CN109133533B - Integrated treatment method for high-concentration liquid crystal wastewater - Google Patents
Integrated treatment method for high-concentration liquid crystal wastewater Download PDFInfo
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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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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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
- C02F3/02—Aerobic processes
- C02F3/12—Activated sludge processes
- C02F3/1236—Particular type of activated sludge installations
- C02F3/1263—Sequencing batch reactors [SBR]
Abstract
The invention belongs to the technical field of chemical production wastewater treatment, and relates to a method for preparing a composite catalystThe integrated treatment method of high-concentration liquid crystal wastewater comprises the steps of firstly adjusting the high-concentration liquid crystal wastewater, then introducing the effluent into a Fenton reactor for reaction, then regulating the pH value of the solution after reaction to 7, standing, taking the supernatant fluid, introducing the supernatant fluid into an SBR reactor for aeration reaction, naturally settling, and then discharging the supernatant fluid to TiO2In the activated carbon photocatalytic reactor, an ultraviolet light source is switched on to start a photocatalytic reaction, iron mud generated by the Fenton reactor and a small amount of sludge generated by the SBR reactor enter a microwave digestion furnace to be dried and digested, and the integrated treatment of the concentration liquid crystal wastewater is realized; the method has the advantages of simple and novel process, convenient operation, low cost, less energy consumption, safe and stable operation, high COD removal efficiency and good iron mud recycling treatment effect.
Description
The technical field is as follows:
the invention belongs to the technical field of chemical production wastewater treatment, and relates to a high-concentration liquid crystal wastewater integrated treatment method based on Fenton pretreatment-SBR-TiO2The novel combined process of activated carbon photocatalytic oxidation and microwave sludge digestion is used for treating high-concentration liquid crystal wastewater and sludge generated in the treatment process.
Background art:
with the rapid development of the information industry and the electronic industry, liquid crystal displays are increasingly widely used in the fields of televisions, mobile phones, instruments, and the like. The monomer liquid crystal is produced by adopting a chemical synthesis method, the concentration of organic pollutants in the produced waste water is high, the components are complex, the toxicity is high, and the waste water is difficult to degrade by microorganisms, the main pollutants in the liquid crystal waste water comprise dodecyl glucoside (95%), olefin, a surfactant (dibutyl phthalate), a plasticizer (perfluorooctanoic acid) and ethanol, wherein the surfactant and the plasticizer are strong carcinogens, have strong inhibiting and poisoning effects on organisms, are slowly metabolized in the organisms, have long retention time, and can damage the water environment, the soil environment and the ecological environment due to the unqualified discharge of the high-concentration liquid crystal waste water. Surfactants and plasticizers are detected in seven water systems in China to different degrees, and particularly, the pollutants are detected in human blood and even found in blood of a newborn.
At present, the method for treating high-concentration liquid crystal chemical wastewater is a Fenton oxidation combined process, such as: the method comprises a Fenton pretreatment + hydrolytic acidification + aerobic + ultrafiltration reverse osmosis combined process, a Fenton pretreatment + hydrolytic acidification + ozone oxidation + aerobic + microfiltration + disinfection, a Fenton oxidation + anaerobic + ultrafiltration, a Fenton oxidation + ultrafiltration + reverse osmosis + desalination and the like. In the prior art, a great amount of iron mud (the main component is Fe (OH)) is generated when Fenton oxidation pretreatment is adopted to pretreat high-concentration liquid crystal chemical wastewater3Precipitation), iron sludge is a hazardous waste, and discharging untreated iron sludge causes environmental pollution. Therefore, a Fenton-SBR-TiO is designed2The novel combination process of/active carbon-microwave digestion realizes the simultaneous disposal of high-concentration liquid crystal wastewater and sludge.
The invention content is as follows:
the invention aims to overcome the defects in the prior art and design a Fenton pretreatment SBR-TiO with the advantages of environmental protection, energy conservation and high efficiency2The novel integrated treatment method of the high-concentration liquid crystal wastewater by activated carbon photocatalytic oxidation-microwave digestion of sludge researches and optimizes treatment parameters of each section, and provides technical support for thorough treatment of the high-concentration liquid crystal wastewater.
In order to realize the aim, the specific process for treating the high-concentration liquid crystal wastewater comprises the following steps:
(1) in an adjusting tank, HCl with the concentration of 31 percent and tap water are used for adjusting the pH and COD concentration of the high-concentration liquid crystal wastewater, and the COD concentration of the effluent after adjustment is controlled below 150000mg/L and the pH is about 3;
(2) enabling the effluent of the regulating reservoir to enter a Fenton reactor for reaction, wherein the reaction time is 30-60 min, introducing the reacted solution into a pH regulating reservoir after the reaction is finished, regulating the pH value to be about 7, standing for 2-3h, and enabling the supernatant to enter an SBR reactor; the ratio of the supernatant to the activated sludge entering the SBR reactor is 1: 3-1: 1, aeration is stopped after 18-22 h of aeration reaction, then natural sedimentation is carried out for 2-3h, and the supernatant is discharged to TiO2In the activated carbon photocatalytic reactor, an ultraviolet light source is switched on, the photocatalytic reaction is started, the hydraulic retention time is 2-3h, the COD concentration of the liquid crystal wastewater is reduced from 150000mg/L to 42mg/L, wherein TiO2The dosage of the activated carbon is 5-10 g/L;
(3) and (3) feeding iron mud generated by the Fenton reactor and a small amount of sludge generated by the SBR reactor into a microwave digestion furnace for drying digestion, wherein the microwave radiation power is 300-400W, and the microwave radiation time is 20-40 min, so that the integrated treatment of the liquid crystal wastewater with concentration is realized.
The Fenton reactor is provided with a Fenton reagent dosing pump, and Fe in the Fenton reagent is added2+：H2O2The mass concentration ratio of Fe to Fe is 1: 3-1: 72+The concentration of (A) is 40-80 mg/L.
The activated sludge is the activated sludge taken from an aeration tank of a certain sewage treatment plant, the concentration of the sludge entering an SBR reactor is 3500-4500 mg/L, and the sludge sedimentation ratio is 40-50.
The TiO of the invention2The active carbon catalyst is self-made in a laboratory, and the specific preparation process flow is as follows:
firstly, sequentially performing surface pretreatment on commercially available coconut shell activated carbon with the particle size of 0.2-0.5 mm for 1-2 h by adopting 5-10% of HCl and 5-10% of NaOH by mass, then fishing out the activated carbon, cleaning the activated carbon for 3-5 times by using tap water, and finally transferring the cleaned activated carbon particles to a microwave oven for activation and drying under the power of 200-300W;
② 1-2L of 1-2 percent polyvinyl alcohol solution is prepared by heating and dissolving, and then 5g of TiO2Ultrasonically dispersing the powder in a polyvinyl alcohol solution with the mass fraction of 1-2%, and carrying out ultrasonic treatment for 30-60 min to obtain the powderTiO2-a polyvinyl alcohol mixed solution;
thirdly, the activated carbon treated in the step one is put into the TiO prepared in the step two2Continuing ultrasonic treatment in the polyvinyl alcohol mixed solution for 30-60 min, draining, taking out the activated carbon, putting the activated carbon into an oven at 80-100 ℃ for drying, and sealing and storing for later use; wherein the TiO is2Selecting commercial P25TiO2。
The sludge generated in the Fenton reactor is digested by microwave, dried and digested, the weight of the sludge is reduced to 1/4, and the main component is Fe (OH)3The sediment can be used as a raw material of other industries, and the reduction, harmlessness and volume reduction treatment of the dangerous waste iron mud are realized.
The working principle of the invention is as follows: the main pollutants of dodecyl glucoside and surfactant in the liquid crystal wastewater are easily oxidized and degraded into micromolecular organic acid by Fenton reagent, and the micromolecular organic acid is aerobically biodegraded into CO by SBR process2And H2The microorganisms such as O, residual trace pollutants and bacteria in the water body pass through the TiO2The water quality of the effluent meets the first-grade A standard of sewage discharge, can meet the requirements of production or living use in a garden, and realizes the recycling of water resources; and iron sludge generated by Fenton reaction and a small amount of sludge generated by SBR process are directly subjected to microwave digestion to obtain a byproduct with high iron content, so that the reduction, harmlessness and recycling of hazardous waste treatment are realized.
Compared with the prior art, the method has the advantages of simple and novel process, convenient operation, low cost, less energy consumption, safe and stable operation, high COD removal efficiency and good iron sludge recycling treatment effect.
Description of the drawings:
FIG. 1 shows Fenton-SBR-TiO of an example of the present invention2A technical route chart of a novel combination process for digesting sludge by activated carbon and microwave to treat high-concentration liquid crystal wastewater.
FIG. 2 shows the example of the present invention in which the high concentration liquid crystal wastewater is treated with Fenton-SBR-TiO2The COD removal condition of each section of the active carbon combined process.
Fig. 3 shows the weight change of the sludge (mainly iron sludge) generated in the embodiment of the invention after microwave digestion.
The specific implementation mode is as follows:
the invention is further illustrated by the following examples in conjunction with the accompanying drawings.
The specific process for treating the high-concentration liquid crystal wastewater comprises the following steps:
(2) in an adjusting tank, HCl with the concentration of 31 percent and tap water are used for adjusting the pH and COD concentration of the high-concentration liquid crystal wastewater, and the COD concentration of the effluent after adjustment is controlled below 150000mg/L and the pH is about 3;
(2) the effluent of the regulating reservoir enters a Fenton reactor (a Fenton reactor in figure 1) for reaction, the reaction time is 30-60 min, after the reaction is finished, the reacted solution is introduced into a pH regulating reservoir to regulate the pH value to about 7, and after the reaction is stopped for 2-3h, the supernatant enters an SBR reactor; the ratio of the supernatant to the activated sludge entering the SBR reactor is 1: 3-1: 1, aeration is stopped after 18-22 h of aeration reaction, then natural sedimentation is carried out for 2-3h, and the supernatant is discharged to TiO2In the activated carbon photocatalytic reactor, an ultraviolet light source is switched on, the photocatalytic reaction is started, the hydraulic retention time is 2-3h, the COD concentration of the liquid crystal wastewater is reduced from 150000mg/L to 42mg/L, wherein TiO2The dosage of the activated carbon is 5-10 g/L;
(3) and (3) feeding iron mud generated by the Fenton reactor and a small amount of sludge generated by the SBR reactor into a microwave digestion furnace for drying digestion, wherein the microwave radiation power is 300-400W, and the microwave radiation time is 20-40 min, so that the integrated treatment of the liquid crystal wastewater with concentration is realized.
In this example, the Fenton reactor was equipped with a Fenton reagent dosing pump, where Fe is contained in the Fenton reagent2+：H2O2The mass concentration ratio of Fe to Fe is 1: 3-1: 72+The concentration of (A) is 40-80 mg/L.
The activated sludge is the activated sludge taken from an aeration tank of a certain sewage treatment plant, the concentration of the sludge entering an SBR reactor is 3500-4500 mg/L, and the sludge sedimentation ratio is 40-50.
TiO as described in this example2The active carbon catalyst is self-made in a laboratory, and the specific preparation process flow is as follows:
firstly, sequentially performing surface pretreatment on commercially available coconut shell activated carbon with the particle size of 0.2-0.5 mm for 1-2 h by adopting 5-10% of HCl and 5-10% of NaOH by mass, then fishing out the activated carbon, cleaning the activated carbon for 3-5 times by using tap water, and finally transferring the cleaned activated carbon particles to a microwave oven for activation and drying under the power of 200-300W;
② 1-2L of 1-2 percent polyvinyl alcohol solution is prepared by heating and dissolving, and then 5g of TiO2Ultrasonically dispersing the powder in a polyvinyl alcohol solution with the mass fraction of 1-2%, and carrying out ultrasonic treatment for 30-60 min to obtain TiO2-a polyvinyl alcohol mixed solution;
thirdly, the activated carbon treated in the step one is put into the TiO prepared in the step two2Continuing ultrasonic treatment in the polyvinyl alcohol mixed solution for 30-60 min, draining, taking out the activated carbon, putting the activated carbon into an oven at 80-100 ℃ for drying, and sealing and storing for later use; wherein the TiO is2Selecting commercial P25TiO2。
The example used Fenton-SBR-TiO2Firstly, researching Fenton, SBR and TiO in treating high-concentration liquid crystal wastewater by using a novel combination process of/active carbon-microwave sludge digestion2The removal condition of liquid crystal wastewater COD by three sections of photocatalytic degradation of activated carbon is examined, and then the resource treatment condition of the generated iron mud by the microwave digestion process is examined.
Example 1: Fenton-SBR-TiO2Novel combined process for treating high-concentration liquid crystal wastewater by/active carbon-microwave digestion of sludge
In the embodiment, liquid crystal wastewater generated by a certain chemical plant is selected, the COD concentration of the liquid crystal wastewater reaches 300000mg/L, the pH value is 5-6, and in order to improve the safety and the efficiency of the Fenton reaction, the liquid crystal wastewater is firstly subjected to water quality regulation by a regulating tank before entering a Fenton reactor, so that the COD concentration of the wastewater entering the Fenton reactor is 150000mg/L, and the pH value is about 3; the wastewater is oxidized in a Fenton reactor for about 30-60 min, the reaction is stopped, supernatant and iron mud are separated, the iron mud is subjected to microwave digestion and then recycled, supernatant effluent enters an SBR reactor after pH adjustment, the reaction is stopped after the supernatant effluent reacts in the SBR reactor for about 20h, and the supernatant enters TiO after standing for a period of time2Photocatalytic oxidation degradation of residue by activated carbon reactorThe water retention time is about 2 hours, and the effluent can be reused in a park or a workshop.
Example 2: removal of COD from high-concentration liquid crystal wastewater
This example was carried out by subjecting the high concentration liquid crystal wastewater of example 1 to Fenton-SBR-TiO2After the activated carbon photocatalysis combined process, the removal situation of COD in each section is shown in figure 2, and as can be seen from the figure, after the liquid crystal wastewater is subjected to Fenton oxidation pretreatment for 60min, the COD concentration is reduced from 150000mg/L to 2800mg/L, and the removal rate of the COD in the stage is as high as 98%; then the Fenton effluent enters an SBR unit for treatment for 20 hours, the COD concentration is reduced from 2800mg/L to 512mg/L, and the COD removal rate at the stage is about 82%; finally, the SBR effluent enters TiO2The activated carbon photocatalytic reactor reacts for 2 hours, the COD concentration is reduced from 512mg/L to 42mg/L, the COD water quality index is lower than the first-class A standard (the COD is 50mg/L) of national sewage discharge, and meanwhile, the ultraviolet light and the photocatalytic reaction at the stage play an effective role in sterilizing and disinfecting harmful bacteria in water.
Example 3: weight change of the sludge (mainly iron sludge) after microwave drying
In the embodiment, the sludge generated in the Fenton pretreatment and SBR sections in the embodiment 1 is concentrated and then enters a microwave oven for drying, the change trend of the weight of the sludge along with the microwave digestion time is shown in figure 3, and the figure shows that the weight of the sludge is sharply reduced along with the increase of the microwave digestion time in the first 20 min; within 20-30 min, the weight of the sludge tends to be stable along with the extension of the microwave digestion time, and the weight of the sludge is basically unchanged after 30min, which shows that the sludge is thoroughly dried and the original 100g of the sludge is changed into 24g of the sludge; during the microwave drying process of the sludge, moisture and a part of the sludge are volatilized in the form of steam and ash, and the rest components are mainly Fe (OH)3Meanwhile, bacteria in the sludge can be sterilized by microwave, so that the sludge can be subjected to reduction, recycling and harmless treatment.
Claims (4)
1. A high-concentration liquid crystal wastewater integrated treatment method is characterized by comprising the following specific steps:
(1) adjusting the pH and COD concentration of the high-concentration liquid crystal wastewater by using HCl with the concentration of 31% and tap water in an adjusting tank, and controlling the COD concentration of the adjusted effluent to be less than 150000mg/L and the pH to be 3;
(2) enabling the effluent of the regulating reservoir to enter a Fenton reactor for reaction, wherein the reaction time is 30-60 min, introducing the reacted solution into a pH regulating reservoir to regulate the pH value to 7 after the reaction is finished, and enabling the supernatant to enter an SBR reactor after standing for 2-3 h; the ratio of the supernatant to the activated sludge entering the SBR reactor is 1: 3-1: 1, aeration is stopped after 18-22 h of aeration reaction, then natural sedimentation is carried out for 2-3h, and the supernatant is discharged to TiO2In the activated carbon photocatalytic reactor, an ultraviolet light source is switched on, the photocatalytic reaction is started, the hydraulic retention time is 2-3h, the COD concentration of the liquid crystal wastewater is reduced from 150000mg/L to 42mg/L, wherein TiO2The dosage of the activated carbon is 5-10 g/L;
(3) and (3) feeding iron mud generated by the Fenton reactor and a small amount of sludge generated by the SBR reactor into a microwave digestion furnace for drying digestion, wherein the microwave radiation power is 300-400W, and the microwave radiation time is 20-40 min, so that the integrated treatment of the liquid crystal wastewater with concentration is realized.
2. The integrated treatment method for the liquid crystal wastewater with the concentration as claimed in claim 1, wherein the Fenton reactor is provided with a Fenton reagent dosing pump, and Fe in the Fenton reagent is added2+：H2O2The mass concentration ratio of Fe to Fe is 1: 3-1: 72+The concentration of (A) is 40-80 mg/L.
3. The integrated treatment method of the concentrated liquid crystal wastewater according to claim 1, wherein the activated sludge is activated sludge taken from an aeration tank of a sewage treatment plant, the concentration of the sludge entering the SBR reactor is 3500-4500 mg/L, and the sludge sedimentation ratio is 40-50.
4. The integrated treatment method of the concentrated liquid crystal wastewater according to claim 1, wherein the TiO is selected from the group consisting of2The activated carbon photocatalytic reactor is provided with self-made TiO2Activated carbon catalyst, TiO2The specific preparation process flow of the activated carbon catalyst is as follows:
firstly, sequentially performing surface pretreatment on commercially available coconut shell activated carbon with the particle size of 0.2-0.5 mm for 1-2 h by adopting 5-10% of HCl and 5-10% of NaOH by mass, then fishing out the activated carbon, cleaning the activated carbon for 3-5 times by using tap water, and finally transferring the cleaned activated carbon particles to a microwave oven for activation and drying under the power of 200-300W;
② 1-2L of 1-2 percent polyvinyl alcohol solution is prepared by heating and dissolving, and then 5g of TiO2Ultrasonically dispersing the powder in a polyvinyl alcohol solution with the mass fraction of 1-2%, and carrying out ultrasonic treatment for 30-60 min to obtain TiO2-a polyvinyl alcohol mixed solution;
thirdly, the activated carbon treated in the step one is put into the TiO prepared in the step two2Continuing ultrasonic treatment in the polyvinyl alcohol mixed solution for 30-60 min, draining, taking out the activated carbon, putting the activated carbon into an oven at 80-100 ℃ for drying, and sealing and storing for later use; wherein the TiO is2Selecting commercial P25TiO2。
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