CN110803835B - Recycling treatment method for quaternary ammonium salt wastewater - Google Patents
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Abstract
The invention provides a method for recycling quaternary ammonium salt wastewater, which belongs to the field of sewage treatment methods and comprises the following steps: carrying out air floatation oil removal on the process wastewater to realize oil-water separation in the wastewater, and collecting the treated oil substances and then returning the oil substances to the production recovery process for treatment; adjusting the pH of the air-flotation effluent, concentrating the process wastewater by the wastewater with the adjusted pH through an ultrafiltration-nanofiltration membrane system component, and concentrating the mother liquor of the nanofiltration concentrated solution through evaporation treatment to produce and recycle the process treatment; mixing the evaporated water and the nanofiltration water to carry out biochemical treatment; biochemical effluent is passed through O3/H2O2The advanced oxidation process is connected with a reverse osmosis system after advanced treatment, and reverse osmosis fresh water is reused for production; evaporating the reverse osmosis concentrated solution, and returning the evaporated water to a biochemical treatment system for further treatment; the invention aims at the technical design of the waste water of quaternary ammonium salt production, solves the technical problem that quaternary ammonium salt is difficult to treat after the treatment by the technology of the invention, and can realize the recycling of the waste water for production.
Description
Technical Field
The invention relates to the technical field of treatment processes for salt-containing high-COD production wastewater, in particular to a method for recycling quaternary ammonium salt wastewater.
Background
Quaternary Ammonium Salts (QACs), also known as quaternary ammonium salts, are mainly used in the production of surfactants, softeners, disinfectants, leveling agents, antistatic agents, emulsifiers and other industrial and household fields. The usage amount of quaternary ammonium salt compounds is increased year by year, and the application range is continuously expanded. Statistically, in 1997, the yield of quaternary ammonium salt surfactants was over 1.7 million tons, and the yield is continuously increasing every year, and nearly 70% of quaternary ammonium salts are discharged to municipal sewage plants worldwide.
The quaternary ammonium salt wastewater has wide sources, the water quality is different from common domestic sewage, the wastewater also has the characteristics of high pH value, high COD content, high suspended matter content and the like, the biochemical treatment difficulty is higher, and great threat is caused to the water environment. The treatment of wastewater from quaternary ammonium salt production has been an important issue worldwide, and is especially important in developed countries. The data show that no mature technology is applied to production practice at home and abroad at present. Therefore, the rational treatment and resource utilization of the quaternary ammonium salt production wastewater are problems to be solved at present, and the innovation of the process and the technical method is urgently needed for the treatment of the quaternary ammonium salt production wastewater.
The main problems of the prior art are as follows: because QACs have strong toxicity, are not easy to biodegrade and have strong surface adsorption characteristics, most QACs are adsorbed on sludge and can not be biodegraded under anaerobic conditions, and finally, the QACs enter the natural environment along with the residual sludge, are accumulated in the environment, are harmful to human health and have toxic effects on the growth of soil organisms, aquatic organisms and the like.
Disclosure of Invention
Aiming at solving the technical problems, the invention provides a method for treating quaternary ammonium salt wastewater, which is characterized in that the process design is carried out on the quaternary ammonium salt production wastewater, and an air floatation oil separation, pH adjustment, a membrane technology treatment system, a biochemical system, an advanced oxidation process and a triple effect evaporation process are adopted. After technical treatment, the technical problem that quaternary ammonium salt is difficult to treat is solved, and the waste water can be recycled for production.
The invention is realized by the following steps:
a method for treating quaternary ammonium salt wastewater as a resource is characterized in that the wastewater in the treatment method sequentially passes through an air floatation oil separation section, a membrane technology treatment system, a triple effect evaporation section, a biochemical system, a flocculation precipitation section and an advanced oxidation section, and the specific treatment steps are as follows:
step one, introducing process wastewater into an air floatation oil separation section for air floatation oil removal to realize oil-water separation in the wastewater; removing oil from high-concentration waste water by air floatation, separating oil from water, discharging floating slag into floating slag tank by scraper, discharging via floating slag pipe, and recovering product from the treated oil layer via overflow weir and water outlet pipe
Step two, adjusting the pH of the effluent obtained in the step one to be 1-5, adjusting the pH of the wastewater, controlling the pH of the effluent to be stable in a certain range, and then further concentrating the process wastewater in an ultrafiltration-nanofiltration membrane technology treatment system component;
regulating the pH of the nanofiltration concentrated solution obtained in the second step to be 6-8, allowing the nanofiltration concentrated solution to enter a triple-effect evaporation system for evaporation treatment, performing wastewater resource recovery on the nanofiltration concentrated solution by using a triple-effect evaporation process, and collecting evaporation concentrated mother liquor for recovery of a production recovery process;
step four, mixing the nanofiltration effluent of the step two and the evaporation effluent of the step three, adjusting the pH = 7-8, and carrying out anaerobic reaction treatment through a biochemical system, wherein the temperature is controlled to be 25-35 ℃, and the reaction time is 24-48 hours; the concentration of organic matters in the wastewater is further reduced through the treatment of a biochemical system;
fifthly, carrying out aerobic reaction on the effluent obtained in the fourth step, controlling the temperature to be 25-35 ℃, controlling the dissolved oxygen to be 2-4 mg/L, and controlling the reaction time to be 24-48 hours; the anaerobic reaction and the aerobic reaction are both treated by a biochemical system, which is beneficial to deeply reducing the concentration of organic matters in the wastewater; after membrane treatment, the concentrated solution and triple-effect evaporation effluent are mixed and enter a biochemical system, after sewage enters anaerobic state, a plurality of mixed bacteria and wastewater are fully mixed under the stirring of a submersible stirrer, and macromolecule insolubility is converted into easily biodegradable micromolecule and soluble substances under the action of a large amount of hydrolytic bacteria; in addition, under the action of acid-producing bacteria, macromolecular organic matter is degraded into micromolecular fatty acid and organic acid, and under the action of ammonifying bacteria, micromolecular organic matter is decomposed into CO2、H2O and H2And the like. The waste water is treated aerobically after anaerobic treatment, under the conditions such as suitable carbon-nitrogen ratio, moisture content and oxygen, utilize the metabolism of microorganism, the organic matter in the greatly reduced waste water, the waste water through biochemical system treatment is through carrying in succession to in the flocculation and precipitation.
Step six, the biochemical effluent of the step five is processed by O3/H2O2Advanced oxidation process advanced treatment, namely, the residual organic matters which are difficult to biodegrade are catalyzed and oxidized by using an oxidant under the action of a catalyst; using O3/H2O2Advanced oxidation process for advanced treatment of reverse osmosis effluent, H2O2Addition of and O3Form a double oxidation reaction mode at O3/H2O2In the oxidation system, two different strong oxidants interact and promote each other, H2O2Can accelerate O3More hydroxyl free radicals are generated by decomposition, and the degradation efficiency of the organic matters is improved by utilizing the strong oxidizing property of the hydroxyl free radicals.
And step seven, the effluent of the advanced oxidation treatment in the step six is connected with a reverse osmosis system, reverse osmosis fresh water is reused for production, reverse osmosis concentrated solution is subjected to evaporation treatment, and the evaporated effluent is returned to a biochemical treatment system for further treatment.
Further, the air flotation oil removal mainly comprises: the air floating section adopts a pressurized dissolved air floating method, the air is pressurized and dissolved in water to reach saturation, when the dissolved air flow is depressurized for air floating, the air amount required by air floating is less, a low-power air compressor is selected, the intermittent operation is adopted, and the pressure from a water pump to a container tank is about 0.5 MPa. The pressurized dissolved air water can be all or part of the treated water, and can also be the return water of the air flotation effluent, and the return ratio is controlled to be 80-100%.
Further, the specific parameters of the second step are as follows: and (3) carrying out ultrafiltration membrane filtration treatment on the wastewater subjected to oil-water separation pretreatment by using an immersed ultrafiltration system. The membrane component is mainly divided into a front end ultrafiltration device, a back filtration device and a tail end reverse osmosis device; controlling the pH = 1-5 of ultrafiltration inlet water through acid-base regulation, and carrying out ultrafiltration membrane filtration treatment on pretreated wastewater through an immersed ultrafiltration system, wherein the ultrafiltration system comprises an ultrafiltration device, a backwashing device, a compressed air storage tank, a backwashing pump and other equipment, bacteria, colloid, part of macromolecular substances and the like are intercepted through an ultrafiltration membrane, the temperature is controlled at 15-30 ℃, and the operating pressure is 0.1-0.25 MPa; the effluent after ultrafiltration enters a nanofiltration system, and organic matters with larger relative molecular mass (generally more than 200) and divalent inorganic salts such as Ca in the wastewater are treated2+And SO-24 at 15-30 deg.C and 0.4-0.6 MPa.
Further, the triple-effect evaporation system in the third step: the steam pressure is controlled to be 0.10-0.35 MPa, and the circulating water consumption is 120-150 t/h. In the triple-effect evaporation process: the nanofiltration concentrated solution and the reverse osmosis concentrated solution enter a triple-effect evaporator, a production mode of continuous feeding and continuous discharging is adopted, the wastewater firstly enters a one-effect forced circulation crystallization evaporator, the crystallization evaporator is provided with a circulating pump, the wastewater is pumped into an evaporation heat exchange chamber, and in the evaporation heat exchange chamber, external steam liquefaction is carried out to generate latent heat of vaporization so as to heat the wastewater; the steam after the evaporation of the waste water enters a double-effect forced circulation evaporator as power steam to heat the double-effect evaporator, and the unevaporated waste water and salt are temporarily stored in a crystallization evaporation chamber; the first-effect, second-effect and third-effect forced circulation evaporators are communicated through a balance pipe, under the action of negative pressure, wastewater flows from the first effect to the second effect and the third effect in sequence, and the consumption of circulating water is 120-150 t/h.
Further, the specific steps of the high-grade oxidation section in the sixth step are as follows: using O3/H2O2Advanced oxidation technology advanced treatment reverse osmosis effluent, controlling the pH of inlet water to be 7-10, controlling the adding amount of hydrogen peroxide to be 0.1-0.5 per mill, controlling the adding amount of ozone to be 3-5 times of the residual COD value of the wastewater, and controlling the reaction time to be 4-8 hours.
And further, the wastewater in the fourth step enters a biochemical system, and the organic matters in the wastewater are reduced by utilizing the metabolism of microorganisms.
The beneficial effects of the invention and the prior art are as follows:
1. the invention adopts an air flotation-ultrafiltration-nanofiltration pretreatment process, wherein the air flotation is used for removing the floating oil in the wastewater and recovering the product, and the ultrafiltration-nanofiltration process can remove most organic matters and suspended matters in the wastewater, improve the biodegradability of the wastewater and reduce the difficulty of a back-end biochemical treatment process on one hand, and can further concentrate the wastewater, reduce the amount of the wastewater subjected to triple effect evaporation and reduce the operation cost on the other hand;
2. the invention adopts an anaerobic-aerobic biochemical treatment process, wherein under the anaerobic condition, the biodegradability of the wastewater is improved, and under the metabolism action of aerobic bacteria, the biochemical substances in the wastewater are degraded in an aerobic section, so that the COD is greatly reduced, and the investment cost and the operation cost of the rear-end ozone oxidation organic load are reduced;
3. the invention adopts an ozone-hydrogen peroxide oxidation process, wherein hydrogen peroxide and ozone are used in combination, most of organic matters which are difficult to be biochemically treated in wastewater can be oxidized, the removal rate of COD is up to 70%, and the removal rate of oxidation is improved by 50% compared with that of ozone which is a single oxidant;
4. the invention effectively solves the problem of quaternary ammonium salt wastewater treatment, has high recycling recovery rate of water and products, basically no wastewater discharge and small solid waste generation amount, realizes zero discharge of wastewater and resource utilization of quaternary ammonium salt in production engineering of enterprises, and has important environmental significance.
Drawings
FIG. 1 is a schematic view of a system and method for treating quaternary ammonium salt wastewater as a resource.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention more clear, the present invention is further described in detail by the following examples. It should be noted that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in FIG. 1, the technical scheme of the invention comprises the following steps: 1) carrying out air floatation oil removal on high-concentration wastewater to separate oil and water in the wastewater, discharging floating slag into a floating slag groove by using a scraper, discharging the floating slag through a floating slag pipe, and recovering a product from a treated oil layer through an overflow weir and a water outlet pipe; 2) adjusting the pH value of the wastewater, controlling the pH value of the effluent to be stable in a certain range, and then further concentrating the process wastewater by passing the wastewater through membrane system components such as ultrafiltration-nanofiltration and the like; 3) carrying out resource recovery on the nanofiltration concentrated solution by using a triple-effect evaporation process, and mixing the evaporated water with nanofiltration clear water for next treatment; 4) the concentration of organic matters in the wastewater is further reduced by treating the mixed water of the evaporated water and the nanofiltration clear water through a biochemical system; 5) biochemical effluent using O3/H2O2Advanced oxidation process, the wastewater after advanced oxidation treatment is connected with a reverse osmosis system, reverse osmosis concentrated solution is subjected to triple effect evaporation, and reverse osmosis fresh water is reused for production.
The invention is further described in detail by specific implementation mode by taking the industrial wastewater of a certain enterprise as a research object, and the feasibility and the accuracy of the method are verified.
The main business quaternary ammonium saltIn series, the waste water contains a large amount of tetrabutylammonium bromide and tetrabutylammonium hydroxide organic matters. Enabling the quaternary ammonium salt wastewater to enter an air floatation system, removing floating oil in the wastewater, adjusting the pH =2, and entering an ultrafiltration-nanofiltration system; adjusting the pH of the nanofiltration concentrated solution to be 7, feeding the nanofiltration concentrated solution into a triple-effect evaporator, and recovering the evaporation mother solution as a product; mixing nanofiltration water and evaporated effluent, performing anaerobic treatment, controlling the water temperature to be 25 ℃, adding activated sludge into a water body, controlling the retention time in an anaerobic stage to be 24 hours, hydrolyzing and acidifying organic matters in wastewater in the anaerobic stage, improving the biodegradability of the wastewater, performing aerobic treatment on anaerobic effluent, controlling the water temperature to be 25 ℃, adding activated sludge, performing aerobic reaction for 24 hours, and controlling the aerobic dissolved oxygen to be 1.5 mg/L; adjusting the pH of biochemical effluent to be =8 by using NaOH solution, coagulating by using PAC, and discharging supernatant to a rear-end advanced oxidation device; 0.5mL of 27.5% hydrogen peroxide and O are added into every 1L of supernatant in the advanced oxidation system3The adding amount is 3 times of the residual COD value, and the retention time is 8 hours; the AOP effluent is connected into a reverse osmosis system, and the COD (chemical oxygen demand) of the fresh water is less than 10 mg/L and NH is treated by the reverse osmosis membrane3N is less than 5 mg/L, TN is less than 5 mg/L, and the crystal is reused for production.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.
Claims (7)
1. A method for treating quaternary ammonium salt wastewater as a resource is characterized in that the wastewater in the treatment method sequentially passes through an air floatation oil separation section, a membrane technology treatment system, a triple effect evaporation section, a biochemical system, a flocculation precipitation section and an advanced oxidation section, and the specific treatment steps are as follows:
step one, introducing process wastewater into an air floatation oil separation section for air floatation oil removal to realize oil-water separation in the wastewater;
step two, adjusting the pH of the effluent obtained in the step one to be 1-5, and then further concentrating the process wastewater in a membrane technology treatment system, namely an ultrafiltration-nanofiltration membrane technology treatment system component;
regulating the pH of the nanofiltration concentrated solution obtained in the second step to be 6-8, allowing the nanofiltration concentrated solution to enter a triple-effect evaporation system for evaporation treatment, and collecting evaporation concentrated mother liquor for recycling production;
step four, mixing the nanofiltration effluent of the step two and the evaporation effluent of the step three, adjusting the pH value to 7-8, treating the mixture by a biochemical system, and carrying out anaerobic reaction at the temperature of 25-35 ℃ for 24-48 hours;
fifthly, carrying out aerobic reaction on the anaerobic effluent obtained in the fourth step, controlling the temperature to be 25-35 ℃, controlling the dissolved oxygen to be 2-4 mg/L, and controlling the reaction time to be 24-48 hours;
step six, the biochemical effluent of the step five is processed by O3/H2O2Advanced oxidation process advanced treatment, namely, the residual organic matters which are difficult to biodegrade are catalyzed and oxidized by using an oxidant under the action of a catalyst;
and step seven, the effluent of the advanced oxidation treatment in the step six is connected with a reverse osmosis system, reverse osmosis fresh water is reused for production, reverse osmosis concentrated solution is subjected to evaporation treatment, and the evaporated effluent is returned to a biochemical treatment system for further treatment.
2. The method for recycling the quaternary ammonium salt wastewater according to claim 1, wherein the air flotation oil separation section adopts dissolved air flotation and is operated intermittently.
3. The method for recycling the quaternary ammonium salt wastewater according to claim 1, wherein the specific parameters of the second step are as follows: performing ultrafiltration membrane filtration treatment on the wastewater subjected to oil-water separation pretreatment by using an immersed ultrafiltration system, wherein the temperature is controlled to be 15-30 ℃, and the operating pressure is 0.1-0.25 MPa; after ultrafiltration, the effluent enters a nanofiltration system, the temperature is controlled to be 15-30 ℃, and the operating pressure is 0.4-0.6 MPa; the aperture of the ultrafiltration membrane is 0.1-0.2 μm; the membrane material is polyvinylidene fluoride or polytetrafluoroethylene; the aperture of the nanofiltration membrane is 0.001-0.0001 μm; the membrane material is one of polyamide, polyvinylidene fluoride or polyacrylonitrile.
4. The method for recycling the quaternary ammonium salt wastewater according to claim 1, wherein the triple effect evaporation process comprises the following steps: the nanofiltration concentrated solution and the reverse osmosis concentrated solution enter a triple-effect evaporator, a production mode of continuous feeding and continuous discharging is adopted, the wastewater firstly enters a one-effect forced circulation crystallization evaporator, the crystallization evaporator is provided with a circulating pump, the wastewater is pumped into an evaporation heat exchange chamber, and in the evaporation heat exchange chamber, external steam liquefaction is carried out to generate latent heat of vaporization so as to heat the wastewater; the steam after the evaporation of the waste water enters a double-effect forced circulation evaporator as power steam to heat the double-effect evaporator, and the unevaporated waste water and salt are temporarily stored in a crystallization evaporation chamber; the first effect, the second effect and the third effect forced circulation evaporators are communicated through a balance pipe, and under the action of negative pressure, the wastewater flows from the first effect to the second effect and the third effect in sequence.
5. The method for recycling the quaternary ammonium salt wastewater according to claim 4, wherein the triple effect evaporation system in the third step comprises: the steam pressure is controlled to be 0.10-0.35 MPa, and the circulating water consumption is 120-150 t/h.
6. The method for recycling the quaternary ammonium salt wastewater according to claim 1, wherein the specific steps of the high-grade oxidation stage in the sixth step are as follows: using O3/H2O2Advanced oxidation technology advanced treatment reverse osmosis effluent, controlling the pH of inlet water to be 7-10, controlling the adding amount of hydrogen peroxide to be 0.1-0.5 per mill, controlling the adding amount of ozone to be 3-5 times of the residual COD value of the wastewater, and controlling the reaction time to be 4-8 hours.
7. The method of claim 1, wherein the wastewater from step four is fed into a biochemical system to reduce the organic substances in the wastewater by the metabolism of microorganisms.
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| CN109912118A (en) * | 2018-12-31 | 2019-06-21 | 浙江蓝湖环保有限公司 | Waste water reclaiming Zero discharging system and method are spun in a kind of color separation with high salt |
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| CN105439395A (en) * | 2016-01-04 | 2016-03-30 | 大唐国际化工技术研究院有限公司 | Zero-discharge treatment method of salt-containing organic wastewater |
| CN206799359U (en) * | 2017-06-06 | 2017-12-26 | 南京膜材料产业技术研究院有限公司 | A kind of pigment industry high-salt wastewater reclamation set |
| CN109912118A (en) * | 2018-12-31 | 2019-06-21 | 浙江蓝湖环保有限公司 | Waste water reclaiming Zero discharging system and method are spun in a kind of color separation with high salt |
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