and extract products, and along with the concentration process, the viscosity and the chromaticity of the mother liquor are increased, so that the re-extraction difficulty of the products is increased, and further, the itaconic acid fermentation mother liquor with the COD of 80 ten thousand mg/L is generated. In recent years, the discharge amount of fermentation mother liquor generated by the fermentation of itaconic acid is gradually increased along with the enlargement of the production scale of the fermentation of itaconic acid. Therefore, the development of an economical and efficient itaconic acid mother liquor recycling treatment technology is very urgent.
The itaconic acid fermentation mother liquor has the characteristics of more suspended matters, higher viscosity, strong acidity, deep chroma and the like, and the treatment technology of the itaconic acid fermentation mother liquor is researched at home and abroad, and the current methods for treating the itaconic acid fermentation mother liquor mainly comprise a physical chemical method, a biological method, a crystallization method, an ion exchange resin method, a solvent extraction method and the like.
Chinese patent CN102816055B discloses a new process for treating itaconic acid fermentation waste mother liquor by utilizing a seawater desalination membrane separation technology, which can recycle the itaconic acid fermentation mother liquor, improve the total yield of itaconic acid produced by a fermentation method and reduce the production cost.
Chinese patent CN101085734 discloses a method for purifying itaconic acid fermentation liquor by using nanofiltration membrane, ultrafiltration membrane or microfiltration membrane or further extracting itaconic acid from itaconic acid mother liquor, which has the characteristics of high yield, good product quality, low operation cost, simple and efficient operation, and is suitable for industrial production, but the method has higher energy consumption.
Chinese patent CN202893068U discloses a method for separating itaconic acid mother liquor by a vacuum negative pressure centrifugal separation device, which has the advantages of convenient use, good separation effect and reduced labor intensity of workers.
The prior technology for purifying and treating the itaconic acid fermentation mother liquor has the problems of resource waste, low removal rate and the like, and the technology for separating and treating the itaconic acid fermentation mother liquor has the problems of high energy consumption and the like.
The invention adopts extraction and stripping process to treat the itaconic acid fermentation waste mother liquor, extracts the itaconic acid, ensures that the extraction rate of organic acid is more than or equal to 99.5 percent (mass percentage), the purity of the recovered itaconic acid is more than or equal to 99 percent (mass percentage), reduces the COD (chemical oxygen demand) by more than 95 percent, and adopts the stripping method to separate the extractant from the itaconic acid to obtain the itaconic acid with higher purity and regenerate and recycle the extractant, thereby developing a new technology integrating the high-efficiency extraction of the itaconic acid, the regeneration of the extractant and the purification of the itaconic acid, and having the outstanding advantages of low energy consumption, simple and convenient operation, high treatment efficiency and cyclic utilization of resources.
[ summary of the invention ]
[ problem to be solved ]
The invention aims to provide a device for extracting and stripping itaconic acid fermentation mother liquor.
The invention also aims to provide a method for carrying out extraction stripping treatment on itaconic acid fermentation mother liquor by using the device.
It is another object of the present invention to provide the use of ethyl acetate as an extractant in the extractive stripping treatment of itaconic acid fermentation mother liquor.
[ solution ]
The invention is realized by the following technical scheme.
A method for treating itaconic acid fermentation mother liquor by multi-stage extraction and steam stripping coupling is characterized in that a device for realizing the method mainly comprises the following parts: the device comprises an extraction kettle (V1), an extraction kettle (V2), an extraction kettle (V3), a stripping tower (T), an extractant metering tank (U1), a mother liquor metering tank (U2), an extract phase storage tank (D1), a raffinate phase storage tank (D2), a delayer (B), a raffinate recovery kettle (R) and a condenser (C); wherein the extractant metering tank (U1) and the mother liquor metering tank (U2) are respectively connected to an extraction kettle (V1), an extraction kettle (V2) and the top of the extraction kettle (V3), the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3) are sequentially connected from top to bottom and are connected with an extraction phase storage tank (D1) and a raffinate phase storage tank (D2), the bottom of the raffinate phase storage tank (D2) is connected to a raffinate phase recovery kettle (R), the bottom of the extraction phase storage tank (D1) and the top of the raffinate phase recovery kettle (R) are respectively connected with a stripping tower (T), a condenser (C) is connected to the top of the stripping tower (T), and the condensed extract is connected to a delayer (B) and is connected to a pipeline of an extractant circulating material flow;
the method for treating the itaconic acid fermentation mother liquor by adopting the device through multistage extraction and steam stripping coupling comprises the following steps:
(1) ethyl acetate and itaconic acid fermentation mother liquor respectively enter from the tops of an extraction kettle (V1), an extraction kettle (V2) and an extraction kettle (V3) through an extractant metering tank (U1) and a mother liquor metering tank (U2), after effective contact extraction separation, a mixture of extraction phase itaconic acid and an extractant enters an extraction phase storage tank (D1) from the bottoms of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3), a mixture of raffinate phase water and the extractant enters an extract phase storage tank (D2) from the bottoms of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3), a mixture of the extractant and the itaconic acid fermentation mother liquor enters the top of the extraction kettle (V2) from the bottom of the extraction kettle (V1), and a mixture of the extraction kettle (V7378) enters the top of the extraction kettle (V3) from the bottom of the top of the extraction kettle (V6866), and a mixture of the extraction kettle (V3) enters the top of the extraction kettle (V1);
(2) after the extraction agent is recovered by the residual phase recovery kettle (R), the extractant in the extraction residual phase is connected to the bottom of a stripping tower (T) through a top material flow, the extraction phase is connected with the stripping tower (T), saturated liquid containing itaconic acid is extracted from the bottom of the stripping tower, the top of the stripping tower is condensed by a condenser (C) and then connected with a delayer (B), the extractant is extracted in layers for recycling, and the itaconic acid mixed liquid at the bottom of the stripping tower is recycled to the stripping tower (T4);
the extraction agent is ethyl acetate, the mass ratio of the feed flow of the extraction agent to the itaconic acid fermentation mother liquor is 1-3, the operating pressure of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3) is 1atm, the number of tower plates of the stripping tower (T) is 10-20, the purity of the itaconic acid recovered from the bottom of the stripping tower (T) is higher than 99.9%, and the yield is higher than 95%.
[ advantageous effects ]
Compared with the prior art, the invention mainly has the following beneficial effects:
(1) the itaconic acid fermentation mother liquor is purified by adopting the method, so that the extraction rate of the organic acid is over 99 percent, and meanwhile, high-purity itaconic acid resources can be recovered from the wastewater.
(2) The method replaces a chemical method with a physical method for extracting agent regeneration, and solves the problems of long process flow, huge equipment and the like when the extracting agent is recycled.
(3) The method develops a low-energy-consumption high-efficiency extractant regeneration process technology, solves the problem of higher organic acid extraction cost at present, and promotes the popularization and application of a wastewater treatment technology.
[ description of the drawings ]
FIG. 1 is a process flow diagram of the extraction stripping treatment of itaconic acid fermentation mother liquor of the invention.
In the figure, V1, V2 and V3-extraction kettles; a T-stripper; u1-extractant metering tank; u2-mother liquor metering tank; d1-extract phase storage tank; d2-extraction raffinate storage tank; b-a delayer; r-residual phase recovery kettle; c-a condenser; the numbers represent the respective lines.
[ detailed description ] embodiments
Example 1:
the feed flow is 100kg/h, the feed contains 7% of itaconic acid and 93% of water (mass fraction), the operating pressure of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3) is 0.01atm, the mixture of itaconic acid and water enters from the tops of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3), the extractant enters from the tops of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3), the extractant is ethyl acetate, the flow is 100kg/h (the mass ratio of the feeding flow of the extractant to the phenol-water mixture is 1), and the temperatures of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3) are 30 ℃. The number of theoretical plates in the stripping tower (T) is 20, the purity of the separated itaconic acid is 99.9%, and the yield is 95.1%.
Example 2:
the feed flow is 100kg/h, the feed contains 8% of itaconic acid and 92% of water (mass fraction), the operating pressure of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3) is 0.015atm, the mixture of itaconic acid and water enters from the tops of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3), the extractant enters from the tops of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3), the extractant is ethyl acetate, the flow is 200kg/h (the mass ratio of the feeding flow of the extractant to the phenol-water mixture is 2), and the temperatures of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3) are 30 ℃. The number of theoretical plates in the stripping tower (T) is 15, the purity of the separated itaconic acid is 99.96%, and the yield is 95.0%.
Example 3:
the feed flow is 100kg/h, the feed contains 9% of itaconic acid and 91% of water (mass fraction), the operating pressure of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3) is 0.02atm, the mixture of itaconic acid and water enters from the tops of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3), the extractant enters from the tops of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3), the extractant is ethyl acetate, the flow is 300kg/h (the mass ratio of the feeding flow of the extractant to the phenol-water mixture is 3), and the temperatures of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3) are 30 ℃. The number of theoretical plates in the stripping tower (T) is 10, the purity of the separated itaconic acid is 99.98%, and the yield is 95.1%.
Claims (1)
1. A method for treating itaconic acid fermentation mother liquor by multi-stage extraction and steam stripping coupling is characterized in that a device for realizing the method mainly comprises the following parts: the device comprises an extraction kettle (V1), an extraction kettle (V2), an extraction kettle (V3), a stripping tower (T), an extractant metering tank (U1), a mother liquor metering tank (U2), an extract phase storage tank (D1), a raffinate phase storage tank (D2), a delayer (B), a raffinate recovery kettle (R) and a condenser (C); wherein the extractant metering tank (U1) and the mother liquor metering tank (U2) are respectively connected to an extraction kettle (V1), an extraction kettle (V2) and the top of the extraction kettle (V3), the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3) are sequentially connected from top to bottom and are connected with an extraction phase storage tank (D1) and a raffinate phase storage tank (D2), the bottom of the raffinate phase storage tank (D2) is connected to a raffinate phase recovery kettle (R), the bottom of the extraction phase storage tank (D1) and the top of the raffinate phase recovery kettle (R) are respectively connected with a stripping tower (T), a condenser (C) is connected to the top of the stripping tower (T), and the condensed extract is connected to a delayer (B) and is connected to a pipeline of an extractant circulating material flow;
the method for treating the itaconic acid fermentation mother liquor by adopting the device through multistage extraction and steam stripping coupling comprises the following steps:
(1) ethyl acetate and itaconic acid fermentation mother liquor respectively enter from the tops of an extraction kettle (V1), an extraction kettle (V2) and an extraction kettle (V3) through an extractant metering tank (U1) and a mother liquor metering tank (U2), after effective contact extraction separation, a mixture of extraction phase itaconic acid and an extractant enters an extraction phase storage tank (D1) from the bottoms of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3), a mixture of raffinate phase water and the extractant enters an extract phase storage tank (D2) from the bottoms of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3), a mixture of the extractant and the itaconic acid fermentation mother liquor enters the top of the extraction kettle (V2) from the bottom of the extraction kettle (V1), and a mixture of the extraction kettle (V7378) enters the top of the extraction kettle (V3) from the bottom of the top of the extraction kettle (V6866), and a mixture of the extraction kettle (V3) enters the top of the extraction kettle (V1);
(2) after the extraction agent is recovered by the residual phase recovery kettle (R), the extractant in the extraction residual phase is connected to the bottom of a stripping tower (T) through a top material flow, the extraction phase is connected with the stripping tower (T), saturated liquid containing itaconic acid is extracted from the bottom of the stripping tower, the top of the stripping tower is condensed by a condenser (C) and then connected with a delayer (B), the extractant is extracted in layers for recycling, and the itaconic acid mixed liquid at the bottom of the stripping tower is recycled to the stripping tower (T4);
the extraction agent is ethyl acetate, the mass ratio of the feed flow of the extraction agent to the itaconic acid fermentation mother liquor is 1-3, the operating pressure of the extraction kettle (V1), the extraction kettle (V2) and the extraction kettle (V3) is 1atm, the number of tower plates of the stripping tower (T) is 10-20, the purity of the itaconic acid recovered from the bottom of the stripping tower (T) is higher than 99.9%, and the yield is higher than 95%.
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