CN113213632B - Nano-hydroxyapatite loofah sponge composite filler and preparation method and application thereof - Google Patents
Nano-hydroxyapatite loofah sponge composite filler and preparation method and application thereof Download PDFInfo
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- CN113213632B CN113213632B CN202110662307.8A CN202110662307A CN113213632B CN 113213632 B CN113213632 B CN 113213632B CN 202110662307 A CN202110662307 A CN 202110662307A CN 113213632 B CN113213632 B CN 113213632B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/30—Aerobic and anaerobic processes
- C02F3/302—Nitrification and denitrification treatment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/30—Aerobic and anaerobic processes
- C02F3/301—Aerobic and anaerobic treatment in the same reactor
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/06—Contaminated groundwater or leachate
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a nano hydroxyapatite and loofah sponge composite filler, a preparation method and application thereof, and relates to a wastewater treatment technologyA field; the method comprises the following steps: soaking retinervus Luffae fructus with water content of 5-10% in 30% hydrogen peroxide for 2 hr, taking out, and air drying; placing the dried retinervus Luffae fructus in Ca (NO) 3 ) 2 ·4H 2 Soaking in the O solution for 8 hours; according to the molar ratio of Ca to P of 1.67 3 ) 2 ·4H 2 Adding diammonium hydrogen phosphate dropwise into the O solution, then adjusting the pH to 9-9.5 by adopting ammonia water with the volume concentration of 10-15%, and stirring for 4-5h; cleaning the loofah sponge obtained in the previous step, and drying for 24 hours at the temperature of 75-78 ℃; repeating the steps for three times to obtain the nano hydroxyapatite and loofah sponge composite filler. The nano hydroxyapatite and loofah sponge composite filler is adopted to adsorb heavy metals in landfill leachate, the optimal adsorption rate of Pb is up to 59%, the optimal adsorption rate of Cr is up to 92.31%, and the adsorption effect is remarkable.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a nano hydroxyapatite and loofah sponge composite filler as well as a preparation method and application thereof.
Background
In about 2000 years, the urban domestic garbage in China is rapidly increased, and therefore, the nation is energetically built with a garbage landfill. The service life of most landfill sites reaches 20 years till now, the content of heavy metals in landfill leachate tends to increase along with the increase of landfill time, and the content of heavy metals such As As, mn, zn, pb, cd, cr, ni and the like is higher.
In order to solve the problem, a biochemical method is adopted to treat the landfill leachate, but the biodegradability of the landfill leachate is poor, and most heavy metals have an inhibiting effect on nitrification and denitrification floras, so that the conditions of poor activity of the floras, unstable yielding water and the like gradually occur in the later stage of CMBR operation and maintenance.
Aiming at the treatment of organic wastewater with high ammonia nitrogen and heavy metal, as most heavy metals have certain inhibition effect on nitrification and denitrification flora, the method for treating the landfill leachate by adopting a biochemical method A2/O process is a main application technology at present. In order to improve the treatment effect of microorganisms, common filler is adopted in the O tank in the field construction of most projects, so that the effects of increasing the contact area of the microorganisms and the wastewater and improving the sewage treatment effect are achieved, but the effect is single.
Loofah serving as an environment-friendly and low-cost material has been widely applied to various water treatment fields as a biomembrane carrier or a carbon source, and the loofah relates to the fields of heavy metal adsorption, fiber modification, petroleum pollutant adsorption, a biological contact oxidation bed carrier, a porous microorganism carrier and the like. Some students adopt a high-temperature drying method to modify hydroxyapatite in the loofah sponge to prepare the loofah sponge into a powder shape, so that the loofah sponge has a certain heavy metal adsorption effect, but the original porous shape of the loofah sponge is destroyed, and the effect that the biological filler is an activated sludge net cannot be realized.
Disclosure of Invention
In order to solve the problems, the invention provides a nano hydroxyapatite and loofah sponge composite filler as well as a preparation method and application thereof.
In order to achieve the purpose, one of the technical schemes adopted by the invention is as follows: the preparation method of the nano hydroxyapatite and loofah sponge composite filler comprises the following steps:
s1: soaking retinervus Luffae fructus with water content of 5-10% in 30% hydrogen peroxide for 2 hr, taking out, and air drying;
s2: placing the loofah sponge dried in the step S1 in Ca (NO) 3 ) 2 ·4H 2 Soaking in the O solution for 8 hours;
s3: dropwise adding diammonium hydrogen phosphate into the solution obtained in the step S2 according to the molar ratio of Ca to P of 1.67, then adjusting the pH value to 9-9.5 by adopting ammonia water with the volume concentration of 10-15%, and stirring for 4-5h;
s4: cleaning the loofah obtained in the step S3, and drying for 24 hours at the temperature of 75-78 ℃;
s5: and repeating the steps S2-S4 for three times to obtain the nano hydroxyapatite and loofah sponge composite filler.
Further, the Ca (NO) 3 ) 2 ·4H 2 The concentration of the O solution was 0.0334moL/L.
Further, the concentration of diammonium hydrogen phosphate was 0.02moL/L.
In order to achieve the purpose, the invention adopts the second technical scheme as follows: the invention provides a nano hydroxyapatite and loofah sponge composite filler prepared by the method.
In order to achieve the purpose, the invention adopts the third technical scheme that: the nano-hydroxyapatite loofah sponge composite filler prepared by the method is applied to but not limited to the treatment of landfill leachate.
In order to achieve the purpose, the invention adopts the fourth technical scheme that: the invention provides a bioreactor for treating landfill leachate, and the filler adopted by the reactor is the nano-hydroxyapatite and loofah sponge composite filler prepared by the invention.
Furthermore, a plurality of porous suspension balls are arranged in the bioreactor, and the nano hydroxyapatite and loofah sponge composite filler is filled in the porous suspension balls.
The invention has the beneficial effects that:
the nano-hydroxyapatite loofah sponge composite material prepared by the method is used as the filler of the bioreactor, so that the problem of heavy metal pretreatment in landfill leachate is effectively solved, engineering equipment is reduced, and Hydraulic Retention Time (HRT) is shortened; solves the problems that the traditional adsorption method can generate a large amount of sludge containing heavy metals when used for treating the heavy metals, and the sludge treatment cost is high.
The invention utilizes the porous multi-stage structure of the loofah sponge to realize integrated synchronous nitrification and denitrification, and replaces the traditional A2/O pool with one reaction pool, thereby not only reducing the size of the pool body and simplifying the equipment, but also reducing the energy consumption and the cost, in addition, the denitrification effect of the synchronous nitrification and denitrification is better, the problem of insufficient C/N ratio of the percolate of old and old refuse landfills is avoided, and the problem of difficult operation or the need of adding a C source is avoided, meanwhile, the loofah sponge is composed of 65.5 percent of cellulose, 17.5 percent of hemicellulose and 15.2 percent of lignin, and can be used as part of the C source to supply nitrobacteria and denitrifying bacteria for metabolic propagation; the loofah sponge is rural solid waste and low in price, and the composite material prepared by using the loofah sponge as a raw material is an environment-friendly and low-cost material. And the lignin in the loofah sponge is degraded by microorganisms, so that the recycling and reduction of the loofah sponge can be realized.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic diagram of the appearance of a loofah sponge material according to an embodiment of the present invention;
FIG. 2 is a scanning electron microscope image of a retinervus Luffae fructus material according to an embodiment of the present invention;
FIG. 3 is a scanning electron microscope image of the nano-hydroxyapatite and loofah sponge composite filler according to the embodiment of the present invention;
fig. 4 is a schematic view of the porous suspension ball filled with the nano-hydroxyapatite and loofah sponge composite filler in the embodiment of the present invention;
fig. 5 is a diagram of a synchronous nitrification-denitrification biological nitrogen removal system with an anaerobic exterior, an anoxic middle and an aerobic interior formed on the surface of the nano-hydroxyapatite and loofah sponge composite filler according to the embodiment of the present invention;
FIG. 6 is a schematic view of the structure of a bioreactor according to an embodiment of the present invention;
FIG. 7 is a graph showing the effect of retinervus Luffae fructus on removing Pb from landfill leachate before and after treatment by the method of the present invention;
FIG. 8 is a graph showing the effect of retinervus Luffae fructus on removing Cr from landfill leachate before and after treatment by the method of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1
A preparation method of a nano hydroxyapatite and loofah sponge composite filler comprises the following steps:
referring to fig. 1, S1: soaking retinervus Luffae fructus with water content of 5-10% in 30% hydrogen peroxide for 2 hr, taking out, and air drying; specifically, finished loofah sponge can be directly bought and aired until the water content is 5-10%, or picked loofah can be aired until the water content is 5-10%, then peeled, seeds are removed, and two ends are removed to obtain loofah sponge; soaking retinervus Luffae fructus with water content of 5-10% in 30% hydrogen peroxide for removing colloid in retinervus Luffae fructus, increasing fiber content of retinervus Luffae fructus, soaking for 2 hr, taking out, and air drying.
S2: placing the loofah sponge dried in the step S1 in Ca (NO) 3 ) 2 ·4H 2 Soaking in the O solution for 8 hours; specifically, first, ca (NO) is weighed 3 ) 2 ·4H 2 Mixing with purified water to obtain paste, adding 60-65 deg.C water, and stirring to obtain Ca (NO) 3 ) 2 ·4H 2 The concentration of O is 0.0334moL/L; then soaking the loofah dried in the step S1 in Ca (NO) 3 ) 2 ·4H 2 In O solution, the aim is to evenly distribute calcium ions around the loofah sponge functional groups, thereby positioning the sites for generating hydroxyapatite and soaking for 8 hours.
S3: dropwise adding diammonium hydrogen phosphate into the solution obtained in the step S2 according to the molar ratio of Ca to P of 1.67, then adjusting the pH value to 9-9.5 by adopting ammonia water with the volume concentration of 10-15%, and stirring for 4-5h; specifically, a diammonium hydrogen phosphate solution with the concentration of 0.02moL/L is prepared, and then Ca (NO) soaked with loofah sponge is added into the prepared diammonium hydrogen phosphate solution according to the proportion of n (Ca)/n (P) =1.67 3 ) 2 ·4H 2 In the O solution, phosphate ions are combined with calcium ions on the surface of the loofah sponge to generate hydroxyapatite, ammonia water with the volume concentration of 10-15% is adopted to adjust the pH value to 9-9.5, and low-speed stirring is carried out for 4-4.5h.
S4: cleaning the loofah obtained in the step S3, and drying for 24 hours at the temperature of 75-78 ℃; specifically, the water for cleaning the loofah sponge is purified water, and the drying is carried out in an oven.
S5: and repeating the steps S2-S4 for three times to obtain the nano hydroxyapatite and loofah sponge composite filler.
In order to verify the modification effect of the method on the loofah sponge, the loofah sponge raw material and the nano-hydroxyapatite loofah sponge composite filler prepared by the method are observed under SEM, and the result is shown in figures 2 and 3, and it can be seen from the figures that the surface of the nano-hydroxyapatite loofah sponge composite filler modified by the method provided by the invention has obviously formed a porous hydroxyapatite adhesive material, the aperture is clear, the size distribution is uniform, and the specific surface area of adsorption is greatly increased.
Example 2
The method comprises the steps of treating landfill leachate of a certain waste incineration plant by using a bioreactor shown in fig. 6, wherein the filler used in the bioreactor is the nano-hydroxyapatite loofah sponge composite filler prepared in example 1, cutting the nano-hydroxyapatite loofah sponge composite filler into a square with the side length of 80mm, filling the square into phi 100 PP porous suspension balls, and connecting the porous suspension balls by using yarns, as shown in fig. 4.
Through analysis, the COD value in the landfill leachate is higher, the B/C ratio is 0.22, the biodegradability is poor, and the water quality is shown in the table 1.
TABLE 1 water quality of landfill leachate
As can be seen from Table 1, the main heavy metal pollution in the landfill leachate is Cr and Pb, so the nano-hydroxyapatite loofah sponge composite filler and the loofah sponge raw material which is not treated by the method are respectively filled with the same amount of porous suspension balls, and the Cr and the Pb in the landfill leachate are subjected to comparative adsorption experiments.
Adjusting the pH value of the landfill leachate to 6.5-7.5, and respectively adsorbing the landfill leachate for 30min, 1h, 2h, 4h, 8h, 12h, 24h and 48h under continuous aeration, and investigating the adsorption effect of the loofah sponge before and after treatment by the method on Cr and Pb in the landfill leachate, wherein the experimental effect is shown in figure 7, and as can be seen from figure 7, the optimal adsorption rate of the nano-hydroxyapatite loofah sponge composite filler prepared by the method on Pb in the landfill leachate reaches 59%, and is increased by 41.85% compared with the optimal adsorption rate of 17.15% of the loofah sponge raw material; the Pb concentration in the effluent after adsorption is as low as 0.098mg/L. Can meet the first class A standard of pollutant discharge standard of urban sewage treatment plants (GB 18918-2002).
As can be seen from FIG. 8, the optimum adsorption rate of the nano-hydroxyapatite and loofah sponge composite filler prepared by the method of the invention to Cr in landfill leachate is as high as 92.31%, which is increased by 34.7% compared with 57.69% of the optimum adsorption rate of loofah sponge raw material; the concentration of the adsorbed Cr in the effluent is as low as 0.02mg/L. Can meet the first class A standard of pollutant discharge standard of urban sewage treatment plants (GB 18918-2002).
The nano-hydroxyapatite loofah sponge composite material prepared by the method is used as a filler of a bioreactor, so that the problem of heavy metal pretreatment in landfill leachate is effectively solved, engineering equipment is reduced, and Hydraulic Retention Time (HRT) is shortened; solves the problems that the traditional adsorption method can generate a large amount of sludge containing heavy metals when used for treating the heavy metals, and the sludge treatment cost is high.
As shown in figure 5, the invention utilizes the porous multi-stage structure of the loofah sponge to realize integrated synchronous nitrification and denitrification, replaces the traditional A2/O pool with one reaction pool, not only reduces the size of the pool body, simplifies the equipment, but also reduces the energy consumption and lowers the cost, in addition, the denitrification effect of the synchronous nitrification and denitrification is better, the problem of insufficient C/N ratio of percolate in old and old refuse landfills is avoided, and the problem of difficult operation or the need of adding a C source is avoided, meanwhile, the loofah sponge is composed of 65.5 percent of cellulose, 17.5 percent of hemicellulose and 15.2 percent of lignin, and can be used as part of the C source for supplying nitrobacteria and denitrifying bacteria for metabolic propagation; the loofah sponge is rural solid waste and low in price, and the composite material prepared by using the loofah sponge as a raw material is an environment-friendly and low-cost material. And the lignin in the loofah sponge is degraded by microorganisms, so that the recycling and reduction of the loofah sponge can be realized.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (7)
1. A preparation method of a nano hydroxyapatite and loofah sponge composite filler is characterized by comprising the following steps:
s1: soaking retinervus Luffae fructus with water content of 5-10% in 30% hydrogen peroxide for 2 hr, taking out, and air drying;
s2: placing the loofah sponge dried in the step S1 in Ca (NO) 3 ) 2 ·4H 2 Soaking in the O solution for 8 hours;
s3: dropwise adding diammonium hydrogen phosphate into the solution obtained in the step S2 according to the molar ratio of Ca to P of 1.67, then adjusting the pH value to 9-9.5 by adopting ammonia water with the volume concentration of 10-15%, and stirring for 4-5h;
s4: cleaning the loofah obtained in the step S3, and drying for 24 hours at 75-78 ℃;
s5: and repeating the steps S2-S4 for three times to obtain the nano hydroxyapatite and loofah sponge composite filler.
2. The method for preparing nano hydroxyapatite and loofah sponge composite filler according to claim 1, wherein the Ca (NO) is 3 ) 2 ·4H 2 The concentration of the O solution was 0.0334moL/L.
3. The method for preparing nano hydroxyapatite and loofah sponge composite filler according to claim 1, wherein the concentration of diammonium phosphate is 0.02moL/L.
4. A nano hydroxyapatite and loofah sponge composite filler, which is characterized in that the nano hydroxyapatite and loofah sponge composite filler is prepared by the method of any one of claims 1 to 3.
5. An application of the nano-hydroxyapatite and loofah sponge composite filler of claim 4 in landfill leachate treatment.
6. A bioreactor for treating landfill leachate, wherein the filler in the bioreactor is the nano hydroxyapatite and loofah sponge composite filler according to claim 4.
7. The bioreactor for treating landfill leachate according to claim 6, wherein a plurality of porous suspension balls are further disposed in the reactor, and the nano hydroxyapatite and loofah sponge composite filler is filled in the porous suspension balls.
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