CN110921996A - Glyphosate wastewater treatment method - Google Patents
Glyphosate wastewater treatment method Download PDFInfo
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- CN110921996A CN110921996A CN201911307799.8A CN201911307799A CN110921996A CN 110921996 A CN110921996 A CN 110921996A CN 201911307799 A CN201911307799 A CN 201911307799A CN 110921996 A CN110921996 A CN 110921996A
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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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
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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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
- C02F11/122—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering using filter presses
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/30—Aerobic and anaerobic processes
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention relates to the technical field of wastewater treatment, and discloses a glyphosate wastewater treatment method, which comprises the steps of firstly removing formaldehyde from wastewater and then carrying out biochemical treatment; the method comprises the following steps: (1) introducing ammonia gas into the glyphosate wastewater, and continuing the reaction after the ammonia gas is introduced; (2) carrying out membrane treatment on the reaction liquid obtained in the step (1), continuously distilling the obtained solid until a large amount of solid is separated out, and filtering and collecting filter residues; (3) performing biochemical treatment on the waste liquid obtained by membrane treatment and distillation in the step (2), and discharging or recycling the waste water after the treated waste water reaches the discharge standard; (4) recycling the filtrate obtained by filtering in the step (2); according to the glyphosate wastewater treatment method, ammonia gas is introduced to remove formaldehyde in wastewater, and the wastewater after membrane treatment enters a biochemical treatment system to reach the national wastewater discharge standard and then is discharged.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a glyphosate wastewater treatment method.
Background
Glyphosate, the chemical name of which is N-phosphono methyl glycine, is a biocidal herbicide with excellent performance, high efficiency, no pollution and broad spectrum, has good systemic and conductive performance, is a post-emergence weeding penalty sprayed on non-selective leaf surfaces, and is widely used in the world. The preparation of the glyphosate is mainly carried out by taking glycine, paraformaldehyde and dimethyl phosphite as raw materials, obtaining a glyphosate product through condensation, hydrolysis, crystallization and filtration, and neutralizing a filtered mother liquor with alkali to recover a catalyst to generate wastewater with high formaldehyde and high COD. Wherein the COD concentration is more than or equal to 5000 mg/L, and the waste water is difficult to treat because the waste water contains a certain amount of glyphosate.
The traditional treatment method is to concentrate the high-alkali mother liquor after the catalyst is recovered and prepare the high-alkali mother liquor into 10 percent aqueous solution for sale. For example, in chinese patent CN101328182, hexamethylenetetramine and glyphosate aqueous solution are produced by using glyphosate waste water, and hexamethylenetetramine finished product is obtained, and the filtrate is neutralized by sulfuric acid to obtain ammonium-containing glyphosate aqueous solution. However, as the glyphosate aqueous solution with the content below 30% stops registering and selling, the traditional diluent selling treatment method is not applicable any more.
The current common treatment method for glyphosate production wastewater comprises the following steps: firstly, the glyphosate and other organic components are recovered by methods such as multi-effect evaporation or membrane filtration, and then the subsequent treatment is carried out by a biological or chemical method. For example, chinese patents CN101428935 and CN101717131 adopt multiple-effect evaporation; the method for treating the glyphosate wastewater disclosed by the Chinese patent CN101591084 comprises the steps of adding alkali to adjust the pH value of 3-5, concentrating by adopting a multi-stage membrane filtration method, evaporating and dehydrating the concentrated solution to recover part of substances in the concentrated solution, and reusing the wastewater subjected to membrane filtration in oxidation production. The multi-effect evaporation has high energy consumption and high treatment cost, and solid waste is generated after evaporation and needs to be treated additionally, so that the treatment cost is increased. And the residual formaldehyde in the wastewater is not treated.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a glyphosate wastewater treatment method, which is characterized in that ammonia gas is introduced to remove formaldehyde in wastewater, and the wastewater after membrane treatment enters a biochemical treatment system to reach the national wastewater discharge standard and then is discharged.
In order to achieve the above purpose, the invention provides the following technical scheme:
a glyphosate waste water treatment method comprises the steps of firstly carrying out formaldehyde removal treatment on waste water and then carrying out biochemical treatment; the method comprises the following steps:
(1) introducing ammonia gas into the glyphosate wastewater, and continuing the reaction after the ammonia gas is introduced;
(2) carrying out membrane treatment on the reaction liquid obtained in the step (1), continuously distilling the obtained solid until a large amount of solid is separated out, and filtering and collecting filter residues;
(3) performing biochemical treatment on the waste liquid obtained by membrane treatment and distillation in the step (2), and discharging or recycling the waste water after the treated waste water reaches the discharge standard;
preferably, after the membrane wastewater and the distilled wastewater in the step (3) are subjected to biochemical treatment, the COD value of the effluent is less than 100mg/L, the effluent reaches the discharge standard, and the effluent can be recycled to the glyphosate synthesis stage.
(4) And (3) recycling the filtrate obtained by filtering in the step (2).
Preferably, the filtrate contains glyphosate and trace urotropine, and tests prove that the filtrate can be recycled to the glyphosate synthesis stage.
In the invention, preferably, the temperature of the ammonia gas introduced in the step (1) is 30-80 ℃; preferably, the temperature of the introduced ammonia gas is 35-50 ℃; more preferably, the temperature of the introduced ammonia gas is 40-45 ℃.
In the invention, preferably, the end point of introducing the ammonia gas in the step (1) is pH 8.0-9.0; preferably, the pH value of the ammonia gas is 8.25-9.85 at the end point of introducing the ammonia gas; more preferably, the end point of the ammonia gas feed is pH 8.7.
In the invention, preferably, the ammonia gas is introduced into the step (1) for reaction for 5-10 hours.
In the present invention, it is preferable that the degree of vacuum in the distillation in the step (2) is at least-0.085 MPa, and the end point is that a large amount of solids are precipitated.
In the present invention, preferably, the biochemical treatment includes an anaerobic biochemical tank, a facultative biochemical tank, an aerobic biochemical tank and a sedimentation tank, and the anaerobic biochemical tank, the facultative biochemical tank, the aerobic biochemical tank and the sedimentation tank are connected in sequence.
The anaerobic biochemical tank is used for anaerobic hydrolytic acidification to convert non-dissolved organic matters in the wastewater into dissolved organic matters, mainly converts microorganism refractory substances into easily biodegradable substances, and improves the biodegradability of the wastewater so as to be beneficial to subsequent aerobic biological treatment. The anaerobic biochemical tank adopts an up-flow anaerobic sludge bed, the effective retention time is about 3 days, and the lower part is provided with a special water distribution device to finish the contact and mass transfer of sewage and microorganisms; the upper part is provided with a three-phase separator to realize the separation of sewage, anaerobic granular sludge, methane gas and the like.
Then, the wastewater sequentially enters a facultative biochemical pool and an aerobic biochemical pool, and effectively stays in the facultative biochemical pool for 12 hours and stays in the aerobic biochemical pool for about 36 hours; the wastewater degrades organic pollutants in the facultative tank and the aerobic tank through the assimilation and dissimilation of the facultative bacteria and the aerobic bacteria, so that the wastewater reaches the discharge standard.
In the invention, preferably, perforated aeration pipes are arranged in the anaerobic biochemical tank, the facultative biochemical tank and the aerobic biochemical tank, and the air inlet ends of the perforated aeration pipes are connected with a fan; the blower blows the oxygen, so that the contact between the oxygen and the microorganisms is effectively improved, and the utilization rate of the oxygen is improved.
In the present invention, it is preferable that the sedimentation tank is connected to a sludge concentration tank connected to a sludge dewatering system; the sludge collected in the sludge concentration tank is naturally settled by gravity, the concentrated sludge is dehydrated by a screw pump to a plate-and-frame filter press, and the dehydrated sludge is convenient for post-treatment or recycling.
In the invention, preferably, before the ammonia gas is introduced, the glyphosate wastewater is pretreated to remove suspended matters and large-particle impurities in the glyphosate wastewater.
Compared with the prior art, the invention has the beneficial effects that:
according to the method, ammonia gas is added to react with formaldehyde in glyphosate wastewater to generate urotropine, the formaldehyde is removed, and urotropine byproducts can be obtained through membrane treatment, distillation and filtration, wherein the membrane treatment wastewater and the distillation wastewater directly enter a biochemical treatment system for treatment, are discharged after reaching the national wastewater discharge standard, and the treatment of the glyphosate wastewater is basically realized. And then, the filtered filtrate contains glyphosate and trace urotropine, and tests prove that the filtrate can be recycled to the glyphosate synthesis stage, so that the filtered waste liquid is recycled, the waste is reduced, and the formaldehyde pollution is avoided.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the embodiment. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The raw materials used in the invention can be purchased from the market.
Example 1: taking 1000g of glyphosate wastewater, detecting the content of formaldehyde to be 1.57%, introducing ammonia gas into the wastewater, controlling the temperature to be 40-45 ℃, introducing the ammonia gas to the terminal pH of 8.70, introducing 22.6g of ammonia gas, stopping introducing ammonia gas when the formaldehyde is not detected, keeping the temperature to be 40-45 ℃ for reaction for 4h, performing biomembrane treatment to obtain a high-concentration urotropine solution, continuously distilling the solution under the vacuum of-0.092 MPa until a large amount of solids are separated out, filtering the solution to obtain urotropine wet products, and drying the wet products at the temperature of 110 ℃ to obtain 11.5g of urotropine with white crystals in appearance and the content of 97.02%.
Wherein formaldehyde in the membrane wastewater is not detected, and the COD value is 4570mg/L, and the wastewater directly enters a biochemical treatment system; the formaldehyde in the distilled wastewater is not detected, and the COD value is 2273mg/L and directly enters a biochemical treatment system; the content of urotropine in the filtrate is 1680 ppm.
After the membrane wastewater and the distilled wastewater are subjected to biochemical treatment, the COD value of the effluent is detected to be 91.5 mg/L.
Example 2: taking 2000g of glyphosate wastewater, detecting the content of formaldehyde to be 1.99%, introducing ammonia gas into the wastewater, controlling the temperature to be 35-40 ℃, introducing ammonia gas to the terminal pH of 8.25, introducing 46.8g of ammonia gas, stopping introducing ammonia gas when the formaldehyde is not detected, keeping the temperature to be 35-40 ℃ for reaction for 5h, performing biomembrane treatment to obtain a highly concentrated urotropine solution, continuously distilling the solution under the vacuum of-0.09 MPa until a large amount of solids are separated out, filtering the solution to obtain a urotropine wet product, and drying the wet product at the temperature of 110 ℃ to obtain 24.6g of urotropine with white crystal appearance and 96.85% of content.
Wherein the formaldehyde in the membrane wastewater is not detected, and the COD value is 5280mg/L, and the wastewater directly enters a biochemical treatment system; the formaldehyde in the distilled wastewater is not detected, and the COD value is 2565mg/L and directly enters a biochemical treatment system; the content of urotropine in the filtrate was 1860 ppm.
After the membrane wastewater and the distilled wastewater are subjected to biochemical treatment, the COD value of the effluent is detected to be 95.7 mg/L.
Example 3: taking 2000g of glyphosate wastewater, detecting the content of formaldehyde by 2.05%, introducing ammonia gas into the wastewater, controlling the temperature to be 40-50 ℃, introducing the ammonia gas to achieve the end point pH =8.85, introducing 59.2g of ammonia gas, stopping introducing ammonia gas when the formaldehyde is not detected, keeping the temperature of 40-50 ℃ for reacting for 6h, performing biomembrane treatment to obtain a high-concentration urotropine solution, continuously distilling the solution under the vacuum of-0.095 MPa until a large amount of solids are separated out, filtering the solution to obtain urotropine wet products, and drying the wet products at the temperature of 110 ℃ to obtain 26.3g of urotropine with white crystals in appearance and the content of 96.25%.
Wherein formaldehyde in the membrane wastewater is not detected, and the COD value is 4755mg/L, and the wastewater directly enters a biochemical treatment system; the distilled wastewater formaldehyde is not detected, and the COD value of 2350mg/L directly enters a biochemical treatment system; the content of urotropine in the filtrate was 1535 ppm.
After the membrane wastewater and the distilled wastewater are subjected to biochemical treatment, the COD value of the effluent is detected to be 94.0 mg/L.
According to the method, ammonia gas is added to react with formaldehyde in glyphosate wastewater to generate urotropine, the formaldehyde is removed, and urotropine byproducts can be obtained through membrane treatment, distillation and filtration, wherein the membrane treatment wastewater and the distillation wastewater directly enter a biochemical treatment system for treatment, are discharged after reaching the national wastewater discharge standard, and the treatment of the glyphosate wastewater is basically realized. And then, the filtered filtrate contains glyphosate and trace urotropine, and tests prove that the filtrate can be recycled to the glyphosate synthesis stage, so that the filtered waste liquid is recycled, the waste is reduced, and the formaldehyde pollution is avoided.
The invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
Claims (10)
1. A glyphosate waste water treatment method is characterized in that the waste water is firstly treated by formaldehyde removal and then treated by biochemical treatment; the method comprises the following steps:
(1) introducing ammonia gas into the glyphosate wastewater, and continuing the reaction after the ammonia gas is introduced;
(2) carrying out membrane treatment on the reaction liquid obtained in the step (1), continuously distilling the obtained solid until a large amount of solid is separated out, and filtering and collecting filter residues;
(3) performing biochemical treatment on the waste liquid obtained by membrane treatment and distillation in the step (2), and discharging or recycling the waste water after the treated waste water reaches the discharge standard;
(4) and (3) recycling the filtrate obtained by filtering in the step (2).
2. The glyphosate wastewater treatment method of claim 1, wherein the temperature of the ammonia gas introduced in the step (1) is 30-80 ℃; preferably, the temperature of the introduced ammonia gas is 35-50 ℃; more preferably, the temperature of the introduced ammonia gas is 40-45 ℃.
3. The glyphosate wastewater treatment method of claim 1, wherein the end point of the ammonia gas introduction in the step (1) is pH 8.0-9.0; preferably, the pH value of the ammonia gas is 8.25-9.85 at the end point of introducing the ammonia gas; more preferably, the end point of the ammonia gas feed is pH 8.7.
4. The glyphosate wastewater treatment method of claim 1, wherein ammonia gas is introduced into the step (1) for reaction for 5-10 h.
5. The glyphosate waste water treatment method of claim 1, wherein the vacuum degree in the distillation in the step (2) is greater than or equal to-0.085 MPa, and the end point is that a large amount of solid is separated out.
6. The glyphosate wastewater treatment method of claim 1, wherein the biochemical treatment comprises an anaerobic biochemical tank, a facultative biochemical tank, an aerobic biochemical tank and a sedimentation tank, and the anaerobic biochemical tank, the facultative biochemical tank, the aerobic biochemical tank and the sedimentation tank are connected in sequence.
7. The glyphosate wastewater treatment method of claim 6, wherein the anaerobic biochemical tank, the facultative biochemical tank and the aerobic biochemical tank are all provided with perforated aeration pipes, and the air inlet ends of the perforated aeration pipes are connected with fans.
8. The glyphosate wastewater treatment method of claim 7, wherein the sedimentation tank is connected to a sludge concentration tank, and the sludge concentration tank is connected with a sludge dewatering system.
9. The glyphosate waste water treatment method of claim 1, wherein the filtrate in the step (4) is recycled and reused to return the filtrate to the glyphosate synthesis stage.
10. The method for treating glyphosate waste water as claimed in claim 1, wherein before the ammonia gas is introduced, the glyphosate waste water is pretreated to remove suspended substances and large-particle impurities.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911307799.8A CN110921996A (en) | 2019-12-18 | 2019-12-18 | Glyphosate wastewater treatment method |
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| CN201911307799.8A CN110921996A (en) | 2019-12-18 | 2019-12-18 | Glyphosate wastewater treatment method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101328182A (en) * | 2008-07-17 | 2008-12-24 | 湖北励创科技开发有限公司 | Method for producing urotropine and gyphosate solution by using glyphosate waste water |
| CN101497617A (en) * | 2009-03-19 | 2009-08-05 | 杭州天创净水设备有限公司 | Method for producing hexamethylene tetramin by formaldehyde-containing wastewater |
| CN102206219A (en) * | 2011-01-14 | 2011-10-05 | 捷马化工股份有限公司 | Method for preparing urotropine by using glyphosate by-product ammonia gas and formaldehyde |
| CN103524554A (en) * | 2013-10-21 | 2014-01-22 | 沙隆达集团公司 | Method for recycling glyphosate from glyphosate wastewater |
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- 2019-12-18 CN CN201911307799.8A patent/CN110921996A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101328182A (en) * | 2008-07-17 | 2008-12-24 | 湖北励创科技开发有限公司 | Method for producing urotropine and gyphosate solution by using glyphosate waste water |
| CN101497617A (en) * | 2009-03-19 | 2009-08-05 | 杭州天创净水设备有限公司 | Method for producing hexamethylene tetramin by formaldehyde-containing wastewater |
| CN102206219A (en) * | 2011-01-14 | 2011-10-05 | 捷马化工股份有限公司 | Method for preparing urotropine by using glyphosate by-product ammonia gas and formaldehyde |
| CN103524554A (en) * | 2013-10-21 | 2014-01-22 | 沙隆达集团公司 | Method for recycling glyphosate from glyphosate wastewater |
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