CN111410336A - Method and treatment process for precipitating and separating humic acid in landfill leachate - Google Patents
Method and treatment process for precipitating and separating humic acid in landfill leachate Download PDFInfo
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- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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Abstract
The invention discloses a method for separating humic acid from landfill leachate by precipitation, which comprises the following steps: (1) adjusting the pH value: adjusting the pH value of the landfill leachate to 6-9; (2) and (3) precipitation reaction: adding water-soluble barium salt into the landfill leachate, and reacting the water-soluble barium salt with humic acid to generate water-insoluble humate to form humate suspension; (3) coagulation reaction: adding a coagulant and a flocculant into the humate suspension in sequence to enable the humate suspension to form floccules; (4) standing for precipitation, and performing solid-liquid separation. The method for separating humic acid from landfill leachate can be carried out under the conditions of pH value of 6-9 and normal temperature, has mild reaction conditions, is simple to operate, needs cheap and easily available reagents, and can effectively separate humic acid from landfill leachate. The invention also relates to a landfill leachate treatment process based on the method.
Description
Technical Field
The invention relates to a treatment method of landfill leachate, in particular to a method for precipitating and separating humic acid in the landfill leachate. Meanwhile, the invention also relates to a landfill leachate treatment process based on the method.
Background
The landfill leachate is mainly characterized in that the landfill leachate is high in pollutant concentration and wide in variation range, the COD value is thousands to tens of thousands mg/L, the ammonia nitrogen concentration is hundreds to thousands mg/L, and the treatment difficulty is very large.
Humic acid substances in the landfill leachate are extremely difficult to degrade biochemically, and after the landfill leachate is biochemically treated, residual humic acid substances in tail water are main factors influencing the unqualified COD of the effluent. In order to remove humic acid substances in landfill leachate, the current main treatment methods comprise an advanced oxidation method, a membrane filtration method, a resin adsorption method, a flocculation method, an acid precipitation method and the like.
The advanced oxidation method includes a Fenton method, an ozone oxidation method, a persulfate oxidation method and the like. The advanced oxidation method is not used independently, and is generally matched with a biochemical system for application, and common processes include a biochemical process, a Fenton oxidation process and a BAF process, a biochemical process, an ozone oxidation process and a biological contact process and the like. The advanced oxidation technology generates OH and SO under certain conditions4 -And the chemical structure of the refractory organic matters is subjected to oxidative decomposition by using the free radicals, so that the biodegradability is improved. The reaction conditions of the advanced oxidation method are severe, for example, the fenton reaction needs to be carried out under the condition that the pH value is 3, the dosage of the medicament is large, and the treatment cost is high. The single treatment is difficult to achieve the preset effect, and needs to be matched with biochemical reaction, thereby increasing the engineering investment. Even if the device is matched with a biochemical system for application, reaction conditions are difficult to control due to the fluctuation of water quality, and the treatment effect is unstable.
The membrane filtration method is to adopt a nanofiltration membrane or a reverse osmosis membrane to retain pollutants such as humic acid in the landfill leachate in a membrane concentrated solution. The membrane filtration method generally has two treatment processes, namely an MBR (membrane bioreactor) and membrane filtration process and a precipitation and sand filtration and high-pressure reverse osmosis process.
The membrane filtration method can not degrade humic acid of the landfill leachate, but retains the humic acid in a membrane concentrated solution by a physical method, the amount of the membrane concentrated solution accounts for 15 to 30 percent of the total amount of the leachate stock solution, and the concentration of refractory pollutants such as humic acid and the like is higher, so that the method is a difficult problem in the sewage treatment industry. Typical membrane concentrate treatment methods currently include: recharging process, furnace spraying process, advanced oxidation technology and the like. The recharging process method is simple, but long-term recharging can cause unstable garbage piles, humic acid and other difficultly-degraded pollutants in the garbage percolate are accumulated continuously, and the concentration is increased. The furnace spraying process is mainly used for treating the garbage leachate of a garbage incineration plant, the water content of the garbage can be increased by the furnace spraying process, the heat value of the garbage is influenced, and the working condition of an incinerator is further influenced. Meanwhile, the salt content in the concentrated solution is high, and the back spraying to the hearth also has influence on the service life of the fire grate. The advanced oxidation technology of the concentrated solution is the same as the treatment of the percolate, and comprises a Fenton method, an ozone oxidation method, an electrochemical method and the like. The advanced oxidation method has higher cost, the single advanced oxidation technology can not stably degrade the humic acid until the humic acid is treated to reach the standard and is discharged, and the biochemical treatment system is matched with the biochemical treatment system to be applied, thereby increasing the construction investment.
The resin adsorption method utilizes the adsorption and elution performances of resin on organic compounds with similar polarities to separate organic matters from water, wherein the common XAD series resin is used for humic acid separation in water and has higher adsorption and elution efficiency, so the resin adsorption method is often used in the field of humic acid extraction and purification.
The flocculation method is characterized in that coal humic acid substances have the characteristic of being flocculated by aluminum ions. This property exists in fulvic acid, ulmic acid, humic acid and salts thereof, but this method has little effect on landfill leachate.
The acid precipitation method is to precipitate humic acid from water by utilizing the characteristic that the humic acid is insoluble in water in a strong acid environment. When the pH value of the landfill leachate is adjusted to about 1, a large amount of humic acid is precipitated to form a suspension. However, under the condition of pH 1, most coagulants are ineffective, so that the humic acid is very difficult to separate well. Under the condition that the pH value is 1, the requirements on the corrosion resistance of treatment facilities, the material of separation equipment and pipelines are high, and the construction cost is high. The addition amount of acid and alkali is large, and the operation cost is high. The factors restrict the application of the acidification method in the separation of humic acid in the landfill leachate.
Therefore, research and development of a simple and efficient method for removing humic acid in landfill leachate are important in research of landfill leachate treatment industry.
Disclosure of Invention
The invention aims to provide a method for precipitating and separating humic acid in landfill leachate, which can simply and efficiently remove the humic acid in the landfill leachate.
Specifically, the invention adopts the following technical scheme: a method for separating humic acid from landfill leachate by precipitation comprises the following steps:
(1) adjusting the pH value: adjusting the pH value of the landfill leachate to 6-9;
(2) and (3) precipitation reaction: adding water-soluble barium salt into the landfill leachate, and reacting the water-soluble barium salt with humic acid to generate water-insoluble humate to form humate suspension;
(3) coagulation reaction: adding a coagulant and a flocculant into the humate suspension in sequence to enable the humate suspension to form floccules;
(4) standing for precipitation, and performing solid-liquid separation.
The invention adopts water-soluble barium salt as a precipitating agent to react with humic acid to generate humate which is insoluble in water, so that garbage percolate forms humate suspension, floccule is formed after coagulation treatment, and solid-liquid separation can be realized only by standing and precipitating.
In the step (1) of the invention, acid and alkali are adopted to adjust the pH value according to the property of the landfill leachate. The acid is inorganic acid or organic acid, the inorganic acid can be hydrochloric acid, etc., and the organic acid can be formic acid or acetic acid. The alkali is sodium hydroxide, potassium hydroxide or calcium hydroxide.
The adding mode of the water-soluble barium salt in the step (2) can be a barium salt solution or a water-soluble barium salt solid, the adding amount of the water-soluble barium salt can be determined according to the content of humic acid in the landfill leachate, and as an embodiment of the invention, the adding concentration of the water-soluble barium salt is 500 mg/L-5000 mg/L.
The reaction time of the step (2) is 0.5-2.0 h.
As an embodiment of the invention, in the step (3), the coagulant is polyaluminium chloride, the flocculant is polyacrylamide, the adding mass concentration of the polyaluminium chloride is 100 mg/L-1000 mg/L, and the adding mass concentration of the polyacrylamide is 1 mg/L-5 mg/L.
The reaction time of the step (3) is 10-20 min.
And (4) performing solid-liquid separation in a precipitation mode, namely standing the landfill leachate subjected to coagulation treatment in the step (3) until solid and liquid are completely layered. As an embodiment of the invention, the standing time of the step (4) is 1-2.5 h.
On the basis of the scheme, the method can further remove the residual barium ions in the landfill leachate after the humic acid is precipitated and separated. Specifically, the present invention further comprises step (5): and (4) adding water-soluble sulfate into the landfill leachate obtained after the precipitation obtained in the step (4) is used for separating humic acid, reacting to generate barium sulfate precipitate, and standing for separating the precipitate.
The adding mode of the water-soluble sulfate is sulfate solution or water-soluble sulfate solid, the adding amount is determined according to the barium ion content in the landfill leachate, in one embodiment of the invention, the adding mass concentration of the sulfate is 100 mg/L-500 mg/L, the reaction time is 10 min-30 min, and the standing separation time is 1 h-2.5 h.
The invention also provides a method for separating humic acid from landfill leachate by precipitation, which is applied to a landfill leachate treatment process, and can be arranged before biochemical treatment or after biochemical treatment. The invention also provides a landfill leachate treatment process based on the method for separating humic acid precipitate in landfill leachate, and specifically comprises a step of separating humic acid precipitate on the basis of the steps of landfill leachate regulation treatment, UASB reaction treatment, biochemical treatment and the like, and the step is arranged before or after the biochemical treatment step. Humic acid in the landfill leachate is removed, the landfill leachate treatment process does not need treatment steps such as membrane advanced treatment, advanced oxidation treatment of humic acid and the like, effluent can meet the discharge standard, the tank capacity of biochemical treatment structures of an MBR system can be reduced by 15-20%, and the construction cost is reduced.
The invention has the following beneficial effects:
1. the method for separating humic acid from landfill leachate can be carried out under the conditions of pH value of 6-9 and normal temperature, has mild reaction conditions, is simple to operate, needs cheap and easily available reagents, and can effectively separate humic acid from landfill leachate.
2. Compared with the existing landfill leachate humic acid treatment process, the method for precipitating and separating humic acid in landfill leachate has the advantages of small investment, low operation cost and no secondary pollution.
3. Compared with the existing landfill leachate humic acid treatment process, the method for separating humic acid sediment in landfill leachate of the invention, while separating humic acid in landfill leachate, about 10% -20% of partial ammonia nitrogen is removed in the form of humic acid barium ammonium complex salt, reduce carbon source and oxygen demand required by biological denitrification, have saved the running cost.
4. The invention is applied to the treatment process of the landfill leachate, removes the humic acid, does not need to carry out treatment steps such as advanced membrane treatment, advanced oxidation treatment of the humic acid and the like, can also lead the effluent to accord with the discharge standard, reduces the treatment of the landfill leachate, saves the investment and reduces the treatment cost; but also can reduce the tank volume of biochemical treatment structures of an MBR system by 15-20 percent and reduce the construction cost of landfill leachate treatment facilities.
Drawings
Embodiments of the present invention are described in further detail below with reference to the accompanying drawings.
FIG. 1 is a diagram showing the effect of landfill leachate after precipitation reaction and coagulation reaction.
FIG. 2 is a comparison graph of the effect before and after humic acid separation in landfill leachate.
FIG. 3 is a graph comparing the separation of humic acid in landfill leachate at different dosage of chemicals.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to specific examples and drawings, but the embodiments and the scope of the present invention are not limited thereto.
Example 1
Taking 100m L of landfill leachate, measuring the pH value of the landfill leachate by using a portable pH meter, adjusting the pH value by using hydrochloric acid and sodium hydroxide if the pH value is not within the range of 6-9, wherein the pH value of the landfill leachate is measured to be 8.3 in the embodiment, taking 50m L of the landfill leachate, putting the landfill leachate into a test tube with a plug, adding a barium chloride solution with the mass concentration of 7% 2m L, namely adding the barium chloride solution with the mass concentration of 2800 mg/L, quickly shaking for 2min, standing, shaking for 1 time every 14min, reacting for 1 hour to form humate, adding polyaluminium chloride with the mass concentration of 10% in the suspension, quickly shaking for 0.5m L, then dripping 1 drop of polyacrylamide with the mass concentration of 0.1% by using a dropper, and standing and precipitating for 1.5 hours.
Separating humic acid precipitate, adding sodium sulfate solution with mass concentration of 5% 0.4m L into the supernatant, shaking rapidly, shaking 1 time every 5min, reacting for 20min, adding 10% polyaluminum chloride with mass concentration of 0.4m L, shaking rapidly, adding 1 drop polyacrylamide with mass concentration of 0.1% into a dropper, shaking rapidly, standing for 1.0h, and separating barium sulfate precipitate.
As shown in FIG. 1, after the precipitation reaction, humic acid alum floc formed by adding coagulant and flocculant, i.e., a humic acid salt suspension, is formed into floc. And (4) carrying out contrast photo on the landfill leachate stock solution after humic acid in the landfill leachate is precipitated and separated (the left is the stock solution). As shown in figure 2, the color of the landfill leachate stock solution is dark brown black, the color of the landfill leachate after humic acid precipitation separation is semitransparent earthy yellow, and the flocculent humic acid precipitate at the bottom of the test tube accounts for about 20 percent of the water.
The change of the water quality index of the landfill leachate before and after the reaction is analyzed and is shown in the table I.
TABLE I landfill leachate Water quality index Table Unit before and after reaction mg/L (except pH)
As can be seen from the water quality analysis indexes in Table I, after the humic acid is precipitated and separated, the pH value of a water sample is basically unchanged, and the COD (chemical oxygen demand) isCrThe removal rate is about 42 percent, the removal rate of NH3-N is about 15 percent, and the better precipitation separation of humic acid in the landfill leachate can be seen.
Example 2
Taking 750m L landfill leachate, measuring the pH value of the landfill leachate by using a portable pH meter, if the pH value is not within the range of 6-9, adjusting the pH value by using hydrochloric acid and sodium hydroxide, wherein the pH value of the landfill leachate is measured to be 8.4 in the embodiment, the landfill leachate is evenly divided into five beakers with the serial numbers of 0#, 1#, 2#, 3#, and 4#, wherein the 0# sample is an original water sample, respectively adding 7 mass percent barium chloride solutions of 3m L, 6m L, 9m L, and 12m L into the 1#, 2#, 3#, and 4# beakers, respectively, stirring for 1h, adding 10 mass percent polyaluminium chloride of 1.0m L, then dropping 3 drops of polyacrylamide with the mass percent of 0.1% by using a dropper, stirring at a slow speed of 30rpm, reacting for 15min, and standing for 1.5 h.
Separating humic acid precipitate, adding sodium sulfate solution with mass concentration of 5% 0.75m L, 1.5m L, 2.5m L and 3m L into the supernatant of water samples No. 1, No. 2, No. 3 and No. 4 respectively, stirring for reaction for 20min, adding polyaluminum chloride with mass concentration of 10% 1.0m L, quickly shaking uniformly, dripping 3 drops of polyacrylamide with mass concentration of 0.1% by using a dropper, quickly shaking uniformly, standing for 1.0h, and separating barium sulfate precipitate.
And analyzing the influence of different barium chloride adding amounts on the water quality change of the landfill leachate, and showing in a second table. As shown in fig. 3, five water samples 0#, 1#, 2#, 3# and 4# with different barium chloride adding amounts are reacted and then compared, the water sample 0# is dark brown black, while with the increase of the barium chloride adding amount, the water sample 1# is semitransparent earthy yellow, the water sample 2# is semitransparent yellow, the color of the water sample 1# is lighter and clearer than that of the water sample 1# but the color of the water sample 3# and the water sample 4# is not obviously different from that of the water sample 2# in comparison.
In the second table, different dosages correspond to the unit of the water quality index table of the landfill leachate, namely mg/L (except pH value)
As can be seen from the water quality analysis indexes of Table II, different amounts of barium chloride are used to treat CODCrHas better removal effect and removal rate of about 10 to 15 percent for ammonia nitrogen, when the adding amount of the barium chloride solution with the mass concentration of 7 percent is 6m L, the adding amount is increased, and the COD is increasedCrThe increase in removal rate was not significant. After the humic acid is precipitated and separated, the pH value of a water sample is basically unchanged. Therefore, the humic acid in the barium chloride landfill leachate has better precipitation separation effect.
Example 3
In the embodiment, the raw water quality of the landfill leachate is COD 25000 mg/L3-N1430 mg/L1700 mg/L, and the treatment process and the results are as follows:
the landfill leachate firstly enters an adjusting tank, the hydraulic retention time of the adjusting tank is 7 days, and the water quality and the water quantity of the leachate are balanced. And then, inputting the landfill leachate of the regulating tank into a UASB reaction tank for further treatment through a lift pump. After the landfill leachate enters the UASB reaction tank, the volume load of the UASB reaction tank 2 is controlled at 6kgCOD/m3D, the ascending flow velocity of the reaction tank is 0.8m/h, the height-diameter ratio of the tank body is 2:1, the COD removal efficiency is 75%, and the effluent quality of the UASB reaction tank 2 is that COD is 6250 mg/L3-N＝1360mg/L，TN＝1550mg/L。
Humic acid precipitation separation is carried out on effluent of the UASB reaction tank, and large water in the effluent is removed by a chemical precipitation modeThe method comprises the steps of measuring the pH value of the garbage leachate by using a portable pH meter, adjusting the pH value by using organic acid and sodium hydroxide if the pH value is not within the range of 6-9, measuring the pH value of the garbage leachate to be 6.4 in the embodiment, adding a barium chloride solution with the mass concentration of 7%, uniformly stirring the barium chloride solution according to the measured content of the humic acid, reacting for 2 hours, adding polyaluminum chloride with the mass concentration of 10% and uniformly stirring the polyaluminum chloride solution, adding polyacrylamide with the mass concentration of 0.1% and uniformly stirring the polyacrylamide, reacting for 20 minutes to generate humic acid alum, precipitating for 2.5 hours, feeding the supernatant of a sedimentation tank into a reaction tank, adding a sodium sulfate solution with the mass concentration of 5% into the reaction tank, uniformly stirring the sodium sulfate solution, reacting for 30 minutes, adding polyaluminum chloride with the mass concentration of 10% and uniformly stirring the polyaluminum chloride, adding polyacrylamide with the mass concentration of 0.1% and uniformly stirring the supernatant, reacting for 20 minutes to generate alum, precipitating for 1.0 hour, feeding the supernatant into a first-stage denitrification tank, filtering the supernatant into a first-stage nitrification tank, performing a second-stage nitrification process, wherein the supernatant of the nitrifying sludge is carried out, the nitrifying sludge, the sewage is carried out by a first-stage nitrification process, wherein the sewage is carried out by a first-stage nitrification process comprising the first-stage nitrifying process comprising the steps of COD load sewage treatment of COD, COD < 60 mg/NO < 2, COD < 2 > 4060 < 2 < 200 < 2 > 2 < 2 > denitrification, COD < 2 < 200 < 2 > denitrification, COD < 2 < 200 < 2 > denitrification, COD < 23N/kgM L SS d, the membrane flux of the ultrafiltration membrane is controlled at 60L/m2∙ h or less. The COD removal rate of the percolate in the MBR biochemical tank reaches more than 98 percent, and TN and NH3The removal rate of N reaches more than 99%, and the water quality of the effluent of the MBR biochemical tank is COD which is 85 mg/L3The effluent quality meets the standard requirement of table 2 in the national standard of pollutant control Standard for municipal solid waste landfill (GB16889-2008), and the COD is less than or equal to 100 mg/L is less than or equal to 40 mg/L3-N≤25mg/L。
Claims (10)
1. A method for precipitating and separating humic acid in landfill leachate is characterized by comprising the following steps:
(1) adjusting the pH value: adjusting the pH value of the landfill leachate to 6-9;
(2) and (3) precipitation reaction: adding water-soluble barium salt into the landfill leachate, and reacting the water-soluble barium salt with humic acid to generate water-insoluble humate to form humate suspension;
(3) coagulation reaction: adding a coagulant and a flocculant into the humate suspension in sequence to enable the humate suspension to form floccules;
(4) standing for precipitation, and performing solid-liquid separation.
2. The method for separating humic acid from landfill leachate of claim 1, wherein in the step (1), the acid is inorganic acid or organic acid; the alkali is sodium hydroxide, potassium hydroxide or calcium hydroxide.
3. The method for precipitation and separation of humic acid in landfill leachate of claim 1, wherein the water-soluble barium salt of step (2) is added in the form of barium salt solution or water-soluble barium salt solid, and the amount of water-soluble barium salt is determined according to the content of humic acid in landfill leachate.
4. The method for precipitating and separating humic acid in landfill leachate according to claim 3, wherein the adding concentration of the water-soluble barium salt is 500 mg/L-5000 mg/L.
5. The method for separating and precipitating humic acid in landfill leachate according to claim 3, wherein the reaction time of the step (2) is 0.5h to 2.0 h.
6. The method for precipitating and separating humic acid in landfill leachate according to claim 1, wherein in the step (3), the coagulant is polyaluminum chloride and is added at a mass concentration of 100 mg/L-1000 mg/L, the flocculant is polyacrylamide and is added at a mass concentration of 1 mg/L-5 mg/L, and the reaction time in the step (3) is 10 min-20 min.
7. The method for separating humic acid from landfill leachate according to claim 3, further comprising the step (5): and (4) adding water-soluble sulfate into the landfill leachate obtained after the precipitation of the step (4) and the separation of humic acid to react to generate barium sulfate precipitate, and standing to separate the precipitate.
8. The method of claim 7, wherein the water-soluble sulfate is added as a sulfate solution or as a water-soluble sulfate solid in an amount determined by the barium ion content of the landfill leachate.
9. The method for precipitating and separating humic acid in landfill leachate according to claim 7, wherein the adding mass concentration of the water-soluble sulfate is 100 mg/L-500 mg/L, and the reaction time is 10 min-30 min.
10. The landfill leachate treatment process based on the method for precipitation and separation of humic acid in landfill leachate according to any one of claims 1 to 9, comprising the following steps: the method comprises the steps of garbage leachate adjusting treatment, UASB reaction treatment and biochemical treatment, and is characterized by further comprising a humic acid precipitation separation treatment step which is arranged before or after the biochemical treatment step.
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| CN113003856A (en) * | 2021-02-02 | 2021-06-22 | 广东远帆环保科技有限公司 | Landfill leachate treatment method and sewage treatment facility |
| CN113955879A (en) * | 2021-11-09 | 2022-01-21 | 遵义师范学院 | Flocculation method for treating landfill leachate |
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| CN102295382A (en) * | 2010-06-28 | 2011-12-28 | 中国石油化工股份有限公司 | Treatment method of two-step wet acrylic fiber production wastewater |
| CN110294573A (en) * | 2019-07-10 | 2019-10-01 | 哈尔滨锅炉厂有限责任公司 | It is a kind of to utilize UASB anaerobic reactor, MBR, ultrafiltration and reverse osmosis treatment landfill leachate system |
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| CN113003856A (en) * | 2021-02-02 | 2021-06-22 | 广东远帆环保科技有限公司 | Landfill leachate treatment method and sewage treatment facility |
| CN113955879A (en) * | 2021-11-09 | 2022-01-21 | 遵义师范学院 | Flocculation method for treating landfill leachate |
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