CN114409850B - Antibacterial water purifying agent and preparation method thereof - Google Patents
Antibacterial water purifying agent and preparation method thereof Download PDFInfo
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- CN114409850B CN114409850B CN202210125049.4A CN202210125049A CN114409850B CN 114409850 B CN114409850 B CN 114409850B CN 202210125049 A CN202210125049 A CN 202210125049A CN 114409850 B CN114409850 B CN 114409850B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 239000012629 purifying agent Substances 0.000 title claims abstract description 73
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
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- 125000002091 cationic group Chemical group 0.000 claims abstract description 46
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- 238000003756 stirring Methods 0.000 claims abstract description 32
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 239000003999 initiator Substances 0.000 claims abstract description 21
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- LBSPZZSGTIBOFG-UHFFFAOYSA-N bis[2-(4,5-dihydro-1h-imidazol-2-yl)propan-2-yl]diazene;dihydrochloride Chemical compound Cl.Cl.N=1CCNC=1C(C)(C)N=NC(C)(C)C1=NCCN1 LBSPZZSGTIBOFG-UHFFFAOYSA-N 0.000 claims description 8
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- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 claims description 4
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 3
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- RRHXZLALVWBDKH-UHFFFAOYSA-M trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)C RRHXZLALVWBDKH-UHFFFAOYSA-M 0.000 claims description 2
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- 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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- 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
- C02F1/5263—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to the technical field of water purification treatment, and particularly discloses a bacteriostatic water purifying agent and a preparation method thereof. The preparation method of the antibacterial water purifying agent comprises the following steps: s1, dissolving chitosan in an acetic acid aqueous solution, stirring, and then adding a sodium tripolyphosphate aqueous solution for ultrasonic treatment to obtain a nano chitosan solution; s2, adding acrylamide, a cationic monomer, a template agent, a bacteriostatic agent and an additive into the nano chitosan solution, stirring, then introducing nitrogen, adding an initiator for sealing, placing in an ultraviolet light initiating device for radiation reaction, standing after the completion of the radiation reaction, washing a product, drying and crushing to obtain the bacteriostatic water purifying agent. The technical scheme has the advantages of simple preparation process and high raw material utilization rate, and the prepared water purifying agent has the dual functions of flocculation and bacteriostasis, and has good market prospect.
Description
Technical Field
The invention relates to the technical field of water purification treatment, in particular to a bacteriostatic water purifying agent and a preparation method thereof.
Background
The water resource is an important substance resource of the natural ecological system and is also an important basic substance resource for supporting the development of the human economic and social system. Along with the acceleration of the industrialization process, a large amount of sewage is directly or indirectly discharged into rivers, lakes and seas, so that fresh water is seriously polluted. The water purifying agent is an important fine chemical product and has important effect in purifying industrial sewage and domestic wastewater. The large-scale use of the water purifying agent not only provides a large amount of clean drinking water and industrial and agricultural water for human beings, greatly relieves the harm of polluted water bodies to the environment, but also effectively maintains the balance of an ecological system.
The production and development processes of the domestic and foreign water purifying agents are comprehensively observed, and the development trend is from low molecular weight to high molecular weight, single type to compound type, and single function to multiple functions. The water purifying agent can be mainly used for removing suspended matters in water, deodorizing and decolorizing, inhibiting bacteria and killing bacteria, softening water quality, reducing scale formation, reducing the damage of raw water to equipment and the like. According to the functional characteristics, the water purifying agent can be divided into flocculating agent, bactericide, scale inhibitor, adsorbent, corrosion inhibitor and the like. In the face of various water bodies with complex conditions, a plurality of water purifying agents are often required to be added to meet the purifying requirement. The commonly used water purifying agents include aluminum salt water treatment agents, synthetic organic polymer water treatment agents mainly comprising polyacrylamide and the like, and have the advantages of small addition amount, large flocs, small influence on water quality and the like, but the post-treatment is difficult, and potential safety hazards exist for aquatic organisms and human health. Therefore, the development direction of the future water purifying agent is green, efficient and multifunctional, and the water purifying agent has one or more functions of bacteriostasis/sterilization, scale inhibition, corrosion inhibition and the like while meeting the basic function of flocculation.
A wide variety of microorganisms are widely distributed in nature, and harmful bacteria in the microorganisms can not only prevent industrial and agricultural production, but also cause serious threat to human health. Water is a material resource for human living, and is relevant to human life, and harmful bacteria in water can directly enter human bodies along with water to cause harm to the human bodies. In water treatment, particularly drinking water treatment processes, microorganisms such as bacteria in water and suspended impurity particles are the target contaminants that are primarily removed in water treatment processes. Therefore, the development of the safe, efficient and bacteriostatic water purifying agent capable of simultaneously removing main target pollutants in water is one of the important directions of the current water treatment agent research.
The invention patent with application number 201811286940.6 discloses a novel particle nano water purifying agent and a preparation method thereof, and the novel particle nano water purifying agent is prepared from the following components in detail: 30-60 parts of modified diatomite, 10-30 parts of bentonite, 10-30 parts of polyaluminium chloride, 5-10 parts of plant bacteriostat, 5-10 parts of dispersing agent, 10-20 parts of expanding agent, 10-20 parts of matrix, 10-20 parts of divinyl sulfone and 10-20 parts of polyacrylamide. The preparation method comprises the following steps: firstly, weighing modified diatomite, putting the modified diatomite into a beaker, adding polyaluminium chloride, a dispersing agent and an extender, and performing ultrasonic treatment; step two, putting the solution into a heating and stirring device, and heating and stirring the solution into paste; adding divinyl sulfone, bentonite and polyacrylamide into the paste, uniformly stirring, and drying in a vacuum drying oven; and fourthly, grinding the dried material into powder, adding the powder into a matrix, uniformly stirring, injecting the mixture into a designated die, and heating the mixture in a muffle furnace. Although the application has a certain water purifying effect, the raw materials are various, the preparation process is complex, the production cost is high, and the adopted plant bacteriostatic agent is only one or a mixture of more than one of the eupatorium adenophorum stems and leaves, moringa seeds, mugwort leaves and aloe, so that the bacteriostatic effect is poor, and the bacteriostatic requirement of the water purifying agent cannot be met.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a bacteriostatic water purifying agent and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
chitosan is a polysaccharide obtained by deacetylation of a natural polymer compound extracted from shells of crustaceans such as shrimps and crabs, and is used as a rich natural organic resource, and has the advantages of no harm to the environment, biodegradability and easiness in chemical modification. Researches show that some natural high molecular compounds such as chitosan, lignin, starch and the like have flocculation and bacteriostasis functions to a certain extent, but the natural organic compounds have weak bacteriostasis/flocculation functions, so that the water treatment requirement is difficult to reach. Compared with starch, the molecular main chain of chitosan contains rich amino, hydroxyl and other functional groups, and the chitosan can promote the absorption of impurities through complexation effect and hydrogen bond to perform adsorption flocculation and can utilize a large amount of amino structures to perform inhibition/sterilization. However, the application of chitosan is limited due to the problems of relatively low molecular weight, weak electropositivity and the like. Therefore, the invention utilizes amino and hydroxyl in chitosan molecules to prepare the water purifying agent with micro-block structure and double functions of bacteriostasis and flocculation through free radical initiated grafting.
The preparation method of the antibacterial water purifying agent comprises the following steps:
s1, dissolving 0.3-0.8 part by weight of chitosan into 20-50 parts by weight of acetic acid aqueous solution with the volume fraction of 0.5-1.5v/v%, and stirring at the room temperature for 15-30min at the speed of 300-500rpm to obtain chitosan solution;
s2, adding 2-5 parts by weight of acrylamide, 1-3 parts by weight of cationic monomer, 0.2-0.8 part by weight of bacteriostat and 0.1-0.3 part by weight of additive into the chitosan solution, stirring at 500-800rpm for 10-20min at room temperature, then introducing nitrogen to purge for 10-20min, adding 0.01-0.05 part by weight of initiator, immediately sealing, placing into an ultraviolet light initiating device, wherein the radiation power is 100-150W, the dominant wavelength is 300-400nm, and the average light intensity is 1000-1500 mu W/cm 3 And (3) carrying out ultraviolet radiation reaction for 90-150min, standing for 1-3h after finishing, washing the product with absolute ethyl alcohol and acetone for 2-5 times, drying at 50-70 ℃ for 20-30h, and crushing to obtain the antibacterial water purifying agent.
Further, the preparation method of the antibacterial water purifying agent comprises the following steps:
s1, dissolving 0.3-0.8 part by weight of chitosan into 20-50 parts by weight of acetic acid aqueous solution with the volume fraction of 0.5-1.5v/v%, stirring at the room temperature at the speed of 300-500rpm for 15-30min, then adding 4-7 parts by weight of sodium tripolyphosphate aqueous solution with the mass fraction of 1-3wt%, and carrying out ultrasonic treatment for 3-8min at the ultrasonic power of 150-300W and the ultrasonic frequency of 15-30kHz to obtain a nano chitosan solution;
s2, adding 2-5 parts by weight of acrylamide, 1-3 parts by weight of cationic monomer, 0.2-0.8 part by weight of bacteriostat and 0.1-0.3 part by weight of additive into the nano chitosan solution, stirring at 500-800rpm for 10-20min at room temperature, then introducing nitrogen to purge for 10-20min, adding 0.01-0.05 part by weight of initiator, immediately sealing, placing into an ultraviolet light initiating device, wherein the radiation power is 100-150W, the dominant wavelength is 300-400nm, and the average light intensity is 1000-1500 mu W/cm 3 And (3) carrying out ultraviolet radiation reaction for 90-150min, standing for 1-3h after finishing, washing the product with absolute ethyl alcohol and acetone for 2-5 times, drying at 50-70 ℃ for 20-30h, and crushing to obtain the antibacterial water purifying agent.
Chitosan is a cationic polysaccharide, and after being mixed with a polyvalent polyanion crosslinking agent, intermolecular and/or intramolecular crosslinking can rapidly occur to form nano chitosan; after the chitosan is prepared into nano chitosan particles, the unique size effect of the nano material can be utilized, and the physicochemical property and antibacterial property of the chitosan can be obviously improved while the excellent property of the chitosan is maintained.
According to the invention, positively charged chitosan and negatively charged sodium tripolyphosphate are mixed together, and the positively charged chitosan and the negatively charged sodium tripolyphosphate are automatically gelled to form nano chitosan particles with a large number of amino groups on the surfaces, the surfaces of the nano chitosan contain a large number of amino groups, nucleophilic substitution reaction can be carried out with cationic monomers, the nano chitosan is grafted on the molecular chain of the cationic monomers, the molecular weight of the water purifying agent is increased, and the formation of adsorption flocs is facilitated; meanwhile, as the nano chitosan is a weak cationic flocculant, the nano chitosan shows stronger electropositivity after being grafted with a cationic monomer, and is easier to generate the electric neutralization effect so as to destabilize and settle the pollutant colloid, thereby achieving the purpose of purifying water.
Further, the preparation method of the antibacterial water purifying agent comprises the following steps:
s1, dissolving 0.3-0.8 part by weight of chitosan into 20-50 parts by weight of acetic acid aqueous solution with the volume fraction of 0.5-1.5v/v%, stirring at the room temperature at the speed of 300-500rpm for 15-30min, then adding 4-7 parts by weight of sodium tripolyphosphate aqueous solution with the mass fraction of 1-3wt%, and carrying out ultrasonic treatment for 3-8min at the ultrasonic power of 150-300W and the ultrasonic frequency of 15-30kHz to obtain a nano chitosan solution;
s2, adding 2-5 parts by weight of acrylamide, 1-3 parts by weight of cationic monomer, 1-3 parts by weight of template agent, 0.2-0.8 part by weight of bacteriostat and 0.1-0.3 part by weight of additive into the nano chitosan solution, stirring at the room temperature at the speed of 500-800rpm for 10-20min, then introducing nitrogen to purge for 10-20min, adding 0.01-0.05 part by weight of initiator and immediately sealing, placing into an ultraviolet light initiating device, wherein the radiation power is 100-150W, the dominant wavelength is 300-400nm, and the average light intensity is 1000-1500 mu W/cm 3 And (3) carrying out ultraviolet radiation reaction for 90-150min, standing for 1-3h after finishing, washing the product with absolute ethyl alcohol and acetone for 2-5 times, drying at 50-70 ℃ for 20-30h, and crushing to obtain the antibacterial water purifying agent.
The template agent is sodium polyacrylate.
The template agent-sodium polyacrylate is added, and mainly probably because the sodium polyacrylate can be used as an anion template, the sodium polyacrylate is firstly subjected to pre-adsorption with a strong quaternary ammonium group in a cation monomer-nucleophilic reagent molecular chain through electrostatic attraction, and is directionally arranged along the template molecular chain to form an association body, and after the polymerization reaction is started, the continuous adjacent cation monomers are easy to preferentially undergo a synthetic reaction, so that a micro-block structure with continuous adjacent cation units in a polymer molecule is generated, and a copolymer with a cation block structure is obtained, and further, the charge density and positive charge utilization rate are improved, and the electric neutralization performance is enhanced; meanwhile, after nucleophilic substitution with bacitracin, bacitracin can be orderly combined on a molecular chain, so that the density of bacitracin in the water purifying agent is improved, and the antibacterial performance of the water purifying agent is further improved.
According to the invention, the sodium polyacrylate is added as the template agent, so that the ordered and concentrated arrangement of the cationic monomers can be promoted, the utilization rate of the cationic monomers is improved, the dosage of the cationic monomers is reduced, the cost is saved, the electrostatic adsorption area between a molecular chain and sewage colloid particles can be increased, the adsorption acting force is enhanced, the floc strength of the water purifying agent is improved, the quantity of bacitracin on a macromolecular chain in the water purifying agent is increased, and the antibacterial performance of the water purifying agent is promoted. In addition, the concentrated arrangement of the cationic monomers ensures that the electrostatic repulsive force between cationic blocks on molecular chains is stronger, so that the high molecular long chains of the water purifying agent are more linear and stretched in configuration in aqueous solution, thereby being beneficial to adsorbing and combining more colloid particles and bacteria, enhancing the bridging effect and improving flocculation and bacteriostasis effects.
The cationic monomer is any one of dimethyl diallyl ammonium chloride, methacryloxyethyl trimethyl ammonium chloride and acryloxyethyl trimethyl ammonium chloride.
Preferably, the cationic monomer is acryloyloxyethyl trimethyl ammonium chloride.
The bacteriostat is bacitracin.
Bacitracin is a polypeptide antibiotic, is mainly a small peptide substance separated from special Lei Suku bacillus subtilis and bacillus licheniformis, has stable structure and high temperature resistance, has higher efficiency in bacteriostasis, has broad-spectrum antibacterial activity on various bacteria, has strong killing effect on fungi, pathogens, viruses with envelopes, tumor cells and the like, has higher inhibitory activity, has no toxic effect on normal cells, and is not easy to cause the target strain to generate drug resistance. Bacitracin has a similar antimicrobial spectrum as compared with penicillin, and has a strong bactericidal effect on both gram-negative and gram-positive bacteria.
The additive is one or more of linseed oil, ethylene glycol butyl ether, polyether F-68, sodium dodecyl benzene sulfonate and cetyltrimethylammonium bromide.
Preferably, the additive is a mixture of ethylene glycol butyl ether and polyether F-68, wherein the mass ratio of the ethylene glycol butyl ether to the polyether F-68 is (1-3): (2-5).
The ethylene glycol butyl ether and the polyether F-68 are nonionic surfactants, do not ionize in aqueous solution, have high stability, are not easy to be influenced by other additives and acid-base salts, and the ether bond can play a role in chain transfer in polymerization reaction, promote the growth of polymer chains, increase the molecular weight of the water purifying agent and promote the formation of adsorption flocs. The ethylene glycol butyl ether has low molecular weight, can rapidly enter water, increases monomer activity and collision probability, promotes rapid reaction, can promote large liquid drops to be small liquid drops, forms a protective film to be attached to the surfaces of nano chitosan particles, prevents nano chitosan from being aggregated due to the change of the reaction process of a homogeneous system, promotes uniform and stable grafting of the nano chitosan on a polymer molecular chain, and further promotes the improvement of the antibacterial performance of the water purifying agent; the polyoxyethylene chain contained in the polyether F-68 can be intertwined with the polymer molecular chain and attached to the polymer molecular chain, so that the solubility of the polymer is improved, the bridging effect can be achieved, and the flocculation and bacteriostasis effects of the water purifying agent are improved.
The initiator is any one of azo diiso Ding Mi hydrochloride VA-044, potassium persulfate, azo diisobutyronitrile and azo diisobutyl amidine V-50.
The invention has the beneficial effects that: according to the invention, chitosan and sodium tripolyphosphate are reacted by utilizing an ionic gel method to prepare nano chitosan, then the nano chitosan is mixed with monomer-acrylamide, a cationic monomer template agent, a bacteriostat and an additive, the ordered and concentrated arrangement of the cationic monomers is promoted under the action of the template agent, then nucleophilic substitution reaction is carried out between amino groups on the nano chitosan and bacitracin and electrophilic reagent-cationic monomers under the action of an initiator, the grafting of the chitosan and bacitracin on molecular chains of the cationic monomers is promoted, then the free radical polymerization reaction is carried out on quaternary ammonium groups on acrylamide and nucleophilic monomers through ultraviolet irradiation, and the nano chitosan, bacitracin and cationic polyacrylamide are successfully grafted to obtain the bacteriostat. The technical scheme has the advantages of simple preparation process and high raw material utilization rate, and the prepared water purifying agent has the dual functions of flocculation and bacteriostasis, and has good market prospect.
Detailed Description
The above summary of the present invention is described in further detail below in conjunction with the detailed description, but it should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
Introduction of some of the raw materials in this application:
chitosan, CAS number: 9012-76-4, degree of deacetylation: 95% by Shaanxi Xinkang biotechnology Co.
Sodium polyacrylate, molecular weight: 2000-5000, model: derin 42N, offered by Pingxian Delin New Material technologies Co.
Bacitracin, CAS no: 1405-87-4, activity: 60U/mg, supplied by Shanghai Jizhui Biochemical technology Co., ltd.
Polyether F-68, CAS number: 9003-11-6, supplied by Jiangsu province sea-An petrochemical plant.
Example 1
The preparation method of the antibacterial water purifying agent comprises the following steps:
s1, dissolving 0.5 part by weight of chitosan into 30 parts by weight of acetic acid aqueous solution with volume fraction of 1v/v%, and stirring at room temperature at 400rpm for 20min to obtain chitosan solution;
s2, will 3 weight percentAdding acrylamide, 1.5 parts by weight of cationic monomer, 0.5 part by weight of bacteriostat and 0.15 part by weight of additive into the chitosan solution, stirring at 600rpm for 15min at room temperature, then introducing nitrogen for purging for 15min, adding 0.03 part by weight of initiator, immediately sealing, placing into an ultraviolet light initiating device, wherein the radiation power is 125W, the dominant wavelength is 365nm, and the average light intensity is 1200 mu W/cm 3 And (3) carrying out ultraviolet radiation reaction for 120min, standing for 2h after finishing, washing the product with absolute ethyl alcohol and acetone for 3 times, drying at 60 ℃ for 24h, and crushing to obtain the antibacterial water purifying agent.
The cationic monomer is dimethyl diallyl ammonium chloride.
The bacteriostat is bacitracin.
The additive is polyether F-68.
The initiator is azo diiso Ding Mi hydrochloride VA-044.
Example 2
The preparation method of the antibacterial water purifying agent comprises the following steps:
s1, dissolving 0.5 part by weight of chitosan into 30 parts by weight of acetic acid aqueous solution with volume fraction of 1v/v%, stirring at room temperature at 400rpm for 20min, then adding 5 parts by weight of sodium tripolyphosphate aqueous solution with mass fraction of 2.0wt%, and performing ultrasonic treatment at ultrasonic power of 200W and ultrasonic frequency of 20kHz for 5min to obtain a nano chitosan solution;
s2, adding 3 parts by weight of acrylamide, 1.5 parts by weight of cationic monomer, 0.5 part by weight of bacteriostat and 0.15 part by weight of additive into the nano chitosan solution, stirring at room temperature for 15min at 600rpm, then introducing nitrogen to purge for 15min, adding 0.03 part by weight of initiator and immediately sealing, placing into an ultraviolet light initiating device, wherein the radiation power is 125W, the dominant wavelength is 365nm, and the average light intensity is 1200 mu W/cm 3 And (3) carrying out ultraviolet radiation reaction for 120min, standing for 2h after finishing, washing the product with absolute ethyl alcohol and acetone for 3 times, drying at 60 ℃ for 24h, and crushing to obtain the antibacterial water purifying agent.
The cationic monomer is dimethyl diallyl ammonium chloride.
The bacteriostat is bacitracin.
The additive is polyether F-68.
The initiator is azo diiso Ding Mi hydrochloride VA-044.
Example 3
The preparation method of the antibacterial water purifying agent comprises the following steps:
s1, dissolving 0.5 part by weight of chitosan into 30 parts by weight of acetic acid aqueous solution with volume fraction of 1v/v%, stirring at room temperature at 400rpm for 20min, then adding 5 parts by weight of sodium tripolyphosphate aqueous solution with mass fraction of 2.0wt%, and performing ultrasonic treatment at ultrasonic power of 200W and ultrasonic frequency of 20kHz for 5min to obtain a nano chitosan solution;
s2, adding 3 parts by weight of acrylamide, 1.5 parts by weight of cationic monomer, 0.5 part by weight of bacteriostat and 0.15 part by weight of additive into the nano chitosan solution, stirring at room temperature for 15min at 600rpm, then introducing nitrogen to purge for 15min, adding 0.03 part by weight of initiator and immediately sealing, placing into an ultraviolet light initiating device, wherein the radiation power is 125W, the dominant wavelength is 365nm, and the average light intensity is 1200 mu W/cm 3 And (3) carrying out ultraviolet radiation reaction for 120min, standing for 2h after finishing, washing the product with absolute ethyl alcohol and acetone for 3 times, drying at 60 ℃ for 24h, and crushing to obtain the antibacterial water purifying agent.
The cationic monomer is acryloyloxyethyl trimethyl ammonium chloride.
The bacteriostat is bacitracin.
The additive is polyether F-68.
The initiator is azo diiso Ding Mi hydrochloride VA-044.
Example 4
The preparation method of the antibacterial water purifying agent comprises the following steps:
s1, dissolving 0.5 part by weight of chitosan into 30 parts by weight of acetic acid aqueous solution with volume fraction of 1v/v%, stirring at room temperature at 400rpm for 20min, then adding 5 parts by weight of sodium tripolyphosphate aqueous solution with mass fraction of 2.0wt%, and performing ultrasonic treatment at ultrasonic power of 200W and ultrasonic frequency of 20kHz for 5min to obtain a nano chitosan solution;
s2, 3 parts by weight of acrylamide and 1.5 parts by weight of sunAdding an ionic monomer, 1.8 parts by weight of a template agent, 0.5 part by weight of a bacteriostat and 0.15 part by weight of an additive into the nano chitosan solution, stirring at 600rpm for 15min at room temperature, then introducing nitrogen to purge for 15min, adding 0.03 part by weight of an initiator, immediately sealing, placing in an ultraviolet light initiating device, wherein the radiation power is 125W, the dominant wavelength is 365nm, and the average light intensity is 1200 mu W/cm 3 And (3) carrying out ultraviolet radiation reaction for 120min, standing for 2h after finishing, washing the product with absolute ethyl alcohol and acetone for 3 times, drying at 60 ℃ for 24h, and crushing to obtain the antibacterial water purifying agent.
The cationic monomer is acryloyloxyethyl trimethyl ammonium chloride.
The template agent is sodium polyacrylate.
The bacteriostat is bacitracin.
The additive is polyether F-68.
The initiator is azo diiso Ding Mi hydrochloride VA-044.
Example 5
The preparation method of the antibacterial water purifying agent comprises the following steps:
s1, dissolving 0.5 part by weight of chitosan into 30 parts by weight of acetic acid aqueous solution with volume fraction of 1v/v%, stirring at room temperature at 400rpm for 20min, then adding 5 parts by weight of sodium tripolyphosphate aqueous solution with mass fraction of 2.0wt%, and performing ultrasonic treatment at ultrasonic power of 200W and ultrasonic frequency of 20kHz for 5min to obtain a nano chitosan solution;
s2, adding 3 parts by weight of acrylamide, 1.5 parts by weight of cationic monomer, 1.8 parts by weight of template agent, 0.5 part by weight of bacteriostat and 0.15 part by weight of additive into the nano chitosan solution, stirring at 600rpm for 15min at room temperature, then introducing nitrogen to purge for 15min, adding 0.03 part by weight of initiator, immediately sealing, placing into an ultraviolet light initiating device, wherein the radiation power is 125W, the dominant wavelength is 365nm, and the average light intensity is 1200 mu W/cm 3 And (3) carrying out ultraviolet radiation reaction for 120min, standing for 2h after finishing, washing the product with absolute ethyl alcohol and acetone for 3 times, drying at 60 ℃ for 24h, and crushing to obtain the antibacterial water purifying agent.
The cationic monomer is acryloyloxyethyl trimethyl ammonium chloride.
The template agent is sodium polyacrylate.
The bacteriostat is bacitracin.
The additive is ethylene glycol butyl ether.
The initiator is azo diiso Ding Mi hydrochloride VA-044.
Example 6
The preparation method of the antibacterial water purifying agent comprises the following steps:
s1, dissolving 0.5 part by weight of chitosan into 30 parts by weight of acetic acid aqueous solution with volume fraction of 1v/v%, stirring at room temperature at 400rpm for 20min, then adding 5 parts by weight of sodium tripolyphosphate aqueous solution with mass fraction of 2.0wt%, and performing ultrasonic treatment at ultrasonic power of 200W and ultrasonic frequency of 20kHz for 5min to obtain a nano chitosan solution;
s2, adding 3 parts by weight of acrylamide, 1.5 parts by weight of cationic monomer, 1.8 parts by weight of template agent, 0.5 part by weight of bacteriostat and 0.15 part by weight of additive into the nano chitosan solution, stirring at 600rpm for 15min at room temperature, then introducing nitrogen to purge for 15min, adding 0.03 part by weight of initiator, immediately sealing, placing into an ultraviolet light initiating device, wherein the radiation power is 125W, the dominant wavelength is 365nm, and the average light intensity is 1200 mu W/cm 3 And (3) carrying out ultraviolet radiation reaction for 120min, standing for 2h after finishing, washing the product with absolute ethyl alcohol and acetone for 3 times, drying at 60 ℃ for 24h, and crushing to obtain the antibacterial water purifying agent.
The cationic monomer is acryloyloxyethyl trimethyl ammonium chloride.
The template agent is sodium polyacrylate.
The bacteriostat is bacitracin.
The additive is a mixture of ethylene glycol butyl ether and polyether F-68, wherein the mass ratio of the ethylene glycol butyl ether to the polyether F-68 is 2:3.
The initiator is azo diiso Ding Mi hydrochloride VA-044.
Test example 1
Escherichia coli is a representative bacterium of the genus Escherichia and is transmitted to people through food, drinking water and other routes, and once it invades the inside of the human body, it causes intestinal infection, diarrhea, vomiting, cholecystitis and other diseases.
Antibacterial performance test: the method comprises the following specific steps:
(1) Preparation of E.coli suspension: weighing 25.0g of LB agar powder, dissolving in 1.0L of distilled water, regulating the pH to 7, transferring into an conical flask, sterilizing at 121 ℃ for 15min, cooling at room temperature for standby, adding Escherichia coli (E.coli) (CMCC 44102) bacterial liquid, and culturing for 12 hours under shaking at 37 ℃; centrifuging the Escherichia coli suspension at 3000rpm for 5min, standing to remove supernatant, washing the rest bottom bacterial liquid with pure water for 3 times, and diluting and dispersing with 0.9wt% physiological saline to obtain 1×l0 7 CFU/mL of Escherichia coli suspension;
(2) The antibacterial water purifying agent prepared in each example is respectively weighed and dissolved in distilled water to prepare 1.0g/L antibacterial water purifying agent mother liquor;
(3) Taking 100mL of the escherichia coli suspension prepared in the step (1), adding 3mL of the antibacterial water purifying agent mother liquor prepared in the step (2), stirring for 3min at a rotating speed of 200r/min, stirring for 10min at a rotating speed of 40r/min, standing for 30min, and extracting the supernatant from a position 1cm below the liquid surface by using a syringe for testing; wherein the blank group only contains the escherichia coli suspension prepared in the step (1); each group of experiments was performed 5 times in parallel and the average was taken;
(4) The bactericidal effect of the antibacterial water purifying agent on escherichia coli is measured by measuring the Optical Density (OD) in the supernatant after the reaction 600 ) Analyzing; the light transmittance (T) of the supernatant after the reaction was measured at 600nm using a TU-1901 type double beam ultraviolet spectrophotometer, and since LB agar in the blank group had an effect on the optical density, the relative optical density was calculated using the relative optical density, and the OD was used 600 The specific numerical value is a value obtained by subtracting a blank control, and the calculation formula is as follows: OD (optical density) 600 ＝lg(1/T)。
Wherein T represents the light transmittance at 600nm in the supernatant after the reaction minus the light transmittance at the place of the blank control.
Table 1 results of antibacterial property test
| Relative optical density OD 600 | |
| Example 1 | 0.906 |
| Example 2 | 0.721 |
| Example 3 | 0.578 |
| Example 4 | 0.192 |
| Example 5 | 0.185 |
| Example 6 | 0.130 |
The above results show that the antibacterial effect of example 2 is more remarkable than that of example 1, probably because the nano chitosan has better solubility than that of chitosan, and the amino groups on the surface of the nano chitosan are more compact after grafting with cationic monomers, so that the antibacterial effect is better. The bacteriostatic effect of example 3 is superior to that of example 2, and is mainly probably due to the fact that the cationic monomer-acryloyloxyethyl trimethyl ammonium chloride in example 3 shows better water solubility and reactivity than the cationic monomer-dimethyldiallyl ammonium chloride in example 2, the free radical reaction efficiency is high, the quantity of quaternary ammonium salt is increased, and the bacteriostatic performance is promoted. Compared with the embodiment 3, the template agent is used in the embodiment 4, the antibacterial effect is obviously improved, and the addition of the template agent can not only promote the orderly and concentrated arrangement of the cationic monomers and improve the utilization rate of the cationic monomers, so that the electrostatic repulsive force effect among cationic blocks on molecular chains is stronger, the configuration of a high molecular long chain of the water purifying agent in an aqueous solution is more linear and stretched, the adsorption and the combination of more bacteria are facilitated, the bridging effect is enhanced, the quantity of bacitracin on the high molecular chain in the water purifying agent is increased, and the improvement of the antibacterial performance of the water purifying agent is jointly promoted. Compared with the single additive used in the embodiments 4 and 5, the embodiment 6 adopts ethylene glycol butyl ether and polyether F-68 together as the additive, so that not only can the uniform and stable grafting of nano chitosan on a polymer molecular chain be promoted, but also the nano chitosan and the polymer molecular chain are mutually entangled and attached to the polymer molecular chain, the solubility of the polymer is improved, and the nano chitosan can also play a bridging role, so that a layer of powder bread can be formed on the surface of bacteria, the energy exchange of substances inside and outside the cells is hindered, the normal metabolism of the bacteria is influenced, and the antibacterial performance of the water purifying agent is promoted.
Test example 2
The kaolin belongs to aluminosilicate with a double-layer structure, waste water containing kaolin particles has high water turbidity and small particle size, is in a stable dispersion state in water, is difficult to settle and separate, and can cause pollution of surrounding water and influence on agricultural production and waste of a large amount of water resources if directly discharged.
Flocculation performance test: the method comprises the following specific steps:
(1) 1.0g of the dried kaolin particles was weighed and dissolved in 1.0L of distilled water to obtain a simulated kaolin suspension with a mass fraction of 0.1 wt%;
(2) The antibacterial water purifying agent prepared in each example is respectively weighed and dissolved in distilled water to obtain 1.0g/L antibacterial water purifying agent mother liquor;
(3) Taking 100mL of the 0.1wt% simulated kaolin suspension prepared in the step (1), regulating the pH to 5, adding 3mL of the antibacterial water purifier mother liquor prepared in the step (2), stirring for 3min at a rotating speed of 200r/min, stirring for 10min at a rotating speed of 40r/min, standing for 30min, and extracting the supernatant from a position 1cm below the liquid surface by using a syringe for testing; each group of experiments was performed 5 times in parallel and the average was taken;
(4) Turbidity measurement was performed with a 2100Q-type nephelometer, and the supernatant turbidity after flocculation (T i ) Simulated kaolin turbidity before flocculation (T 0 ) The percent residual turbidity (RT%) was calculated as follows: RT (%) =t i /T 0 ×100％。
TABLE 2 flocculation performance test results
| Percent turbidity remaining (RT%) (%) | |
| Example 1 | 17.57 |
| Example 2 | 11.83 |
| Example 3 | 7.96 |
| Example 4 | 1.64 |
| Example 5 | 1.55 |
| Example 6 | 1.32 |
The kaolin surface has negative charge lattice points and is electronegative as a whole, and the antibacterial water purifying agent prepared by the invention belongs to a cationic water purifying agent, so that the antibacterial water purifying agent has a relatively excellent water purifying effect. Compared with example 1, the flocculation performance of example 2 is obviously improved, probably because the nano chitosan has better dissolution performance, long linear molecular chains of the nano chitosan are easier to stretch, after the nano chitosan is grafted with a cationic monomer, the steric hindrance of the molecular chains is increased, the nano chitosan is easier to stretch, and the flocculation performance is improved. The flocculation effect of example 3 is superior to that of example 2, and is mainly probably due to the fact that the cationic monomer-acryloyloxyethyl trimethyl ammonium chloride in example 3 shows better water solubility and reactivity than the cationic monomer-dimethyldiallyl ammonium chloride in example 2, the free radical reaction efficiency is high, the cationic degree in the main chain is further improved, the electropositivity of the water purifying agent is improved, and the water purifying agent has stronger electric neutralization effect with the electronegative kaolin suspension, so that the flocculation performance of the water purifying agent is improved. Compared with example 3, the preparation of example 4 introduces the template agent, and the flocculation effect is greatly improved, probably because the introduction of the template agent promotes the orderly and centralized arrangement of the cationic monomers, so that the electrostatic repulsive force effect among the cationic blocks on the molecular chains is stronger, the configuration of the high molecular long chains of the water purifying agent in the aqueous solution is more linear and stretched, the specific surface area is increased, the void distribution range is wide, the bridging effect is enhanced, the adsorption and net patch-scanning capacity of kaolin is facilitated, and the improvement of the flocculation effect is promoted. In example 6, ethylene glycol butyl ether and polyether F-68 are used as additives together, and compared with the single additives in examples 4 and 5, the flocculation performance of the water purifying agent is improved, and the flocculation performance of the water purifying agent is improved due to the fact that the ethylene glycol butyl ether and the polyether F-68 are mainly used together.
Claims (6)
1. The preparation method of the antibacterial water purifying agent is characterized by comprising the following steps of:
s1, dissolving chitosan in an acetic acid aqueous solution, stirring, and then adding a sodium tripolyphosphate aqueous solution for ultrasonic treatment to obtain a nano chitosan solution;
s2, adding acrylamide, a cationic monomer, a template agent, a bacteriostatic agent and an additive into the nano chitosan solution, stirring, then introducing nitrogen, adding an initiator, immediately sealing, placing in an ultraviolet initiating device for ultraviolet radiation reaction, standing after finishing, washing, drying and crushing the product to obtain a bacteriostatic water purifying agent;
the cationic monomer is any one of dimethyl diallyl ammonium chloride, methacryloxyethyl trimethyl ammonium chloride and acryloxyethyl trimethyl ammonium chloride;
the bacteriostat is bacitracin;
the template agent is sodium polyacrylate;
the additive is ethylene glycol butyl ether, polyether F-68 or a mixture of the two.
2. The method for preparing the bacteriostatic water purifier according to claim 1, which comprises the following steps:
s1, dissolving 0.3-0.8 part by weight of chitosan into 20-50 parts by weight of acetic acid aqueous solution with the volume fraction of 0.5-1.5v/v%, stirring at the room temperature at the speed of 300-500rpm for 15-30min, then adding 4-7 parts by weight of sodium tripolyphosphate aqueous solution with the mass fraction of 1-3wt%, and carrying out ultrasonic treatment for 3-8min to obtain a nano chitosan solution;
s2, adding 2-5 parts by weight of acrylamide, 1-3 parts by weight of cationic monomer, 1-3 parts by weight of template agent, 0.2-0.8 part by weight of bacteriostat and 0.1-0.3 part by weight of additive into the nano chitosan solution, stirring at the room temperature at 500-800rpm for 10-20min, then introducing nitrogen to purge for 10-20min, adding 0.01-0.05 part by weight of initiator, immediately sealing, placing into an ultraviolet light initiating device, ultraviolet radiation reacting for 90-150min, standing for 1-3h after finishing, washing the product with absolute ethyl alcohol and acetone for 2-5 times, drying at 50-70 ℃ for 20-30h, and crushing to obtain the bacteriostasis water purifying agent.
3. The method for preparing a bacteriostatic water purifier according to claim 1 or 2, characterized in that the ultrasonic treatment process parameters in step S1 are as follows: ultrasonic power 150-300W and ultrasonic frequency 15-30kHz.
4. The method for preparing a bacteriostatic water purifier according to claim 1 or 2, characterized in that the process parameters of the ultraviolet radiation reaction in step S2 are as follows: the radiation power is 100-150W, the dominant wavelength is 300-400nm, and the average light intensity is 1000-1500 mu W/cm 3 。
5. The method for preparing a bacteriostatic water purifier according to claim 1 or 2, wherein the initiator is any one of azobisisobutyronitrile, azobisisobutylamino amidine V-50, potassium persulfate, and azobisisobutylamino hydrochloride VA-044.
6. A bacteriostatic water purifier prepared by the method of any one of claims 1-5.
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