CN112023894A - Sewage treatment additive and preparation method thereof - Google Patents
Sewage treatment additive and preparation method thereof Download PDFInfo
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- CN112023894A CN112023894A CN202010868347.3A CN202010868347A CN112023894A CN 112023894 A CN112023894 A CN 112023894A CN 202010868347 A CN202010868347 A CN 202010868347A CN 112023894 A CN112023894 A CN 112023894A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Biodiversity & Conservation Biology (AREA)
- Microbiology (AREA)
- Water Treatment By Sorption (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The scheme relates to a sewage treatment additive and a preparation method thereof, and the additive suitable for sewage treatment is prepared by utilizing a series of acidification, acylation and esterification reactions of carbon nano tubes and cellulose. The invention has moderate cost, simple preparation process and good operability; the carbon nano tube/cellulose compound provided by the invention is used as an additive of a water treatment agent, so that the decolorization and COD removal rate can be effectively improved, and the sedimentation rate is increased; can be used as a carrier of microbial flora to further improve the sterilization and antibacterial performance of the microbial agent; the sewage treatment agent with different functions can be formed by adding functional components according to the pollution degree of the wastewater, and the application range is wide.
Description
Technical Field
The invention relates to the field of sewage treatment, in particular to a sewage treatment additive and a preparation method thereof.
Background
Water resources are the premise on which the human society lives and are directly related to the sustainable development of the society. However, with the rapid development of our society, the urbanization process is accelerated continuously, and the scale is also enlarged remarkably. The problems are obvious, industrial wastewater, medical wastewater, urban wastewater, agricultural wastewater and the like are generated in large quantities, water resource pollution is increasingly serious, and physical and psychological health and living environment of people are seriously influenced.
The currently used methods for treating wastewater mainly comprise: physical separation method, biological degradation method and chemical decomposition method, but the methods have certain limitations, and the biological method has long treatment time, slow speed and low efficiency; the physical method has high treatment cost and incomplete treatment; the chemical method is usually added with more chemical substances, is easy to cause secondary pollution to water and is not beneficial to sustainable development. Therefore, there is a need to develop a water treatment material which is efficient, environment-friendly, economical and free from secondary pollution, and can improve the water treatment effect to meet the purpose of higher sewage discharge standard.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to utilize the carbon nano tube and the cellulose to carry out serial modification and apply the carbon nano tube and the cellulose to sewage treatment so as to achieve the aims of fast adsorption and sedimentation and reducing COD (chemical oxygen demand) and chroma.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a sewage treatment additive comprises the following steps:
1): modification of carbon nanotubes: placing Carbon Nano Tubes (CNT) in a mixed solution of sulfuric acid and nitric acid for ultrasonic dispersion for 1h, then refluxing in a water bath at 80 ℃ for 4h, filtering, washing until the filtrate is neutral, drying, and grinding to obtain acidified carbon nano tubes; placing the acidified carbon nanotubes in SOCl2Performing ultrasonic treatment for 0.5h, stirring and refluxing for 2h at 80 ℃ under the action of DMF, filtering, cleaning with acetone, drying, and grinding to obtain the carbon nanotube chloride; placing the acyl chlorinated carbon nano tube into a reaction bottle, adding toluene/tetrahydrofuran, performing ultrasonic treatment to uniformly disperse the carbon nano tube, then adding polyethylene glycol and triethylamine, performing nitrogen protection on a mixed system, stirring and reacting for 48 hours at 80 ℃, filtering, washing with water and ethanol, drying, and grinding to obtain polyethylene glycol-carbon nano tube PEG-CNTs.
2): modification of cellulose: adding carboxymethyl cellulose (CMC) into a dimethyl sulfoxide DMSO solvent, adding a catalyst, stirring for 30 minutes at 50 ℃, then adding long-chain alkyl acyl chloride and pyridine, and reacting for 2 hours at 90 ℃ to obtain the long-chain alkyl grafted carboxymethyl cellulose.
3): dissolving the long-chain alkyl grafted carboxymethyl cellulose in dichloromethane, adding 20% of N, N' -Dicyclohexylcarbodiimide (DCC), and stirring for 2 hours by blowing nitrogen; adding the polyethylene glycol-carbon nano tube into a reaction bottle, adding dichloromethane solution, performing ultrasonic treatment to uniformly disperse the polyethylene glycol-carbon nano tube, adding 10% of 4-Dimethylaminopyridine (DMAP), introducing nitrogen, dropwise adding the dichloromethane solution of the long-chain alkyl grafted carboxymethyl cellulose at normal temperature, stirring for 48 hours at normal temperature after dropwise adding, and filtering, cleaning, drying and grinding the mixture after the reaction is finished to obtain the modified carbon nano tube/cellulose composite CNTs-CMC.
Preferably, in the preparation method, the solution volume ratio of the mixed solution of sulfuric acid and nitric acid is 3: 1.
Preferably, in the preparation method, the molecular weight of the polyethylene glycol is 1000-4000 g/mol.
Preferably, in the preparation method, the catalyst is p-toluenesulfonic acid TSA.
Preferably, in the preparation method, the long-chain alkyl acyl chloride is C12～C14Straight chain acid chlorides of (1).
A sewage treatment additive prepared by the method.
Compared with the prior art, the invention has the beneficial effects that: the invention has moderate cost, simple preparation process and good operability; the carbon nano tube/cellulose compound provided by the invention is used as an additive of a water treatment agent, so that the decolorization and COD removal rate can be effectively improved, and the sedimentation rate is increased; can be used as a carrier of microbial flora to further improve the sterilization and antibacterial performance of the microbial agent; the sewage treatment agent with different functions can be formed by adding functional components according to the pollution degree of the wastewater, and the application range is wide.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and 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.
S1: modification of carbon nanotubes:
a) putting 10g CNT in 200mL mixed solution of sulfuric acid and nitric acid (v/v 3:1), ultrasonically dispersing for 1h, refluxing in 80 ℃ water bath for 4h, filtering, repeatedly washing with a large amount of deionized water and acetone until the filtrate is neutral, drying, and grinding to obtain acidified carbon nano tubes;
b) placing the acidified carbon nanotubes in 200mL of SOCl2Performing ultrasonic treatment for 0.5h, stirring and refluxing for 2h at 80 ℃ under the action of DMF, filtering, cleaning with acetone, drying, and grinding to obtain the carbon nanotube chloride;
c) placing the acyl chlorinated carbon nano tube into a reaction bottle, adding 100mL of toluene/tetrahydrofuran, performing ultrasonic treatment to uniformly disperse the carbon nano tube, then adding polyethylene glycol and 10mL of triethylamine with equal mass, performing nitrogen protection on a mixed system, stirring and reacting at 80 ℃ for 48 hours, filtering, washing with water and ethanol, drying, and grinding to obtain the polyethylene glycol-carbon nano tube PEG-CNTs.
The surface of the carbon nano tube is a porous structure, and has stronger adsorption capacity due to the structural particularity, but the practical application of the carbon nano tube is limited due to the poor dispersibility of the carbon nano tube, so researchers usually modify the surface of the carbon nano tube to improve the dispersibility.
S2: modification of cellulose: 10g of carboxymethyl cellulose is added into 200mL of DMSO solvent, 10mL of p-toluenesulfonic acid is added, stirring is carried out at 50 ℃ for 30 minutes, and then long-chain alkyl acyl chloride and 5mL of pyridine with equal mass are added, and reaction is carried out at 90 ℃ for 2 hours to obtain long-chain alkyl grafted carboxymethyl cellulose.
In general water purifying agents, cellulose is usually added as a flocculating agent, the cellulose is a natural polymer, a large number of reactive hydroxyl groups exist in a molecular chain, and long-chain hydrocarbon groups are usually grafted on the surface of the cellulose to increase the hydrophobicity of the cellulose in a chemical reaction so as to improve the surface activity of the cellulose.
According to the invention, the carbon nano tube and the cellulose are modified and skillfully connected through esterification reaction, so that the dispersibility of the carbon nano tube is increased, the surface activity of the cellulose is increased, and the modified product can adsorb a large amount of organic matters in sewage treatment to achieve the purposes of removing COD and reducing chroma.
S3: dissolving the long-chain alkyl grafted carboxymethyl cellulose in dichloromethane, adding 20% of DCC, and stirring for 2 hours by blowing nitrogen; adding the polyethylene glycol-carbon nano tube into a reaction bottle, adding dichloromethane solution, performing ultrasonic treatment to uniformly disperse the polyethylene glycol-carbon nano tube, adding 10% DMAP, introducing nitrogen, dropwise adding the dichloromethane solution of the long-chain alkyl grafted carboxymethyl cellulose at normal temperature, stirring for 48 hours at normal temperature after dropwise adding, and filtering, cleaning, drying and grinding the mixture after the reaction is finished to obtain the modified carbon nano tube/cellulose composite CNTs-CMC.
The compound contains a large amount of hydroxyl groups, ether groups and hydrocarbon groups, and the hydrophilic and oleophilic groups are used for demulsifying oil-water pollutants in water, so that flocculation and precipitation of harmful substances are facilitated, the pollutants are prevented from floating upwards, and the adsorption and sedimentation rate is high; meanwhile, the carbon nano tube with a porous structure and a nano size can also be used as a carrier of microbial flora, and a microbial agent is added into the water treatment agent to have a synergistic effect with the water treatment agent, so that the performance of degerming and antibiosis can be greatly improved.
The embodiment of the invention further discloses a sewage treatment agent prepared by mixing the carbon nano tube/cellulose composite additive prepared by the method, and the sewage treatment agent comprises the following raw materials in parts by weight: 8-15 parts of CNTs-CMC, 30-45 parts of flocculant, 3-5 parts of microbial agent and 6-13 parts of adsorbent.
When in use, the sewage treatment agent is uniformly scattered in the secondary sedimentation tank water after biochemical treatment according to the adding amount of 100mg/L, stirred for 1 minute at 80-140r/min and then kept stand, and various performance parameters before and after treatment are tested.
Further, the flocculating agent is selected from one or more of cationic polyacrylamide, aluminum sulfate and polymeric ferric sulfate.
Further, the adsorbent is selected from one or more of bentonite, diatomite or activated carbon.
Example 1: the weight fractions of the components are as follows: 8 parts of CNTs-CMC, 20 parts of cationic polyacrylamide, 5 parts of aluminum sulfate, 10 parts of polymeric ferric sulfate, 3 parts of microbial agent and 6 parts of diatomite.
Example 2: the weight fractions of the components are as follows: 11 parts of CNTs-CMC, 8 parts of diatomite, 22 parts of cationic polyacrylamide, 15 parts of aluminum sulfate and 3 parts of microbial agent.
Example 3: the weight fractions of the components are as follows: 13 parts of CNTs-CMC, 10 parts of diatomite, 25 parts of cationic polyacrylamide, 13 parts of polymeric ferric sulfate and 4 parts of microbial agent.
Example 4: the weight fractions of the components are as follows: 15 parts of CNTs-CMC, 13 parts of diatomite, 28 parts of cationic polyacrylamide, 8 parts of aluminum sulfate and 5 parts of microbial agent.
Comparative example 1: the weight fractions of the components are as follows: 10 parts of diatomite, 3 parts of bentonite, 28 parts of cationic polyacrylamide, 8 parts of aluminum sulfate and 5 parts of microbial agent.
As shown in the data in Table 1, the CNTs-CMC is added into the water treatment agent, so that the adsorption capacity can be effectively improved, the effect of rapid sedimentation is achieved, meanwhile, the COD removal rate and the decolorization rate are further improved, and the carbon nano tube with the nano structure can be used as a carrier of microbial flora, so that the antibacterial and bactericidal capacity of the microbial agent is effectively improved.
TABLE 1
While the invention has been described above with reference to an embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the various features of the embodiments disclosed herein may be used in any combination, provided that there is no structural conflict, and the combinations are not exhaustively described in this specification merely for the sake of brevity and conservation of resources. Therefore, it is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (6)
1. The preparation method of the sewage treatment additive is characterized by comprising the following steps:
1): modification of carbon nanotubes: placing the carbon nano tube in a mixed solution of sulfuric acid and nitric acid, performing ultrasonic dispersion for 1h, then refluxing in a water bath at the temperature of 80 ℃ for 4h, filtering, washing until the filtrate is neutral, drying, and grinding to obtain an acidified carbon nano tube; it was placed in SOCl2Performing ultrasonic treatment for 0.5h, stirring and refluxing for 2h at 80 ℃ under the action of DMF, filtering, cleaning with acetone, drying, and grinding to obtain the carbon nanotube chloride; placing the acyl chlorinated carbon nano tube into a reaction bottle, adding toluene/tetrahydrofuran, performing ultrasonic treatment to uniformly disperse the carbon nano tube, then adding polyethylene glycol and triethylamine, performing nitrogen protection on a mixed system, stirring and reacting for 48 hours at 80 ℃, filtering, washing with water and ethanol, drying, and grinding to obtain the polyethylene glycol-carbon nano tube.
2): modification of cellulose: adding carboxymethyl cellulose into a dimethyl sulfoxide solvent, adding a catalyst, stirring for 30 minutes at 50 ℃, then adding long-chain alkyl acyl chloride and pyridine, and reacting for 2 hours at 90 ℃ to obtain the long-chain alkyl grafted carboxymethyl cellulose.
3): dissolving the long-chain alkyl grafted carboxymethyl cellulose in dichloromethane, adding 20% of N, N' -dicyclohexylcarbodiimide, and stirring for 2 hours by blowing nitrogen; adding the polyethylene glycol-carbon nano tube into a reaction bottle, adding dichloromethane solution, performing ultrasonic treatment to uniformly disperse the polyethylene glycol-carbon nano tube, adding 10% of 4-dimethylaminopyridine, introducing nitrogen, dropwise adding the dichloromethane solution of the long-chain alkyl grafted carboxymethyl cellulose at normal temperature, stirring for 48 hours at normal temperature after dropwise adding, filtering, washing, drying and grinding to obtain the modified carbon nano tube/cellulose composite.
2. The method for preparing an additive for sewage treatment according to claim 1, wherein the solution volume ratio of the mixed solution of sulfuric acid and nitric acid is 3: 1.
3. The method for preparing sewage treatment additive according to claim 1, wherein the molecular weight of the polyethylene glycol is 1000-4000 g/mol.
4. The method of claim 1, wherein the catalyst is p-toluenesulfonic acid.
5. The method of claim 1, wherein the long-chain hydrocarbyl acid chloride is C12～C14Straight chain acid chlorides of (1).
6. A sewage treatment additive prepared by the preparation method according to any one of claims 1 to 5.
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| CN202010868347.3A CN112023894B (en) | 2020-08-26 | 2020-08-26 | Sewage treatment additive and preparation method thereof |
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| CN202010868347.3A CN112023894B (en) | 2020-08-26 | 2020-08-26 | Sewage treatment additive and preparation method thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1563211A (en) * | 2004-04-15 | 2005-01-12 | 上海交通大学 | Nano carbon tube grafted with super branched polymer synthesized in situ and preparation method |
| CN101215361A (en) * | 2008-01-16 | 2008-07-09 | 青岛大学 | Method for preparing graft polymer containing carbon nano-tube |
| CN101239714A (en) * | 2008-03-06 | 2008-08-13 | 广州大学 | Ethoxyl cellulose-carbon nano-tube derivatives and preparation method thereof |
| CN102942810A (en) * | 2012-11-21 | 2013-02-27 | 太原理工大学 | Surface modification method for carbon nano tube |
| CN105289527A (en) * | 2015-12-03 | 2016-02-03 | 南京林业大学 | Preparation method of cellulose ester aerogel material for adsorbing organic matters in wastewater |
| WO2018028365A1 (en) * | 2016-08-09 | 2018-02-15 | 翁秋梅 | Dynamic polymer with hybrid cross-linked network and application thereof |
-
2020
- 2020-08-26 CN CN202010868347.3A patent/CN112023894B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1563211A (en) * | 2004-04-15 | 2005-01-12 | 上海交通大学 | Nano carbon tube grafted with super branched polymer synthesized in situ and preparation method |
| CN101215361A (en) * | 2008-01-16 | 2008-07-09 | 青岛大学 | Method for preparing graft polymer containing carbon nano-tube |
| CN101239714A (en) * | 2008-03-06 | 2008-08-13 | 广州大学 | Ethoxyl cellulose-carbon nano-tube derivatives and preparation method thereof |
| CN102942810A (en) * | 2012-11-21 | 2013-02-27 | 太原理工大学 | Surface modification method for carbon nano tube |
| CN105289527A (en) * | 2015-12-03 | 2016-02-03 | 南京林业大学 | Preparation method of cellulose ester aerogel material for adsorbing organic matters in wastewater |
| WO2018028365A1 (en) * | 2016-08-09 | 2018-02-15 | 翁秋梅 | Dynamic polymer with hybrid cross-linked network and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| MARGARET J. SOBKOWICZ ET AL.: ""Decorating in green: surface esterification of carbon and cellulosic nanoparticles"", 《GREEN CHEM.》 * |
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