CN109796101B - Highly-efficient and resource-utilization treatment process for paraquat wastewater - Google Patents
Highly-efficient and resource-utilization treatment process for paraquat wastewater Download PDFInfo
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Abstract
The invention provides a high-efficiency and resource utilization treatment process technology for paraquat wastewater, which comprises the steps of wastewater pre-evaporation and PH value adjustment pretreatment; rectifying the mixed solution, and cooling and recovering the methanol solution; ammonia rectification and ammonia water cooling and recycling; the waste water cod after the paraquat waste water treatment process is less than 3000mg/L and the ammonia nitrogen is less than 350mg/L, and can be applied to a production working section.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a treatment process for efficiently and resourcefully utilizing paraquat wastewater.
Background
Paraquat, the chemical name of which is 1-1-dimethyl-4-4-bipyridine cation salt, is a quick biocidal herbicide. A large amount of wastewater is generated in the production process of paraquat herbicide, and indexes of COD (chemical oxygen demand) and ammonia nitrogen content in the wastewater are very high, so that the wastewater can be discharged after being treated.
In the existing paraquat wastewater treatment process, paraquat wastewater generates a strand of secondary steam condensate containing methanol and high ammonia nitrogen after being subjected to evaporation concentration treatment, it is known that most of wastewater containing low-boiling-point solvent is treated by a rectification method, the low-boiling-point solvent can be effectively removed, the COD of the wastewater is reduced, but the ammonia nitrogen, especially ionic ammonium radicals, cannot be efficiently removed, the biodegradability of the wastewater is low, an additional ammonia nitrogen removal device needs to be added, the ammonia nitrogen in the wastewater is reduced, and the ammonia nitrogen reduction device can generally produce an ammonium salt solution as a byproduct, so that the ammonium salt solution cannot be directly utilized, and needs to concentrate crystals again, so that the process is long, the efficiency is low, and the operation cost is high. Aiming at the problems, the invention provides a process for treating paraquat wastewater efficiently and resourcefully, which is a pending technical problem.
Disclosure of Invention
Technical problem to be solved
In order to solve the problem that the COD and ammonia nitrogen in the wastewater cannot be simultaneously reduced by the existing treatment process for the secondary condensate containing methanol and having high ammonia nitrogen content, the invention provides a treatment process for efficiently treating and recycling the wastewater with high COD and high ammonia nitrogen.
(II) technical scheme
The invention is realized by the following technical scheme:
a high-efficiency and resource utilization treatment process technology for paraquat wastewater comprises the following steps:
1) wastewater pretreatment: heating and concentrating paraquat wastewater, performing secondary evaporation on the concentrated wastewater, and dropwise adding alkali liquor into condensed water generated by the secondary evaporation, wherein the pH value is controlled to be 9-12;
2) and (3) rectifying mixed liquor: conveying the mixed liquor obtained in the step 1 into a rectifying device through a conveying pump, rectifying the mixed liquor when the temperature of a reboiler is controlled to be 100-105 ℃, introducing gas generated at the top in the rectifying process into a condensing system to be cooled and recovered to obtain a methanol solution, collecting waste water from the bottom of the rectifying device after the rectification is finished, and directly using the waste water for production and recycling or directly discharging the waste water into a biochemical system;
3) ammonia recovery: and (3) introducing the ammonia gas which is not liquefied by the condensation system in the step (2) into an ammonia absorption system to prepare dilute ammonia water, conveying the dilute ammonia water into an ammonia rectification device through a conveying pump, controlling the temperature of a reboiler at 100-120 ℃ and the top temperature at 25-35 ℃ to recover liquid ammonia, simultaneously extracting a bottom liquid from the bottom of the ammonia rectification device, cooling the bottom liquid through a heat exchanger, and introducing the cooled bottom liquid into the ammonia absorption system for recycling.
Preferably, the concentration of the alkali liquor in the step 1 is 32%.
Preferably, the transportation speed of the delivery pump in the step 2 is 6-7 m3/h。
Preferably, the rectification device in the step 2 is one of a rectification column or a gravity bed.
Preferably, the refrigerant in the condensation system in the step 2 is circulating water, and the reflux ratio is adjusted to control the top temperature of the wastewater rectification section to be 85-95 ℃.
Preferably, the concentration of the methanol solution recovered in the step 2 is 35-45%.
Preferably, the refrigerant of the heat exchanger in the step 3 is circulating water.
Preferably, before the paraquat wastewater is treated, the indexes are that the COD content is more than 50000mg/L, the ammonia nitrogen content is more than 3000mg/L, after the paraquat wastewater is rectified, the COD content is less than 3000mg/L, and the ammonia nitrogen content is less than 300 mg/L.
(III) advantageous effects
1. In the process of reducing COD of the wastewater rectification device, liquid caustic soda is dripped to adjust the pH value of the feed of the wastewater rectification device, so that a solvent and ammonia nitrogen in the wastewater are fully volatilized, the solvent and ammonia nitrogen in the wastewater are removed, a certain content of methanol solvent is recovered through the top temperature adjustment of the rectification device, ammonia gas in a gas phase is absorbed by an ammonia absorption system to prepare ammonia water with lower concentration, the ammonia water with lower concentration enters an ammonia rectification tower to prepare liquid ammonia for recovery, produced liquid at the bottom of the tower is cooled and then returns to the ammonia absorption system for reuse, the aim of recovering ammonia is fulfilled, the treated wastewater can be directly applied to a production working section, and the aim of recycling is fulfilled;
2. after the wastewater treated by the method is treated, COD is less than 3000mg/L, ammonia nitrogen is less than 300mg/L, and the wastewater can be directly used for production and application or directly discharged into a biochemical system;
3. the invention has simple process for treating the wastewater, high efficiency and low operation cost.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without inventive labor.
FIG. 1 is a flow chart of the wastewater treatment process of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a highly effective and resource utilization treatment process for paraquat waste water comprises the following steps:
heating and concentrating 1t of paraquat wastewater to 45% of the original volume, performing secondary evaporation on the concentrated wastewater, dropwise adding 32% alkali liquor into condensed water generated by the secondary evaporation, and controlling the pH value to be about 10;
the mixed solution after the alkali liquor is dripped is mixed by a delivery pump at the speed of 6m3The transportation speed of/h is transported to a rectifying tower, when the temperature of a reboiler is controlled to be 100 ℃, the mixed liquid is rectified, gas generated at the top in the rectifying process is introduced into a condensing system, wherein a refrigerant in the condensing system is circulating water, the temperature of the top of a wastewater rectifying section is controlled to be 90 ℃ by adjusting a reflux ratio, a methanol solution with the concentration of 40% is obtained by cooling and recycling, after the rectification is finished, wastewater is extracted from the bottom of a rectifying device and is directly used for production and recycling or is directly discharged into a biochemical system;
in the rectification process, ammonia gas which is not liquefied by a condensing system is introduced into an ammonia absorption system to prepare dilute ammonia water, the dilute ammonia water is conveyed into an ammonia rectification device by a delivery pump, then the temperature of a reboiler is controlled to be 110 ℃, the top temperature is controlled to be 30 ℃ to recover liquid ammonia, meanwhile, bottom liquid is extracted from the bottom of the ammonia rectification device, the bottom liquid passes through a heat exchanger, wherein a refrigerant of the heat exchanger is circulating water, and the cooled bottom liquid is introduced into the ammonia absorption system for cyclic utilization.
Example 2:
a highly effective and resource utilization treatment process for paraquat waste water comprises the following steps:
heating and concentrating 1t of paraquat wastewater to 45% of the original volume, performing secondary evaporation on the concentrated wastewater, dropwise adding 32% alkali liquor into condensed water generated by the secondary evaporation, and controlling the pH value to be about 12;
the mixed solution after the alkali liquor is dripped is mixed by a delivery pump at the speed of 6m3The transportation speed of/h is transported to a rectifying tower, when the temperature of a reboiler is controlled to be 100 ℃, the mixed liquid is rectified, gas generated at the top in the rectifying process is introduced into a condensing system, wherein a refrigerant in the condensing system is circulating water, the temperature of the top of a wastewater rectifying section is controlled to be 90 ℃ by adjusting a reflux ratio, a methanol solution with the concentration of 42% is obtained by cooling and recycling, after the rectification is finished, wastewater is extracted from the bottom of a rectifying device, and the wastewater is directly used for production and recycling or is directly discharged into a biochemical system;
in the rectification process, ammonia gas which is not liquefied by a condensing system is introduced into an ammonia absorption system to prepare dilute ammonia water, the dilute ammonia water is conveyed into an ammonia rectification device by a delivery pump, then the temperature of a reboiler is controlled to be 110 ℃, the top temperature is controlled to be 30 ℃ to recover liquid ammonia, meanwhile, bottom liquid is extracted from the bottom of the ammonia rectification device, the bottom liquid passes through a heat exchanger, wherein a refrigerant of the heat exchanger is circulating water, and the cooled bottom liquid is introduced into the ammonia absorption system for cyclic utilization.
Example 3:
a highly effective and resource utilization treatment process for paraquat waste water comprises the following steps:
heating and concentrating 1t of paraquat wastewater to 45% of the original volume, performing secondary evaporation on the concentrated wastewater, dropwise adding 32% alkali liquor into condensed water generated by the secondary evaporation, and controlling the pH value to be about 11;
the mixed solution after the alkali liquor is dripped is 7m by a delivery pump3The transportation speed of the/h is transported to a rectifying tower, when the temperature of a reboiler is controlled to be 105 ℃, the mixed liquid is rectified, the gas generated at the top in the rectifying process is introduced into a condensing system, wherein the condensing systemThe refrigerant in the process is circulating water, the temperature of the top of a wastewater rectification section is controlled to be 95 ℃ by adjusting the reflux ratio, a methanol solution with the concentration of 37% is obtained by cooling and recycling, after the rectification is finished, wastewater is extracted from the bottom of a rectification device, and the wastewater is directly used for production and is used for production or is directly discharged into a biochemical system;
in the rectification process, ammonia gas which is not liquefied by a condensing system is introduced into an ammonia absorption system to prepare dilute ammonia water, the dilute ammonia water is conveyed into an ammonia rectification device by a delivery pump, then the temperature of a reboiler is controlled to be 115 ℃, the top temperature is controlled to be 25 ℃ to recover liquid ammonia, meanwhile, bottom liquid is extracted from the bottom of the ammonia rectification device, the bottom liquid passes through a heat exchanger, wherein a refrigerant of the heat exchanger is circulating water, and the cooled bottom liquid is introduced into the ammonia absorption system to be recycled.
Example 4:
a highly effective and resource utilization treatment process for paraquat waste water comprises the following steps:
heating and concentrating 1t of paraquat wastewater to 40% of the original volume, performing secondary evaporation on the concentrated wastewater, dropwise adding 32% alkali liquor into condensed water generated by the secondary evaporation, and controlling the pH value to be about 9;
the mixed solution after the alkali liquor is dripped is mixed by a delivery pump at the speed of 6m3The transportation speed of/h is transported to a rectifying tower, when the temperature of a reboiler is controlled to be 105 ℃, the mixed liquid is rectified, gas generated at the top in the rectifying process is introduced into a condensing system, wherein a refrigerant in the condensing system is circulating water, the temperature of the top of a wastewater rectifying section is controlled to be 85 ℃ by adjusting a reflux ratio, a methanol solution with the concentration of 43% is obtained by cooling and recycling, after the rectification is finished, wastewater is extracted from the bottom of a rectifying device, and the wastewater is directly used for production and recycling or is directly discharged into a biochemical system;
in the rectification process, ammonia gas which is not liquefied by a condensing system is introduced into an ammonia absorption system to prepare dilute ammonia water, the dilute ammonia water is conveyed into an ammonia rectification device by a delivery pump, then the temperature of a reboiler is controlled to be 105 ℃, the top temperature is controlled to be 25 ℃ to recover liquid ammonia, meanwhile, bottom liquid is extracted from the bottom of the ammonia rectification device, the bottom liquid passes through a heat exchanger, wherein a refrigerant of the heat exchanger is circulating water, and the cooled bottom liquid is introduced into the ammonia absorption system to be recycled.
Example 5:
a highly effective and resource utilization treatment process for paraquat waste water comprises the following steps:
heating and concentrating 1t of paraquat wastewater to 45% of the original volume, performing secondary evaporation on the concentrated wastewater, dropwise adding 32% alkali liquor into condensed water generated by the secondary evaporation, and controlling the pH value to be about 10;
the mixed solution after the alkali liquor is dripped is mixed by a delivery pump at the speed of 6m3The transportation speed of/h is transported to a rectifying tower, when the temperature of a reboiler is controlled to be 100 ℃, the mixed liquid is rectified, gas generated at the top in the rectifying process is introduced into a condensing system, wherein a refrigerant in the condensing system is circulating water, the temperature of the top of a wastewater rectifying section is controlled to be 85 ℃ by adjusting a reflux ratio, a methanol solution with the concentration of 42% is obtained by cooling and recycling, after the rectification is finished, wastewater is extracted from the bottom of a rectifying device, and the wastewater is directly used for production and recycling or is directly discharged into a biochemical system;
in the rectification process, ammonia gas which is not liquefied by a condensing system is introduced into an ammonia absorption system to prepare dilute ammonia water, the dilute ammonia water is conveyed into an ammonia rectification device by a delivery pump, then the temperature of a reboiler is controlled to be 105 ℃, the top temperature is controlled to be 25 ℃ to recover liquid ammonia, meanwhile, bottom liquid is extracted from the bottom of the ammonia rectification device, the bottom liquid passes through a heat exchanger, wherein a refrigerant of the heat exchanger is circulating water, and the cooled bottom liquid is introduced into the ammonia absorption system to be recycled.
Example 6:
a highly effective and resource utilization treatment process for paraquat waste water comprises the following steps:
heating and concentrating 1t of paraquat wastewater to 40% of the original volume, performing secondary evaporation on the concentrated wastewater, dropwise adding 32% alkali liquor into condensed water generated by the secondary evaporation, and controlling the pH value to be about 10;
the mixed solution after the alkali liquor is dripped is mixed by a delivery pump at the speed of 6m3The transportation speed of the/h is transported to a rectifying tower, when the temperature of a reboiler is controlled to be 105 ℃, the mixed liquid is rectified, and the top of the rectifying tower generatesIntroducing the gas into a condensation system, wherein a refrigerant in the condensation system is circulating water, controlling the temperature of the top of a wastewater rectification section to be 90 ℃ by adjusting a reflux ratio, cooling and recovering to obtain a methanol solution with the concentration of 38%, collecting wastewater from the bottom of a rectification device after rectification is finished, and directly using the wastewater for production and recycling or directly discharging the wastewater into a biochemical system;
in the rectification process, ammonia gas which is not liquefied by a condensing system is introduced into an ammonia absorption system to prepare dilute ammonia water, the dilute ammonia water is conveyed into an ammonia rectification device by a delivery pump, then the temperature of a reboiler is controlled to be 120 ℃, the top temperature is controlled to be 25 ℃ to recover liquid ammonia, meanwhile, bottom liquid is extracted from the bottom of the ammonia rectification device, the bottom liquid passes through a heat exchanger, wherein a refrigerant of the heat exchanger is circulating water, and the cooled bottom liquid is introduced into the ammonia absorption system to be recycled.
Before the treatment of the waste water of the invention, the COD is more than 50000mg/L and the ammonia nitrogen content is more than 3000 mg/L.
The concentration and volume of the methanol solution recovered in examples 1 to 6 were measured, and the COD and ammonia nitrogen content of the paraquat wastewater treated in each group of examples were measured, and the obtained data were recorded, to obtain table 1:
TABLE 1
The above examples are only used to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A highly-efficient and resource-utilization treatment process for paraquat wastewater is characterized by comprising the following steps:
1) wastewater pretreatment: heating and concentrating paraquat wastewater, performing secondary evaporation on the concentrated wastewater, and dropwise adding alkali liquor into condensed water generated by the secondary evaporation, wherein the pH value is controlled to be 9-12;
2) and (3) rectifying mixed liquor: conveying the mixed liquor obtained in the step 1 into a rectifying device through a conveying pump, rectifying the mixed liquor when the temperature of a reboiler is controlled to be 100-105 ℃, introducing gas generated at the top in the rectifying process into a condensing system to be cooled and recovered to obtain a methanol solution, collecting waste water from the bottom of the rectifying device after the rectification is finished, and directly using the waste water for production and recycling or directly discharging the waste water into a biochemical system;
3) ammonia recovery: and (3) introducing the ammonia gas which is not liquefied by the condensation system in the step (2) into an ammonia absorption system to prepare dilute ammonia water, conveying the dilute ammonia water into an ammonia rectification device through a conveying pump, controlling the temperature of a reboiler at 100-120 ℃ and the top temperature at 25-35 ℃ to recover liquid ammonia, simultaneously extracting a bottom liquid from the bottom of the ammonia rectification device, cooling the bottom liquid through a heat exchanger, and introducing the cooled bottom liquid into the ammonia absorption system for recycling.
2. The efficient and resource utilization treatment process for paraquat wastewater according to claim 1, wherein the concentration of the alkali liquor in the step 1 is 32% by mass.
3. The efficient and resource utilization treatment process for paraquat wastewater according to claim 1, wherein the transportation speed of the delivery pump in the step 2 is 6-7 m3/h。
4. The process for efficiently and resource-efficiently utilizing paraquat waste water according to claim 1, wherein the rectifying device in the step 2 is one of a rectifying tower and a gravity bed.
5. The process for efficiently and resourcefully utilizing paraquat waste water according to claim 1, wherein the refrigerant in the condensation system in the step 2 is circulating water, and the reflux ratio is adjusted to control the temperature of the top of the rectifying section to be 85-95 ℃.
6. The efficient and resource utilization treatment process for paraquat wastewater according to claim 1, wherein the mass percentage concentration of the methanol solution recovered in the step 2 is 35-45%.
7. The process for efficiently and resource-efficiently utilizing paraquat wastewater according to claim 1, wherein the refrigerant of the heat exchanger in the step 3 is circulating water.
8. The process for efficient and resource utilization of paraquat wastewater according to claim 1, wherein indexes before treatment of paraquat wastewater are that COD content is more than 50000mg/L, ammonia nitrogen content is more than 3000mg/L, COD is less than 3000mg/L after rectification treatment, and ammonia nitrogen content is less than 300 mg/L.
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| CN1415396A (en) * | 2001-10-30 | 2003-05-07 | 浙江工业大学 | Deflection of jet type revolving bed equipment in hyper gravity field |
| CN101628767A (en) * | 2009-08-14 | 2010-01-20 | 山东科信生物化学有限公司 | Waste water integrated treatment method of paraquat produced by cyanamideprocess |
| CN104230081A (en) * | 2014-07-16 | 2014-12-24 | 湖北仙隆化工股份有限公司 | Paraquat pesticide wastewater treatment process |
| CN107500463A (en) * | 2017-09-26 | 2017-12-22 | 安徽国星生物化学有限公司 | A kind of paraquat wastewater treatment and resource utilization process |
| CN207632536U (en) * | 2017-09-07 | 2018-07-20 | 北京赛科康仑环保科技有限公司 | A kind of recycling treatment system of high ammonia nitrogen and high salt waste water |
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- 2019-02-25 CN CN201910137117.7A patent/CN109796101B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415396A (en) * | 2001-10-30 | 2003-05-07 | 浙江工业大学 | Deflection of jet type revolving bed equipment in hyper gravity field |
| CN101628767A (en) * | 2009-08-14 | 2010-01-20 | 山东科信生物化学有限公司 | Waste water integrated treatment method of paraquat produced by cyanamideprocess |
| CN104230081A (en) * | 2014-07-16 | 2014-12-24 | 湖北仙隆化工股份有限公司 | Paraquat pesticide wastewater treatment process |
| CN207632536U (en) * | 2017-09-07 | 2018-07-20 | 北京赛科康仑环保科技有限公司 | A kind of recycling treatment system of high ammonia nitrogen and high salt waste water |
| CN107500463A (en) * | 2017-09-26 | 2017-12-22 | 安徽国星生物化学有限公司 | A kind of paraquat wastewater treatment and resource utilization process |
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