CN113457639B - Manganese-loaded loofah sponge fiber for adsorption catalytic denitrification and preparation and application thereof - Google Patents
Manganese-loaded loofah sponge fiber for adsorption catalytic denitrification and preparation and application thereof Download PDFInfo
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- 235000009814 Luffa aegyptiaca Nutrition 0.000 title claims abstract description 66
- 239000000835 fiber Substances 0.000 title claims abstract description 48
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 44
- 239000011572 manganese Substances 0.000 title claims abstract description 44
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 40
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 244000280244 Luffa acutangula Species 0.000 title claims abstract 27
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000002351 wastewater Substances 0.000 claims abstract description 15
- 230000015556 catabolic process Effects 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000006731 degradation reaction Methods 0.000 claims abstract description 12
- 229940099596 manganese sulfate Drugs 0.000 claims abstract description 12
- 239000011702 manganese sulphate Substances 0.000 claims abstract description 12
- 235000007079 manganese sulphate Nutrition 0.000 claims abstract description 12
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000010802 sludge Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 10
- 238000005273 aeration Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 239000008399 tap water Substances 0.000 claims description 4
- 235000020679 tap water Nutrition 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- 238000004886 process control Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000000274 adsorptive effect Effects 0.000 claims 5
- 230000004048 modification Effects 0.000 claims 1
- 238000012986 modification Methods 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 2
- 244000302544 Luffa aegyptiaca Species 0.000 description 40
- 239000000203 mixture Substances 0.000 description 9
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical group O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- -1 polyethylene Polymers 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000012487 rinsing solution Substances 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 102000019197 Superoxide Dismutase Human genes 0.000 description 1
- 108010012715 Superoxide dismutase Proteins 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000032770 biofilm formation Effects 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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Abstract
The invention discloses a manganese-loaded fiber for adsorption catalytic denitrification and preparation and application thereof. The loofah sponge fiber loaded with manganese oxide is prepared by taking loofah sponge as a raw material and mixing and modifying the loofah sponge with sodium hydroxide, potassium permanganate and manganese sulfate. Adding the manganese-loaded loofah sponge fiber subjected to adsorption catalytic denitrification into wastewater containing ammonia nitrogen, inoculating sludge, and then aerating, reacting to complete ammonia nitrogen adsorption degradation. The preparation method is simple, the prepared manganese-loaded loofah sponge fiber can efficiently remove ammonia nitrogen in water at normal temperature, the ammonia nitrogen in the water can be quickly adsorbed on the surface of the loofah sponge, the aim of quick catalytic degradation is fulfilled, and meanwhile, the loofah sponge fiber can also be used as a slow-release carbon source for denitrification reaction. The invention is suitable for denitrification treatment of ammonia nitrogen wastewater.
Description
Technical Field
The invention relates to a manganese-loaded fiber for adsorption catalytic denitrification and preparation and application thereof, belonging to the technical field of water pollution treatment.
Background
Water pollution is one of the most important environmental pollutants. In recent years, with the gradual development of various large industries, the problem of waste water discharge has become a key environmental problem, and random discharge of a large amount of waste water not only poses a serious threat to the ecological environment, but also has many negative effects on the health development of human beings.
Ammonia nitrogen is a typical form of nitrogen pollution of water, and the commonly used denitrification technologies at present comprise air stripping, chemical precipitation, advanced oxidation, biological treatment and the like. But the cost is high, the efficiency is low, and the low ammonia nitrogen wastewater is difficult to treat. Aiming at the problems, the adsorption method is more and more widely applied to the treatment of ammonia nitrogen wastewater, and common adsorbents such as zeolite, biochar and the like have high adsorption capacity, but have the defects of large adsorbent consumption, complex preparation process, long adsorption balance period and the like.
In recent years, manganese has become one of the important elements of interest because of its significant influence on biological denitrification efficiency. Manganese is a ubiquitous metal element in the environment and is also an essential part of microbial activity. The manganese element can participate in the activity of bacterial superoxide dismutase and plays an important role in the synthesis of microbial enzymes in the denitrification process. Meanwhile, the manganese oxide is used as an eco-friendly adsorbent with good adsorption capacity and strong oxidation performance, and has the advantages of simple preparation method, high removal rate, wide application conditions and the like.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the prior common denitrification technology has the problems of high cost, low efficiency and difficult treatment of low ammonia nitrogen wastewater.
In order to solve the technical problems, the invention provides manganese-loaded loofah sponge fiber for adsorption catalytic denitrification, which takes loofah sponge as a raw material and is prepared by mixing and modifying the raw material with sodium hydroxide, potassium permanganate and manganese sulfate.
The invention also provides a preparation method of the manganese-loaded loofah sponge fiber for adsorption catalytic denitrification, which comprises the steps of completely immersing loofah sponge segments in a sodium hydroxide solution, taking out the loofah sponge segments after soaking for 30-120 min, washing to be neutral, and drying; and then soaking the loofah sponge in a manganese sulfate aqueous solution, adding a potassium permanganate solution, placing the obtained reaction system on a shaking table to react at room temperature, taking out the reaction system, and drying to obtain the manganese-loaded loofah sponge fiber.
Preferably, the mass concentration of the sodium hydroxide solution is 1 to 10%.
Preferably, the washing method specifically comprises the following steps: washing with tap water, and then rinsing with deionized water until the rinsing liquid is neutral.
Preferably, the mass ratio of the potassium permanganate to the manganese sulfate is (1-3): (1-3); the proportion of the potassium permanganate to the reaction system is (1-5) g, (200-1000) mL.
Preferably, the loofah sponge is completely soaked in the aqueous solution of manganese sulfate and is subjected to ultrasonic treatment for 10min.
Preferably, the reaction time is 1 to 24 hours.
Preferably, the drying temperature of the two times is 50-70 ℃ and the drying time is 1-3 h.
The invention also provides application of the manganese-loaded loofah sponge fiber for adsorption catalytic denitrification in adsorption degradation of ammonia nitrogen in water, and is characterized in that the manganese-loaded loofah sponge fiber for adsorption catalytic denitrification is added into wastewater containing ammonia nitrogen, sludge is inoculated, aeration and reaction are carried out, and ammonia nitrogen adsorption degradation is completed.
Preferably, the manganese-loaded loofah sponge fiber for adsorption catalytic denitrification is used as a filler and placed in a porous structure to prevent the manganese-loaded loofah sponge fiber from being dispersed by water flow, and then the porous structure filled with the filler is placed in a biological filter reactor to enable the wastewater to be treated to pass through the reactor from bottom to top; the aeration is specifically air or oxygen, and the aeration process controls the dissolved oxygen in the water body to be 2-5mg/L; the addition amount of the manganese-loaded loofah sponge fiber for adsorption catalytic denitrification is as follows: the filling rate (volume) of the biological filter is 30-40%.
According to the invention, manganese oxide is originally generated on the loofah sponge fiber through an oxidation-reduction reaction, the main component of the manganese oxide is manganese dioxide, and the obtained manganese-loaded loofah sponge fiber can efficiently remove ammonia nitrogen in water at normal temperature, so that the ammonia nitrogen in water can be rapidly adsorbed on the surface of the loofah sponge, the purpose of rapid catalytic degradation is achieved, and the efficient treatment of wastewater is realized.
The method has more advantages in treating the nitrogen-containing wastewater by using the loofah sponge fiber loaded manganese oxide as a fixed carbon source for adsorption, catalysis and denitrification. The loofah sponge filler has low manufacturing cost, can be used as a slow-release carbon source to provide nutrition for water microorganisms, and has a remarkable effect of treating nitrogen-containing wastewater by loading manganese oxide on loofah sponge, and short treatment time. The characterization property of the modified loofah sponge is changed, and the curing and stabilizing capability of pollutants is improved.
Compared with the prior art, the invention has the beneficial effects that:
(1) The manganese-loaded loofah sponge fiber for adsorption catalytic denitrification, which is prepared by the invention, has a loose and porous spatial structure, is beneficial to quick biofilm formation of microorganisms, and achieves the purpose of quickly starting denitrification reaction.
(2) The manganese-loaded loofah sponge fiber for adsorption catalytic denitrification prepared by the invention has the advantages that the loaded manganese oxide is mainly manganese dioxide, and the properties of the manganese dioxide are not changed before and after the reaction, so that the manganese-loaded loofah sponge fiber can be recycled.
(3) According to the manganese-loaded loofah sponge fiber for adsorption catalytic denitrification, which is prepared by the invention, the loofah sponge carrier can be used as a fixed slow-release carbon source, so that the effect of long-term denitrification is achieved.
(4) For ammonia nitrogen wastewater adsorbed, catalyzed and degraded at normal temperature, 1L of initial water sample has the ammonia nitrogen concentration of 31.2772mg/L and the COD value of 90.763; after 12 hours, the ammonia nitrogen concentration of the water sample is reduced to 28.1802mg/L, and the COD value is reduced to 64.964; after 24 hours, the ammonia nitrogen concentration of the water sample is reduced to 21.6543mg/L, and the COD value is reduced to 27.091. The degradation rate of ammonia nitrogen is 0.0128 mg/(L.h).
(5) The manganese-loaded loofah sponge fiber for adsorption catalytic denitrification, prepared by the invention, has the advantages of rich source of production raw materials, low price, simple preparation process and mass production.
(6) Compared with the traditional denitrification method, the adsorption and catalytic denitrification manganese-loaded loofah sponge fiber prepared by the invention combines adsorption denitrification with a biological method, and is more energy-saving, efficient and lower in cost.
Drawings
FIG. 1 is an SEM image of manganese-loaded loofah sponge fibers for adsorption catalytic denitrification in example 1;
fig. 2 is an SEM image of the manganese-supported loofah sponge fiber for adsorption catalytic denitrification in example 2.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
(1) Cutting retinervus Luffae fructus into 1cm × 1cm segments, soaking in 1.5% sodium hydroxide solution for 30min, taking out, washing with tap water, and rinsing with deionized water until the rinsing solution is neutral to obtain alkali modified retinervus Luffae fructus.
(2) Weighing 1g of manganese sulfate, completely dissolving in 100mL of deionized water, adding 2g of alkali modified loofah sponge, and carrying out ultrasonic treatment for 10min. Then, 100mL of a 10g/L potassium permanganate solution was added dropwise thereto, and the mixture was allowed to react at room temperature at 100rpm on a shaker for 24 hours. And aging the mixture for 4 hours, taking out the mixture, and putting the mixture into a forced air drier to dry the mixture for 3 hours at the temperature of 60 ℃ until the weight of the mixture is constant, thus obtaining the manganese-loaded loofah sponge.
(3) Weighing 2g of manganese-loaded loofah sponge fiber for adsorption catalytic denitrification, filling the manganese-loaded loofah sponge fiber into a semicircular porous sphere processed by polyethylene, polypropylene and other materials, measuring 1L of distilled water, adding ammonium chloride to prepare test water with the ammonia nitrogen concentration of 20mg/L, inoculating 3.5g/L of activated sludge, controlling the dissolved oxygen in the water to be 2-5mg/L by aeration, and measuring the ammonia nitrogen concentration after 3h, 6h, 9h, 12h and 24h respectively.
Fig. 1 is an SEM image of manganese-supported loofah sponge fibers for adsorption catalytic denitrification in example 1. Table 1 shows the degradation data of example 1 for ammonia nitrogen.
Table 1 degradation data for ammonia nitrogen in example 1
| Time (h) | 0 | 3 | 6 | 9 | 12 | 24 |
| Ammonia nitrogen concentration (mg/L) | 31.2772 | 31.8856 | 29.3416 | 29.3416 | 28.1802 | 21.6543 |
Example 2
(1) Cutting retinervus Luffae fructus into 1cm × 1cm segments, soaking in 1.5% sodium hydroxide solution for 30min, taking out, washing with tap water, and rinsing with deionized water until the rinsing solution is neutral to obtain alkali modified retinervus Luffae fructus.
(2) Weighing 1g of manganese sulfate, completely dissolving the manganese sulfate in 100mL of deionized water, adding 2g of alkali modified loofah sponge, and carrying out ultrasonic treatment for 10min. Then, 100mL of a 10g/L potassium permanganate solution was added dropwise thereto, and the mixture was placed on a shaker at 100rpm and reacted at room temperature for 24 hours. And aging the mixture for 4 hours, taking out, and putting the mixture into a blast drier to be dried for 3 hours at the temperature of 60 ℃ until the weight is constant, thus obtaining the manganese-loaded loofah sponge.
(3) Weighing 2g of manganese-loaded loofah sponge fiber for adsorption and catalytic denitrification, filling the manganese-loaded loofah sponge fiber into a semicircular porous sphere processed by polyethylene, polypropylene and other materials, measuring 1L of distilled water, adding ammonium chloride to prepare test water with ammonia nitrogen concentration of 20mg/L, inoculating 3.5g/L of activated sludge, controlling dissolved oxygen in the water to be 2-5mg/L by aeration, and measuring COD (chemical oxygen demand) values after 3h, 6h, 9h, 12h and 24h respectively. Fig. 2 is an SEM image of manganese-supported luffa vegetable sponge fibers for adsorption catalytic denitrification in example 2. Table 2 shows the degradation data of example 2 on COD.
Table 2 degradation data for COD in example 2
| Time (h) | 0 | 3 | 6 | 9 | 12 | 24 |
| COD(mg/L) | 90.763 | 43.704 | 109.410 | 82.987 | 64.964 | 27.091 |
Claims (9)
1. The manganese-loaded loofah sponge fiber for adsorption catalytic denitrification is characterized in that loofah sponge is used as a raw material, and is mixed with sodium hydroxide, potassium permanganate and manganese sulfate for modification to prepare the loofah sponge fiber loaded with manganese oxide; the preparation method of the manganese-loaded loofah sponge fiber for adsorption catalytic denitrification comprises the following steps: completely immersing the loofah sponge segments in a sodium hydroxide solution, taking out after soaking for 30-120 min, washing to be neutral, and drying; and then soaking the loofah sponge in a manganese sulfate aqueous solution, adding a potassium permanganate solution, placing the obtained reaction system on a shaking table at room temperature for reaction, taking out the reaction system, and drying to obtain the manganese-loaded loofah sponge fiber with a loose and porous space structure.
2. The manganese-loaded loofah sponge fiber for adsorptive catalytic denitrification according to claim 1, wherein the mass concentration of the sodium hydroxide solution is 1-10%.
3. The manganese-loaded loofah sponge fiber for adsorptive catalytic denitrification according to claim 1, wherein the washing method specifically comprises the following steps: washing with tap water, and then rinsing with deionized water until the rinsing liquid is neutral.
4. The manganese-loaded loofah sponge fiber for adsorptive catalytic denitrification according to claim 1, wherein the mass ratio of potassium permanganate to manganese sulfate is (1-3): (1-3); the proportion of the potassium permanganate to the reaction system is (1-5) g, (200-1000) mL.
5. The manganese-loaded loofah sponge fiber for adsorption catalytic denitrification according to claim 1, wherein the loofah sponge is soaked in the aqueous solution of manganese sulfate completely and ultrasonically for 10min.
6. The manganese-loaded loofah sponge fiber for adsorptive catalytic denitrification according to claim 1, wherein the reaction time is 1-24 h.
7. The manganese-loaded loofah sponge fiber for adsorptive catalytic denitrification according to claim 1, wherein the drying temperature of both times is 50-70 ℃ and the drying time is 1-3 h.
8. The application of the manganese-loaded loofah sponge fiber for adsorption catalytic denitrification disclosed by claim 1 in adsorption degradation of ammonia nitrogen in water is characterized in that the manganese-loaded loofah sponge fiber for adsorption catalytic denitrification is added into wastewater containing ammonia nitrogen, sludge is inoculated, and then aeration and reaction are carried out to complete adsorption degradation of ammonia nitrogen.
9. The use of claim 8, wherein the manganese-loaded loofah sponge fiber for adsorption catalytic denitrification is placed in a porous structure as a filler to prevent the manganese-loaded loofah sponge fiber from being dispersed by water flow, and then the porous structure filled with the filler is placed in a biological filter reactor to allow wastewater to be treated to pass through the reactor from bottom to top; the aeration is specifically air or oxygen, and the aeration process controls the dissolved oxygen in the water body to be 2-5mg/L; the addition amount of the manganese-loaded loofah sponge fiber for adsorption catalytic denitrification is as follows: the filling rate of the biological filter reactor is 30 to 40 percent.
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