CN114380352B - 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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- CN114380352B CN114380352B CN202210096268.4A CN202210096268A CN114380352B CN 114380352 B CN114380352 B CN 114380352B CN 202210096268 A CN202210096268 A CN 202210096268A CN 114380352 B CN114380352 B CN 114380352B
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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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- 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
- 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 the 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 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 discharging pipe, the other end of the desorption outlet pipe is communicated with the inlet of the condenser, and the outlet of the condenser is communicated with the inlet of the layering tank; the recovery method is that an adsorption column filled with macroporous adsorption resin H-01 is used for adsorbing ethyl acetate in beta-carotene extraction wastewater, the ethyl acetate adsorbed by the resin is desorbed by steam after adsorption, desorption liquid is collected, standing is carried out for separating water phase and solvent phase, and the solvent phase is collected. The method can effectively recycle the low-concentration ethyl acetate, has high recovery rate and low energy consumption, can reduce COD in the wastewater, and has good economical efficiency.
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 is a carotenoid of the formula C 40 H 56 Is widely applied to the industries of foods, feeds, medicines and cosmetics. Currently, 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 biological or chemical methods according to different principles.
The production of beta-carotene generally involves an extraction step of beta-carotene, ethyl acetate being one of the solvents mainly used in this step. Therefore, a small amount of ethyl acetate tends to remain in the beta-carotene extraction wastewater, and the recovery is difficult due to the low polarity and low concentration of ethyl acetate, and a distillation tower recovery mode is often adopted at present.
Chinese patent application CN201910867154.3 discloses a method for recovering pharmaceutical ethyl acetate waste solvent, which comprises removing impurities, extracting, rectifying, dehydrating and drying to obtain ethyl acetate with purity up to 99%. However, this recovery method is energy-consuming and costly.
Therefore, there is a need for a recovery apparatus and recovery method for ethyl acetate in beta-carotene extraction wastewater, which have high yields and low energy consumption.
Disclosure of Invention
Aiming at the technical problems that ethyl acetate in beta-carotene extraction wastewater is low in polarity and concentration and difficult to recover, the invention provides the recovery device and the recovery method for the 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 feeding 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 discharging 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 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 a desorption solution, standing and separating an aqueous phase and a solvent phase, and collecting the solvent phase.
Further, the adsorption column is pretreated before the beta-carotene extraction wastewater is adsorbed, and the pretreatment comprises (1) washing the adsorption column with water; (2) ejecting water by using an organic solvent and then soaking; (3) The organic solvent was drained and the column was again washed with water until no organic solvent odor was present.
Further, in the step (1), the adsorption column is washed with water in an amount of 2 to 5 times the 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 to 4 times of the resin volume (BV).
Further, the soaking time in the step (2) is 24-48 hours.
Further, the flow rate of the beta-carotene to the column is 0.5-2 times of the resin volume (BV)/h, and the total amount of the beta-carotene to the column is 5-20 times of the resin volume (BV).
Further, after the adsorption was completed, N was used 2 Drying 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:
according to the invention, the principle that ethyl acetate and the Van der Waals force on the surface of macroporous adsorption resin H-01 are mutually attracted is utilized to carry out physical adsorption, and the resin has large specific area, strong adsorption capacity and easy desorption; the resin is eluted by using steam as desorbent, and the eluted resin can be reused. The method can effectively solve the problem that the recovery of the low-concentration ethyl acetate in the beta-carotene extraction wastewater is difficult.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the prior art will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
Fig. 1 is a schematic structural view of a recovery apparatus of example 1.
FIG. 2 is a gas chromatogram of the beta-carotene extraction wastewater treated in examples 2-4.
FIG. 3 is a gas chromatogram of a water sample after adsorption in example 2.
FIG. 4 is a gas chromatogram of ethyl acetate obtained by distillation recovery after the adsorption column analysis in example 2.
FIG. 5 is a gas chromatogram of a water sample after adsorption in example 3.
FIG. 6 is a gas chromatogram of ethyl acetate obtained by distillation recovery after the adsorption column analysis in example 3.
FIG. 7 is a gas chromatogram of a water sample after adsorption in example 4.
FIG. 8 is a gas chromatogram of ethyl acetate obtained by distillation recovery after the adsorption column analysis in example 4.
In the figure, a 1-adsorption column, a 2-condenser and a 3-layering tank.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
Example 1
The utility model provides a recovery unit of ethyl acetate in beta-carotene extraction waste water, including adsorption column 1, condenser 2 and layering jar 3, the import of adsorption column 1 is passed through main inlet pipe and is advanced pipe, nitrogen gas advances pipe, steam advances pipe, organic solvent advances pipe and wash water and advances the pipe intercommunication respectively, the export of adsorption column 1 is passed through main discharging pipe and is passed through desorption exit tube, waste water exit tube, gas exit tube intercommunication respectively, desorption exit tube other end and condenser 2 import intercommunication, condenser 2 export and layering jar 3's import intercommunication, all be provided with the valve on each connecting tube.
The working principle of the recovery device is as follows: wash water, organic solvent, steam, N 2 And the waste water can be introduced into an 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, N 2 Can be discharged through a gas outlet pipe, a desorption product obtained after the steam is introduced can be discharged through a desorption outlet pipe, is condensed into desorption liquid through a condenser, the desorption liquid is placed in a layering tank for standing, after water and ethyl acetate are layered,and water and ethyl acetate are sequentially discharged, so that recovery of the ethyl acetate is realized.
Example 2
Beta-carotene extraction wastewater with COD value of 3.12×10 4 The results of gas chromatography detection on the wastewater at mg/L are shown in FIG. 2, and the content of ethyl acetate in the wastewater is 0.621% (v/v).
The ethyl acetate in the wastewater was recovered by using the recovery apparatus of example 1, as follows:
s1, 4.07L of macroporous adsorption resin H-01 is taken, wetted with water, uniformly stirred and then packed into a column, wherein the specification of the adsorption column is H=0.12 m and phi=0.36 m;
s2, preprocessing an adsorption column:
(1) Washing the resin with 8.14L of water;
(2) Ejecting water by 8.14L of ethanol, and soaking for 24 hours;
(3) Evacuating ethanol, completely replacing the solvent with water, and washing until the adsorption column has no ethanol smell;
s3, performing column adsorption on the beta-carotene extraction wastewater, controlling the flow rate to be 0.5BV/h, controlling the total column loading amount to be 20BV, taking an instant effluent sample with the column loading amount of 10BV, the column loading amount of 20BV and a mixed effluent sample with the column loading amount of 20BV, and performing ethyl acetate residue test, wherein the detection result of a gas chromatograph is that the ethyl acetate residue concentration of three samples is undetected;
the COD value of the water sample after adsorption is 2.85 multiplied by 10 4 mg/L, and the gas chromatography detection result is shown in FIG. 3;
s4, using N 2 Blowing out water in an adsorption column, then introducing steam, controlling the steam pressure to be 0.02MPa, collecting desorption liquid, standing, separating out water phase, distilling and collecting solvent phase to obtain ethyl acetate 0.463L;
the recovered ethyl acetate was subjected to gas chromatography, and the result was shown in fig. 4, wherein the purity of ethyl acetate was 99.735% and the recovery rate was 91.35%.
Example 3
Beta-carotene extraction wastewater with COD value of 3.12×10 4 mg/L, ethyl acetate content 0.621% (v/v). Ethyl acetate for wastewater using the recovery apparatus of example 1The recovery is carried out, and the steps are as follows:
s1, continuing to use the macroporous adsorption resin H-01 analyzed in the embodiment 1, wetting with water, uniformly stirring, and filling into a column, wherein the specification of the adsorption column is H=0.12 m and phi=0.36 m;
s2, preprocessing an adsorption column:
(1) Washing the resin with 8.14L of water;
(2) Ejecting water by 8.14L of ethanol, and soaking for 24 hours;
(3) Evacuating ethanol, completely replacing the solvent with water, and washing until the adsorption column has no ethanol smell;
s3, performing column adsorption on the beta-carotene extraction wastewater, controlling the flow rate to be 1BV/h, controlling the total column loading amount to be 20BV, taking a 10BV column loading amount, an instantaneous effluent sample when the 20BV column loading amount is adopted, and performing ethyl acetate residue test on the mixed effluent sample when the 20BV column loading amount is adopted, wherein the detection result of a gas chromatograph is that the ethyl acetate residue concentration of the three samples is undetected;
the COD value of the water sample after adsorption is 2.96 multiplied by 10 4 mg/L, and the gas chromatography detection result is shown in FIG. 5;
s4, using N 2 Blowing out water in the adsorption column, then introducing steam, controlling the steam pressure to be 0.08MPa, collecting desorption liquid, standing, separating out water phase, distilling and collecting solvent phase, and obtaining ethyl acetate 0.477L.
The recovered ethyl acetate was subjected to gas chromatography, and the result is shown in fig. 6, wherein the purity of ethyl acetate was 99.724%, and the recovery rate was 94.10%.
Example 4
Beta-carotene extraction wastewater with COD value of 3.12×10 4 mg/L, ethyl acetate content 0.621% (v/v). The ethyl acetate in the wastewater was recovered by using the recovery apparatus of example 1, as follows:
s1, continuing to use the macroporous adsorption resin H-01 analyzed in the embodiment 3, wetting with water, uniformly stirring, and filling into a column, wherein the specification of the adsorption column is H=0.12 m and phi=0.36 m;
s2, preprocessing an adsorption column:
(1) Washing the resin with 8.14L of water;
(2) Ejecting water by 8.14L of ethanol, and soaking for 24 hours;
(3) Evacuating ethanol, completely replacing the solvent with water, and washing until the adsorption column has no ethanol smell;
s3, performing column adsorption on the beta-carotene extraction wastewater, controlling the flow rate to be 1BV/h, controlling the total column loading amount to be 20BV, taking a 10BV column loading amount, an instantaneous effluent sample when the 20BV column loading amount is adopted, and performing ethyl acetate residue test on the mixed effluent sample when the 20BV column loading amount is adopted, wherein the detection result of a gas chromatograph is that the ethyl acetate residue concentration of the three samples is undetected;
the COD value of the water sample after adsorption is 2.90 multiplied by 10 4 mg/L, and the gas chromatography detection result is shown in FIG. 7;
s4, using N 2 Blowing out water in an adsorption column, then introducing steam, controlling the steam pressure to be 0.15MPa, collecting desorption liquid, standing, separating out water phase, distilling and collecting solvent phase to obtain ethyl acetate 0.467L;
the recovered ethyl acetate was subjected to gas chromatography, and the result was shown in fig. 8, wherein the purity of ethyl acetate was 99.687%, and the recovery rate was 92.10%.
Although the present invention has been described in detail by way of preferred embodiments with reference to the accompanying drawings, the present invention is not limited thereto. Various equivalent modifications and substitutions may be made in the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and it is intended that all such modifications and substitutions be within the scope of the present invention/be within the scope of the present invention as defined by the appended claims.
Claims (1)
1. A recovery method of ethyl acetate in 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 beta-carotene extraction wastewater, the flow rate of the beta-carotene on the column is 0.5-2 times of the volume/H of the resin, the total loading amount is 5-20 times of the volume of the resin, and N is used after adsorption 2 Drying the resin, and then using steam with the pressure of 0.02-0.15 MPa to adsorb the ethylene on the resinDesorbing the ethyl acetate, collecting a desorption solution, standing and separating a water phase and a solvent phase, and collecting the solvent phase;
pre-treating an adsorption column before adsorbing beta-carotene extraction wastewater, wherein the pre-treatment comprises (1) washing the adsorption column with 2-5 times of resin volume of water; (2) Ejecting water by using an organic solvent, and then soaking, wherein the organic solvent is selected from acetone, ethanol, isopropanol or methanol, the dosage of the organic solvent is 1-4 times of the volume of the resin, and the soaking time is 24-48 hours; (3) The organic solvent was drained and the column was again washed with water until no organic solvent odor was present.
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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.离子交换与吸附.2016,第32卷(第2期),第1节，第2.1.2节，第2.2.1-2.2.2节. * |
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