CN115259510B - Novel acrylic acid wastewater treatment device and wastewater treatment method - Google Patents
Novel acrylic acid wastewater treatment device and wastewater treatment method Download PDFInfo
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- CN115259510B CN115259510B CN202210632262.4A CN202210632262A CN115259510B CN 115259510 B CN115259510 B CN 115259510B CN 202210632262 A CN202210632262 A CN 202210632262A CN 115259510 B CN115259510 B CN 115259510B
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- 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
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F2001/5218—Crystallization
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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Abstract
The invention belongs to the technical field of acrylic acid wastewater treatment, and particularly relates to a novel acrylic acid wastewater treatment device and a wastewater treatment method. Including anti first reation kettle, centrifugal filter, plate-and-frame filter press, supernatant through pump, second reation kettle, evaporative crystallizer and crystallization through the filter, the cauldron bottom and the centrifugal filter intercommunication of first reation kettle, centrifugal filter's bottom is connected with the frame filter press, and centrifugal filter's upper end is through supernatant through pump and second heat exchanger and second reation kettle intercommunication, second reation kettle and evaporative crystallizer intercommunication, evaporative crystallizer and crystallization through the filter intercommunication. Has the characteristics of environmental protection, low carbon, energy conservation, high efficiency, no material waste and high recovery rate of acetic acid and acrylic acid in water.
Description
Technical Field
The invention belongs to the technical field of acrylic acid wastewater treatment, and particularly relates to a novel acrylic acid wastewater treatment device and a wastewater treatment method.
Background
Olefine acid plays a very important role in the field of fine chemical engineering. Acrylic acid is mainly used for producing acrylic esters (resin) in industry, accounting for about 60 percent of the total consumption of the acrylic acid, and is applied to the fields of construction, papermaking, leather, textile, plastic processing, packaging materials, daily chemical industry, water treatment, oil extraction, metallurgy and the like.
The acrylic acid wastewater has the characteristics of high organic matter content, complex water quality, poor biodegradability and the like. In the aspect of acrylic acid wastewater treatment, the current technology mainly focuses on wastewater treatment technology. The existing acrylic acid wastewater treatment is mainly controlled at the tail end, and the adopted technology is mainly as follows: biochemical, electrochemical, catalytic oxidation, incineration, and the like. Most of the methods stay in a laboratory stage, and the incineration method is applied to engineering, but has the disadvantages of excessively high cost and unfavorable popularization in a large scale. And most of the acrylic acid wastewater treatment at present is not analyzed from the aspects of clean production, water balance and resource recovery, so as to carry out comprehensive treatment on the wastewater.
Disclosure of Invention
The invention aims to provide a novel acrylic acid wastewater treatment device and a wastewater treatment method, which are used for comprehensively treating wastewater from the aspects of clean production, water balance and resource recovery and system analysis.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the utility model provides a novel acrylic acid waste water treatment device, includes first reation kettle, centrifugal filter, plate and frame filter press, supernatant pump, second reation kettle, evaporative crystallizer and crystallization filter, the cauldron bottom and the centrifugal filter intercommunication of first reation kettle, centrifugal filter's bottom is connected with the frame filter press, and centrifugal filter's upper end is through supernatant pump and second heat exchanger and second reation kettle intercommunication, second reation kettle and evaporative crystallizer intercommunication, evaporative crystallizer and crystallization filter intercommunication.
Further, a liquid inlet of the first reaction kettle is provided with a liquid pump and a first heat exchanger, waste water is pumped to the first heat exchanger through the liquid pump, and the first heat exchanger is communicated with the first reaction kettle.
Further, the second reaction kettle steam outlet is communicated with a second heat exchanger.
Further, the second reaction kettle is communicated with the evaporation crystallizer through a third heat exchanger.
The invention also discloses a wastewater treatment method of the novel acrylic acid wastewater treatment device,
s1, preheating acrylic acid wastewater;
s2, carrying out precipitation filtration on the acrylic acid wastewater in the step S1;
s3, carrying out filter pressing separation on the precipitate in the step S2;
s4, evaporating and concentrating the supernatant generated in the step S3;
s5, evaporating and crystallizing the concentrated solution in the step S4.
Further, the acrylic acid wastewater in the step S1 is sent to a first heat exchanger through a liquid pump, preheated to 50-60 ℃ and then put into a first reaction kettle.
Further, in the step S2, zirconium oxychloride as a reaction raw material is continuously added into the first reaction kettle, ammonia water is added to adjust the pH value of the solution in the first reaction kettle to 5.5-6, a large amount of white precipitate is immediately produced in the first reaction kettle, and the suspension in the first reaction kettle is sent to a centrifugal filter.
And in the step S3, the white precipitate in the step S2 is sent into a plate-and-frame filter press for treatment, and filter pressing separation is carried out on filter residues through the plate-and-frame filter press.
And further, pressurizing the supernatant in the centrifugal filter in the step S4 by a pump, sending the supernatant into a second heat exchanger, preheating to 80-90 ℃, then putting the supernatant into a second reaction kettle, continuously adding reaction raw material calcium hydroxide into the second reaction kettle to ensure that the pH value of the solution in the reaction kettle is about 9-10, then evaporating and concentrating the mixed solution in the second reaction kettle, and stopping evaporating when the mixed solution is evaporated and concentrated to 1/5 of the original volume.
Further, the concentrated solution in the step S4 is subjected to further heat exchange by a third heat exchanger to be heated to 120-130 DEG
Sending the solid product to an evaporation crystallizer at the temperature of DEG C to generate a large amount of white crystals of calcium acetate, filtering the crystals at the bottom by a filter 7 to obtain an industrial-grade calcium acetate solid product, collecting and packaging the industrial-grade calcium acetate solid product as a byproduct, and collecting distilled water discharged from the top for direct biochemical treatment.
In summary, due to the adoption of the technical scheme, the beneficial technical effects of the invention are as follows:
the novel acrylic acid wastewater treatment device has the advantages of environmental protection, low carbon, energy conservation, high efficiency, no material waste and the like, the recovery rate of acetic acid and acrylic acid in wastewater reaches more than 98 percent, calcium acetate can be recovered from the wastewater of the acrylic acid device, a high-grade zirconia ceramic coating precursor can be obtained, and purified wastewater can be directly biochemically treated.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
In this embodiment, a novel acrylic acid waste water treatment device, including anti-first reation kettle 1, centrifugal filter 2, plate-and-frame filter press 3, supernatant pump 4, second reation kettle 5, evaporative crystallizer 6 and crystallization filter 7, the cauldron bottom and the centrifugal filter 2 intercommunication of first reation kettle 1, the bottom and the plate-and-frame filter press 3 of centrifugal filter 2 are connected, and the upper end of centrifugal filter 2 is through supernatant pump 4 and second heat exchanger 8 and second reation kettle 5 intercommunication, and second reation kettle 5 and evaporative crystallizer 6 intercommunication, evaporative crystallizer 6 and crystallization filter 7 intercommunication. The liquid inlet of the first reaction kettle 1 is provided with a liquid pump 9 and a first heat exchanger 10, waste water is sent to the first heat exchanger 10 through the liquid pump 9, and the first heat exchanger 10 is communicated with the first reaction kettle 1. The steam outlet of the second reaction kettle 5 is communicated with a second heat exchanger 8. The second reaction kettle 5 is communicated with the evaporative crystallizer 6 through a third heat exchanger 11.
The invention also discloses a wastewater treatment method of the novel acrylic acid wastewater treatment device,
s1, preheating acrylic acid wastewater;
s2, carrying out precipitation filtration on the acrylic acid wastewater in the step S1;
s3, carrying out filter pressing separation on the precipitate in the step S2;
s4, evaporating and concentrating the supernatant generated in the step S3;
s5, evaporating and crystallizing the concentrated solution in the step S4.
The acrylic acid wastewater in the step S1 is sent to a first heat exchanger 10 through a liquid pump 9, preheated to 50-60 ℃ and then put into a first reaction kettle 1.
In the step S2, zirconium oxychloride as a reaction raw material is continuously added into the first reaction kettle 1, ammonia water is added to adjust the pH value of the solution in the first reaction kettle 1 to 5.5-6, a large amount of white precipitate is immediately produced in the first reaction kettle 1, and the suspension in the first reaction kettle 1 is sent to the centrifugal filter 2.
And in the step S3, the white precipitate in the step S2 is sent into a plate-and-frame filter press 3 for treatment, and filter residues are subjected to filter pressing separation through the plate-and-frame filter press 3.
And in the step S4, the supernatant in the centrifugal filter 2 is pressurized by a pump 4, then is sent into a second heat exchanger 8 to be preheated to 80-90 ℃ and then is put into a second reaction kettle 5, and the reaction raw material calcium hydroxide is continuously added into the second reaction kettle 5 to enable the pH value of the solution in the reaction kettle to be 9-10, then the mixed solution in the second reaction kettle 5 is evaporated and concentrated, and when the mixed solution is evaporated and concentrated to 1/5 of the original volume, the evaporation is stopped.
The concentrated solution in the step S4 is further subjected to heat exchange by a third heat exchanger 11 and is sent to an evaporation crystallizer 6 after being heated to 120-130 ℃, a large amount of white crystals of calcium acetate are generated, the crystals at the bottom are filtered by a filter 7, an industrial grade calcium acetate solid product is obtained, the industrial grade calcium acetate solid product is packaged as a byproduct after collection, and distilled water discharged from the top can be directly subjected to biochemical treatment after collection.
Example 1
The method for treating low-concentration acrylic acid wastewater of the following example was carried out, wherein the amount of wastewater produced by an acrylic acid plant of certain petrochemical company was 8.5m 3 And/h, the main pollutants in the wastewater comprise organic matters such as acrylic acid, acetic acid, formaldehyde, acrolein, toluene and the like, the COD is 127832mg/L, the BOD is 26101mg/L, and the main pollutant composition and the content of the wastewater are shown in Table 1.
TABLE 1 acrylic acid plant wastewater composition
| Sequence number | Component (A) | Mass fraction (wt%) |
| 1 | Acetic acid | 4.95 |
| 2 | Acrylic acid | 0.71 |
| 3 | Formaldehyde | 0.11 |
| 4 | Acrolein | 0.03 |
| 5 | Propionic acid | 0.03 |
| 6 | Acetaldehyde | 0.02 |
| 7 | Toluene (toluene) | 0.08 |
The wastewater flow of the acrylic acid device is 8.5m 3 And (3) preheating to 58 ℃ through a first heat exchanger by pumping, then putting the mixture into a first reaction kettle, continuously adding a zirconium oxychloride solution with the mass fraction of 30wt% into the first reaction kettle, adding the mixture with the flow rate of 125.3kg/h, simultaneously adding concentrated ammonia water with the concentration of 26% to adjust the pH value of the mixed solution in the first reaction kettle to be between 5.5 and 6.3, immediately producing a large amount of alkaline zirconium acrylate white precipitate in the first reaction kettle, putting the white suspension precipitate in the first reaction kettle into a centrifugal filter 2, putting the white precipitated alkaline zirconium acrylate at the bottom into a plate-and-frame filter press 3 for treatment, performing filter pressing separation on filter residues through the plate-and-frame filter press 3, and collecting a filter material for use as a precursor of the advanced zirconia ceramic coating.
The supernatant in the centrifugal filter 2 is pressurized by a pump 4, sent to a second heat exchanger to be preheated to 90 ℃, then put into a second reaction kettle 5, and continuously added with 260kg/h of calcium hydroxide into the second reaction kettle 5 to enable the pH value of the solution in the reaction kettle to be 9-10, then the mixed solution in the second reaction kettle is evaporated and concentrated, when the mixed solution is evaporated and concentrated to 1/5 of the original volume, evaporation is stopped, the mixed solution is further heat-exchanged and heated to 125 ℃ by the heat exchanger and then sent to an evaporation crystallizer 6, a large amount of white crystals of calcium acetate are generated, the crystals at the bottom are filtered by a filter 7 to obtain an industrial grade calcium acetate solid product, and the industrial grade calcium acetate solid product is collected and packaged as a byproduct, and analysis and test results of distilled water and filtered water are shown in the following tables 2 and 3 respectively.
TABLE 2 analytical test results for distilled water
| Sequence number | Analyzing content | Detection value |
| 1 | Zirconium ion content | Not detected |
| 2 | Calcium ion content | Not detected |
| 3 | COD | 205mg/ |
| 4 | BOD | 70mg/L |
TABLE 3 analytical test results for filtered Water
| Sequence number | Analyzing content | Detection value |
| 1 | Zirconium ion content | ＜ |
| 2 | Calcium ion content | ＜ |
| 3 | COD | 661mg/ |
| 4 | BOD | 98mg/L |
The distilled water purified by the technology of the invention does not contain inorganic metal ions, the COD removal rate of the acrylic acid wastewater reaches 99.7%, and the BOD removal rate is 99.8%. The inorganic metal ion content in the filtered water is lower than 100ppm, the COD removal rate of the acrylic acid wastewater reaches 99.2%, the BOD removal rate is 99.3%, and the treated wastewater can be directly biochemically treated.
Comparative example 1
The amount of wastewater generated by an acrylic acid device of a petrochemical company is 8.5m3/h, COD of the wastewater is 126528mg/L, BOD of the wastewater is 25710mg/L, and main pollutants in the wastewater comprise organic matters such as acrylic acid, acetic acid, formaldehyde, acrolein, toluene and the like, wherein the main pollutant content of the wastewater is shown in the following table 4.
TABLE 4 organic content in acrylic acid plant wastewater
| Sequence number | Component (A) | Mass fraction (wt%) |
| 1 | Acetic acid | 4.75 |
| 2 | Acrylic acid | 0.61 |
| 3 | Formaldehyde | 0.13 |
| 4 | Acrolein | 0.04 |
| 5 | Propionic acid | 0.03 |
| 6 | Acetaldehyde | 0.02 |
| 7 | Toluene (toluene) | 0.08 |
Loading a certain amount of weak alkaline anion exchange resin D301 into an ion exchange column, loading a small amount of quartz sand at the upper end and the lower end to compact a resin layer, pressurizing the waste water of an acrylic acid device by a pump, flowing through the exchange column at a certain flow rate, collecting the waste water in a liquid storage tank, sampling at fixed time to measure acrylic acid, acetic acid concentration, COD and BOD values in the treated water, and stopping the injection of the waste water until reaching a saturation point in the adsorption process.
In the elution process, naOH solution with the concentration of 15wt% is injected from an alkaline washing tank through a pump, the addition amount is controlled to enable alkali liquor to flow through a saturated resin exchange column at a certain flow rate, the resin exchange column is regenerated, eluent is collected in a waste liquid collecting tank, and pH, COD, acrylic acid and acetic acid concentrations are measured by sampling at regular time.
TABLE 5 detection results of acrylic acid plant wastewater after adsorption treatment with weakly basic anion exchange resin D301
| Sequence number | Analyzing content | Detection value |
| 1 | Acrylic acid content | 1.03 |
| 2 | Acetic acid content | 0.21 |
| 3 | COD | 92386mg/ |
| 4 | BOD | 18292mg/L |
The COD removal rate of the acrylic acid device wastewater treated by the weak-alkaline anion exchange resin D301 is 73.01 percent, and the BOD removal rate is 71.15 percent.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (5)
1. The method is characterized in that a device used by the method comprises a first reaction kettle (1), a centrifugal filter (2), a plate-and-frame filter press (3), a supernatant pump (4), a second reaction kettle (5), an evaporative crystallizer (6) and a crystallization filter (7), wherein the kettle bottom of the first reaction kettle (1) is communicated with the centrifugal filter (2), the bottom end of the centrifugal filter (2) is connected with the plate-and-frame filter press (3), the upper end of the centrifugal filter (2) is communicated with the second reaction kettle (5) through the supernatant pump (4) and the second heat exchanger (8), the second reaction kettle (5) is communicated with the evaporative crystallizer (6), and the evaporative crystallizer (6) is communicated with the crystallization filter (7);
the liquid inlet of the first reaction kettle (1) is provided with a liquid pump (9) and a first heat exchanger (10), waste water is sent to the first heat exchanger (10) through the liquid pump (9), and the first heat exchanger (10) is communicated with the first reaction kettle (1);
the steam outlet of the second reaction kettle (5) is communicated with a second heat exchanger (8);
the second reaction kettle (5) is communicated with the evaporation crystallizer (6) through a third heat exchanger (11);
the method for treating the acrylic acid wastewater comprises the following steps:
s1, preheating acrylic acid wastewater;
s2, carrying out precipitation filtration on the acrylic acid wastewater in the step S1;
s3, carrying out filter pressing separation on the precipitate in the step S2;
s4, evaporating and concentrating the supernatant generated in the step S3;
s5, evaporating and crystallizing the concentrated solution in the step S4;
in the step S2, continuously adding a reaction raw material zirconium oxychloride into the first reaction kettle, simultaneously adding ammonia water to adjust the pH value of the solution in the first reaction kettle to 5.5-6, immediately producing a large amount of white precipitate in the first reaction kettle, and sending the suspension in the first reaction kettle into a centrifugal filter.
2. The method for treating acrylic acid wastewater according to claim 1, wherein the acrylic acid wastewater in the step S1 is sent to the first heat exchanger by a liquid pump, preheated to 50-60 ℃ and then put into the first reaction kettle.
3. The method for treating acrylic acid wastewater according to claim 1, wherein the white precipitate obtained in the step S2 is sent to a plate-and-frame filter press for treatment in the step S3, and filter residues are subjected to filter pressing separation by the plate-and-frame filter press.
4. The method for treating acrylic acid wastewater according to claim 1, wherein the supernatant in the centrifugal filter in the step S4 is pressurized by a supernatant pump, sent to a second heat exchanger, preheated to 80-90 ℃ and then put into a second reaction kettle, and continuously adding reaction raw material calcium hydroxide into the second reaction kettle to make the pH value of the solution in the reaction kettle be 9-10, then evaporating and concentrating the mixed solution in the second reaction kettle, and stopping evaporating when the mixed solution is evaporated and concentrated to 1/5 of the original volume.
5. The method for treating acrylic acid wastewater according to claim 1, wherein the concentrated solution in the step S4 is further heat-exchanged and heated to 120-130 ℃ by a third heat exchanger, and then is sent to an evaporation crystallizer to generate a large amount of white crystals of calcium acetate, the crystals at the bottom are filtered by a filter to obtain an industrial grade calcium acetate solid product, the industrial grade calcium acetate solid product is packaged as a byproduct after collection, and distilled water discharged from the top can be directly biochemically treated after collection.
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| CN103408175A (en) * | 2013-07-22 | 2013-11-27 | 沈阳理工大学 | Treatment and reclamation method of (methyl) acrylic acid production wastewater |
| CN105236649B (en) * | 2015-09-28 | 2017-11-03 | 博天环境集团股份有限公司 | It is a kind of to administer acrylic ester wastewater and the method for acrylic acid sodium |
| CN206204105U (en) * | 2016-09-26 | 2017-05-31 | 克雷伯氏环保科技（苏州）有限公司 | A kind of butyl acrylate production wastewater treatment system |
| CN109126734A (en) * | 2018-10-11 | 2019-01-04 | 成都其其小数科技有限公司 | A kind of high efficiency, low cost adsorbent and preparation method for heavy metal containing wastewater treatment |
| CN210505926U (en) * | 2019-08-15 | 2020-05-12 | 山东开泰石化股份有限公司 | Acrylic acid effluent disposal system |
| CN112745418A (en) * | 2020-12-28 | 2021-05-04 | 江苏利田科技股份有限公司 | Method for preparing low-molecular-weight sodium polyacrylate by using wastewater generated in production of acrylic resin |
| CN216513304U (en) * | 2021-12-29 | 2022-05-13 | 杭州上拓环境科技股份有限公司 | Zero discharge system for acrylic resin production wastewater |
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