CN114380352A - Recovery device and recovery method for ethyl acetate in beta-carotene extraction wastewater - Google Patents
Recovery device and recovery method for ethyl acetate in beta-carotene extraction wastewater Download PDFInfo
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- CN114380352A CN114380352A CN202210096268.4A CN202210096268A CN114380352A CN 114380352 A CN114380352 A CN 114380352A CN 202210096268 A CN202210096268 A CN 202210096268A CN 114380352 A CN114380352 A CN 114380352A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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Abstract
The invention relates to the technical field of solvent recovery, in particular to a recovery device and a recovery method for ethyl acetate in beta-carotene extraction wastewater. The recovery device comprises an adsorption column, a condenser and a layering tank, wherein an inlet of the adsorption column is respectively communicated with a wastewater inlet pipe, a nitrogen inlet pipe, a steam inlet pipe, an organic solvent inlet pipe and a washing water inlet pipe through a main feeding pipe; the recovery method comprises adsorbing ethyl acetate in the beta-carotene extraction wastewater by using an adsorption column filled with macroporous adsorption resin H-01, desorbing the ethyl acetate adsorbed by the resin by using steam after adsorption, collecting desorption liquid, standing to separate a water phase and a solvent phase, and collecting the solvent phase. The method can effectively recover the low-concentration ethyl acetate, has high recovery rate and low energy consumption, can reduce COD in the wastewater, and has good economy.
Description
Technical Field
The invention relates to the technical field of solvent recovery, in particular to a recovery device and a recovery method for ethyl acetate in beta-carotene extraction wastewater.
Background
Beta-carotene belongs to a carotenoid with a chemical formula of C40H56It is widely used in food, feed, medicine and cosmetics industries. At present, the production of beta-carotene mainly comprises two ways of extracting natural beta-carotene and synthesizing beta-carotene, wherein the beta-carotene can be synthesized by a biological method or a chemical method according to different principles.
The beta-carotene production process usually involves an extraction step of beta-carotene, ethyl acetate being one of the main solvents used in this step. Therefore, a small amount of ethyl acetate is often remained in the beta-carotene extraction wastewater, and because the ethyl acetate has very low polarity and low concentration, the ethyl acetate is difficult to recover, and a distillation tower is usually adopted at present for recovery.
Chinese patent application CN201910867154.3 discloses a method for recovering pharmaceutical ethyl acetate waste solvent, which obtains ethyl acetate with purity up to 99% by the processes of impurity removal, extraction, rectification, dehydration and drying. However, the recovery method has large energy consumption and high recovery cost.
Therefore, it is necessary to provide a recovery apparatus and a recovery method for ethyl acetate in β -carotene extraction wastewater with high yield and low energy consumption.
Disclosure of Invention
The invention provides a recovery device and a recovery method of ethyl acetate in beta-carotene extraction wastewater, aiming at the technical problems of low polarity, low concentration and difficult recovery of ethyl acetate in the beta-carotene extraction wastewater.
In a first aspect, the invention provides a recovery device for ethyl acetate in beta-carotene extraction wastewater, which comprises an adsorption column, a condenser and a layering tank, wherein an inlet of the adsorption column is respectively communicated with a wastewater inlet pipe, a nitrogen inlet pipe, a steam inlet pipe, an organic solvent inlet pipe and a washing water inlet pipe through a main feed pipe, an outlet of the adsorption column is respectively communicated with a desorption outlet pipe, a wastewater outlet pipe and a gas outlet pipe through a main discharge pipe, the other end of the desorption outlet pipe is communicated with an inlet of the condenser, and an outlet of the condenser is communicated with an inlet of the layering tank.
In a second aspect, the invention provides a method for recovering ethyl acetate from beta-carotene extraction wastewater, which comprises the steps of adsorbing ethyl acetate in the beta-carotene extraction wastewater by using an adsorption column filled with macroporous adsorption resin H-01, desorbing the ethyl acetate adsorbed by the resin by using steam after adsorption, collecting desorption liquid, standing, separating a water phase and a solvent phase, and collecting the solvent phase.
Further, before adsorbing the beta-carotene extraction wastewater, pretreating an adsorption column, wherein the pretreatment comprises (1) washing the adsorption column with water; (2) ejecting water by using an organic solvent and soaking; (3) the organic solvent was evacuated and washed again with water until the adsorption column was free of organic solvent odor.
Further, in the step (1), washing the adsorption column by using 2-5 times of resin volume (BV).
Further, the organic solvent used in the step (2) is selected from acetone, ethanol, isopropanol or methanol, and the amount of the organic solvent is 1-4 times of the resin volume (BV).
Further, the soaking time in the step (2) is 24-48 h.
Furthermore, the flow rate of the beta-carotene on the column is 0.5-2 times of the resin volume (BV)/h, and the total amount on the column is 5-20 times of the resin volume (BV).
Further, after completion of the adsorption, N was used2Drying the resin, and desorbing the ethyl acetate adsorbed by the resin by using steam with the pressure of 0.02-0.15 MPa.
The invention has the beneficial effects that:
the invention utilizes the principle that van der Waals force on the surfaces of ethyl acetate and macroporous adsorption resin H-01 is mutually attracted to carry out physical adsorption, and the resin has large specific area, strong adsorption capacity and easy desorption; and (3) eluting the resin by using steam as a desorbent, wherein the resin can be repeatedly used after elution. The method can effectively solve the problem that the low-concentration ethyl acetate in the beta-carotene extraction wastewater is difficult to recover.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a schematic view of the structure of a recovery apparatus according to embodiment 1.
FIG. 2 is a gas chromatogram of the wastewater from the extraction of beta-carotene treated in examples 2 to 4.
FIG. 3 is a gas chromatogram of the water sample after adsorption in example 2.
FIG. 4 is a gas chromatogram of ethyl acetate obtained by distillation and recovery after analysis by the adsorption column in example 2.
FIG. 5 is a gas chromatogram of the water sample after adsorption in example 3.
FIG. 6 is a gas chromatogram of ethyl acetate obtained by distillation and recovery after analysis by the adsorption column in example 3.
FIG. 7 is a gas chromatogram of the water sample after adsorption in example 4.
FIG. 8 is a gas chromatogram of ethyl acetate obtained by distillation and recovery after analysis by the adsorption column in example 4.
In the figure, 1-adsorption column, 2-condenser and 3-layering tank.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The utility model provides a recovery unit of ethyl acetate in beta-carotene draws waste water, including adsorption column 1, condenser 2 and layering jar 3, the import of adsorption column 1 advances the pipe with waste water respectively through main inlet pipe, nitrogen gas advances the pipe, the steam advances the pipe, organic solvent advances the pipe and the washing water advances the pipe intercommunication, the export of adsorption column 1 advances the pipe intercommunication with desorption exit tube, waste water exit tube, gas exit tube intercommunication respectively through main discharging pipe, the desorption exit tube other end and 2 import intercommunications of condenser, 2 exports of condenser and the import intercommunication of layering jar 3, all be provided with the valve on each connecting tube.
The working principle of the recovery device is as follows: washing water, organic solvent, steam, N2And the waste water can be introduced into the adsorption column according to a recovery method, wherein the washing water, the organic solvent and the residual waste water after adsorption can be discharged through a waste water outlet pipe, and N2The desorption product obtained after the steam is introduced can be discharged through a desorption outlet pipe, and is condensed into desorption liquid through a condenser, the desorption liquid is stood in a layering tank, and after the water and the ethyl acetate are layered, the water and the ethyl acetate are sequentially discharged, so that the recovery of the ethyl acetate is realized.
Example 2
The COD value of the beta-carotene extraction wastewater is 3.12 multiplied by 104mg/L, the content of ethyl acetate in the wastewater was 0.621% (v/v) as shown in FIG. 2.
The ethyl acetate in the wastewater was recovered by using the recovery apparatus of example 1, and the procedure was as follows:
s1, wetting 4.07L macroporous adsorption resin H-01 with water, stirring uniformly, and loading into a column with specification of H0.12 m and phi 0.36 m;
s2, pretreatment of the adsorption column:
(1) the resin was washed with 8.14L of water;
(2) ejecting the water by using 8.14L of ethanol, and soaking for 24 hours;
(3) emptying ethanol, completely replacing the solvent with water, and washing until the adsorption column has no ethanol smell;
s3, adsorbing the beta-carotene extraction wastewater by column loading, controlling the flow rate to be 0.5BV/h and the total column loading to be 20BV, and performing an ethyl acetate residue test on a 10BV column loading, an instantaneous effluent sample during 20BV column loading and a mixed effluent sample of 20BV column loading, wherein the detection result of a gas chromatograph shows that the ethyl acetate residue concentrations of the three samples are not detected;
the COD value of the water sample after adsorption is 2.85 multiplied by 104mg/L, the gas chromatography detection result is shown in figure 3;
s4, using N2Blowing out water in the adsorption column, introducing steam, controlling the steam pressure to be 0.02MPa, collecting desorption liquid, standing, separating out a water phase, and distilling and collecting a solvent phase to obtain 0.463L of ethyl acetate;
the recovered ethyl acetate was subjected to gas chromatography, and as a result, the purity of ethyl acetate was 99.735% and the recovery rate was 91.35%, as shown in FIG. 4.
Example 3
The COD value of the beta-carotene extraction wastewater is 3.12 multiplied by 104mg/L, ethyl acetate content 0.621% (v/v). The ethyl acetate in the wastewater was recovered by using the recovery apparatus of example 1, and the procedure was as follows:
s1, continuing to use the macroporous adsorption resin H-01 analyzed in example 1, wetting with water, stirring uniformly, and packing into a column, wherein the adsorption column has specifications of H0.12 m and Φ 0.36 m;
s2, pretreatment of the adsorption column:
(1) the resin was washed with 8.14L of water;
(2) ejecting the water by using 8.14L of ethanol, and soaking for 24 hours;
(3) emptying ethanol, completely replacing the solvent with water, and washing until the adsorption column has no ethanol smell;
s3, adsorbing the beta-carotene extraction wastewater on a column, controlling the flow rate to be 1BV/h and the total column loading amount to be 20BV, and performing an ethyl acetate residue test on a 10BV column loading amount, an instantaneous effluent sample during 20BV column loading amount and a mixed effluent sample of 20BV column loading amount, wherein the detection result of a gas chromatograph shows that the ethyl acetate residue concentrations of the three samples are not detected;
the COD value of the water sample after adsorption is 2.96 multiplied by 104mg/L, the gas chromatography detection result is shown in figure 5;
s4, using N2Blowing out water in the adsorption column, introducing steam, controlling steam pressure at 0.08MPa, collecting desorption solution, standing, removing water phase, and distilling solvent phaseCollected to yield 0.477L of ethyl acetate.
The recovered ethyl acetate was analyzed by gas chromatography, and as a result, the purity of ethyl acetate was 99.724% and the recovery rate was 94.10%, as shown in FIG. 6.
Example 4
The COD value of the beta-carotene extraction wastewater is 3.12 multiplied by 104mg/L, ethyl acetate content 0.621% (v/v). The ethyl acetate in the wastewater was recovered by using the recovery apparatus of example 1, and the procedure was as follows:
s1, continuing to use the macroporous adsorption resin H-01 analyzed in example 3, wetting with water, stirring uniformly, and packing into a column, wherein the adsorption column has specifications of H0.12 m and Φ 0.36 m;
s2, pretreatment of the adsorption column:
(1) the resin was washed with 8.14L of water;
(2) ejecting the water by using 8.14L of ethanol, and soaking for 24 hours;
(3) emptying ethanol, completely replacing the solvent with water, and washing until the adsorption column has no ethanol smell;
s3, adsorbing the beta-carotene extraction wastewater on a column, controlling the flow rate to be 1BV/h and the total column loading amount to be 20BV, and performing an ethyl acetate residue test on a 10BV column loading amount, an instantaneous effluent sample during 20BV column loading amount and a mixed effluent sample of 20BV column loading amount, wherein the detection result of a gas chromatograph shows that the ethyl acetate residue concentrations of the three samples are not detected;
the COD value of the water sample after adsorption is 2.90 multiplied by 104mg/L, the gas chromatography detection result is shown in FIG. 7;
s4, using N2Blowing out water in the adsorption column, introducing steam, controlling the steam pressure to be 0.15MPa, collecting desorption liquid, standing, separating out a water phase, and distilling and collecting a solvent phase to obtain 0.467L of ethyl acetate;
the recovered ethyl acetate was analyzed by gas chromatography, and as a result, the purity of ethyl acetate was 99.687% and the recovery rate was 92.10%, as shown in FIG. 8.
Although the present invention has been described in detail by referring to the drawings in connection with the preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention.
Claims (8)
1. The utility model provides a recovery unit of ethyl acetate in beta-carotene draws waste water, which characterized in that, includes adsorption column, condenser and layering jar, the import of adsorption column is advanced the pipe with waste water respectively through main inlet pipe, nitrogen gas advances the pipe, the steam advances the pipe, organic solvent advances the pipe and washing water advances the pipe intercommunication, the export of adsorption column is advanced the pipe intercommunication with desorption exit tube, waste water exit tube, gas exit tube respectively through main discharging pipe, desorption exit tube other end and condenser import intercommunication, the condenser export communicates with the import of layering jar.
2. A method for recovering ethyl acetate from beta-carotene extraction wastewater is characterized in that an adsorption column filled with macroporous adsorption resin H-01 is used for adsorbing ethyl acetate in the beta-carotene extraction wastewater, the ethyl acetate adsorbed by the resin is desorbed by steam after adsorption, desorption liquid is collected and kept stand to separate a water phase and a solvent phase, and the solvent phase is collected.
3. The recovery method according to claim 2, wherein the adsorption column is pretreated before adsorbing the wastewater from the β -carotene extraction, the pretreatment comprising (1) washing the adsorption column with water; (2) ejecting water by using an organic solvent and soaking; (3) the organic solvent was evacuated and washed again with water until the adsorption column was free of organic solvent odor.
4. The recovery method according to claim 3, wherein the adsorption column is washed with 2 to 5 times the volume of the resin in the washing in the step (1).
5. The recycling method according to claim 3, wherein the organic solvent used in the step (2) is selected from acetone, ethanol, isopropanol or methanol, and the amount of the organic solvent is 1 to 4 times the volume of the resin.
6. The recycling method according to claim 3, wherein the soaking time in the step (2) is 24-48 h.
7. The recovery method according to claim 2, wherein the column flow rate of β -carotene is 0.5 to 2 times the volume of the resin per hour, and the total column amount is 5 to 20 times the volume of the resin.
8. The recovery method according to claim 2, wherein N is used after completion of the adsorption2Drying the resin, and desorbing the ethyl acetate adsorbed by the resin by using steam with the pressure of 0.02-0.15 MPa.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1534012A (en) * | 2003-03-28 | 2004-10-06 | 华北制药集团有限责任公司 | Method recovering butylacetate in antibiotic production process |
| CN101066785A (en) * | 2007-06-01 | 2007-11-07 | 浙江工商大学 | Process of separating and recovering extractant from waste erythromycin producing water |
| CN111689857A (en) * | 2020-05-18 | 2020-09-22 | 南京工业大学 | Resource utilization method of ethyl acetate production wastewater |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1534012A (en) * | 2003-03-28 | 2004-10-06 | 华北制药集团有限责任公司 | Method recovering butylacetate in antibiotic production process |
| CN101066785A (en) * | 2007-06-01 | 2007-11-07 | 浙江工商大学 | Process of separating and recovering extractant from waste erythromycin producing water |
| CN111689857A (en) * | 2020-05-18 | 2020-09-22 | 南京工业大学 | Resource utilization method of ethyl acetate production wastewater |
Non-Patent Citations (1)
| Title |
|---|
| 顾霖 等: "超高交联树脂吸附乙酸乙酯蒸汽的动态穿透特性" * |
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