CN112619619A - Modified adsorption material for treating wastewater - Google Patents
Modified adsorption material for treating wastewater Download PDFInfo
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- CN112619619A CN112619619A CN202011424278.3A CN202011424278A CN112619619A CN 112619619 A CN112619619 A CN 112619619A CN 202011424278 A CN202011424278 A CN 202011424278A CN 112619619 A CN112619619 A CN 112619619A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28085—Pore diameter being more than 50 nm, i.e. macropores
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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
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
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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
- C02F2103/20—Nature of the water, waste water, sewage or sludge to be treated from animal husbandry
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Abstract
本案涉及一种用于处理废水的改性吸附材料，包括如下组分：50‑60份改性聚苯乙烯树脂、3‑6份生物菌群、0.5‑1份菌群保护剂、10‑15份絮凝剂和20‑30份无机填料。本发明设计一种改性聚苯乙烯树脂，其具有大孔树脂比表面积大的特点，具有较强的吸附能力，同时聚合物主干可降解，在水体中易水解成小分子，避免大分子聚合物残留而对环境造成二次污染；基于改性大孔吸附树脂添加生物菌群，少量生物菌群的使用达到净化水质的目的，同时由于量少，不会对水体造成富营养化；其它添加剂配合使用，能够更好的处理水产废水中的污染物，促进水体环境改善，实现水体环境的自然平衡。This case relates to a modified adsorption material for wastewater treatment, comprising the following components: 50-60 parts of modified polystyrene resin, 3-6 parts of biological flora, 0.5-1 part of flora protection agent, 10-15 parts of part flocculant and 20-30 parts inorganic filler. The present invention designs a modified polystyrene resin, which has the characteristics of large specific surface area of macroporous resin, strong adsorption capacity, and at the same time the polymer backbone is degradable, easily hydrolyzed into small molecules in water body, and avoids macromolecular polymerization. secondary pollution to the environment due to residues; adding biological flora based on modified macroporous adsorption resin, the use of a small amount of biological flora achieves the purpose of purifying water quality, and at the same time, due to the small amount, it will not cause eutrophication to the water body; other additives When used together, the pollutants in the aquatic wastewater can be better treated, the improvement of the water environment can be promoted, and the natural balance of the water environment can be achieved.
Description
Technical Field
The invention relates to the field of water treatment, in particular to a modified adsorbing material for treating wastewater.
Background
The fresh water resources in China are rich, the aquaculture amount is in the front of the world, but most of the aquaculture in China adopts closed water areas such as ponds, warehouses and the like, the self-purification capacity of the water is not as good as that of a living water source, and the eutrophication of the aquaculture water is caused by the application of a large amount of feed; the addition of the bactericide and the disinfectant and the accumulation of animal and plant corpses directly cause the accumulation of a large amount of organic matters, nitrogen and phosphorus in the water body, and the aquaculture wastewater not only causes damage to aquatic products, but also causes great harm to surrounding water areas and ecological environment.
At present, the general sewage treatment process is generally divided into three major categories, namely physical method, chemical method and biological method. With a single method, a good treatment effect is often difficult to achieve, and for aquaculture water, a water treatment agent remains in the water after use and can also cause harm to the health of fishes.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the degradable macroporous resin which is used as the adsorption material of the aquatic wastewater, has a good adsorption and catalysis function on pollutants in a water body, and can be degraded into small molecules after being treated for a period of time, so that the secondary pollution to the water body can be avoided.
In order to achieve the purpose, the invention provides the following technical scheme:
a modified adsorption material for treating wastewater comprises the following components: modified polystyrene resin, biological flora, a flora protective agent, a flocculating agent and inorganic filler; wherein the preparation process of the modified polystyrene resin comprises the following steps:
s1: adding azobisisobutyronitrile, styrene and divinylbenzene into a reaction bottle, uniformly mixing, adding toluene, heating to 45 ℃, adding 2-methylene-4-phenyl-1, 3-dioxolane, adding a dispersing agent and a dispersion medium while stirring, heating for reaction for a period of time, naturally cooling, centrifugally separating a product, collecting solids, fully washing with methanol, and drying to obtain polystyrene-ester microspheres;
s2: polystyrene-ester microspheres in CCl4Swelling for 3h, adding chlorosulfonic acid while stirring, reacting for 0.5-1h at 50-60 ℃, washing with ethanol and water in sequence after the reaction is finished, and drying to obtain the modified polystyrene resin.
Further, the reaction condition in the S1 is that the temperature is controlled to be 65-80 ℃, and the reaction time is 8-9 h.
Further, the mass ratio of the styrene, the azobisisobutyronitrile, the 2-methylene-4-phenyl-1, 3-dioxolane, the divinylbenzene and the toluene is 1:0.01: 0.5-1.5: 0.1: 0.1.
Further, the dispersing agent is polyvinylpyrrolidone or polyvinyl alcohol; the dispersion medium was methanol/water in a volume ratio of 80/20.
Further, the biological flora is selected from at least two mixed strains of bacillus subtilis, nitrobacteria, yeast, bacillus licheniformis or enterococcus faecalis.
Further, the flora protecting agent is selected from vitamin C, vitamin B1, vitamin B2, choline chloride, vitamin E or thiourea.
Further, the flocculant is selected from polymeric aluminum oxide, ferric sulfate, ferric polysilicate, aluminum chloride or polymeric aluminum sulfate.
Further, the inorganic filler is selected from at least three compositions of active carbon, diatomite, alunite, calcium hydrogen phosphate, sodium sulfite or magnesium sulfate.
Further, the weight parts of the components are as follows: 50-60 parts of modified polystyrene resin, 3-6 parts of biological flora, 0.5-1 part of flora protective agent, 10-15 parts of flocculating agent and 20-30 parts of inorganic filler.
The invention further provides a preparation method of the modified adsorbing material for treating wastewater, which comprises the following steps:
1) mixing the biological flora and the flora protective agent, crushing by using a micronizer, uniformly stirring, and storing for 10 days in a sealed and dark manner;
2) crushing the flocculating agent and the inorganic filler by using a micro-pulverizer, and uniformly mixing and stirring;
3) and (3) uniformly mixing and stirring the modified polystyrene resin, the step 1) and the step 2) to obtain the modified adsorbing material for treating the wastewater.
The macroporous resin can be prepared by utilizing styrene and divinylbenzene, has certain adsorption property due to the larger specific surface area, and can form van der Waals force with organic substances in a water body, so that the macroporous resin can be used as an adsorbent for sewage treatment. However, the density of benzene rings in the polymer chain is high, so that the adsorption capacity is limited, and the bonds between the polymer chain and adsorbates are easy to fall off; and the polystyrene resin has strong hydrophobicity, so that the polystyrene resin is unevenly dispersed in a water body, and the adsorption effect is weakened.
The invention also uses the cyclic ketene acetal (2-methylene-4-phenyl-1, 3-dioxolane) with benzene ring in the process of preparing the polystyrene macroporous adsorption resin, the cyclic ketene acetal monomer introduces ester group in the main chain of the polymer through the ring-opening polymerization of free radicals, and simultaneously keeps the existence of benzene ring in the side chain, thereby ensuring the adsorption characteristic of the macroporous resin; on one hand, the introduction of the ester group enables the main chain of the polymer to have degradability, and the polymer is easily degraded into small molecules after water treatment; on the other hand, the ester-based chain is inserted into the polymer backbone, so that the spacing between benzene rings on the backbone is effectively lengthened, the electron cloud density at the position is diluted, the steric hindrance caused by the aromatic ring is reduced, more space is made for combining adsorbates with larger volume, and the adsorbates are combined more firmly and are not easy to fall off; with introduction of an ester group in the fragment-COOCH2In CH (Ph), because carbon atoms in CH (Ph) are hybridized in sp3 mode, oxygen atoms in ester groups are closer to benzene rings, lone pair electrons in the oxygen atoms generate an induced electron supply effect on the benzene rings, so that sulfonation reaction at the para positions of the benzene rings is easier to occur, the sulfonation reaction is favorably completed under a milder reaction condition, and sulfonic groups are generated on the surfaces of resin microspheres, so that the hydrophilicity of the resin is effectively increased, the resin microspheres are convenient to disperse in a water body, and the adsorption performance is improved.
The biological flora is attached to the surface of the macroporous resin and can form a large microbial environment with indigenous microorganisms in a water body, thereby achieving the functions of purification and adsorption.
The flora protecting agent can improve the storage stability of the strains, increase the storage time and facilitate transportation.
The flocculating agent and the pollutants in the water body form flocculate, so that the cost is low and the flocculating effect is good.
Compared with the prior art, the invention has the beneficial effects that: the invention designs a modified polystyrene resin which has the characteristic of large specific surface area of macroporous resin, has strong adsorption capacity, and simultaneously the polymer backbone can be degraded and hydrolyzed into micromolecules in water, so that secondary pollution to the environment caused by residual macromolecular polymer is avoided; biological flora is added based on the modified macroporous adsorption resin, the purpose of purifying water quality is achieved by using a small amount of biological flora, and meanwhile, due to the small amount, eutrophication can not be caused to a water body; other additives are matched for use, so that pollutants in aquaculture wastewater can be better treated, the water environment is promoted to be improved, and the natural balance of the water environment is realized.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. 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.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1: a modified adsorption material for treating wastewater comprises the following components: 50 parts of modified polystyrene resin, 1 part of bacillus subtilis, 2 parts of nitrobacteria, 0.5 part of vitamin C, 10 parts of ferric sulfate and 20 parts of inorganic filler (the mass ratio of activated carbon to diatomite to alunite is 1:1: 1).
Example 2: a modified adsorption material for treating wastewater comprises the following components: 55 parts of modified polystyrene resin, 2 parts of nitrobacteria, 3 parts of yeast, 0.8 part of vitamin E, 12 parts of aluminum chloride and 25 parts of inorganic filler (the mass ratio of alunite, calcium hydrophosphate and sodium sulfite is 2:1: 1).
Example 3: a modified adsorption material for treating wastewater comprises the following components: 60 parts of modified polystyrene resin, 1 part of bacillus subtilis, 2 parts of bacillus licheniformis, 3 parts of enterococcus faecalis, 1 part of thiourea, 15 parts of ferric polysilicate and 30 parts of inorganic filler (the mass ratio of the diatomite, the alunite and the calcium hydrophosphate is 2:2: 1).
Wherein the preparation process of the modified polystyrene resin comprises the following steps:
s1: adding 0.01mol of azobisisobutyronitrile, 1mol of styrene and 0.1mol of divinylbenzene into a reaction bottle, uniformly mixing, adding 0.1mol of toluene, heating to 45 ℃, adding 1.5mol of 2-methylene-4-phenyl-1, 3-dioxolane (the synthesis method is shown in J.Org.Chem.,1978,43(14) and 2773), adding 20ml of polyvinylpyrrolidone and 130ml of methanol/water (the volume ratio is 80/20) while stirring, reacting for 8 hours, naturally cooling, centrifugally separating a product, collecting solids, fully washing and drying the solids by using methanol, and obtaining the polystyrene-ester microspheres;
s2: polystyrene-ester microspheres in CCl4Swelling for 3h, adding 0.2mol of chlorosulfonic acid while stirring, reacting for 1h at 50 ℃, washing with ethanol and water in sequence after the reaction is finished, and drying to obtain the modified polystyrene resin
Example 4: a modified adsorbing material for treating wastewater comprises the same components and using amount as in example 3, and is characterized in that the modified polystyrene resin is
S2 is absent in the preparation process.
Example 5: a modified adsorbing material for treating wastewater comprises the same components and using amount as in example 3, and is characterized in that the modified polystyrene resin is
The preparation process does not add 2-methylene-4-phenyl-1, 3-dioxolane.
Example 6: the components and the using amount of the modified adsorbing material for treating the wastewater are the same as those of example 3, and the difference is that the using amount of the 2-methylene-4-phenyl-1, 3-dioxolane in the preparation of the modified polystyrene resin is 1 mol.
Example 7: the components and the using amount of the modified adsorbing material for treating the wastewater are the same as those of example 3, and the difference is that the using amount of the 2-methylene-4-phenyl-1, 3-dioxolane in the preparation of the modified polystyrene resin is 0.5 mol.
The modified adsorbent materials for treating wastewater of examples 1 to 6 were prepared by the following steps:
1) mixing the biological flora and the flora protective agent, crushing by using a micronizer, uniformly stirring, and storing for 10 days in a sealed and dark manner;
2) crushing the flocculating agent and the inorganic filler by using a micro-pulverizer, and uniformly mixing and stirring;
3) and (3) uniformly mixing and stirring the modified polystyrene resin, the step 1) and the step 2) to obtain the modified adsorbing material for treating the aquaculture wastewater.
The application comprises the following steps: diluting the prepared wastewater adsorbing material with water, and uniformly splashing the wastewater adsorbing material on the surface of a water body to be treated, wherein the water body is sprayed on every 1000m310g of the adsorbent described in examples 1 to 6 was used in aquaculture wastewater, and the treatment was described as application examples 1 to 6.
Detecting COD value and ammonia nitrogen concentration (NH) before and after treatment3-N), Total Phosphorus (TP) and total solids concentration (SS), the removal of each was calculated and reported in table 1.
TABLE 1
| COD value | NH3-N | TP | SS | |
| Application example 1 | 92.5％ | 94.1％ | 94.5％ | 90.2％ |
| Application example 2 | 93.8％ | 95.8％ | 95.1％ | 91.0％ |
| Application example 3 | 95.1％ | 97.2％ | 96.6％ | 91.9％ |
| Application example 4 | 80.1％ | 82.5％ | 82.2％ | 85.3％ |
| Application example 5 | 82.1％ | 81.5％ | 82.0％ | 83.2％ |
| Application example 6 | 88.4％ | 89.3％ | 90.1％ | 88.6％ |
| Application example 7 | 86.9％ | 88.1％ | 88.8％ | 85.3％ |
From the above table, the adsorption material of the present invention has a good treatment effect on aquaculture wastewater, and the treatment effect of application example 4 is poor, because the modified polystyrene resin is not subjected to sulfonation reaction, the resin exhibits strong hydrophobicity, and has poor dispersibility in water, resulting in weak adsorption force; compared with application examples 1-3 and application examples 5-7, the introduction of the ester group can effectively lengthen the distance between the benzene rings on the main chain, reduce steric hindrance, and make more space for combining adsorbates with larger volume, so that the adsorbates are combined more firmly and are not easy to fall off.
The modified polystyrene resins prepared in examples 3 and 5 to 7 were further subjected to degradation test determination, three 10ml portions of wastewater to be treated were taken, 10mg of modified polystyrene resin was added thereto and stirred uniformly, then the mixture was left to stand, ten days later, samples were taken to test the molecular weight of the modified polystyrene resin, and the degradation rates were calculated, the degradation rates of examples 3 and 5 to 7 were 92%, 10%, 80% and 68%, respectively, example 3 was able to degrade into small molecules in water, whereas the molecular weights of the polymers after degradation of examples 6 and 7 were still large, which may cause secondary pollution to water, and example 5 was only a small portion of molecular weight falling off and could not be degraded well.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (9)
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Cited By (2)
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| CN115180677A (en) * | 2022-07-26 | 2022-10-14 | 厦门钨业股份有限公司 | Tungsten wastewater treatment method |
| CN116119833A (en) * | 2022-11-29 | 2023-05-16 | 嘉兴沃特泰科环保科技股份有限公司 | Nutrient for water recovery system and preparation method and application thereof |
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Effective date of registration: 20240531 Address after: 523000 Room 302, Building 1, No. 115, Guangma Avenue, Machong Town, Dongguan City, Guangdong Province Patentee after: DONGGUAN XINHE ENVIRONMENTAL PROTECTION EQUIPMENT Co.,Ltd. Country or region after: China Address before: Yangzhou Vocational and Technical College of industry, Chahe street, Hanjiang District, Yangzhou City, Jiangsu Province Patentee before: YANGZHOU POLYTECHNIC INSTITUTE Country or region before: China |