CN113396931A - Composite disinfectant and preparation method thereof - Google Patents

Composite disinfectant and preparation method thereof Download PDF

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Publication number
CN113396931A
CN113396931A CN202110621850.3A CN202110621850A CN113396931A CN 113396931 A CN113396931 A CN 113396931A CN 202110621850 A CN202110621850 A CN 202110621850A CN 113396931 A CN113396931 A CN 113396931A
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parts
titanium dioxide
silver
nano silver
composite
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袁树东
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Shanghai Lanyu Water Treatment Co ltd
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Shanghai Lanyu Water Treatment Co ltd
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16—Heavy metals; Compounds thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/02—Sulfur; Selenium; Tellurium; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
    • A61L2/08—Radiation
    • A61L2/088—Radiation using a photocatalyst or photosensitiser
    • 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
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • 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
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/42—Nature of the water, waste water, sewage or sludge to be treated from bathing facilities, e.g. swimming pools
    • 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

Abstract

The invention belongs to the technical field of disinfection, and particularly relates to a composite disinfectant and a preparation method thereof, wherein the composite disinfectant comprises the following components in parts by weight: 50-70 parts of calcium hypochlorite, 2-10 parts of a sodium phosphate compound, 5-10 parts of potassium hydrogen peroxymonosulfate, 8-15 parts of a nano silver-titanium dioxide compound and 2-10 parts of an auxiliary agent; the preparation method comprises the following steps: uniformly mixing calcium hypochlorite, a sodium phosphate compound and potassium peroxymonosulfate, adding a nano silver-titanium dioxide compound, stirring, adding an auxiliary agent while stirring until all components are uniformly mixed to obtain the composite disinfectant; this application is through multiunit material collaborative adjustment in the compound disinfectant, can realize a large amount of effective chlorine outputs to effective chlorine stability is high, and the bactericidal ability is strong.

Description

Composite disinfectant and preparation method thereof
Technical Field
The invention belongs to the technical field of disinfection, and particularly relates to a compound disinfectant and a preparation method thereof.
Background
The disinfection of the swimming pool generally adopts a chemical agent, ultraviolet rays, ozone or metal ions disinfection mode, wherein the chemical agent disinfection has the defects of toxic hazard of the disinfection agent to human bodies, narrow range of disinfection objects, difficult treatment after disinfection and the like;
the ultraviolet disinfection has the defects that a certain water flow thickness must be kept for the disinfected swimming pool, and the maintenance cost of the disinfected equipment is high;
ozone disinfection has the defects of high power consumption of equipment, damage to human bodies caused by excessive use, poor treatment effect of ozone on algae and red line worms and need of synergistic reaction of chlorine series medicaments;
metal ion sterilization has the disadvantage of high sterilization cost.
At present, the latest technology adopted in the domestic swimming pool disinfection stage is a disinfectant formed by combining photocatalytic reaction and silver ions, for example CN201410617021.8, a form of a bactericidal composition consisting of nano titanium dioxide and silver-loaded activated carbon is adopted, and the advantages of good heat resistance, wide antibacterial spectrum and effective period of the nano titanium dioxide high surface activity and the silver-loaded activated carbon are respectively utilized to realize harmless sterilization and disinfection of the swimming pool.
Disclosure of Invention
In view of the above problems, the present invention has been made to provide a composite disinfectant and a method for preparing the same, which overcome or at least partially solve the above problems.
The embodiment of the invention provides a composite disinfectant, which comprises the following components in parts by weight: 50-70 parts of calcium hypochlorite, 2-10 parts of a sodium phosphate compound, 5-10 parts of potassium hydrogen peroxymonosulfate, 8-15 parts of a nano silver-titanium dioxide compound and 2-10 parts of an auxiliary agent.
Optionally, the nano silver-titanium dioxide composite comprises, by weight, 2-10 parts of silver, 60-80 parts of titanium dioxide and 10-15 parts of alumina.
Optionally, the particle size of the silver is 10-15nm, the particle size of the titanium dioxide is 5-20nm, and the particle size of the aluminum oxide is 5-15 nm.
Optionally, the nano silver-titanium dioxide composite is prepared by a sol-gel method, and the sol-gel method further comprises the following steps:
mixing tetrabutyl titanate and isopropanol, and adding an isopropanol aqueous solution into the mixed solution to prepare titanium dioxide powder;
obtaining a silver ammonia solution, adding the silver ammonia solution into a mixed solution of tetrabutyl titanate and isopropanol, and preparing mixed powder of nano silver and titanium dioxide;
adding alumina powder into the prepared titanium dioxide powder and the mixed powder, uniformly mixing, and then jointly and finely grinding to obtain the nano silver-titanium dioxide composite.
Optionally, the auxiliary agent is at least one of potassium dihydrogen phosphate, ferric chloride, aluminum chloride, polyaluminium sulfate, polyferric chloride and polyferric sulfate; furthermore, the auxiliary agent comprises 20-25 parts by weight of polyaluminium sulfate and 2-5 parts by weight of polyferric sulfate.
Optionally, the calcium hypochlorite is sodium-method calcium hypochlorite.
Based on the same inventive concept, the embodiment of the invention also provides a preparation method of the composite disinfectant, which comprises the following steps:
uniformly mixing calcium hypochlorite, a sodium phosphate compound and potassium hydrogen peroxymonosulfate, adding the nano silver-titanium dioxide compound, stirring, adding the auxiliary agent while stirring until all the components are uniformly mixed, and thus obtaining the composite disinfectant.
One or more technical solutions in the embodiments of the present invention have at least the following technical effects or advantages:
the embodiment of the invention provides a composite disinfectant, which comprises the following components in parts by weight: 50-70 parts of calcium hypochlorite, 2-10 parts of a sodium phosphate compound, 5-10 parts of potassium hydrogen peroxymonosulfate, 8-15 parts of a nano silver-titanium dioxide compound and 2-10 parts of an auxiliary agent; by using calcium hypochlorite as a main disinfecting substance and potassium monopersulfate as an auxiliary material, under the condition that the effective chlorine content is 68-70% (w/w), in the titanium dioxide photocatalysis process, the transferred electrons are transferred to other substances for reaction, for example, in the process that the calcium hypochlorite reacts to generate chloride ions or chlorine gas, the transferred electrons accelerate the reaction of the hypochlorite ions, so that the hypochlorite ions in the calcium hypochlorite react to generate the chlorine gas or form the chloride ions, and a part of the added nano silver is converted into silver ions with bactericidal capability, and the other part of the added nano silver forms silver chloride precipitates with the excessive chloride ions, thereby preventing the formation of the excessive chloride or silver ions, and simultaneously, the silver ions and the chloride ions react to further accelerate the reaction of the calcium hypochlorite, and the calcium hypochlorite can form scales such as calcium carbonate and the like in the reaction stage, the photocatalysis process is influenced, active groups in molecules are adsorbed on active points on the surface of calcium carbonate by adding a sodium phosphate compound, the growth of calcium carbonate crystals is slowed down, a large amount of crystals are kept in a microcrystalline state, so that the permeability of the whole water body is increased, the smooth proceeding of the photocatalysis process is further ensured, and the reaction process of calcium hypochlorite is accelerated.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
It should be noted that like reference numerals and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
FIG. 1 is a flow chart of the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying a relative importance or order.
In order to solve the technical problems, the general idea of the embodiment of the application is as follows:
according to a typical embodiment of the present invention, there is provided a composite disinfectant, comprising, in parts by weight: 50-70 parts of calcium hypochlorite, 2-10 parts of a sodium phosphate compound, 5-10 parts of potassium hydrogen peroxymonosulfate, 8-15 parts of a nano silver-titanium dioxide compound and 2-10 parts of an auxiliary agent.
The calcium hypochlorite is used as a main disinfecting and sterilizing component to generate effective chlorine substances capable of disinfecting and sterilizing, and the reason for controlling the weight part of the calcium hypochlorite to be 50-70 parts is that the calcium hypochlorite generates the largest amount of effective chlorine and generates the smallest amount of chloride ions and generated calcium carbonate in the component interval, and when the weight part of the calcium hypochlorite is too large, although more effective chlorine components are generated, the formed calcium carbonate is too much and is easy to precipitate into a swimming pool, so that the titanium dioxide photocatalyst stage reaction in the nano silver-titanium dioxide compound is easily influenced, and the final disinfecting and sterilizing effect is influenced; when the weight part of the calcium hypochlorite is too small, the generation of effective chlorine components is reduced, the disinfection effect is not obvious, the titanium dioxide photocatalysis process in the further nano silver-titanium dioxide compound is intensified, the nano silver-titanium dioxide compound can well play a role in sterilization, but a large amount of generated free radicals and electrons cannot be consumed, so that the nano silver-titanium dioxide compound reacts with an auxiliary agent or potassium hydrogen peroxymonosulfate to cause the internal consumption of the disinfectant and influence the disinfection effect;
the sodium phosphate compound has the function of relieving the influence of calcium carbonate insoluble substances formed in the disinfection and sterilization process of the calcium hypochlorite on the permeability of the swimming pool, when the value of the weight part of the sodium phosphate compound is too large, the sodium phosphate compound can slow down the growth of calcium carbonate crystals in the calcium hypochlorite so as to block the generation of a large amount of calcium carbonate, so that calcium ions generated by the reaction of the calcium hypochlorite cannot be consumed, and when the calcium ions cannot be consumed according to the reaction balance, the reaction of the calcium hypochlorite is insufficient or the reaction speed is slowed down, so that the final disinfection and sterilization effect and the disinfection and sterilization speed are influenced; when the weight part of the sodium phosphate compound is too small, the sodium phosphate compound cannot relieve the generation of calcium carbonate crystals, so that the calcium carbonate in water is crystallized and precipitated, the permeability of the whole water body is influenced, the photocatalytic stage of the nano silver-titanium dioxide compound is not obvious, and the contents of electrons and free radicals generated by the nano silver-titanium dioxide compound are insufficient, so that the content of effective chlorine generated by the calcium hypochlorite receiving electrons is reduced, and the final disinfection and sterilization effects are influenced.
Potassium peroxymonosulfate is an inorganic peroxide, has the effect of widely killing microorganisms, releases active oxygen after being dissolved in water, generates various high-energy and high-activity micromolecule free radicals, nascent atomic oxygen, oxygen radicals, hydroxyl free radicals, sulfuric acid free radicals and other active ingredients through a chain reaction by a high-energy activator, thereby becoming a high-efficiency oxidation disinfectant, can oxidize and decompose organic pollutants which cannot be oxidized by the hydroxyl free radicals due to the existence of other free radicals except the hydroxyl free radicals, and decompose the organic pollutants into water, carbon dioxide and simple inorganic matters, and can remove algae and decompose algal toxins; when the weight part of the potassium monopersulfate is excessively large, a large amount of free radicals can be generated in the potassium monopersulfate and a large amount of electrons are needed in the reaction stage, so that the reaction process of generating electrons by photocatalysis of the nano silver-titanium dioxide composite to participate in calcium hypochlorite can be influenced, the photocatalytic process can be influenced by the large amount of free radicals, and further, the consumption of a large amount of electrons can cause the insufficient yield of effective chlorine generated by the calcium hypochlorite reaction, and the final disinfection and sterilization effect can be influenced; when the weight part of potassium monopersulfate is too small, the potassium monopersulfate provides a large amount of radicals, so that when the content is low, the content of the radicals is low, and the capability of decomposing organic pollutants which cannot be oxidatively decomposed by hydroxyl radicals is reduced, thereby causing poor final disinfection effect.
The nano silver-titanium dioxide compound has the effects that in the whole composite disinfectant system, the nano silver-titanium dioxide compound is utilized, as the silver has a certain sterilization effect, free radicals generated in the photocatalytic reaction stage of titanium dioxide can decompose complex organic matters and can enable the nano silver to partially form silver ions, and then electrons generated in the photocatalytic stage of titanium dioxide are utilized, in the process that calcium hypochlorite receives electrons to generate effective chlorine components, the silver ions can react with excessive chlorine ions after reaction, so that the quantity of the electrons received by the calcium hypochlorite is increased, the photocatalysis of the titanium dioxide is intensified, the reaction stage of the calcium hypochlorite is more sufficient, and the sterilization effect is more obvious; when the weight part of the nano silver-titanium dioxide composite is too large, a large amount of electrons generated by photocatalysis participate in the reaction of calcium hypochlorite to generate a large amount of chloride ions, and because the added nano silver is too much, a large amount of chloride ions are consumed, so that the effective chlorine component of the calcium hypochlorite is reduced, and the final disinfection and sterilization effect is influenced; when the weight part of the nano silver-titanium dioxide composite is too small, the quantity of electrons generated by photocatalysis is insufficient, the content of nano silver is reduced, the quantity of electrons obtained by calcium hypochlorite is reduced, the generation speed and the generation quantity of available chlorine are reduced, and the composite disinfection and sterilization capacity of the nano silver and the calcium hypochlorite is weakened, so that the disinfection and sterilization effect is influenced.
The assistant has the effects that the nano silver-titanium dioxide compound, the calcium hypochlorite, the potassium peroxymonosulfate and the sodium phosphate compound are fully mixed and coagulated, so that the nano silver-titanium dioxide compound and the calcium hypochlorite are directly combined to react, and the phenomenon that the nano silver-titanium dioxide compound starts to react only when the calcium hypochlorite completely reacts due to overlarge gaps is avoided, and the nano silver-titanium dioxide compound cannot cooperate with the calcium hypochlorite compound; when the weight portion of the auxiliary agent is too large, the auxiliary agent has a coagulation effect, so that a coagulated mass is easily formed to precipitate out of a water body, the permeability of the water body is poor, the reaction of the nano silver-dioxide compound is insufficient, and the disinfection and sterilization effects are affected.
Therefore, the technical problem of 'rapidly treating the wastewater of the swimming pool' is solved by selecting the chemical components and the parts by weight, and the technical obstacle to be overcome is how to utilize the nano silver-titanium dioxide compound to synergistically react with the calcium hypochlorite, the potassium hydrogen peroxymonosulfate, the sodium phosphate compound and the auxiliary agent.
As an alternative embodiment, the nano silver-titanium dioxide composite comprises 2 to 10 parts by weight of silver, 60 to 80 parts by weight of titanium dioxide, and 10 to 15 parts by weight of alumina;
the silver in 2-10 weight portions is used as secondary functional matter for sterilization, when the weight portion is too large, the content of free radicals generated by titanium dioxide in a photocatalytic system is limited, and when the content of nano silver is too large, silver which is not converted into silver ions can be deposited to form silver precipitate, so that the permeability of a water body is influenced, and the process of a photocatalytic stage is influenced.
60-80 parts of titanium dioxide is used as a main catalyst of photocatalysis to catalyze water to generate free radicals and electrons, the adverse effect of excessively large part by weight is the existence of a large amount of electrons and free radicals generated in the photocatalysis process, so that the electrons and the free radicals can react with an auxiliary agent or potassium hydrogen peroxymonosulfate to generate internal consumption between the composite disinfectants, the adverse effect of excessively small part by weight is that the electrons and the free radicals generated in the photocatalysis process are insufficient, so that the content of effective chlorine generated by calcium hypochlorite receiving electrons is insufficient, and meanwhile, the disinfection effect of the composite disinfectants is poor due to insufficient content of the free radicals.
10-15 parts of alumina serves as a protective agent and a bonding agent for silver and titanium dioxide, and by utilizing the high stability of alumina, the surface of alumina generates [ Al (H) due to free radicals in a reaction system2O)6]3+In the stage of hydrolysis and polycondensation reaction, titanium dioxide and silver are bonded together through the adsorption bridging effect generated by substances subjected to hydrolysis and polycondensation, and meanwhile, due to the characteristic that aluminum oxide can react with acid and alkali, the acid resistance and alkali resistance of the nano silver-titanium dioxide compound can be protected in the reaction stage, the stable existence of the nano silver-titanium dioxide compound is ensured, and the disinfection and sterilization effects are ensured; an adverse effect of an excessively large part by weight is the formation of [ Al (H)2O)6]3+Too much silver and titanium dioxide are wrapped into balls, so that the silver and the titanium dioxide form particle precipitation, and the final disinfection and sterilization effect is influenced; an adverse effect of too small a weight fraction is the formation of [ Al (H)2O)6]3+The defects result in separation of silver and titanium dioxide, so that the titanium dioxide photocatalysis stage and silver synergistic reaction are not established, the process that the titanium dioxide catalyzes to generate electrons so that chloride ions generated by calcium hypochlorite are removed by silver ions cannot be constructed, the content of effective chlorine components generated by the calcium hypochlorite is reduced, and the final disinfection and sterilization effects are influenced.
The principle of the synergistic effect of 2-10 parts of silver, 60-80 parts of titanium dioxide and 10-15 parts of aluminum oxide (namely 1+1+1 > 3) is as follows:
mainly takes the photocatalysis process of titanium dioxide, and forms [ Al (H) on the surface of alumina by the generated free radical2O)6]3+Titanium dioxide and silver are passed through by hydrolysis and polycondensation [ Al (H)2O)6]3+Adsorption shelf produced by hydrolytic polycondensation of substancesThe electrons generated by titanium dioxide photocatalysis enable calcium hypochlorite to generate enough chloride ions in the stage of generating effective chloride components in the photocatalysis process, so that the calcium hypochlorite can be combined with the silver ions, according to the reaction balance, the calcium hypochlorite can generate more effective chloride components, so that more electrons are consumed, a large amount of free radicals are generated in the photocatalysis reaction stage, and the integral nano silver-titanium dioxide compound can synergistically oxidize and decompose organic impurities through the generated free radicals, thereby improving the disinfection and sterilization effects.
As an optional embodiment, sodium hexametaphosphate is adopted as the phosphate compound, and sodium hexametaphosphate is adopted, so that when sodium hexametaphosphate is combined with calcium carbonate generated by calcium hypochlorite compared with other phosphate compounds, sodium hexametaphosphate can form a soluble complex on the crystal surface of calcium carbonate, so that the surface of calcium carbonate insoluble in water is coated with the soluble complex, thereby slowing down the precipitation of calcium carbonate crystals, increasing the permeability of a water body, and indirectly improving the capacity of a nano silver-titanium dioxide compound in a photocatalytic stage.
As an alternative embodiment, the particle size of the silver is 10 to 15nm, the particle size of the titanium dioxide is 5 to 20nm, and the particle size of the aluminum oxide is 5 to 15 nm;
the particle size of silver of 10-15mm, the particle size of titanium dioxide of 5-20mm and the particle size of alumina of 5-15nm are all limited in the nanometer level, and the particle sizes of the three are all limited in an overlapping range, and because the relative molecular mass is ordered from large to small as silver > alumina > titanium dioxide, under the condition of similar particle size, the particles of the three can be fused and embedded into each other through respective gaps to form dense nanoparticle clusters, so that stable nano silver-titanium dioxide composite particles can be formed, and the photocatalyst stage can be stably carried out; when the particle size values of the three are overlarge, electrons generated in a photocatalysis stage are unstable, so that the electron transfer process is blocked due to overlarge size, the calcium hypochlorite is blocked to receive electrons, and the silver particles are overlarge in size, overlarge in weight and easy to fall off from particle clusters; when the particle size values of the three are all too small, even if gaps can exist, the contact area of the three is reduced, the three are mutually fused and embedded with small force, so that the nano particle clusters are easy to disperse, and the photocatalysis stage is influenced.
As an alternative embodiment, the nano silver-titanium dioxide composite is prepared by a sol-gel method, and the sol-gel method further comprises the following steps:
mixing tetrabutyl titanate and isopropanol, and adding an isopropanol aqueous solution into the mixed solution to prepare titanium dioxide powder;
obtaining a silver ammonia solution, adding the silver ammonia solution into a mixed solution of tetrabutyl titanate and isopropanol, and preparing mixed powder of nano silver and titanium dioxide;
adding alumina powder into the prepared titanium dioxide powder and the mixed powder, uniformly mixing, and then jointly and finely grinding to obtain the nano silver-titanium dioxide composite.
Pure titanium dioxide powder is firstly generated by adopting tetrabutyl titanate and isopropanol, then the bonded mixed powder of nano silver and titanium dioxide is prepared by adopting a mixed solution of a silver ammonia solution and tetrabutyl titanate and isopropanol, the aluminum oxide is utilized in a grinding stage, the friction loss of the silver and the titanium dioxide can be slowed down due to the smooth surface of the aluminum oxide, the aluminum oxide can be used as a filling agent, the distance between the silver and the titanium dioxide is increased, the grinding stage is more sufficient, and the nano silver and the titanium dioxide powder are jointly synthesized, so that the nano silver and the titanium dioxide can coexist in a synthesis stage.
As an optional embodiment, the auxiliary agent is at least one of potassium dihydrogen phosphate, ferric chloride, aluminum chloride, polyaluminum sulfate, polyferric chloride and polyferric sulfate; furthermore, the auxiliary agent comprises 20-25 parts by weight of polyaluminium sulfate and 2-5 parts by weight of polyferric sulfate.
The limiting auxiliary agent comprises 20-25 parts by weight of polyaluminium sulfate and 2-5 parts by weight of polyferric sulfate, and has the function that the polyaluminium sulfate is dissolved in water and then is immediately dissociatedAluminum ion, [ Al (H) ]2O)6]3+When existing, the polymeric ferric sulfate dissolved in water will react with [ Fe (H)2O)6]3+Fe (H) exists because it is extremely unstable, either forms coordinate bonds or hydrolyzes to form colloids2O)6]3+Will react with [ Al (H)2O)6]3+The hydrolysis and polycondensation reaction are carried out jointly to form unhydrolyzed hydrated aluminum ions, unhydrolyzed iron ions, mononuclear hydroxyl complex, polynuclear hydroxyl complex, ferric hydroxide colloid or precipitate, aluminum hydroxide precipitate and other substances, and the substances play a coagulation effect through the actions of adsorption bridging and the like, so that the calcium hypochlorite, the potassium hydrogen peroxymonosulfate, the sodium phosphate compound and the nano silver-titanium dioxide compound are fully mixed and adsorbed and bonded; when the weight fraction of polyaluminium sulfate is too large, a large amount of [ Al (H) is produced due to hydrolysis thereof2O)6]3+The coagulation effect after hydrolysis and polycondensation is too heavy, and the newcastle particles are precipitated, so that the permeability of the water body is influenced; when the weight fraction of polyaluminium sulfate is too small, [ Al (H) is produced by hydrolysis thereof2O)6]3+The content is insufficient, so that each component generated by hydrolysis and polycondensation reaction is insufficient, and coagulation is insufficient, so that the components among the composite disinfectants are insufficiently coagulated, and substance unbalance in the reaction stage is easily caused, and residual reactants exist;
when the weight portion of the polymeric ferric sulfate is too large, the polymeric ferric sulfate is formed into Fe (H)2O)6]3+Easily decomposed and thus large amount of [ Fe (H) ]2O)6]3+Decomposition thereby affecting [ Al (H)2O)6]3+Resulting in [ Al (H) participating in the polycondensation reaction2O)6]3+The content is insufficient, the coagulation effect is not obvious, and thus residual reactants exist; when the weight portion of the polymeric ferric sulfate is too small, Fe (H) is formed2O)6]3+Insufficient amount of [ Al (H) ]2O)6]3+In the hydrolysis and polycondensation reaction, the coagulation effect is not obvious, resulting in the generation of calcium hypochlorite, potassium hydrogen peroxymonosulfate and sodium phosphateAfter the compound and the nano silver-titanium dioxide compound are uniformly mixed, the adsorption and bonding capacity is weak.
As an alternative embodiment, the calcium hypochlorite is sodium calcium hypochlorite, when the sodium calcium hypochlorite is adopted, the calcium chloride is converted into sodium chloride due to the introduction of a sodium hydroxide solution in the preparation stage, potassium ions are introduced by the addition of potassium monopersulfate, so that when potassium monopersulfate is added into the calcium hypochlorite, the calcium hypochlorite can be stimulated to be active by the reaction balance interaction of potassium and sodium ions, and the chloride ions in the sodium calcium hypochlorite can react with the potassium monopersulfate in a non-free radical manner under the action of electrons generated by photocatalysis to generate an active substance Cl2And HClO.
According to another exemplary embodiment of the present invention, there is provided a method for preparing a composite disinfectant, the method including:
uniformly mixing calcium hypochlorite, a sodium phosphate compound and potassium hydrogen peroxymonosulfate, adding the nano silver-titanium dioxide compound, stirring, adding the auxiliary agent while stirring until all the components are uniformly mixed, and thus obtaining the composite disinfectant.
Firstly, calcium hypochlorite, a sodium phosphate compound and potassium peroxymonosulfate are uniformly mixed, the action is that when the powders of the calcium hypochlorite, the potassium peroxymonosulfate and the sodium phosphate compound are uniformly mixed, the three are not in the water solution, so that the mutual reaction can not be started, then a nano silver-titanium dioxide compound is added, the nano silver-titanium dioxide compound has smaller grain diameter, so that the three can be uniformly mixed in the uniformly mixed powder, when the nano silver-titanium dioxide compound is simultaneously added into the mixing stage of the three, the nano silver-titanium dioxide compound has smaller grain diameter, so that the nano silver-titanium dioxide compound is easy to be accumulated on the surface of the mixture in the mixing stage, so that the mixing is insufficient, and finally, the auxiliary agent is doped, so that the nano silver-titanium dioxide compound and other composite disinfectants can be uniformly mixed in the hydrolysis stage, so that the calcium hypochlorite can generate enough effective chlorine to rapidly treat the swimming pool wastewater.
The following will explain in detail a composite disinfectant and a preparation method thereof in the present application with reference to examples, comparative examples and related experiments.
Examples
Example 1
As shown in fig. 1, the composite disinfectant comprises the following components in parts by weight: 60 parts of calcium hypochlorite, 5 parts of sodium hexametaphosphate, 7 parts of potassium peroxymonosulfate, 10 parts of nano silver-titanium dioxide compound and 8 parts of auxiliary agent; the sodium method calcium hypochlorite is purchased from a Xinxin chemical plant in Tianjin, and the effective chlorine content is 65 percent; the nano silver-titanium dioxide compound comprises 8 parts of silver, 70 parts of titanium dioxide and 12 parts of aluminum oxide by weight; the particle size of the silver is 13nm, the particle size of the titanium dioxide is 15nm, and the particle size of the aluminum oxide is 10 nm; the auxiliary agent comprises 22 parts by weight of polyaluminium sulfate and 3 parts by weight of polyferric sulfate.
Example 2
The composite disinfectant comprises the following components in parts by weight: 50 parts of calcium hypochlorite, 2 parts of sodium hexametaphosphate, 5 parts of potassium hydrogen peroxymonosulfate, 8 parts of nano silver-titanium dioxide compound and 2 parts of auxiliary agent; the sodium method calcium hypochlorite is purchased from a Xinxin chemical plant in Tianjin, and the effective chlorine content is 70 percent; the nano silver-titanium dioxide compound comprises 2 parts of silver, 60 parts of titanium dioxide and 10 parts of aluminum oxide in parts by weight; the particle size of the silver is 10nm, the particle size of the titanium dioxide is 5nm, and the particle size of the aluminum oxide is 5 nm; the auxiliary agent comprises 20 parts by weight of polyaluminium sulfate and 2 parts by weight of polyferric sulfate.
Example 3
The composite disinfectant comprises the following components in parts by weight: 70 parts of calcium hypochlorite, 10 parts of sodium hexametaphosphate, 10 parts of potassium hydrogen peroxymonosulfate, 15 parts of nano silver-titanium dioxide compound and 10 parts of auxiliary agent; the sodium method calcium hypochlorite is purchased from a Xinxin chemical plant in Tianjin, and the effective chlorine content is 68 percent; the nano silver-titanium dioxide compound comprises 10 parts of silver, 80 parts of titanium dioxide and 15 parts of aluminum oxide in parts by weight; the particle size of the silver is 15nm, the particle size of the titanium dioxide is 20nm, and the particle size of the aluminum oxide is 15 nm; the auxiliary agent comprises 25 parts of polyaluminium sulfate and 5 parts of polyferric sulfate by weight.
Example 4
The composite disinfectant comprises the following components in parts by weight: 60 parts of calcium hypochlorite, 5 parts of sodium hexametaphosphate, 7 parts of potassium peroxymonosulfate, 10 parts of nano silver-titanium dioxide compound and 8 parts of auxiliary agent; the sodium method calcium hypochlorite is purchased from a Xinxin chemical plant in Tianjin, and the effective chlorine content is 65 percent; the nano silver-titanium dioxide compound comprises 2 parts of silver, 60 parts of titanium dioxide and 10 parts of aluminum oxide in parts by weight; the particle size of the silver is 15nm, the particle size of the titanium dioxide is 15nm, and the particle size of the aluminum oxide is 10 nm; the auxiliary agent comprises 22 parts by weight of polyaluminium sulfate and 3 parts by weight of polyferric sulfate.
Example 5
The composite disinfectant comprises the following components in parts by weight: 60 parts of calcium hypochlorite, 5 parts of sodium hexametaphosphate, 7 parts of potassium peroxymonosulfate, 10 parts of nano silver-titanium dioxide compound and 8 parts of auxiliary agent; the sodium method calcium hypochlorite is purchased from a Xinxin chemical plant in Tianjin, and the effective chlorine content is 65 percent; the nano silver-titanium dioxide compound comprises 10 parts of silver, 80 parts of titanium dioxide and 15 parts of aluminum oxide in parts by weight; the particle size of the silver is 13nm, the particle size of the titanium dioxide is 15nm, and the particle size of the aluminum oxide is 10 nm; the auxiliary agent comprises 22 parts by weight of polyaluminium sulfate and 3 parts by weight of polyferric sulfate.
Comparative example 1
The composite disinfectant comprises the following components in parts by weight: 60 parts of calcium hypochlorite, 5 parts of sodium hexametaphosphate, 7 parts of potassium hydrogen peroxymonosulfate, 10 parts of nano silver-titanium dioxide compound, 8 parts of auxiliary agent and the rest of the formula steps are the same as those in example 1.
Comparative example 2
The composite disinfectant comprises the following components in parts by weight: 60 parts of calcium hypochlorite, 5 parts of sodium hexametaphosphate, 7 parts of potassium hydrogen peroxymonosulfate, 0 part of nano silver-titanium dioxide compound, 8 parts of auxiliary agent and the rest of the formula and the steps are the same as those of the example 1.
Comparative example 3
The nano silver-titanium dioxide composite comprises 10 parts by weight of silver, 80 parts by weight of titanium dioxide and 0 part by weight of aluminum oxide, and the rest of the formula and the steps are the same as those of the example 1.
Comparative example 4
The assistant comprises 22 parts of polyaluminium sulfate and 0 part of polyferric sulfate by weight, and the rest formula and steps are the same as those in example 1.
Comparative example 5
The assistant comprises 0 part of polyaluminium sulfate and 3 parts of polyferric sulfate by weight, and the rest formula and steps are the same as those in example 1.
Related experiments:
the composite disinfectants prepared in examples 1-5 and comparative examples 1-5 were tested and the test results are shown in table 1.
The related test method comprises the following steps:
testing the content of available chlorine: the test was carried out according to the Disinfection protocol (2002 edition) with a standard titration solution of sodium thiosulfate at a concentration of 0.1179mol/L, a test temperature of 23.5 ℃ and a relative humidity of 53%.
And (3) pH test: the test was carried out according to the Disinfection protocol (2002 edition) in a solution of 3mg/L available chlorine.
And (3) stability testing: placing the sample in a constant temperature box at 37 ℃ for 90 days, and then testing the content of available chlorine according to the disinfection technical specification (2002 edition), wherein the concentration of a sodium thiosulfate standard titration solution is 0.1179mol/L, the testing temperature is 23.5 ℃, and the relative humidity is 53%; the decrease in available chlorine after the stability test (i.e., the available chlorine content before storage minus the available chlorine content after storage) was calculated.
And (3) testing the disinfection effect: the test is carried out according to the disinfection technical Specification (2002 edition), GB/T18204.9-2000, GB/T18204.10-2000 and GB/T5750.11-2006; the test water body and the indoor swimming pool are 28m in length, 20m in width and 1.5m in water depth; the effective chlorine in the swimming pool is 3mg/L, the disinfection action time is 30min, viable bacteria culture counting, escherichia coli counting and free residual chlorine content determination are carried out.
The neutralizer is: 0.03mol/L PBS 0.25% sodium thiosulfate + 1.0% Tween 80.
Tests show that the effective chlorine content of the composite disinfectant in the examples 1-5 is 76-81(w/w), the pH value of the prepared solution with the effective chlorine of 3mg/L is 7-8, and the effective chlorine content is reduced by less than 2.3% after the solution is placed in a constant temperature box at 37 ℃ for 90 days; after the indoor swimming pool is disinfected, the total number of bacteria, the number of escherichia coli and the content of free residual chlorine in the pool all meet the sanitary standard of swimming places, and the details are shown in table 1.
Table 1 examples 1-5 results of the disinfection effect test
Figure BDA0003099283030000151
Figure BDA0003099283030000161
Further examination of the composite disinfectants of comparative examples 1-5 as described above, Table 2 was obtained
Table 2 results of the sterilization effect test of examples 1 to 5 and comparative examples 1 to 5
Figure BDA0003099283030000162
The effective chlorine decreasing rate refers to the consumption rate of the effective chlorine component in the storage stage when the disinfectant is not carried out, and the over-large decreasing rate indicates that the stability of the effective chlorine component of the disinfectant is poor, and otherwise indicates that the stability of the effective chlorine component of the disinfectant is stable.
The total number of bacteria before disinfection refers to the total number of bacteria in the sampled water of the swimming pool before disinfection, and the total number of bacteria before disinfection fluctuates due to the difference of the total number of bacteria in different conditions of the same water body.
The total number of bacteria after disinfection refers to the total number of bacteria existing in the disinfected sampling water, and the final total number of bacteria after disinfection is different according to different disinfection conditions.
From the data of examples 1-5 in tables 1 and 2, it can be seen that:
the composite disinfectant composed of 60 parts of calcium hypochlorite, 5 parts of sodium hexametaphosphate, 7 parts of potassium hydrogen peroxymonosulfate, 10 parts of nano silver-titanium dioxide composite and 8 parts of auxiliary agent has the strongest and most stable disinfection and sterilization capability, wherein, when the parts by weight of the silver, the titanium dioxide and the aluminum oxide which form the nano silver-titanium dioxide composite are different, the stability and the sterilization capability of the effective chlorine show different changing trends, in particular, when the weight ratio of the silver to the aluminum oxide is smaller (reference example 4), the reduction rate of the effective chlorine is larger, and the difference value before and after sterilization is 1126CFU/mL, and when the weight ratio of the silver to the aluminum oxide is larger (reference example 5), the reduction rate of available chlorine is small, and the difference value before and after sterilization is 1251CFU/mL, but the reduction rate and the difference value before and after sterilization are obvious compared with those in example 1, probably because when silver and alumina are excessive, electrons and free radicals generated in the photocatalytic stage of titanium dioxide can not completely convert silver and alumina, and the excessive alumina causes [ Al (H) to be2O)6]3+Too much, part of the silver and titanium dioxide is encapsulated and does not react.
Therefore, the nano silver-titanium dioxide composite is composed of 8 parts of silver, 70 parts of titanium dioxide and 12 parts of aluminum oxide in parts by weight.
From the data of comparative examples 1-5 in Table 2, it can be seen that:
as can be seen from comparative example 1, the difference of the disinfection and sterilization effects of calcium hypochlorite in different processes may be caused by the synergistic reaction between sodium hydroxide added to sodium-method calcium hypochlorite and potassium peroxymonosulfate, which increases the generation of available chlorine.
From the data of comparative example 2, it can be seen that the nano silver-titanium dioxide composite has a great influence on the overall composite disinfectant, and the composite disinfectant lacking the nano silver-titanium dioxide composite has a great difference in the stability of available chlorine and bactericidal ability.
From the data of comparative example 3, it can be seen that the lack of alumina component in the nano silver-titanium dioxide composite has a certain effect on the stability and bactericidal ability of available chlorine, but the effect is smaller.
From the data of comparative examples 4 to 5, it can be seen that when polyaluminium sulfate or polymeric ferric pomegranate is used as the auxiliary, the stability and bactericidal activity of available chlorine are affected, and polyaluminium sulfate is the most influential factor.
One or more technical solutions in the embodiments of the present invention at least have the following technical effects or advantages:
(1) in the embodiment of the invention, the disinfection time of different embodiments is different, the total number of bacteria is 0CFU/mL, the shortest time is 10min in the embodiment 1, and the time of other embodiments is more than 12 min;
(2) because the embodiment of the invention adopts the photocatalysis method, the photocatalysis energy can be provided by means of the ultraviolet disinfection stage, and the ultraviolet broad-spectrum disinfection and sterilization can be utilized, and the chemical components in the compound disinfectant can be utilized for further disinfection and sterilization;
(3) the compound disinfectant provided by the embodiment of the invention has the advantages that the content of the rest chlorine can be maintained at 0.282-0.296mg/L, the reduction rate of the effective chlorine is lower than 2.3%, and the total number of bacteria after disinfection is maintained below 4 CFU/mL.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims (9)

1. The composite disinfectant is characterized by comprising the following components in parts by weight: 50-70 parts of calcium hypochlorite, 2-10 parts of a sodium phosphate compound, 5-10 parts of potassium hydrogen peroxymonosulfate, 8-15 parts of a nano silver-titanium dioxide compound and 2-10 parts of an auxiliary agent.
2. The composite disinfectant as set forth in claim 1, wherein said nano silver-titanium dioxide composite comprises silver in an amount of 2-10 parts by weight, titanium dioxide in an amount of 60-80 parts by weight, and alumina in an amount of 10-15 parts by weight.
3. The composite disinfectant as set forth in claim 2, wherein said silver has a particle size of 10-15nm, said titanium dioxide has a particle size of 5-20nm, and said aluminum oxide has a particle size of 5-15 nm.
4. A composite disinfectant as set forth in claim 2, wherein: the nano silver-titanium dioxide composite is prepared by a sol-gel method.
5. A composite disinfectant as set forth in claim 4, wherein: the sol-gel method comprises the following steps:
mixing tetrabutyl titanate and isopropanol, and adding an isopropanol aqueous solution into the mixed solution to prepare titanium dioxide powder;
obtaining a silver ammonia solution, adding the silver ammonia solution into a mixed solution of tetrabutyl titanate and isopropanol, and preparing mixed powder of nano silver and titanium dioxide;
adding alumina powder into the prepared titanium dioxide powder and the mixed powder, uniformly mixing, and then jointly and finely grinding to obtain the nano silver-titanium dioxide composite.
6. A composite disinfectant as set forth in claim 1, wherein: the auxiliary agent is at least one of potassium dihydrogen phosphate, ferric chloride, aluminum chloride, polyaluminum sulfate, polyferric chloride and polyferric sulfate.
7. A composite disinfectant as set forth in claim 6, wherein: the auxiliary agent comprises 20-25 parts of polyaluminium sulfate and 2-5 parts of polyferric sulfate by weight.
8. A composite disinfectant as set forth in claim 1, wherein: the calcium hypochlorite is sodium-method calcium hypochlorite.
9. A method of preparing a composite disinfectant as claimed in any of claims 1 to 8, said method comprising: uniformly mixing calcium hypochlorite, a sodium phosphate compound and potassium hydrogen peroxymonosulfate, adding the nano silver-titanium dioxide compound, stirring, adding the auxiliary agent while stirring until all the components are uniformly mixed, and thus obtaining the composite disinfectant.
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