CN112136821A - Reusable novel dehumidifying antibacterial agent and preparation method thereof - Google Patents
Reusable novel dehumidifying antibacterial agent and preparation method thereof Download PDFInfo
- Publication number
- CN112136821A CN112136821A CN202010991040.2A CN202010991040A CN112136821A CN 112136821 A CN112136821 A CN 112136821A CN 202010991040 A CN202010991040 A CN 202010991040A CN 112136821 A CN112136821 A CN 112136821A
- Authority
- CN
- China
- Prior art keywords
- weight
- antibacterial agent
- parts
- dehumidifying
- nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
-
- 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- 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
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/02—Amines; Quaternary ammonium compounds
- A01N33/12—Quaternary ammonium 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
-
- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
-
- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- 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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
- A01N47/42—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —N=CX2 groups, e.g. isothiourea
- A01N47/44—Guanidine; Derivatives 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
- A01N59/08—Alkali metal chlorides; Alkaline earth metal chlorides
-
- 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
- A01N59/16—Heavy metals; Compounds thereof
- A01N59/20—Copper
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Environmental Sciences (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Plant Pathology (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Drying Of Gases (AREA)
Abstract
The invention discloses a novel reusable dehumidifying antibacterial agent and a preparation method thereof. The novel dehumidifying antibacterial agent prepared by the invention has the advantages of strong dehumidifying capacity, large moisture absorption capacity, lower resolving temperature, wide antibacterial spectrum, high antibacterial activity, long antibacterial aging, environmental friendliness, reusability and the like, can effectively sterilize and efficiently remove moisture in air, and has great application prospect in the fields of storage and the like.
Description
[ technical field ]: the invention mainly applies to the dehumidification and sterilization of air, in particular to a novel recyclable dehumidification antibacterial agent and a preparation method thereof.
[ background Art ] A method of: the warehousing technology has great influence on our lives, and different warehousing environments need to be selected for different articles. In the warehousing field, the most common concerns are moisture and mold. Particularly, some cotton and hemp products are easy to generate damp and mildewed phenomena during the preservation process, and how to effectively solve the problem is a big problem (H B Gonzales, P R Armstrong, R G Magranging. Simulans monitoring of stored grain with relative humidity, temperature, and carbon dioxide sensors [ J ]. Applied Engineering in Agriculture,2009,25(4): 595-604).
At present, common dehumidifying agents on the market are mainly divided into two types, one type is a non-deliquescent dehumidifying agent which comprises silica gel, a molecular sieve, vermiculite, activated carbon and the like, the principle of the dehumidifying agent is mainly physical adsorption, and the dehumidifying agent has huge specific surface area due to a large number of pores, and can adsorb moisture through capillary adsorption, but the dehumidifying agent has the common defects of weak moisture absorption capacity, slow speed, small capacity, high resolving temperature and the like; another is a deliquescent desiccant, such as hygroscopic salts, including calcium chloride, lithium chloride, whose mechanism is mainly chemical absorption, which, although it is strong in moisture absorption capacity, rate block, large capacity, low desorption temperature, often accompanies the generation of liquid, which is inconvenient to use, and some salts are also strongly corrosive, which limits its application to a large extent (Thomas Nonnen, Hannes Prei β -ler, Steffen Beckert, et al, salt inclusion and deliquesce in salt X complexes for thermal chemical heat storage [ J ]. Microporous and meso Materials,2020,303: 110239).
The two common dehumidifying agents can only dehumidify, and almost have no sterilizing effect. Therefore, in order to solve the problem, it is urgently needed to prepare a dehumidifying antibacterial agent which can effectively remove moisture in the air and kill various bacteria, molds and viruses while removing the moisture. Aiming at the problem, the invention provides a novel recyclable dehumidifying antibacterial agent and a preparation method thereof, wherein components with antibacterial effects are organically combined with the dehumidifying agent, so that the effects of removing moisture in air and inhibiting bacteria and mould are achieved, and the novel dehumidifying antibacterial agent has novelty, novelty and practicability.
[ summary of the invention ]: the invention provides a novel reusable dehumidifying antibacterial agent and a preparation method thereof, wherein a non-deliquescent adsorbent is used as a carrier, and hygroscopic salt and an antibacterial agent are loaded in pores of the adsorbent.
[ technical solution of the present invention ]: the invention provides a novel reusable dehumidifying antibacterial agent and a preparation method thereof, wherein the dehumidifying antibacterial agent comprises a moisture absorbent and an antibacterial agent; the moisture absorbent comprises an adsorbent and a moisture absorbent salt, the antibacterial agent comprises an organic antibacterial agent and an inorganic nano antibacterial agent, and the target product is realized by the following steps:
first, dissolution of organic antibacterial agent and hygroscopic salt
Weighing 0.0-1.0 part by weight of 4, 5-dichloro-N-octyl-4-isothiazolin-3-one, 0.0-1.0 part by weight of polyhexamethylene guanidine, 0.0-1.0 part by weight of coconut diethanolamide, 0.0-1.0 part by weight of dodecyl alanine, 0.0-1.0 part by weight of sulfamethoxydiazine sodium, 0.0-1.0 part by weight of didecyl dimethyl ammonium chloride, 0.0-1.0 part by weight of dimethoxy methyl benzyl amino pyrimidine sodium, 0.0-1.0 part by weight of clavulanate potassium, 5.0-10.0 parts by weight of calcium chloride, 5.0-10.0 parts by weight of sodium carbonate and 10.0-80.0 parts by weight of solvent at room temperature, mixing, stirring at a rotating speed of 200-700 r/min for 10-60 min to obtain fully dissolved organic antibacterial agent and hygroscopic salt, wherein the solvent is water or ethanol or the volume ratio of ethanol to water is (3-5): (1-3) mixing the solution;
second, mixing the adsorbent, hygroscopic salt and antimicrobial agent
Adding 0.0-1.0 part by weight of nano silver, 0.0-1.0 part by weight of nano copper oxide, 20.0-30.0 parts by weight of silver zeolite, 5.0-10.0 parts by weight of zinc zeolite, 5.0-10.0 parts by weight of copper zeolite, 5.0-20.0 parts by weight of microporous molecular sieve, 5.0-20.0 parts by weight of active carbon, 5.0-20.0 parts by weight of C-type coarse pore silica gel, 5.0-20.0 parts by weight of A-type fine pore silica gel and 5.0-10.0 parts by weight of alumina powder into the solution obtained in the first step in sequence, firstly stirring at the rotating speed of 200-700 r/min for 10-60 min, and then carrying out ultrasonic treatment for 30-100 min to obtain a mixed solution of a target adsorbent, a hygroscopic salt and an antibacterial agent;
thirdly, preparing the target dehumidifying antibacterial agent
Placing the mixed solution of the target adsorbent, the hygroscopic salt and the antibacterial agent obtained in the second step into a 50-200 mL three-neck quartz flask, transferring the three-neck quartz flask into an XH-300UP computer microwave ultrasonic ultraviolet light combined catalytic synthesizer, starting microwave, ultrasound and ultraviolet at the same time, carrying out constant-temperature reflux reaction on the mixed solution at the temperature of 10-100 ℃ for 10-60 min, stopping heating when the temperature exceeds a set temperature, and continuing heating when the temperature is lower than the set temperature; the conditions of microwave, ultrasonic and ultraviolet of the synthesizer are set as follows: the microwave frequency is 2450MHz, and the microwave power is 1-1000W; the ultrasonic power is 0-1500W, and the ultrasonic frequency is 24-26 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 0.1 multiplied by 105μW/cm2～1.999×105μW/cm2(ii) a And finally, under the conditions of-0.09 MPa and 50-90 ℃, rotationally evaporating at the speed of 50-100 r/min for 30-120 min to remove the solvent, and placing in a vacuum dryer at the temperature of 40-80 ℃ for 10-100 min to obtain the target dehumidifying antibacterial agent.
In the second step, an adsorbent, a hygroscopic salt and an antibacterial agent are mixed, wherein: the particle size of the nano silver is 5-50 nm, and the surface dispersant is 4-sulfocalixarene [6]]The anti-discoloration agent is branched polyethyleneAmines of nano silver, 4-sulfocalixarenes [6]]And branched polyethyleneimine in a mass ratio of (3-5): (5-8): 1, the agglomeration phenomenon and the oxidation phenomenon of nano particles can be effectively inhibited, and the excellent antibacterial activity of nano silver is maintained; the particle size of the nano copper oxide is 30-50 nm, the length of the nano copper oxide is 1-2 mu m, the surface dispersing agent is polyethylene glycol, and the mass ratio of the polyethylene glycol to the nano copper oxide is (3-5): 1, the agglomeration phenomenon of nano copper oxide particles can be effectively inhibited; the silver content of the silver zeolite is 0.5-2.5%, and the aperture is 50-100 mu m; the zinc content of the zinc zeolite is 1% -5%, and the aperture is 50-100 mu m; the copper content of the copper zeolite is 1% -5%, and the aperture is 50-100 mu m; the microporous molecular sieve is a mixed molecular sieve with the weight ratio of the A-type molecular sieve to the X-type molecular sieve being (1-3) to (1-3), and the average pore diameter is 0.5-2.0 nm, wherein the Si/Al of the A-type molecular sieve is 1, and the Si/Al of the X-type molecular sieve is 1.0-1.5; the specific surface area of the activated carbon is 200-1500 m2(ii)/g, the average pore diameter is 1-50 nm; the specific surface area of the C-type coarse-pore silica gel is 300-600 m2Per g, the average pore diameter is 8-16 nm, the pore volume is 0.80-1.00 mL/g, and the molecular formula is mSiO2·nH2O; the specific surface area of the A-type fine-pore silica gel is 650-800 m2(ii) per gram, the average pore diameter is 2-3 nm, the pore volume is 0.35-0.45 mL/g, and the molecular formula is SiO2·nH2O; the alumina powder has a particle size of 50 to 200 nm.
[ advantages and effects of the invention ]: compared with the prior art, the invention provides a novel reusable dehumidifying antibacterial agent and a preparation method thereof, and the novel reusable dehumidifying antibacterial agent has the following advantages: (1) the target product disclosed by the invention is a novel dehumidifying antibacterial agent which is prepared by taking a non-deliquescent adsorbent as a carrier, loading hygroscopic salt and an antibacterial agent in pores of the adsorbent and combining dehumidifying components and antibacterial components into a whole, and has strong moisture absorption capacity and excellent antibacterial effect; (2) the novel dehumidifying antibacterial agent prepared by the invention has the advantages of large moisture absorption capacity, low resolving temperature, no liquid generation and good antibacterial ability by controlling the proportion of the hygroscopic salt to the adsorbent; (3) the novel dehumidifying antibacterial agent prepared by the invention can be recycled after being dried by heat treatment, saves cost, is environment-friendly, and accords with the concept of green sustainable development; (4) the novel dehumidifying antibacterial agent provided by the invention utilizes microwave, ultrasonic and ultraviolet combined technology to enable all components to fully interact, the humidity resistance and bacteria removal performance of the product is regulated and controlled by controlling reaction conditions, the preparation process is simple, the operation is convenient, and the novel dehumidifying antibacterial agent has great commercial popularization and use potential.
[ description of the drawings ]
FIG. 1 is a schematic diagram of the synthetic route of the patent of the present invention, wherein: a is an organic antibacterial agent, B is a hygroscopic salt, C is an adsorbent, and D is a target dehumidifying antibacterial agent sample.
The specific implementation mode is as follows:
in order to more clearly illustrate the advantages of the present patent, the following embodiments and effects of the present invention are further illustrated with reference to the following examples; it is to be understood that not all embodiments described herein are provided. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments disclosed herein are intended to be within the scope of the present invention.
Example 1: preparation of a recyclable novel dehumidifying antimicrobial agent sample 1
The invention provides a novel reusable dehumidifying antibacterial agent and a preparation method thereof, wherein the dehumidifying antibacterial agent comprises a moisture absorbent and an antibacterial agent; as shown in fig. 1, the target product is specifically realized by the following steps:
first, dissolution of organic antibacterial agent and hygroscopic salt
Weighing 1.0 part by weight of 4, 5-dichloro-N-octyl-4-isothiazolin-3-one, 1.0 part by weight of dodecyl alanine, 1.0 part by weight of sulfamethoxydiazine sodium, 1.0 part by weight of didecyl dimethyl ammonium chloride, 1.0 part by weight of dimethoxy methyl benzyl aminopyrimidine sodium, 10.0 parts by weight of calcium chloride, 10.0 parts by weight of sodium carbonate and 75.0 parts by weight of ethanol at room temperature, mixing, and stirring at the rotating speed of 500r/min for 30min to obtain fully dissolved organic antibacterial agent and hygroscopic salt;
second, mixing the adsorbent, hygroscopic salt and antimicrobial agent
To the solution obtained in the first step, 0.5 part by weight of sodium salt having a particle size of 50nm was addedMiyasilver, 0.5 part by weight of nano copper oxide with the particle size of 50nm and the length of 2 mu m, 20.0 parts by weight of silver zeolite with the pore diameter of 60 mu m, 10.0 parts by weight of zinc zeolite with the zinc content of 3% and the pore diameter of 60 mu m, 10.0 parts by weight of copper zeolite with the copper content of 4% and the pore diameter of 60 mu m, 10.0 parts by weight of mixed type molecular sieve with the pore diameter of 1nm (wherein the weight ratio of the A type molecular sieve to the X type molecular sieve is 1:2, the Si/Al of the A type molecular sieve is 1, and the Si/Al of the X type molecular sieve is 1), and 14.0 parts by weight of activated carbon (the specific surface area of 1200 m)2Per g, mean pore diameter 2nm), 15.0 parts by weight of coarse-pored silica gel in the form of C (specific surface area 600 m)2(ii)/g, average pore diameter of 10nm, pore volume of 0.9mL/g, molecular formula of mSiO2·nH2O) 15.0 parts by weight of A-type fine-pored silica gel (the specific surface area of the A-type fine-pored silica gel was 800 m)2(ii)/g, average pore diameter of 3nm, pore volume of 0.4mL/g, molecular formula of SiO2·nH2O) and 5.0 parts by weight of alumina powder with the grain diameter of 100nm, stirring for 30min at the rotating speed of 400r/min, and then carrying out ultrasonic treatment for 60min to obtain a mixed solution of a target adsorbent, hygroscopic salt and an antibacterial agent;
the following steps: the surface dispersant of the nano silver is 4-sulfocalixarene [6], the anti-discoloration agent is branched polyethyleneimine, and the mass ratio of the nano silver to the 4-sulfocalixarene [6] to the branched polyethyleneimine is 3: 5: 1, the agglomeration phenomenon and the oxidation phenomenon of nano particles can be effectively inhibited, and the excellent antibacterial activity of nano silver is maintained; the nano copper oxide surface dispersant is polyethylene glycol, wherein the mass ratio of the polyethylene glycol to the nano copper oxide is 4: 1, the agglomeration phenomenon of nano copper oxide particles can be effectively inhibited;
thirdly, preparing the target dehumidifying antibacterial agent
Placing the mixed solution of the target adsorbent, the hygroscopic salt and the antibacterial agent obtained in the second step into a 150mL three-neck quartz flask, then transferring the three-neck quartz flask into an XH-300UP computer microwave ultrasonic ultraviolet light combined catalytic synthesizer, simultaneously starting microwave, ultrasound and ultraviolet, enabling the mixed solution to perform reflux reaction at a constant temperature of 50 ℃ for 30min, stopping heating when the temperature exceeds a set temperature, and continuing heating when the temperature is lower than the set temperature; microwave and ultrasonic wave with the synthesizerAnd the ultraviolet condition is as follows: microwave frequency 2450MHz and microwave power 900W; the ultrasonic power is 1000W, and the ultrasonic frequency is 25 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 1 multiplied by 105μW/cm2(ii) a And finally, rotationally evaporating at the temperature of 80 ℃ and the pressure of-0.09 MPa for 60min at the speed of 60r/min to remove the solvent, and then placing in a vacuum drier at the temperature of 60 ℃ for 80min to obtain the novel dehumidifying antibacterial agent sample 1 which can be recycled.
The moisture absorption and antimicrobial properties of the desiccant antimicrobial were tested by exposing the prepared target novel desiccant antimicrobial sample 1 to air at a relative humidity of 70% at room temperature, wherein: the dehumidifying antibacterial agent adsorbs moisture in the air until the weight of the dehumidifying antibacterial agent is not increased any more; the antibacterial performance adopts escherichia coli and staphylococcus aureus as test strains. Through the test: the moisture absorption amount is 34g, the sterilization rate of escherichia coli is 95.7%, the sterilization rate of staphylococcus aureus is 95.2%, the moisture absorption and the antibacterial performance of the novel dehumidifying antibacterial agent sample 1 are excellent, moisture can be removed through heat treatment after moisture absorption is saturated, and the dehumidifying antibacterial agent can be recycled.
Example 2: preparation of a recyclable novel dehumidifying antimicrobial agent sample 2
The invention provides a novel reusable dehumidifying antibacterial agent and a preparation method thereof, wherein the dehumidifying antibacterial agent comprises a moisture absorbent and an antibacterial agent; the target product is realized by the following steps:
first, dissolution of organic antibacterial agent and hygroscopic salt
Weighing 0.5 part by weight of 4, 5-dichloro-N-octyl-4-isothiazolin-3-one, 0.5 part by weight of dodecyl alanine, 0.5 part by weight of sulfamethoxydiazine sodium, 0.5 part by weight of didecyl dimethyl ammonium chloride, 0.2 part by weight of dimethoxy methyl benzyl aminopyrimidine sodium, 5.0 parts by weight of calcium chloride, 5.0 parts by weight of sodium carbonate and 87.8 parts by weight of ethanol at room temperature, mixing, and stirring at the rotating speed of 500r/min for 60min to obtain fully dissolved organic antibacterial agent and hygroscopic salt;
second, mixing the adsorbent, hygroscopic salt and antimicrobial agent
To the first0.5 part by weight of nano silver with the particle size of 50nm, 0.5 part by weight of nano copper oxide with the particle size of 50nm and the length of 2 mu m, 30.0 parts by weight of silver zeolite with the silver content of 2.0 percent and the pore size of 60 mu m, 5.0 parts by weight of zinc zeolite with the zinc content of 3 percent and the pore size of 60 mu m, 5.0 parts by weight of copper zeolite with the copper content of 4 percent and the pore size of 60 mu m, 10.0 parts by weight of mixed type molecular sieve with the pore size of 1nm (wherein the weight ratio of the A type molecular sieve to the X type molecular sieve is 1:2, the Si/Al of the A type molecular sieve is 1, the Si/Al of the X type molecular sieve is 1) and 15.0 parts by weight of activated carbon (the specific surface area is 1200 m) are sequentially added into the solution obtained in the first step2Per g, mean pore diameter 2nm), 14.0 parts by weight of coarse-pore silica gel in the form of C (specific surface area 600 m)2(ii)/g, average pore diameter of 10nm, pore volume of 0.9mL/g, molecular formula of mSiO2·nH2O) 15.0 parts by weight of A-type fine-pored silica gel (the specific surface area of the A-type fine-pored silica gel was 800 m)2(ii)/g, average pore diameter of 3nm, pore volume of 0.4mL/g, molecular formula of SiO2·nH2O) and 5.0 parts by weight of alumina powder with the grain diameter of 100nm, stirring for 30min at the rotating speed of 500r/min, and then carrying out ultrasonic treatment for 60min to obtain a mixed solution of a target adsorbent, hygroscopic salt and an antibacterial agent;
the following steps: the surface dispersant of the nano silver is 4-sulfocalixarene [6], the anti-discoloration agent is branched polyethyleneimine, and the mass ratio of the nano silver to the 4-sulfocalixarene [6] to the branched polyethyleneimine is 3: 5: 1, the agglomeration phenomenon and the oxidation phenomenon of nano particles can be effectively inhibited, and the excellent antibacterial activity of nano silver is maintained; the nano copper oxide surface dispersant is polyethylene glycol, wherein the mass ratio of the polyethylene glycol to the nano copper oxide is 4: 1, the agglomeration phenomenon of nano copper oxide particles can be effectively inhibited;
thirdly, preparing the target dehumidifying antibacterial agent
Placing the mixed solution of the target adsorbent, the hygroscopic salt and the antibacterial agent obtained in the second step into a 150mL three-neck quartz flask, transferring the three-neck quartz flask into an XH-300UP computer microwave ultrasonic ultraviolet light combined catalytic synthesizer, simultaneously starting microwave, ultrasonic and ultraviolet light, enabling the mixed solution to perform reflux reaction at a constant temperature of 50 ℃ for 30min, stopping heating when the temperature exceeds a set temperature, and stopping heating when the temperature is lower than the set temperatureThe heating is continued at the set temperature; the conditions of microwave, ultrasonic and ultraviolet of the synthesizer are set as follows: microwave frequency 2450MHz and microwave power 900W; the ultrasonic power is 1000W, and the ultrasonic frequency is 25 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 1 multiplied by 105μW/cm2(ii) a And finally, rotationally evaporating at the temperature of 80 ℃ and the pressure of-0.09 MPa for 60min at the speed of 60r/min to remove the solvent, and then placing in a vacuum drier at the temperature of 60 ℃ for 80min to obtain the novel dehumidifying antibacterial agent sample 2 with the target being recyclable.
The moisture absorption and antimicrobial properties of the desiccant antimicrobial were tested by exposing sample 2 of the prepared target novel desiccant antimicrobial to air at a relative humidity of 70% at room temperature, wherein: the dehumidifying antibacterial agent adsorbs moisture in the air until the weight of the dehumidifying antibacterial agent is not increased any more; the antibacterial performance adopts escherichia coli and staphylococcus aureus as test strains. Through the test: the moisture absorption amount is 41g, the sterilization rate of escherichia coli is 95.6%, the sterilization rate of staphylococcus aureus is 95.0%, the moisture absorption and the antibacterial performance of the novel dehumidifying antibacterial agent sample 2 are excellent, moisture can be removed through heat treatment after moisture absorption is saturated, and the dehumidifying antibacterial agent can be recycled.
Example 3: preparation of a recyclable novel dehumidifying antimicrobial agent sample 3
The invention provides a novel reusable dehumidifying antibacterial agent and a preparation method thereof, wherein the dehumidifying antibacterial agent comprises a moisture absorbent and an antibacterial agent; the target product is realized by the following steps:
first, dissolution of organic antibacterial agent and hygroscopic salt
Weighing 1.0 part by weight of 4, 5-dichloro-N-octyl-4-isothiazolin-3-one, 1.0 part by weight of dodecyl alanine, 1.0 part by weight of sulfamethoxydiazine sodium, 1.0 part by weight of didecyl dimethyl ammonium chloride, 1.0 part by weight of dimethoxy methyl benzyl aminopyrimidine sodium, 7.0 parts by weight of calcium chloride, 7.0 parts by weight of sodium carbonate and 81.0 parts by weight of ethanol at room temperature, mixing, and stirring at the rotating speed of 500r/min for 20min to obtain fully dissolved organic antibacterial agent and hygroscopic salt;
second, mixing the adsorbent, hygroscopic salt and antimicrobial agent
To the solution obtained in the first step were added, in order, 0.5 part by weight of nano silver having a particle diameter of 40nm, 0.5 part by weight of nano copper oxide having a particle diameter of 40nm and a length of 2 μm, 20.0 parts by weight of silver zeolite having a silver content of 2.0% and a pore diameter of 60 μm, 5.0 parts by weight of zinc zeolite having a zinc content of 3% and a pore diameter of 60 μm, 10.0 parts by weight of copper zeolite having a copper content of 4% and a pore diameter of 60 μm, 20.0 parts by weight of mixed type molecular sieve having a pore diameter of 1nm (wherein the weight ratio of the type A molecular sieve to the type X molecular sieve is 1:2, the type A molecular sieve has Si/Al of 1 and the type X molecular sieve has Si/Al of 1), and 9.0 parts by weight of activated carbon (having a specific surface area of 1200 m)2Per g, mean pore diameter 2nm), 15.0 parts by weight of coarse-pored silica gel in the form of C (specific surface area 600 m)2(ii)/g, average pore diameter of 10nm, pore volume of 0.9mL/g, molecular formula of mSiO2·nH2O) 15.0 parts by weight of A-type fine-pored silica gel (the specific surface area of the A-type fine-pored silica gel was 800 m)2(ii)/g, average pore diameter of 3nm, pore volume of 0.4mL/g, molecular formula of SiO2·nH2O) and 5.0 parts by weight of alumina powder with the grain diameter of 100nm, stirring for 30min at the rotating speed of 500r/min, and then carrying out ultrasonic treatment for 60min to obtain a mixed solution of a target adsorbent, hygroscopic salt and an antibacterial agent;
the following steps: the surface dispersant of the nano silver is 4-sulfocalixarene [6], the anti-discoloration agent is branched polyethyleneimine, and the mass ratio of the nano silver to the 4-sulfocalixarene [6] to the branched polyethyleneimine is 3: 5: 1, the agglomeration phenomenon and the oxidation phenomenon of nano particles can be effectively inhibited, and the excellent antibacterial activity of nano silver is maintained; the nano copper oxide surface dispersant is polyethylene glycol, wherein the mass ratio of the polyethylene glycol to the nano copper oxide is 4: 1, the agglomeration phenomenon of nano copper oxide particles can be effectively inhibited;
thirdly, preparing the target dehumidifying antibacterial agent
Placing the mixed solution of the target adsorbent, the hygroscopic salt and the antibacterial agent obtained in the second step into a 150mL three-neck quartz flask, transferring the three-neck quartz flask into a computer microwave ultrasonic ultraviolet light combined catalytic synthesizer with the model of XH-300UP, and simultaneously starting microwave, ultrasonic and ultraviolet to ensure that the mixed solution is back-heated at the constant temperature of 50 DEG CPerforming flow reaction for 30min, stopping heating when the temperature exceeds the set temperature, and continuing heating when the temperature is lower than the set temperature; the conditions of microwave, ultrasonic and ultraviolet of the synthesizer are set as follows: microwave frequency 2450MHz and microwave power 900W; the ultrasonic power is 1000W, and the ultrasonic frequency is 25 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 1 multiplied by 105μW/cm2(ii) a And finally, rotationally evaporating at the temperature of 80 ℃ and the pressure of-0.09 MPa for 60min at the speed of 60r/min to remove the solvent, and then placing in a vacuum drier at the temperature of 60 ℃ for 80min to obtain a novel dehumidifying antibacterial agent sample 3 with the target being recyclable.
The moisture absorption and antimicrobial properties of the desiccant antimicrobial were tested by exposing the prepared target novel desiccant antimicrobial sample 3 to air at a relative humidity of 70% at room temperature, wherein: the dehumidifying antibacterial agent adsorbs moisture in the air until the weight of the dehumidifying antibacterial agent is not increased any more; the antibacterial performance adopts escherichia coli and staphylococcus aureus as test strains. Through the test: the moisture absorption amount is 45g, the sterilization rate of escherichia coli is 95.3%, the sterilization rate of staphylococcus aureus is 95.1%, the moisture absorption and the antibacterial performance of the novel dehumidifying antibacterial agent sample 3 are excellent, moisture can be removed through heat treatment after moisture absorption is saturated, and the dehumidifying antibacterial agent can be recycled.
Example 4: preparation of a recyclable novel dehumidifying antimicrobial agent sample 4
The invention provides a novel reusable dehumidifying antibacterial agent and a preparation method thereof, wherein the dehumidifying antibacterial agent comprises a moisture absorbent and an antibacterial agent; the target product is realized by the following steps:
first, dissolution of organic antibacterial agent and hygroscopic salt
Weighing 1.0 part by weight of 4, 5-dichloro-N-octyl-4-isothiazolin-3-one, 1.0 part by weight of polyhexamethylene guanidine, 0.5 part by weight of coconut diethanolamide, 0.5 part by weight of dodecyl alanine, 1.0 part by weight of sodium sulfamethoxydiazine, 0.5 part by weight of didecyldimethylammonium chloride, 1.0 part by weight of sodium dimethoxymethylbenzamide, 10.0 parts by weight of calcium chloride, 5.0 parts by weight of sodium carbonate and 79.5 parts by weight of ethanol, mixing at room temperature, and stirring at the rotating speed of 500r/min for 40min to obtain fully dissolved organic antibacterial agent and hygroscopic salt;
second, mixing the adsorbent, hygroscopic salt and antimicrobial agent
To the solution obtained in the first step were added, in order, 1.0 part by weight of nano silver having a particle diameter of 40nm, 1.0 part by weight of nano copper oxide having a particle diameter of 40nm and a length of 2 μm, 20.0 parts by weight of silver zeolite having a silver content of 2.0% and a pore diameter of 60 μm, 10.0 parts by weight of zinc zeolite having a zinc content of 3% and a pore diameter of 60 μm, 10.0 parts by weight of copper zeolite having a copper content of 4% and a pore diameter of 60 μm, 20.0 parts by weight of mixed type molecular sieve having a pore diameter of 1nm (wherein the weight ratio of the type A molecular sieve to the type X molecular sieve is 1:2, the type A molecular sieve has Si/Al of 1 and the type X molecular sieve has Si/Al of 1), and 10.0 parts by weight of activated carbon (having a specific surface area of 1200 m)2Per g, mean pore diameter 2nm), 10.0 parts by weight of coarse-pored silica gel in the form of C (specific surface area 600 m)2(ii)/g, average pore diameter of 10nm, pore volume of 0.9mL/g, molecular formula of mSiO2·nH2O), 10.0 parts by weight of A-type fine-pored silica gel (the specific surface area of the A-type fine-pored silica gel was 800 m)2(ii)/g, average pore diameter of 3nm, pore volume of 0.4mL/g, molecular formula of SiO2·nH2O) and 8.0 parts by weight of alumina powder with the grain diameter of 100nm, stirring for 30min at the rotating speed of 500r/min, and then carrying out ultrasonic treatment for 60min to obtain a mixed solution of a target adsorbent, a hygroscopic salt and an antibacterial agent;
the following steps: the surface dispersant of the nano silver is 4-sulfocalixarene [6], the anti-discoloration agent is branched polyethyleneimine, and the mass ratio of the nano silver to the 4-sulfocalixarene [6] to the branched polyethyleneimine is 3: 5: 1, the agglomeration phenomenon and the oxidation phenomenon of nano particles can be effectively inhibited, and the excellent antibacterial activity of nano silver is maintained; the nano copper oxide surface dispersant is polyethylene glycol, wherein the mass ratio of the polyethylene glycol to the nano copper oxide is 4: 1, the agglomeration phenomenon of nano copper oxide particles can be effectively inhibited;
thirdly, preparing the target dehumidifying antibacterial agent
The mixture of the objective adsorbent, hygroscopic salt and antibacterial agent obtained in the second step was placed in a 150mL three-necked quartz flask, which was then transferred toIn a computer microwave ultrasonic ultraviolet light combined catalytic synthesizer with the model of XH-300UP, simultaneously starting microwave, ultrasonic and ultraviolet light, leading the mixed solution to carry out reflux reaction for 30min at constant temperature of 50 ℃, stopping heating when the temperature exceeds the set temperature, and continuing heating when the temperature is lower than the set temperature; the conditions of microwave, ultrasonic and ultraviolet of the synthesizer are set as follows: microwave frequency 2450MHz and microwave power 900W; the ultrasonic power is 1000W, and the ultrasonic frequency is 25 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 1 multiplied by 105μW/cm2(ii) a And finally, rotationally evaporating at the temperature of 80 ℃ and the pressure of-0.09 MPa for 60min at the speed of 60r/min to remove the solvent, and then placing in a vacuum drier at the temperature of 60 ℃ for 80min to obtain a novel dehumidifying antibacterial agent sample 4 with the target being recyclable.
The moisture absorption and antimicrobial properties of the desiccant antimicrobial were tested by exposing the prepared target novel desiccant antimicrobial sample 4 to air at a relative humidity of 70% at room temperature, wherein: the dehumidifying antibacterial agent adsorbs moisture in the air until the weight of the dehumidifying antibacterial agent is not increased any more; the antibacterial performance adopts escherichia coli and staphylococcus aureus as test strains. Through the test: the moisture absorption amount is 36g, the sterilization rate of escherichia coli is 97.8%, the sterilization rate of staphylococcus aureus is 96.9%, the moisture absorption and the antibacterial performance of the novel dehumidifying antibacterial agent sample 4 are excellent, moisture can be removed through heat treatment after moisture absorption is saturated, and the dehumidifying antibacterial agent can be recycled.
Example 5: preparation of a recyclable novel dehumidifying antimicrobial sample 5
The invention provides a novel reusable dehumidifying antibacterial agent and a preparation method thereof, wherein the dehumidifying antibacterial agent comprises a moisture absorbent and an antibacterial agent; the target product is realized by the following steps:
first, dissolution of organic antibacterial agent and hygroscopic salt
Weighing 0.5 part by weight of 4, 5-dichloro-N-octyl-4-isothiazolin-3-one, 1.0 part by weight of polyhexamethylene guanidine, 1.0 part by weight of coconut diethanolamide, 1.0 part by weight of dodecyl alanine, 1.0 part by weight of sodium sulfamethoxydiazine, 0.5 part by weight of didecyldimethylammonium chloride, 0.5 part by weight of sodium dimethoxymethylbenzylaminopyrimidine, 5.0 parts by weight of calcium chloride, 5.0 parts by weight of sodium carbonate and 84.5 parts by weight of ethanol at room temperature, mixing, and stirring at the rotating speed of 500r/min for 40min to obtain fully dissolved organic antibacterial agent and hygroscopic salt;
second, mixing the adsorbent, hygroscopic salt and antimicrobial agent
To the solution obtained in the first step were added, in order, 1.0 part by weight of nano silver having a particle diameter of 50nm, 1.0 part by weight of nano copper oxide having a particle diameter of 50nm and a length of 2 μm, 30.0 parts by weight of silver zeolite having a silver content of 2.0% and a pore diameter of 60 μm, 8.0 parts by weight of zinc zeolite having a zinc content of 3% and a pore diameter of 60 μm, 5.0 parts by weight of copper zeolite having a copper content of 4% and a pore diameter of 60 μm, 15.0 parts by weight of mixed type molecular sieve having a pore diameter of 1nm (wherein the weight ratio of the type A molecular sieve to the type X molecular sieve is 2:3, the type A molecular sieve has Si/Al of 1 and the type X molecular sieve has Si/Al of 1), and 15.0 parts by weight of activated carbon (having a specific surface area of 1200 m)2Per g, mean pore diameter 2nm), 5.0 parts by weight of coarse-pored silica gel in the form of C (specific surface area 600 m)2(ii)/g, average pore diameter of 10nm, pore volume of 0.9mL/g, molecular formula of mSiO2·nH2O) 15.0 parts by weight of A-type fine-pored silica gel (the specific surface area of the A-type fine-pored silica gel was 800 m)2(ii)/g, average pore diameter of 3nm, pore volume of 0.4mL/g, molecular formula of SiO2·nH2O) and 5.0 parts by weight of alumina powder with the grain diameter of 100nm, stirring for 30min at the rotating speed of 500r/min, and then carrying out ultrasonic treatment for 60min to obtain a mixed solution of a target adsorbent, hygroscopic salt and an antibacterial agent;
the following steps: the surface dispersant of the nano silver is 4-sulfocalixarene [6], the anti-discoloration agent is branched polyethyleneimine, and the mass ratio of the nano silver to the 4-sulfocalixarene [6] to the branched polyethyleneimine is 3: 5: 1, the agglomeration phenomenon and the oxidation phenomenon of nano particles can be effectively inhibited, and the excellent antibacterial activity of nano silver is maintained; the nano copper oxide surface dispersant is polyethylene glycol, wherein the mass ratio of the polyethylene glycol to the nano copper oxide is 4: 1, the agglomeration phenomenon of nano copper oxide particles can be effectively inhibited;
thirdly, preparing the target dehumidifying antibacterial agent
Will be secondPlacing the mixed solution of the target adsorbent, the hygroscopic salt and the antibacterial agent obtained in the step into a 150mL three-neck quartz flask, then transferring the three-neck quartz flask into an XH-300UP computer microwave ultrasonic ultraviolet light combined catalytic synthesizer, simultaneously starting microwave, ultrasonic and ultraviolet light, enabling the mixed solution to perform constant temperature reflux reaction for 30min at the temperature of 50 ℃, stopping heating when the temperature exceeds a set temperature, and continuing heating when the temperature is lower than the set temperature; the conditions of microwave, ultrasonic and ultraviolet of the synthesizer are set as follows: microwave frequency 2450MHz and microwave power 900W; the ultrasonic power is 1000W, and the ultrasonic frequency is 25 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 1 multiplied by 105μW/cm2(ii) a And finally, rotationally evaporating at the temperature of 80 ℃ and the pressure of-0.09 MPa for 60min at the speed of 60r/min to remove the solvent, and then placing in a vacuum drier at the temperature of 60 ℃ for 80min to obtain the novel dehumidifying antibacterial agent sample 5 which can be recycled.
The moisture absorption and antimicrobial properties of the desiccant antimicrobial were tested by exposing the prepared sample 5 of the target novel desiccant antimicrobial to air at a relative humidity of 70% at room temperature, wherein: the dehumidifying antibacterial agent adsorbs moisture in the air until the weight of the dehumidifying antibacterial agent is not increased any more; the antibacterial performance adopts escherichia coli and staphylococcus aureus as test strains. Through the test: the moisture absorption amount is 40g, the sterilization rate of escherichia coli is 98.3%, the sterilization rate of staphylococcus aureus is 97.8%, the moisture absorption and the antibacterial performance of the novel dehumidifying antibacterial agent sample 5 are excellent, moisture can be removed through heat treatment after moisture absorption is saturated, and the dehumidifying antibacterial agent can be recycled.
Example 6: preparation of a recyclable novel dehumidifying antimicrobial agent sample 6
The invention provides a novel reusable dehumidifying antibacterial agent and a preparation method thereof, wherein the dehumidifying antibacterial agent comprises a moisture absorbent and an antibacterial agent; the target product is realized by the following steps:
first, dissolution of organic antibacterial agent and hygroscopic salt
Weighing 0.5 part by weight of 4, 5-dichloro-N-octyl-4-isothiazolin-3-one, 0.5 part by weight of polyhexamethylene guanidine, 1.0 part by weight of coconut diethanolamide, 1.0 part by weight of dodecyl alanine, 1.0 part by weight of sodium sulfamethoxydiazine, 0.5 part by weight of didecyldimethylammonium chloride, 0.5 part by weight of sodium dimethoxymethylbenzylaminopyrimidine, 5.0 parts by weight of calcium chloride, 5.0 parts by weight of sodium carbonate and 85.0 parts by weight of ethanol at room temperature, mixing, and stirring at the rotating speed of 500r/min for 50min to obtain fully dissolved organic antibacterial agent and hygroscopic salt;
second, mixing the adsorbent, hygroscopic salt and antimicrobial agent
To the solution obtained in the first step were added, in order, 0.5 part by weight of nano silver having a particle diameter of 50nm, 0.5 part by weight of nano copper oxide having a particle diameter of 50nm and a length of 2 μm, 25 parts by weight of silver zeolite having a silver content of 2.0% and a pore diameter of 60 μm, 7.0 parts by weight of zinc zeolite having a zinc content of 3% and a pore diameter of 60 μm, 7.0 parts by weight of copper zeolite having a copper content of 4% and a pore diameter of 60 μm, 20.0 parts by weight of mixed type molecular sieve having a pore diameter of 1nm (wherein the weight ratio of the type A molecular sieve to the type X molecular sieve is 2:3, the type A molecular sieve has Si/Al of 1, and the type X molecular sieve has Si/Al of 1), and 5.0 parts by weight of activated carbon (having a specific surface area of 1200 m)2Per g, mean pore diameter 2nm), 15.0 parts by weight of coarse-pored silica gel in the form of C (specific surface area 600 m)2(ii)/g, average pore diameter of 10nm, pore volume of 0.9mL/g, molecular formula of mSiO2·nH2O) 15.0 parts by weight of A-type fine-pored silica gel (the specific surface area of the A-type fine-pored silica gel was 800 m)2(ii)/g, average pore diameter of 3nm, pore volume of 0.4mL/g, molecular formula of SiO2·nH2O) and 5.0 parts by weight of alumina powder with the grain diameter of 100nm, stirring for 30min at the rotating speed of 500r/min, and then carrying out ultrasonic treatment for 60min to obtain a mixed solution of a target adsorbent, hygroscopic salt and an antibacterial agent;
the following steps: the surface dispersant of the nano silver is 4-sulfocalixarene [6], the anti-discoloration agent is branched polyethyleneimine, and the mass ratio of the nano silver to the 4-sulfocalixarene [6] to the branched polyethyleneimine is 3: 5: 1, the agglomeration phenomenon and the oxidation phenomenon of nano particles can be effectively inhibited, and the excellent antibacterial activity of nano silver is maintained; the nano copper oxide surface dispersant is polyethylene glycol, wherein the mass ratio of the polyethylene glycol to the nano copper oxide is 4: 1, the agglomeration phenomenon of nano copper oxide particles can be effectively inhibited;
thirdly, preparing the target dehumidifying antibacterial agent
Placing the mixed solution of the target adsorbent, the hygroscopic salt and the antibacterial agent obtained in the second step into a 150mL three-neck quartz flask, then transferring the three-neck quartz flask into an XH-300UP computer microwave ultrasonic ultraviolet light combined catalytic synthesizer, simultaneously starting microwave, ultrasound and ultraviolet, enabling the mixed solution to perform reflux reaction at a constant temperature of 50 ℃ for 30min, stopping heating when the temperature exceeds a set temperature, and continuing heating when the temperature is lower than the set temperature; the conditions of microwave, ultrasonic and ultraviolet of the synthesizer are set as follows: microwave frequency 2450MHz and microwave power 900W; the ultrasonic power is 1000W, and the ultrasonic frequency is 25 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 1 multiplied by 105μW/cm2(ii) a And finally, rotationally evaporating at the temperature of 80 ℃ and the pressure of-0.09 MPa for 60min at the speed of 60r/min to remove the solvent, and then placing in a vacuum drier at the temperature of 60 ℃ for 80min to obtain a novel dehumidifying antibacterial agent sample 6 with the target being recyclable.
The moisture absorption and antimicrobial properties of the desiccant antimicrobial were tested by exposing the prepared sample of the target novel desiccant antimicrobial 6 to air at a relative humidity of 70% at room temperature, said: the dehumidifying antibacterial agent adsorbs moisture in the air until the weight of the dehumidifying antibacterial agent is not increased any more; the antibacterial performance adopts escherichia coli and staphylococcus aureus as test strains. Through the test: the moisture absorption amount is 44g, the sterilization rate of escherichia coli is 98.1%, the sterilization rate of staphylococcus aureus is 98.0%, the moisture absorption and the antibacterial performance of the novel dehumidifying antibacterial agent sample 6 are excellent, and after moisture absorption is saturated, moisture can be removed through heat treatment, so that the dehumidifying antibacterial agent can be recycled.
TABLE 1 tables of the test results of the performance of the samples of the dehumidifying antibacterial agent in each example
Claims (2)
1. The invention provides a novel reusable dehumidifying antibacterial agent and a preparation method thereof, wherein the dehumidifying antibacterial agent comprises a moisture absorbent and an antibacterial agent; the moisture absorbent comprises an adsorbent and a moisture absorbent salt, the antibacterial agent comprises an organic antibacterial agent and an inorganic nano antibacterial agent, and the target product is realized by the following steps:
first, dissolution of organic antibacterial agent and hygroscopic salt
Weighing 0.0-1.0 part by weight of 4, 5-dichloro-N-octyl-4-isothiazolin-3-one, 0.0-1.0 part by weight of polyhexamethylene guanidine, 0.0-1.0 part by weight of coconut diethanolamide, 0.0-1.0 part by weight of dodecyl alanine, 0.0-1.0 part by weight of sulfamethoxydiazine sodium, 0.0-1.0 part by weight of didecyl dimethyl ammonium chloride, 0.0-1.0 part by weight of dimethoxy methyl benzyl amino pyrimidine sodium, 0.0-1.0 part by weight of clavulanate potassium, 5.0-10.0 parts by weight of calcium chloride, 5.0-10.0 parts by weight of sodium carbonate and 10.0-80.0 parts by weight of solvent at room temperature, mixing, stirring at a rotating speed of 200-700 r/min for 10-60 min to obtain fully dissolved organic antibacterial agent and hygroscopic salt, wherein the solvent is water or ethanol or the volume ratio of ethanol to water is (3-5): (1-3) mixing the solution;
second, mixing the adsorbent, hygroscopic salt and antimicrobial agent
Adding 0.0-1.0 part by weight of nano silver, 0.0-1.0 part by weight of nano copper oxide, 20.0-30.0 parts by weight of silver zeolite, 5.0-10.0 parts by weight of zinc zeolite, 5.0-10.0 parts by weight of copper zeolite, 5.0-20.0 parts by weight of microporous molecular sieve, 5.0-20.0 parts by weight of active carbon, 5.0-20.0 parts by weight of C-type coarse pore silica gel, 5.0-20.0 parts by weight of A-type fine pore silica gel and 5.0-10.0 parts by weight of alumina powder into the solution obtained in the first step in sequence, firstly stirring at the rotating speed of 200-700 r/min for 10-60 min, and then carrying out ultrasonic treatment for 30-100 min to obtain a mixed solution of a target adsorbent, a hygroscopic salt and an antibacterial agent;
thirdly, preparing the target dehumidifying antibacterial agent
Placing the mixed solution of the target adsorbent, the hygroscopic salt and the antibacterial agent obtained in the second step into a 50-200 mL three-neck quartz flask, and transferring the three-neck quartz flask to a computer microwave ultrasonic ultraviolet light combination with the model of XH-300UPIn a catalytic synthesizer, simultaneously starting microwave, ultrasound and ultraviolet to enable the mixed solution to perform reflux reaction at a constant temperature of 10-100 ℃ for 10-60 min, stopping heating when the temperature exceeds a set temperature, and continuing heating when the temperature is lower than the set temperature; the conditions of microwave, ultrasonic and ultraviolet of the synthesizer are set as follows: the microwave frequency is 2450MHz, and the microwave power is 1-1000W; the ultrasonic power is 0-1500W, and the ultrasonic frequency is 24-26 KHz; the ultraviolet wavelength is 365nm, the power is 250W, and the measurement range is 0.1 multiplied by 105μW/cm2～1.999×105μW/cm2(ii) a And finally, under the conditions of-0.09 MPa and 50-90 ℃, rotationally evaporating at the speed of 50-100 r/min for 30-120 min to remove the solvent, and placing in a vacuum dryer at the temperature of 40-80 ℃ for 10-100 min to obtain the target dehumidifying antibacterial agent.
2. The novel reusable dehumidifying antibacterial agent and the preparation method thereof according to claim 1, wherein: in the second step, an adsorbent, a hygroscopic salt and an antibacterial agent are mixed, wherein: the particle size of the nano silver is 5-50 nm, and the surface dispersant is 4-sulfocalixarene [6]]The anti-discoloration agent is branched polyethyleneimine, wherein the nano silver and the 4-sulfocalixarene [6]]And branched polyethyleneimine in a mass ratio of (3-5): (5-8): 1, the agglomeration phenomenon and the oxidation phenomenon of nano particles can be effectively inhibited, and the excellent antibacterial activity of nano silver is maintained; the particle size of the nano copper oxide is 30-50 nm, the length of the nano copper oxide is 1-2 mu m, the surface dispersing agent is polyethylene glycol, and the mass ratio of the polyethylene glycol to the nano copper oxide is (3-5): 1, the agglomeration phenomenon of nano copper oxide particles can be effectively inhibited; the silver content of the silver zeolite is 0.5-2.5%, and the aperture is 50-100 mu m; the zinc content of the zinc zeolite is 1% -5%, and the aperture is 50-100 mu m; the copper content of the copper zeolite is 1% -5%, and the aperture is 50-100 mu m; the microporous molecular sieve is a mixed molecular sieve with the weight ratio of the A-type molecular sieve to the X-type molecular sieve being (1-3) to (1-3), and the average pore diameter is 0.5-2.0 nm, wherein the Si/Al of the A-type molecular sieve is 1, and the Si/Al of the X-type molecular sieve is 1.0-1.5; the specific surface area of the activated carbon is 200-1500 m2(ii)/g, the average pore diameter is 1-50 nm; the specific surface area of the C-type coarse-pore silica gel is 300-600 m2Per g, mean pore diameter of 8About 16nm, the pore volume of 0.80-1.00 mL/g and the molecular formula of mSiO2·nH2O; the specific surface area of the A-type fine-pore silica gel is 650-800 m2(ii) per gram, the average pore diameter is 2-3 nm, the pore volume is 0.35-0.45 mL/g, and the molecular formula is SiO2·nH2O; the alumina powder has a particle size of 50 to 200 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010991040.2A CN112136821A (en) | 2020-09-20 | 2020-09-20 | Reusable novel dehumidifying antibacterial agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010991040.2A CN112136821A (en) | 2020-09-20 | 2020-09-20 | Reusable novel dehumidifying antibacterial agent and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112136821A true CN112136821A (en) | 2020-12-29 |
Family
ID=73892458
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010991040.2A Pending CN112136821A (en) | 2020-09-20 | 2020-09-20 | Reusable novel dehumidifying antibacterial agent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112136821A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0585174A1 (en) * | 1992-08-26 | 1994-03-02 | Ram Lavie | Apparatus for a rapid drying of compressed air |
| CN107118654A (en) * | 2017-05-11 | 2017-09-01 | 南通美亚新型活性炭制品有限公司 | A kind of antibacterial moisture adsorption and releasing coating and manufacture method |
| CN109380298A (en) * | 2017-08-08 | 2019-02-26 | 电子科技大学中山学院 | Colorless and transparent anti-color-change nano-silver composite antibacterial agent solution |
| CN110432420A (en) * | 2019-03-15 | 2019-11-12 | 珠海市自然之旅生物技术有限公司 | Plant-derived composite mildewproof bacteriostatic agent and its preparation method and application |
| CN111670912A (en) * | 2020-06-28 | 2020-09-18 | 南京优写智能科技有限公司 | Synthetic method of water-soluble antibacterial mildew inhibitor containing graphene oxide and nano-silver |
-
2020
- 2020-09-20 CN CN202010991040.2A patent/CN112136821A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0585174A1 (en) * | 1992-08-26 | 1994-03-02 | Ram Lavie | Apparatus for a rapid drying of compressed air |
| CN107118654A (en) * | 2017-05-11 | 2017-09-01 | 南通美亚新型活性炭制品有限公司 | A kind of antibacterial moisture adsorption and releasing coating and manufacture method |
| CN109380298A (en) * | 2017-08-08 | 2019-02-26 | 电子科技大学中山学院 | Colorless and transparent anti-color-change nano-silver composite antibacterial agent solution |
| CN110432420A (en) * | 2019-03-15 | 2019-11-12 | 珠海市自然之旅生物技术有限公司 | Plant-derived composite mildewproof bacteriostatic agent and its preparation method and application |
| CN111670912A (en) * | 2020-06-28 | 2020-09-18 | 南京优写智能科技有限公司 | Synthetic method of water-soluble antibacterial mildew inhibitor containing graphene oxide and nano-silver |
Non-Patent Citations (1)
| Title |
|---|
| 丁浩等: "《纳米抗菌技术》", 31 January 2008, 化学工业出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20210197172A1 (en) | Regenerative adsorbents of modified amines on solid supports | |
| JP6273015B2 (en) | Renewable adsorbent of modified amines on nanostructured supports | |
| CN101910062B (en) | Aluminum silicate complex, and high-performance adsorbent comprising the same | |
| Tan et al. | Composite salt in MIL-101 (Cr) with high water uptake and fast adsorption kinetics for adsorption heat pumps | |
| Rekha et al. | Unprecedented adsorptive removal of Cr 2 O 7 2− and methyl orange by using a low surface area organosilica | |
| US20090211453A1 (en) | Filtration Media for the Removal of Basic Molecular Contaminants for Use in a Clean Environment | |
| JP2006240956A (en) | Amorphous aluminum silicate, adsorbent having the same, dehumidifying rotor and air conditioner | |
| US11045785B2 (en) | Metal-organic framework, method for preparing the same, and adsorption device employing the same | |
| Dinda et al. | A study on zeolite-based adsorbents for CO 2 capture | |
| Chen et al. | Mesoporous silica impregnated with organoamines for post‐combustion CO2 capture: a comparison of introduced amine types | |
| Ma et al. | Carbon dioxide adsorption using amine-functionalized mesocellular siliceous foams | |
| Li et al. | Toluene and water vapor adsorption characteristics and selectivity on hydrophobic resin-based activated carbon | |
| WO2010082456A1 (en) | Regenerative moisture absorbent | |
| JP2021062344A (en) | Prussian blue derivative-containing composite using silicon oxide as substrate, ammonia absorption/desorption method using the composite and ammonia recovery apparatus | |
| JP5392121B2 (en) | Method for producing hygroscopic agent | |
| CN112136821A (en) | Reusable novel dehumidifying antibacterial agent and preparation method thereof | |
| JP5140278B2 (en) | Desiccant material and air dehumidification method using the same | |
| JP2001334120A (en) | Moisture absorbent and moisture absorption element using the same | |
| JP2009233647A (en) | Natural zeolite for ammonia adsorption to which sulfate group is imparted, and its manufacturing method | |
| JP3050139B2 (en) | Activated carbon reforming method | |
| JP2024508533A (en) | functionalized hydrogel | |
| Yang et al. | Preparation of triethylenetetramine‐modified zirconosilicate molecular sieve for carbon dioxide adsorption | |
| Mittal et al. | Development of high efficacy super-porous hydrogel composites-based polymer desiccants to capture water vapors from moist air | |
| Bai et al. | Performance evaluation of PVA/PEO/LiCl composite as coated heat exchangers desiccants | |
| Sivadas et al. | Supramolecular β-cyclodextrin–aniline system: a new class of amine on solid support for carbon dioxide capture with high amine efficiency |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |