CN115259510A - 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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- CN115259510A CN115259510A CN202210632262.4A CN202210632262A CN115259510A CN 115259510 A CN115259510 A CN 115259510A CN 202210632262 A CN202210632262 A CN 202210632262A CN 115259510 A CN115259510 A CN 115259510A
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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
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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, evaporation crystallizer and crystallization process filter, first reation kettle's the cauldron bottom and centrifugal filter intercommunication, centrifugal filter's bottom and frame filter press are connected, and the upper end of centrifugal filter is passed through the supernatant and is passed through pump and second heat exchanger and second reation kettle intercommunication, second reation kettle and evaporation crystallizer intercommunication, evaporation crystallizer and brilliant process filter intercommunication. The method 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, accounts for about 60 percent of the total consumption of the acrylic acid, and is applied to the fields of building, 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 treatment of acrylic acid wastewater, the treatment process of wastewater is mainly focused at present. And the existing treatment of acrylic acid wastewater mainly adopts end control, and the adopted technology mainly comprises the following steps: biochemical method, electrochemical method, catalytic oxidation method, incineration method, etc. Most of the methods are in the laboratory stage, and although the incineration method is applied in engineering, the cost is too high, and the method is not beneficial to large-scale popularization. Most of the existing acrylic acid wastewater treatment processes do not perform systematic analysis from the aspects of clean production, water balance and resource recovery, and the wastewater is comprehensively treated.
Disclosure of Invention
The invention aims to provide a novel acrylic acid wastewater treatment device and a wastewater treatment method, which are used for carrying out comprehensive treatment on wastewater from the aspects of clean production, water balance and resource recovery.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the utility model provides a novel acrylic acid waste water treatment device, includes anti-first reation kettle, centrifugal filter, plate and frame filter press, supernatant through pump, second reation kettle, evaporation crystallizer and crystallization process filter, first reation kettle's the cauldron end and centrifugal filter intercommunication, centrifugal filter's bottom and frame filter press are connected, and centrifugal filter's upper end is passed through the supernatant through pump and second heat exchanger and second reation kettle intercommunication, second reation kettle and evaporation crystallizer intercommunication, evaporation crystallizer and brilliant process filter intercommunication.
Further, a liquid pump and a first heat exchanger are arranged on a liquid inlet of the first reaction kettle, wastewater is conveyed to the first heat exchanger through the liquid pump, and the first heat exchanger is communicated with the first reaction kettle.
Further, the steam outlet of the second reaction kettle is communicated with a second heat exchanger.
Further, the second reaction kettle is communicated with the evaporative 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, precipitating and filtering the acrylic acid wastewater in the step S1;
s3, performing 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, in the step S1, the acrylic acid wastewater 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 precipitates are immediately produced in the first reaction kettle, and the suspension in the first reaction kettle is sent to a centrifugal filter.
Further, in the step S3, the white precipitate in the step S2 is sent to a plate-and-frame filter press for treatment, and filter residue is subjected to filter pressing separation through the plate-and-frame filter press.
And further, pumping the supernatant in the centrifugal filter in the step S4, preheating the supernatant in a second heat exchanger to 80-90 ℃, putting the supernatant into a second reaction kettle, continuously adding a reaction raw material calcium hydroxide into the second reaction kettle to enable the pH value of the solution in the reaction kettle to be about 9-10, then evaporating and concentrating the mixed solution in the second reaction kettle, and stopping evaporation when the mixed solution is evaporated and concentrated to 1/5 of the original volume.
Further, the concentrated solution in the step S4 is further subjected to heat exchange by a third heat exchanger and is heated to 120 to E
And (3) after 130 ℃, sending the mixture to an evaporation crystallizer 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 product as a byproduct, and directly performing biochemical treatment on the distilled water discharged from the top after collecting.
In conclusion, 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 the purified wastewater can be directly subjected to biochemical treatment.
Drawings
FIG. 1 is a schematic 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 is further described in detail below with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit 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 through pump 4, second reation kettle 5, evaporative crystallizer 6 and crystallization process filter 7, the cauldron bottom and the centrifugal filter 2 intercommunication of first reation kettle 1, centrifugal filter 2's bottom and frame filter press 3 are connected, and centrifugal filter 2's upper end is passed through supernatant through 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 brilliant process filter 7 intercommunication. A liquid pump 9 and a first heat exchanger 10 are arranged at a liquid inlet of the first reaction kettle 1, wastewater 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. And a 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, precipitating and filtering the acrylic acid wastewater in the step S1;
s3, performing 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 S1, the acrylic acid wastewater 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 precipitates are 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 to a plate-and-frame filter press 3 for treatment, and filter pressing separation is carried out on filter residues through the plate-and-frame filter press 3.
And S4, pressurizing the supernatant in the centrifugal filter 2 in the step S4 through a pump 4, sending the supernatant into a second heat exchanger 8, preheating the supernatant to 80-90 ℃, putting the supernatant into a second reaction kettle 5, continuously adding a reaction raw material calcium hydroxide into the second reaction kettle 5 to ensure that the pH value of the solution in the reaction kettle is 9-10, then carrying out evaporation concentration on the mixed solution in the second reaction kettle 5, and stopping evaporation when the mixed solution is evaporated and concentrated to 1/5 of the original volume.
And (4) further exchanging heat of the concentrated solution in the step (S4) by a third heat exchanger (11), heating to 120-130 ℃, sending to an evaporative crystallizer (6) 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 directly performing biochemical treatment on the distilled water discharged from the top after collecting.
Example 1
The following examples are given as a method for treating low concentration acrylic acid waste water, in which the amount of waste water generated from an acrylic acid plant of a petrochemical company is 8.5m3H, main pollutants in the wastewaterOrganic 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 composition and the content of main pollutants of the wastewater are shown in Table 1.
TABLE 1 acrylic acid plant wastewater composition
| Serial number | Components | Mass fraction (wt%) |
| 1 | Acetic acid | 4.95 |
| 2 | Acrylic acid | 0.71 |
| 3 | Formaldehyde (I) | 0.11 |
| 4 | Acrolein | 0.03 |
| 5 | Propionic acid | 0.03 |
| 6 | Acetaldehyde | 0.02 |
| 7 | Toluene | 0.08 |
The flow rate of waste water of the acrylic acid device is 8.5m3And h, pumping the mixture through a first heat exchanger by a pump, preheating the mixture to 58 ℃, putting the mixture into a first reaction kettle, continuously adding 30wt% of zirconium oxychloride solution into the first reaction kettle, adding 125.3kg/h of the solution, adding 26% of concentrated ammonia water to adjust the pH value of the mixed solution in the first reaction kettle to be 5.5-6.3, immediately producing a large amount of alkaline zirconium acrylate white precipitate in the first reaction kettle, sending the white turbid liquid precipitate in the first reaction kettle into a centrifugal filter 2, sending the alkaline zirconium acrylate white precipitate at the bottom into a plate-and-frame filter press 3 for treatment, performing filter pressing separation on filter residues by the plate-and-frame filter press 3, and collecting a filtrate to be used as a precursor of the high-grade zirconium oxide ceramic coating.
After the supernatant in the centrifugal filter 2 is pressurized by a pump 4, the supernatant is sent to a second heat exchanger to be preheated to 90 ℃, then the supernatant is put into a second reaction kettle 5, 260kg/h of calcium hydroxide is continuously added into the second reaction kettle 5, the pH value of the solution in the reaction kettle is between 9 and 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, the evaporation is stopped, the mixed solution is further subjected to heat exchange by the heat exchanger and is heated to 125 ℃, then the mixed solution is sent to an evaporation crystallizer 6 to generate a large amount of white crystals of calcium acetate, the crystals at the bottom are filtered by a filter 7 to obtain an industrial-grade calcium acetate solid product, the industrial-grade calcium acetate solid product is collected and packaged as a byproduct, and the analysis results of distilled water and filtered water are respectively shown in the following table 2 and table 3.
TABLE 2 analytical test results for distilled water
| Serial number | Analyzing content | Detection value |
| 1 | Zirconium ion content | Not detected out |
| 2 | Calcium ion content | Not detected out |
| 3 | COD | 205mg/ |
| 4 | BOD | 70mg/L |
TABLE 3 analysis and test results of filtered water
| Serial 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 removal rate of COD in the acrylic acid wastewater reaches 99.7 percent, and the removal rate of BOD is 99.8 percent. The content of inorganic metal ions in the filtered water is lower than 100ppm, the COD removal rate of the acrylic acid wastewater reaches 99.2 percent, the BOD removal rate is 99.3 percent, and the treated wastewater can be directly biochemically treated.
Comparative example 1
The amount of wastewater generated by an acrylic acid device of a certain petrochemical company is 8.5m3/h, the COD of the wastewater is determined to be 126528mg/L, the BOD of the wastewater is determined to be 25710mg/L, the main pollutants in the wastewater comprise organic matters such as acrylic acid, acetic acid, formaldehyde, acrolein, toluene and the like, and the content of the main pollutants in the wastewater is shown in the following table 4.
TABLE 4 organic content in acrylic acid plant wastewater
| Serial number | Components | Mass fraction (wt%) |
| 1 | Acetic acid | 4.75 |
| 2 | Acrylic Acid (AA) | 0.61 |
| 3 | Formaldehyde (I) | 0.13 |
| 4 | Acrolein | 0.04 |
| 5 | Propionic acid | 0.03 |
| 6 | Acetaldehyde | 0.02 |
| 7 | Toluene | 0.08 |
A certain amount of weakly basic anion exchange resin D301 is filled into an ion exchange column, a small amount of quartz sand is filled at the upper end and the lower end to tightly press a resin layer, acrylic acid device wastewater flows through the exchange column at a certain flow rate after being pressurized by a pump and is collected in a liquid storage tank, the acrylic acid, acetic acid concentration, COD (chemical oxygen demand) and BOD (biochemical oxygen demand) values in the treated water are measured by timing sampling, and the wastewater injection is stopped when the adsorption process reaches a saturation point.
And in the elution process, injecting a NaOH solution with the concentration of 15wt% from an alkaline washing tank through a pump, controlling the addition amount to enable the alkaline solution to flow through a saturated resin exchange column at a certain flow rate, regenerating the resin exchange column, collecting eluent in a waste liquid collecting tank, and sampling at regular time to measure the pH, the COD and the concentrations of acrylic acid and acetic acid.
TABLE 5 detection results of acrylic acid device wastewater after adsorption treatment with weakly basic anion exchange resin D301
| Serial 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 acrylic acid device wastewater treated by the weak base anion exchange resin D301 has COD removal rate of 73.01 percent and BOD removal rate of 71.15 percent.
The above-described preferred embodiments of the invention are not intended to be limiting, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the invention are intended to be included within the scope of the invention.
Claims (10)
1. The utility model provides a novel acrylic acid waste water treatment device, its characterized in that, includes anti-first reation kettle (1), centrifugal filter (2), plate and frame filter press (3), supernatant through pump (4), second reation kettle (5), evaporative crystallizer (6) and crystallization process 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 supernatant is passed through pump (4) and second heat exchanger (8) and second reation kettle (5) intercommunication in the upper end of centrifugal filter (2), and second reation kettle (5) and evaporative crystallizer (6) intercommunication, evaporative crystallizer (6) and brilliant process filter (7) intercommunication.
2. The novel acrylic acid wastewater treatment device according to claim 1, characterized in that: a liquid pump (9) and a first heat exchanger (10) are arranged at a liquid inlet of the first reaction kettle (1), wastewater 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).
3. The novel acrylic acid wastewater treatment device according to claim 1, characterized in that: and a steam outlet of the second reaction kettle (5) is communicated with a second heat exchanger (8).
4. The novel acrylic acid wastewater treatment device according to claim 1, characterized in that: the second reaction kettle (5) is communicated with the evaporative crystallizer (6) through a third heat exchanger (11).
5. The wastewater treatment method of the novel acrylic acid wastewater treatment plant as set forth in claim 1, comprising the steps of:
s1, preheating acrylic acid wastewater;
s2, precipitating and filtering the acrylic acid wastewater in the step S1;
s3, performing 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.
6. The wastewater treatment method of the novel acrylic acid wastewater treatment device according to claim 5, wherein the acrylic acid wastewater in the step S1 is sent to the first heat exchanger through a liquid pump, preheated to 50-60 ℃ and then put into the first reaction kettle.
7. The wastewater treatment method of the novel acrylic acid wastewater treatment device according to claim 5, wherein in step S2, zirconium oxychloride as a reaction raw material is continuously added into the first reaction vessel, ammonia water is added to adjust the pH value of the solution in the first reaction vessel to 5.5-6, a large amount of white precipitates are immediately produced in the first reaction vessel, and the suspension in the first reaction vessel is sent to a centrifugal filter.
8. The method for treating wastewater of a novel acrylic acid wastewater treatment plant as set forth in claim 5, wherein the white precipitate in the step S2 is sent to a plate and frame filter press for treatment in the step S3, and the filter residue is subjected to pressure filtration separation by the plate and frame filter press.
9. The wastewater treatment method of the novel acrylic acid wastewater treatment device according to claim 5, characterized in that the supernatant in the centrifugal filter in the step S4 is pressurized by a pump, sent into a second heat exchanger to be preheated to 80-90 ℃, and then put into a second reaction kettle, and calcium hydroxide as a reaction raw material is continuously added into the second reaction kettle to adjust the pH value of the solution in the reaction kettle to 9-10, and then the mixed solution in the second reaction kettle is evaporated and concentrated, and when the mixed solution is evaporated and concentrated to 1/5 of the original volume, the evaporation is stopped.
10. The wastewater treatment method of the novel acrylic acid wastewater treatment device according to claim 5, wherein the concentrated solution obtained in the step S4 is further subjected to heat exchange by a third heat exchanger, heated to 120-130 ℃, sent to an evaporative 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 collected and packaged as a byproduct, and the distilled water discharged from the top can be directly subjected to biochemical treatment after being collected.
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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 |
| 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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