CN112340842A - Preparation method of denitrification solid carbon source - Google Patents
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- CN112340842A CN112340842A CN202011072564.8A CN202011072564A CN112340842A CN 112340842 A CN112340842 A CN 112340842A CN 202011072564 A CN202011072564 A CN 202011072564A CN 112340842 A CN112340842 A CN 112340842A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000007787 solid Substances 0.000 title claims abstract description 13
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 60
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 claims abstract description 23
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 23
- 239000004626 polylactic acid Substances 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 229910052786 argon Inorganic materials 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000012467 final product Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 229920000642 polymer Polymers 0.000 claims abstract description 5
- 239000000853 adhesive Substances 0.000 claims abstract description 4
- 230000001070 adhesive effect Effects 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000006185 dispersion Substances 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical group ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 239000002135 nanosheet Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 5
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 4
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 4
- 239000000839 emulsion Substances 0.000 claims description 4
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 4
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 4
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
- 239000012286 potassium permanganate Substances 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 2
- 239000002174 Styrene-butadiene Substances 0.000 claims description 2
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- 239000011115 styrene butadiene Substances 0.000 claims description 2
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- OCKPCBLVNKHBMX-UHFFFAOYSA-N butylbenzene Chemical compound CCCCC1=CC=CC=C1 OCKPCBLVNKHBMX-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229960001701 chloroform Drugs 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 230000004060 metabolic process Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000149 chemical water pollutant Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- 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
- C02F3/28—Anaerobic digestion processes
-
- 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
- C02F2305/06—Nutrients for stimulating the growth of microorganisms
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- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Biodiversity & Conservation Biology (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a denitrification solid carbon source, which comprises the following steps: (1) preparing modified polylactic acid; (2) preparing a graphene oxide nano roll modified by poly (diallyldimethylammonium chloride); (3) mixing the obtained modified polylactic acid and a polymer according to the mass ratio of 1: (1-2) and uniformly stirring to obtain a mixed solution, and then mixing the mixed solution, an adhesive and the poly (diallyldimethylammonium chloride) -modified graphene oxide nano roll according to a mass ratio of 4: 2: 1 in THF, stirring the mixture at room temperature for 2-4 hours under the protection of argon, centrifuging the mixture, washing the mixture with THF, and finally performing heat treatment under the protection of argon to obtain a final product. The solid carbon source of the invention releases COD mildly, has long duration and moderate dosage.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a preparation method of a denitrification solid carbon source.
Background
Research shows that insufficient carbon source supplement or unstable supply becomes an important factor for restricting biological denitrification efficiency, and sufficient carbon source can provide sufficient nutrient source for growth and metabolism of microorganisms. Therefore, the solution of the problem of low denitrification efficiency by adding carbon source is becoming a hot point of research in the field of water treatment.
As known from research reports on carbon source supplement, liquid carbon sources such as short-chain organic carbon such as methanol, ethanol, glucose and the like are mainly mature and most widely used, but the problems of high cost, toxicity, uncertain dosage, difficult transportation and the like also lead researchers to start to search and try for additional carbon sources. The hot spots mostly concentrate on how to optimize the traditional carbon source, such as adding a hydrolysis acidification process before a denitrification process, so as to improve the biodegradability and treatment rate of the raw sewage; developing non-traditional carbon sources as carbon sources which can be selected in the denitrification process, such as industrial wastewater, primary sludge hydrolysate, landfill leachate, plant straws and the like. However, these carbon sources have problems such as difficulty in controlling the amount of supply and insufficient supply at the early stage, which affect the metabolism of the microorganism and further the effect of the treatment.
Graphene is a compound represented by sp2The two-dimensional nano material composed of hybridized carbon atoms has a hexagonal honeycomb structure, and has excellent performance and wide application prospect. Materials such as graphene sheets, graphene fibers, graphene hydrogel or aerogel, graphene nanocoils and the like can be prepared by various methods at present. The graphene oxide nano roll composite material is formed by wrapping other nano substances with two-dimensional graphene oxide nano sheets and curling, and is a carbon nano material with an open structure. At present, the graphene oxide nano roll is mainly applied to the aspects of energy conversion and storage, electronic devices, quantum transportation, flexible materials, optical devices, catalysis, aerospace and the like, and few literature reports are used in the denitrification process of sewage treatment.
According to the invention, the graphene oxide nano roll is used as a carrier matrix, and a carbon source is loaded on the surface of the graphene oxide nano roll, so that on one hand, more carbon sources can be loaded due to the larger interface area of the graphene oxide nano roll, and on the other hand, the graphene oxide nano roll has good mechanical properties, so that the stability in the denitrification process can be ensured, and a sufficient and stable carbon source can be provided for flora.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a denitrification solid carbon source. According to the invention, the graphene oxide nano roll is used as a carrier matrix, and a carbon source material is loaded on the surface of the graphene oxide nano roll, so that an adequate and stable carbon source is provided for flora.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme.
The invention provides a preparation method of a denitrification solid carbon source, which comprises the following steps:
(1) dissolving polylactic acid in an organic solvent, then dropwise adding a strong oxidant solution, carrying out oxidation pretreatment at the temperature of not higher than 60 ℃, and then adjusting the pH of the solution to 6-8 to obtain modified polylactic acid;
(2) uniformly dispersing graphene oxide nanosheets in deionized water, heating the obtained graphene oxide dispersion liquid in a water bath, quickly immersing the graphene oxide dispersion liquid in liquid nitrogen until the graphene oxide dispersion liquid is completely frozen, finally, obtaining graphene nano rolls through freeze drying, carrying out ultrasonic treatment on the graphene oxide nano rolls in 100ml of aqueous solution containing 1 wt% of poly (diallyldimethylammonium chloride) for 2-4 hours, filtering and carrying out vacuum drying to obtain poly (diallyldimethylammonium chloride) -modified graphene oxide nano rolls;
(3) mixing the obtained modified polylactic acid and a polymer according to the mass ratio of 1: (1-2) and uniformly stirring to obtain a mixed solution, and then mixing the mixed solution, an adhesive and the poly (diallyldimethylammonium chloride) -modified graphene oxide nano roll according to a mass ratio of 4: 2: 1 in THF, stirring the mixture at room temperature for 2-4 hours under the protection of argon, centrifuging the mixture, washing the mixture with THF, and finally performing heat treatment under the protection of argon to obtain a final product.
The preparation method, wherein the organic solvent is dichloromethane or trichloromethane.
The above preparation method, wherein the strong oxidant is selected from any one of nitric acid, sulfuric acid, potassium permanganate, or a mixed solution thereof.
In the preparation method, the water bath heating temperature is 70-80 ℃, and the time is 1-3 hours.
In the preparation method, the vacuum drying temperature is 40-50 ℃ and the time is 12-24 hours.
In the preparation method, the polymer is PMMA or PDMS.
In the preparation method, the adhesive includes one or more of aqueous LA-132, aqueous hydroxymethyl cellulose, aqueous styrene-butadiene emulsion, and oil-based polyvinylidene fluoride.
In the preparation method, the heat treatment temperature is 200-400 ℃ and the time is 1-3 hours.
By the technical scheme, the invention at least has the following advantages: according to the invention, the graphene oxide nano roll is used as a carrier matrix, and a carbon source is loaded on the surface of the graphene oxide nano roll, so that on one hand, more carbon sources can be loaded due to the larger interface area of the graphene oxide nano roll, and on the other hand, the graphene oxide nano roll has good mechanical properties, so that the stability in the denitrification process can be ensured, and a sufficient and stable carbon source can be provided for flora. The solid carbon source has large surface area, is beneficial to microorganism attachment and improves the utilization rate of the carbon source.
In conclusion, the special denitrification solid carbon source has good mechanical property and can effectively improve the denitrification rate. The method has the advantages and practical value, does not have similar design publication or use in the similar products and methods, is innovative, has great improvement on the method or the function, has great technical progress, produces good and practical effects, has multiple enhanced efficacies compared with the prior products, is more suitable for practical use, has industrial wide utilization value, and is a novel, improved and practical new design.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Dissolving 100g of polylactic acid in 50mL of dichloromethane, then dropwise adding a nitric acid solution (60 wt%), carrying out oxidation pretreatment at a temperature of not higher than 60 ℃, and then adjusting the pH value of the solution to 6-8 to obtain the modified polylactic acid. Uniformly dispersing graphene oxide nano sheets in deionized water, heating the obtained graphene oxide dispersion liquid in a water bath at 70 ℃ for 2 hours, then quickly immersing the graphene oxide dispersion liquid in liquid nitrogen until the graphene oxide dispersion liquid is completely frozen, and finally, obtaining the graphene nano roll through freeze drying. And then carrying out ultrasonic treatment on the graphene oxide nano roll in 100ml of aqueous solution containing 1 wt% of poly (diallyldimethylammonium chloride) for 3h, then filtering and carrying out vacuum drying at 50 ℃ for 12h to obtain the poly (diallyldimethylammonium chloride) -modified graphene oxide nano roll. Mixing the obtained modified polylactic acid and PMMA according to the mass ratio of 1: 2 to obtain a mixed solution, and then mixing the mixed solution, the water-based butylbenzene emulsion and the poly diallyl dimethyl ammonium chloride modified graphene oxide nano roll according to the mass ratio of 4: 2: 1 in THF and the mixture was stirred at room temperature under argon for 3h, after which the mixture was centrifuged and washed with THF and finally heat treated at 300 ℃ under argon for 2h to give the final product.
Example 2
Dissolving 100g of polylactic acid in 80mL of trichloromethane, then dropwise adding a nitric acid solution (60 wt%), carrying out oxidation pretreatment at a temperature of not higher than 60 ℃, and then adjusting the pH value of the solution to 6-8 to obtain the modified polylactic acid. Uniformly dispersing graphene oxide nano sheets in deionized water, heating the obtained graphene oxide dispersion liquid in a water bath at 70 ℃ for 2 hours, then quickly immersing the graphene oxide dispersion liquid in liquid nitrogen until the graphene oxide dispersion liquid is completely frozen, and finally, obtaining the graphene nano roll through freeze drying. And then carrying out ultrasonic treatment on the graphene oxide nano roll in 100ml of aqueous solution containing 1 wt% of poly (diallyldimethylammonium chloride) for 4 hours, then filtering and carrying out vacuum drying at 50 ℃ for 12 hours to obtain the poly (diallyldimethylammonium chloride) -modified graphene oxide nano roll. Mixing the obtained modified polylactic acid and PMMA according to the mass ratio of 1: 1 to obtain a mixed solution, and then mixing the mixed solution, a water system LA-132 and a poly diallyl dimethyl ammonium chloride modified graphene oxide nano roll according to a mass ratio of 4: 2: 1 in THF and the mixture was stirred at room temperature under argon for 2h, after which the mixture was centrifuged and washed with THF and finally heat treated at 400 ℃ under argon for 2h to give the final product.
Example 3
Dissolving 100g of polylactic acid in 100mL of dichloromethane, then dropwise adding a potassium permanganate solution (55 wt%) and carrying out oxidation pretreatment at a temperature of not higher than 60 ℃, and then adjusting the pH value of the solution to 6-8 to obtain the modified polylactic acid. Uniformly dispersing graphene oxide nano sheets in deionized water, heating the obtained graphene oxide dispersion liquid in water bath at 80 ℃ for 1h, then quickly immersing in liquid nitrogen until the graphene oxide dispersion liquid is completely frozen, and finally, obtaining the graphene nano roll through freeze drying. And then carrying out ultrasonic treatment on the graphene oxide nano roll in 100ml of aqueous solution containing 1 wt% of poly (diallyldimethylammonium chloride) for 4 hours, then filtering and carrying out vacuum drying at 40 ℃ for 24 hours to obtain the poly (diallyldimethylammonium chloride) -modified graphene oxide nano roll. And (3) mixing the obtained modified polylactic acid with PDMS according to the mass ratio of 1: 1.5 to obtain a mixed solution, and then mixing the mixed solution, water-based hydroxymethyl cellulose and poly diallyl dimethyl ammonium chloride modified graphene oxide nano-roll according to a mass ratio of 4: 2: 1 in THF and the mixture was stirred at room temperature under argon for 2h, after which the mixture was centrifuged and washed with THF and finally heat treated at 200 ℃ under argon for 4h to give the final product.
Example 4
Dissolving 100g of polylactic acid in 40mL of trichloromethane, then dripping a potassium permanganate solution (50 wt%) and carrying out oxidation pretreatment at a temperature of not higher than 60 ℃, and then adjusting the pH value of the solution to 6-8 to obtain the modified polylactic acid. Uniformly dispersing graphene oxide nano sheets in deionized water, heating the obtained graphene oxide dispersion liquid in a water bath at 70 ℃ for 3h, then quickly immersing the graphene oxide dispersion liquid in liquid nitrogen until the graphene oxide dispersion liquid is completely frozen, and finally, obtaining the graphene nano roll through freeze drying. And then carrying out ultrasonic treatment on the graphene oxide nano roll in 100ml of aqueous solution containing 1 wt% of poly (diallyldimethylammonium chloride) for 2h, then filtering and carrying out vacuum drying at 45 ℃ for 18h to obtain the poly (diallyldimethylammonium chloride) -modified graphene oxide nano roll. Mixing the obtained modified polylactic acid and PMMA according to the mass ratio of 1: 2 to obtain a mixed solution, and then mixing the mixed solution, the water-based butylbenzene emulsion and the poly diallyl dimethyl ammonium chloride modified graphene oxide nano roll according to the mass ratio of 4: 2: 1 in THF and the mixture was stirred at room temperature under argon for 3h, after which the mixture was centrifuged and washed with THF and finally heat treated at 300 ℃ under argon for 3h to give the final product.
Example 5
Dissolving 100g of polylactic acid in 60mL of dichloromethane, then dropwise adding a nitric acid solution (50 wt%), carrying out oxidation pretreatment at a temperature of not higher than 60 ℃, and then adjusting the pH value of the solution to 6-8 to obtain the modified polylactic acid. Uniformly dispersing graphene oxide nano sheets in deionized water, heating the obtained graphene oxide dispersion liquid in a water bath at 70 ℃ for 3h, then quickly immersing the graphene oxide dispersion liquid in liquid nitrogen until the graphene oxide dispersion liquid is completely frozen, and finally, obtaining the graphene nano roll through freeze drying. And then carrying out ultrasonic treatment on the graphene oxide nano roll in 100ml of aqueous solution containing 1 wt% of poly (diallyldimethylammonium chloride) for 2h, then filtering and carrying out vacuum drying at 45 ℃ for 24h to obtain the poly (diallyldimethylammonium chloride) -modified graphene oxide nano roll. And (3) mixing the obtained modified polylactic acid with PDMS according to the mass ratio of 1: 1 to obtain a mixed solution, and then mixing the mixed solution, water-based hydroxymethyl cellulose and poly diallyl dimethyl ammonium chloride modified graphene oxide nano-roll according to a mass ratio of 4: 2: 1 in THF and the mixture was stirred at room temperature under argon for 3h, after which the mixture was centrifuged and washed with THF and finally heat treated at 300 ℃ under argon for 3h to give the final product.
Application example
The solid carbon sources prepared in examples 1 to 5 were respectively added to the denitrification filter tank at a dosage of 8 kg/ton/hour, and the monitoring time was continued for 8 days after the addition. As for the control group, COD (mg/L) and TN (mg/L) indexes of effluent were measured respectively in the case of adding glucose as a carbon source, and the results are shown in Table 1.
TABLE 1 effluent COD (mg/L) and effluent TN (mg/L) indices
From the results in table 1, under the condition of the same inlet water, the COD of the outlet water of the denitrification filter added with the solid carbon source of the invention is obviously higher than that of the control group, and the TN of the outlet water is always lower than that of the total nitrogen of the outlet water of the control group. The solid carbon source of the invention releases COD mildly, has long duration and moderate dosage.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A method for preparing a denitrification solid carbon source, which comprises the following steps:
(1) dissolving polylactic acid in an organic solvent, then dropwise adding a strong oxidant solution, carrying out oxidation pretreatment at the temperature of not higher than 60 ℃, and then adjusting the pH of the solution to 6-8 to obtain modified polylactic acid;
(2) uniformly dispersing graphene oxide nanosheets in deionized water, heating the obtained graphene oxide dispersion liquid in a water bath, quickly immersing the graphene oxide dispersion liquid in liquid nitrogen until the graphene oxide dispersion liquid is completely frozen, finally, obtaining graphene nano rolls through freeze drying, carrying out ultrasonic treatment on the graphene oxide nano rolls in 100ml of aqueous solution containing 1 wt% of poly (diallyldimethylammonium chloride) for 2-4 hours, filtering and carrying out vacuum drying to obtain poly (diallyldimethylammonium chloride) -modified graphene oxide nano rolls;
(3) mixing the obtained modified polylactic acid and a polymer according to the mass ratio of 1: (1-2) and uniformly stirring to obtain a mixed solution, and then mixing the mixed solution, an adhesive and the poly (diallyldimethylammonium chloride) -modified graphene oxide nano roll according to a mass ratio of 4: 2: 1 in THF, stirring the mixture at room temperature for 2-4 hours under the protection of argon, centrifuging the mixture, washing the mixture with THF, and finally performing heat treatment under the protection of argon to obtain a final product.
2. The method according to claim 1, wherein the organic solvent is selected from dichloromethane or chloroform.
3. The preparation method according to claim 1, wherein the strong oxidant is selected from any one of nitric acid, sulfuric acid, potassium permanganate, or a mixed solution thereof.
4. The preparation method of claim 1, wherein the water bath heating temperature is 70-80 ℃ and the time is 1-3 h.
5. The preparation method according to claim 1, wherein the vacuum drying temperature is 40-50 ℃ and the time is 12-24 h.
6. The production method according to claim 1, wherein the polymer is PMMA or PDMS.
7. The method according to claim 1, wherein the binder comprises one or more of aqueous LA-132, aqueous hydroxymethylcellulose, aqueous styrene-butadiene emulsion, and oil-based polyvinylidene fluoride.
8. The method according to claim 1, wherein the heat treatment temperature is 200 to 400 ℃ and the time is 1 to 3 hours.
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| CN107841037A (en) * | 2016-09-20 | 2018-03-27 | 河南智联寰宇知识产权运营有限公司 | High adsorption polylactic acid composite biological membrane carrier materials and preparation method thereof |
| CN107141082A (en) * | 2017-05-24 | 2017-09-08 | 安徽恒海生态农业观光园有限公司 | A kind of vegetable cultivation is with the organic slow-release fertilizer that concave convex rod is major ingredient |
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