CN113527083A - Method for treating tail water from butyl acrylate production and extracting sodium acrylate from tail water - Google Patents
Method for treating tail water from butyl acrylate production and extracting sodium acrylate from tail water Download PDFInfo
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- CN113527083A CN113527083A CN202110710201.0A CN202110710201A CN113527083A CN 113527083 A CN113527083 A CN 113527083A CN 202110710201 A CN202110710201 A CN 202110710201A CN 113527083 A CN113527083 A CN 113527083A
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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
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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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
- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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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Abstract
The invention provides a method for treating tail water in butyl acrylate production and extracting sodium acrylate from the tail water, which comprises the following steps: adding a powdery activated carbon adsorbent into butyl acrylate production tail water, stirring at a medium speed for 10-30 min at a reaction temperature of 20-25 ℃, filtering, and collecting filtrate; transferring the filtrate to a rotary evaporator for evaporation treatment under a vacuum condition to obtain a concentrated solution and an evaporation condensate with the concentration ratio of 2.5-2.7 times; the obtained evaporation condensate is the treated butyl acrylate production tail water; and (3) drying the concentrated solution in a vacuum drying oven at 105-120 ℃ to constant weight to obtain sodium acrylate solid. The COD removal rate of the butyl acrylate production tail water treated by the method is more than 99.95 percent, the COD is lower than 100mg/L, the solid sodium acrylate obtained by extraction can be discharged through a nano tube or directly, the purity of the solid sodium acrylate reaches 98.6 percent, and the problems of high treatment difficulty and high cost of the butyl acrylate production tail water are solved.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a method for producing tail water from butyl acrylate and extracting sodium acrylate from the tail water.
Background
In recent years, acrylic acid and esters have rapidly developed as important industrial derivatives of propylene. Acrylic acid is the simplest ethylenic monomer of the monocarboxylic acid group type, which is easily copolymerized with other monomers, and as a monomer of a high molecular compound, the world's total production has exceeded millions of tons. One of the factors affecting the development of the acrylic acid and ester industry is the generation of large amounts of waste water from the production of acrylic acid and acrylic esters, water-soluble resins, dispersants, flocculants. Because of high concentration and high toxicity, the treatment difficulty is high and the direct biochemistry is difficult.
At present, the resource research of the acrylic acid wastewater is more, but the specific water quality conditions are different, and the resource method is different. The tail water produced by butyl acrylate is used as organic salt-containing wastewater to be incinerated at present, but the tail water is low in heat value, needs to consume a large amount of fuel oil, is high in investment and running cost, and due to high salt content, an incinerator is frequently scaled, and needs to be periodically stopped for descaling, so that part of treatment cost is increased. The treatment method for the butyl acrylate production tail water with simple process and low operation cost is lacked at present.
Disclosure of Invention
The invention aims to provide a method for treating butyl acrylate production tail water and extracting sodium acrylate from the butyl acrylate production tail water, which can solve the problems of high difficulty and high cost in butyl acrylate production tail water treatment in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for treating butyl acrylate production tail water and extracting sodium acrylate from the tail water comprises the following steps:
a method for treating butyl acrylate production tail water and extracting sodium acrylate from the tail water is characterized by comprising the following steps:
s1, adding an adsorbent into the butyl acrylate production tail water, stirring at a medium speed for 10-30 min at a reaction temperature of 20-25 ℃, filtering, and collecting filtrate; the adding amount of the adsorbent is 5-10% of the mass of the butyl acrylate production tail water;
s2, transferring the filtrate obtained in the step S1 to a rotary evaporator for evaporation treatment to obtain a concentrated solution and an evaporation condensate with the concentration ratio of 2.5-5 times;
s3, drying the concentrated solution in a vacuum drying oven at the temperature of 105-120 ℃ to constant weight to obtain sodium acrylate solid;
the evaporation condensate obtained in the step S2 is the treated butyl acrylate production tail water; and (3) obtaining a dried solid obtained in the step S3, namely sodium acrylate extracted from the tail water of butyl acrylate production.
Preferably, in the step S1, the content of sodium acrylate in the butyl acrylate production tail water is 12-14%, the COD concentration is 130000-150000 mg/L, and the chroma is 400-450.
Preferably, in step S2, the evaporation concentration ratio is 2.5-2.7.
Preferably, the mass fraction of sodium acrylate in the evaporation condensate is below 0.01%.
Preferably, the purity of the solid sodium acrylate obtained by drying in the step S3 is as high as 98.6%.
Preferably, the adsorbent is one or both of powdered activated carbon and resin.
Preferably, the adsorbent adopts powdered activated carbon, and the adding amount of the powdered activated carbon is 7.5% of the mass of the tail water produced by the butyl acrylate.
The method for treating the tail water from butyl acrylate production and extracting the sodium acrylate from the tail water has the advantages of simple process and low cost, and can extract high-purity solid sodium acrylate. The COD removal rate of the tail water of butyl acrylate production treated by the method is more than 99.95 percent, the COD is lower than 100mg/L, and the tail water can be discharged through a nano tube or directly.
Drawings
FIG. 1 is a flow chart of a preparation method of treating tail water from butyl acrylate production and extracting sodium acrylate from the tail water.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
The invention discloses a method for treating tail water from butyl acrylate production and extracting sodium acrylate from the tail water, and the method for treating the tail water from butyl acrylate production and extracting sodium acrylate from the tail water comprises the following steps:
s1, adding an adsorbent into the butyl acrylate production tail water, stirring at a medium speed for 10-30 min, reacting at a temperature of 20-25 ℃ (the stirring time and the reaction temperature are not limited to the parameters provided by the invention), filtering, and collecting filtrate; the adding amount of the adsorbent is 5-10% of the mass of the butyl acrylate production tail water; the adsorbent is one or two of powdered activated carbon and resin;
it should be noted that, after the adsorbent is added to the butyl acrylate production tail water in the step S1, the organic matter with color-developing groups in the butyl acrylate production tail water is adsorbed by physical action, so as to achieve the effect of decoloring the butyl acrylate production tail water, and the method is very beneficial to obtaining high-purity sodium acrylate by subsequent evaporation and concentration. When the resin is used as an adsorbent, methanol is required for activation treatment. Those skilled in the art can grasp the present invention from practical experience, and the present invention is not particularly limited herein.
S2, transferring the filtrate obtained in the step S1 to a rotary evaporator for evaporation treatment to obtain a concentrated solution and an evaporation condensate with the concentration ratio of 2.5-5 times;
s3, drying the concentrated solution in a vacuum drying oven at the temperature of 105-120 ℃ to constant weight to obtain sodium acrylate solid;
the evaporation condensate obtained in the step S2 is the treated butyl acrylate production tail water; and (3) obtaining a dried solid obtained in the step S3, namely sodium acrylate extracted from the tail water of butyl acrylate production.
It should be noted that, in the evaporation concentration process in step S2, the evaporation pressure may be vacuum or normal pressure, and when drying the concentrated solution, the drying temperature and the drying time provided by the present invention are not limited, and those skilled in the art can grasp the drying temperature and the drying time according to practical experience.
Further, in the technical scheme of the invention, the content of sodium acrylate in the tail water of butyl acrylate production is 12-14%, the COD concentration is 130000-150000 mg/L, and the chroma is 400-450.
Furthermore, the evaporation concentration ratio is controlled to be 2.5-2.7 in the step S2, so that the concentrated solution can be poured out of the distillation flask without being glued on the flask wall.
Further, the mass fraction of sodium acrylate in the evaporation condensate is below 0.01%.
Further, the solid sodium acrylate obtained by drying in the step of S3 had a purity as high as 98.6%.
Furthermore, the adsorbent adopted in the invention preferably adopts powdered activated carbon, and the powdered activated carbon which is saturated in adsorption is separated from the tail water of butyl acrylate production through filtration, thereby being beneficial to the subsequent treatment of the tail water of butyl acrylate production.
Further, the adsorbent adopts powdered activated carbon, and the adding amount of the powdered activated carbon is 7.5% of the mass of the tail water in the butyl acrylate production.
The technical solutions of the present invention will be described below with reference to specific embodiments, and the described embodiments are only a part of embodiments of the present invention, but not all embodiments.
The reagents required in the examples of the present invention are all commercially available.
Specification of powdered activated carbon: iodine value is 1000mg/g, methylene blue adsorbs 150mg/g, ash content is 10%, water content is 10%, pH is 9-10, and the manufacturer Shandonnake activated carbon Co.
Resin model Seplite XDA-1G, Sean blue, scientific New materials, Inc.
The rotary evaporator model RE-52A, manufacturer Shanghai Yanglong Biochemical apparatus factory.
Example 1
Taking 500g of butyl acrylate production tail water, wherein the initial index of the butyl acrylate production tail water is as follows: the sodium acrylate content is 13.20%, the COD is 137580mg/L, the pH value is 8.03, and the color value is 432.
Adding 37.5g of powdered activated carbon into tail water of butyl acrylate production, stirring at medium speed for 30min, and filtering to obtain filtrate; evaporating and concentrating the filtrate at 67 ℃ in vacuum, and collecting an evaporation condensate and a concentrated solution when the concentration multiple reaches 2.5; and transferring the concentrated solution to a vacuum drying oven, drying for 24h at 105 ℃ to obtain sodium acrylate solid, wherein the evaporation condensate is the treated butyl acrylate production tail water.
The COD concentration in the treated butyl acrylate production tail water is 63mg/L, the chroma is 6, the removal rate of the COD reaches 99.95 percent, and the treated butyl acrylate production tail water can be subjected to pipeline collection or directly discharged. The purity of the solid sodium acrylate obtained by concentration and drying is 98.58 percent, and the appearance is white.
Example 2
Taking 1000g of butyl acrylate production tail water, wherein the initial index of the butyl acrylate production tail water is as follows: the sodium acrylate content is 13.82%, the COD is 143450mg/L, the pH value is 8.11, and the chromatic value is 444.
Adding 100g of powdered activated carbon into the tail water of butyl acrylate production, stirring at medium speed for 30min, and filtering to obtain filtrate; evaporating and concentrating the filtrate at 70 ℃ in vacuum, and collecting an evaporation condensate and a concentrated solution when the concentration multiple reaches 2.7; and transferring the concentrated solution to a vacuum drying oven, drying for 24h at 105 ℃ to obtain sodium acrylate solid, wherein the evaporation condensate is the treated butyl acrylate production tail water.
The COD concentration in the treated butyl acrylate production tail water is 54mg/L, the chroma is 4, the removal rate of the COD is 99.96 percent, and the treated butyl acrylate production tail water can be subjected to pipeline collection or directly discharged. The solid sodium acrylate obtained by concentration and drying had a purity of 98.60% and was white in appearance.
Example 3
Taking 1000g of butyl acrylate production tail water, wherein the initial index of the butyl acrylate production tail water is as follows: the sodium acrylate content is 13.82%, the COD is 143450mg/L, the pH value is 8.11, and the chromatic value is 444.
Adding 100g of resin into the tail water of butyl acrylate production, stirring at medium speed for 30min, filtering to obtain a primary filtrate, adding 50g of powdered activated carbon into the primary filtrate, stirring at medium speed for 30min, and filtering to obtain a secondary filtrate; evaporating and concentrating the secondary filtrate at 72 ℃ in vacuum, and collecting an evaporation condensate and a concentrated solution when the concentration multiple reaches 2.7; and transferring the concentrated solution to a vacuum drying oven, drying for 24h at 105 ℃ to obtain sodium acrylate solid, wherein the evaporation condensate is the treated butyl acrylate production tail water.
The COD concentration in the treated butyl acrylate production tail water is 76mg/L, the chroma is 6, the removal rate of the COD is 99.95 percent, and the treated butyl acrylate production tail water can be subjected to pipeline collection or directly discharged. The purity of the solid sodium acrylate obtained by concentration and drying is 98.59 percent, and the appearance is white.
From the examples 1 to 3, it can be seen that the method of the present invention has a simple process and a low cost. The method for treating the tail water of butyl acrylate production has the COD removal rate of over 99.95 percent, and the purity of the extracted sodium acrylate is as high as 98.6 percent, so the method has high secondary utilization value. After the treatment by the method, the COD of the tail water of butyl acrylate production is lower than 100mg/L, and the tail water can be contained in a pipe or directly discharged.
Comparative example 1
Taking 500g of butyl acrylate production tail water, wherein the initial index of the butyl acrylate production tail water is as follows: the sodium acrylate content is 13.20%, the COD is 137580mg/L, the pH value is 8.03, and the color value is 432.
Directly transferring the butyl acrylate production tail water to vacuum at 74 ℃ for evaporation concentration, collecting evaporation condensate and concentrated solution when the concentration multiple reaches 2.6, transferring the concentrated solution to a vacuum drying oven, and drying at 105 ℃ for 24h to obtain sodium acrylate solid, wherein the evaporation condensate is the treated butyl acrylate production tail water.
The COD concentration in the treated butyl acrylate production tail water is 403mg/L, the removal rate of the COD is 99.68 percent, the COD concentration is higher, the chroma is 496, and the chroma exceeds the standard and cannot be contained in a pipe or directly discharged. The sodium acrylate obtained by concentration and drying has the purity of 95.26 percent and the appearance of gray.
Comparative example 2
Taking 1000g of butyl acrylate production tail water, wherein the initial index of the butyl acrylate production tail water is as follows: the sodium acrylate content is 13.82%, the COD is 143450mg/L, the pH value is 8.11, and the chromatic value is 444.
Adding 100g of resin into the tail water of butyl acrylate production, stirring at medium speed for 30min, and filtering to obtain filtrate; and (3) evaporating and concentrating the filtrate at 72 ℃ in vacuum, collecting evaporation condensate and concentrated solution when the concentration multiple reaches 2.7, transferring the concentrated solution to a vacuum drying oven, and drying for 24 hours at 105 ℃ to obtain sodium acrylate solid, wherein the evaporation condensate is the treated butyl acrylate production tail water.
The COD concentration in the treated butyl acrylate production tail water is 379mg/L, the removal rate of COD is 99.74%, the chroma is 125, the chroma exceeds the standard, and the tail water cannot be contained in a pipe or directly discharged. The sodium acrylate obtained by concentration and drying has the purity of 96.98 percent and the appearance of light gray.
The chemical oxygen demand COD is a chemical method for measuring the amount of reducing substances to be oxidized in water. COD in the present invention means the chemical oxygen demand measured using potassium dichromate as an oxidizing agent, i.e., CODCr。
As shown in table 1, experimental data and experimental results are compared between examples 1 to 3 provided for the present invention and comparative examples 1 and 2. From table 1, it can be seen that, in the case of comparative example 1 and comparative example 2, neither the adsorption decoloring pretreatment nor the resin adsorption pretreatment was performed, the decoloring effect by the addition of the powdered activated carbon or the combined action of the resin and the powdered activated carbon used in the present invention was achieved, and the COD and color in the treated butyl acrylate production tail water and the purity and appearance of the sodium acrylate solid obtained by concentration and drying were far from those obtained in examples 1 to 3.
TABLE 1
The method for treating the tail water from butyl acrylate production and extracting the sodium acrylate from the tail water is described in detail above. The principles and practice of the present invention are illustrated herein using specific embodiments, which are presented only to aid in the understanding of the method and its central concept. It should be noted that it is possible for those skilled in the art to make improvements or modifications to the present invention without departing from the principle of the present invention, and such improvements and modifications also fall within the scope of the claims of the present invention.
Claims (7)
1. A method for treating butyl acrylate production tail water and extracting sodium acrylate from the tail water is characterized by comprising the following steps:
s1, adding an adsorbent into the butyl acrylate production tail water, stirring at a medium speed for 10-30 min at a reaction temperature of 20-25 ℃, filtering, and collecting filtrate; the adding amount of the adsorbent is 5-10% of the mass of the butyl acrylate production tail water;
s2, transferring the filtrate obtained in the step S1 to a rotary evaporator for evaporation treatment to obtain a concentrated solution and an evaporation condensate with the concentration ratio of 2.5-5 times;
s3, drying the concentrated solution in a vacuum drying oven at the temperature of 105-120 ℃ to constant weight to obtain sodium acrylate solid;
the evaporation condensate obtained in the step S2 is the treated butyl acrylate production tail water; and (3) obtaining a dried solid obtained in the step S3, namely sodium acrylate extracted from the tail water of butyl acrylate production.
2. The method for treating the tail water from butyl acrylate production and extracting the sodium acrylate from the tail water from butyl acrylate production according to claim 1, wherein the tail water from butyl acrylate production in the step S1 has the sodium acrylate content of 12-14%, the COD concentration of 130000-150000 mg/L and the chroma of 400-450.
3. The method for treating tail water from butyl acrylate production and extracting sodium acrylate from tail water according to any one of claims 1 or 2, wherein in step S2, the evaporation concentration ratio is 2.5-2.7.
4. The method for processing the tail water from the production of butyl acrylate and extracting sodium acrylate from the tail water according to claim 3, wherein the mass fraction of sodium acrylate in the evaporation condensate is below 0.01 percent.
5. The method for processing the tail water from the production of butyl acrylate and extracting sodium acrylate from the tail water according to any one of claims 1 and 4, wherein the purity of the solid sodium acrylate obtained by evaporation and drying in the step S3 is up to 98.6%.
6. The method for treating tail water from butyl acrylate production and extracting sodium acrylate from the tail water according to claim 1, wherein the adsorbent is one or both of powdered activated carbon and resin.
7. The method for treating tail water from butyl acrylate production and extracting sodium acrylate from the tail water from butyl acrylate production as claimed in claim 3, wherein the adsorbent is powdered activated carbon, and the addition amount of the powdered activated carbon is 7.5% of the mass of the tail water from butyl acrylate production.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236649A (en) * | 2015-09-28 | 2016-01-13 | 博天环境集团股份有限公司 | Method for processing acrylate wastewater and recovering sodium acrylate |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236649A (en) * | 2015-09-28 | 2016-01-13 | 博天环境集团股份有限公司 | Method for processing acrylate wastewater and recovering sodium acrylate |
Non-Patent Citations (3)
| Title |
|---|
| 何领好 等: "《功能高分子材料》", 31 August 2016, 华中科技大学出版社 * |
| 吴骏等: "丙烯酸酯废水处理工艺的研究", 《化肥设计》 * |
| 祁鲁梁 等: "《水处理药剂及材料实用手册》", 31 March 2000, 中国石化出版社 * |
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Inventor after: Wang Wenbiao Inventor after: Wang Meijing Inventor after: Zhao Zhiwen Inventor after: Zhang Kai Inventor after: Sun Tian Inventor before: Wang Wenbiao Inventor before: Wang Meijing Inventor before: Zhao Zhiwen Inventor before: Zhang Kai Inventor before: Sun Tian Inventor before: Qiao Ruiping |
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Application publication date: 20211022 |