CN115316384B - Antibacterial slow-release granule and preparation method thereof - Google Patents
Antibacterial slow-release granule and preparation method thereof Download PDFInfo
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- CN115316384B CN115316384B CN202211035706.2A CN202211035706A CN115316384B CN 115316384 B CN115316384 B CN 115316384B CN 202211035706 A CN202211035706 A CN 202211035706A CN 115316384 B CN115316384 B CN 115316384B
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 79
- 239000008187 granular material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 48
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 32
- 239000003463 adsorbent Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000000853 adhesive Substances 0.000 claims abstract description 10
- 230000001070 adhesive effect Effects 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 36
- 239000011347 resin Substances 0.000 claims description 36
- 229920005989 resin Polymers 0.000 claims description 35
- 239000000243 solution Substances 0.000 claims description 34
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 33
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 33
- 239000010410 layer Substances 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 230000000845 anti-microbial effect Effects 0.000 claims description 20
- 239000004599 antimicrobial Substances 0.000 claims description 20
- 239000011248 coating agent Substances 0.000 claims description 19
- 239000011247 coating layer Substances 0.000 claims description 19
- 238000000576 coating method Methods 0.000 claims description 19
- 238000013268 sustained release Methods 0.000 claims description 19
- 239000012730 sustained-release form Substances 0.000 claims description 19
- 238000002791 soaking Methods 0.000 claims description 17
- -1 alkyl quaternary ammonium salt Chemical class 0.000 claims description 16
- 239000000839 emulsion Substances 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 12
- 239000001913 cellulose Substances 0.000 claims description 7
- 229920002678 cellulose Polymers 0.000 claims description 7
- 235000010980 cellulose Nutrition 0.000 claims description 7
- 229920002472 Starch Polymers 0.000 claims description 6
- 235000019270 ammonium chloride Nutrition 0.000 claims description 6
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- 235000019698 starch Nutrition 0.000 claims description 6
- 239000008107 starch Substances 0.000 claims description 6
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 5
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 5
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 5
- UXFBJATYVZPQTG-UHFFFAOYSA-N dimethoxysilicon Chemical compound CO[Si]OC UXFBJATYVZPQTG-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 2
- 229920000178 Acrylic resin Polymers 0.000 claims description 2
- 239000004925 Acrylic resin Substances 0.000 claims description 2
- DJDCAVIWCPSDKS-UHFFFAOYSA-M CCCCCCCCCCCCCCCCCCCCCC[N+](C)(CCCCCCCCCCCCCCCCCCCCCC)CCC[SiH](OC)OC.[Cl-] Chemical compound CCCCCCCCCCCCCCCCCCCCCC[N+](C)(CCCCCCCCCCCCCCCCCCCCCC)CCC[SiH](OC)OC.[Cl-] DJDCAVIWCPSDKS-UHFFFAOYSA-M 0.000 claims description 2
- XTAFLMIQGZBUNN-UHFFFAOYSA-M CCCCCCCCCCCCCCCCCC[N+](C)(CCCCCCCCCCCCCCCCCC)CCC[SiH](OC)OC.[Cl-] Chemical compound CCCCCCCCCCCCCCCCCC[N+](C)(CCCCCCCCCCCCCCCCCC)CCC[SiH](OC)OC.[Cl-] XTAFLMIQGZBUNN-UHFFFAOYSA-M 0.000 claims description 2
- XXKKNRFXTOSEOE-UHFFFAOYSA-M CCCCCCCCCCCCCCCC[N+](C)(CCCCCCCCCCCCCCCC)CCC[SiH](OC)OC.[Cl-] Chemical compound CCCCCCCCCCCCCCCC[N+](C)(CCCCCCCCCCCCCCCC)CCC[SiH](OC)OC.[Cl-] XXKKNRFXTOSEOE-UHFFFAOYSA-M 0.000 claims description 2
- UNSYLLOKGUWESH-UHFFFAOYSA-M CCCCCCCCCCCCCC[N+](C)(CCCCCCCCCCCCCC)CCC[SiH](OC)OC.[Cl-] Chemical compound CCCCCCCCCCCCCC[N+](C)(CCCCCCCCCCCCCC)CCC[SiH](OC)OC.[Cl-] UNSYLLOKGUWESH-UHFFFAOYSA-M 0.000 claims description 2
- IKKSLZZVRCRVBC-UHFFFAOYSA-M CCCCCCCCCCCC[N+](C)(CCCCCCCCCCCC)CCC[SiH](OC)OC.[Cl-] Chemical compound CCCCCCCCCCCC[N+](C)(CCCCCCCCCCCC)CCC[SiH](OC)OC.[Cl-] IKKSLZZVRCRVBC-UHFFFAOYSA-M 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 2
- 229920000881 Modified starch Polymers 0.000 claims description 2
- 239000004368 Modified starch Substances 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- SOPZLXDKMICEMF-UHFFFAOYSA-N diethoxysilicon Chemical compound CCO[Si]OCC SOPZLXDKMICEMF-UHFFFAOYSA-N 0.000 claims description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 2
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 2
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 2
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 2
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 2
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 2
- 239000011630 iodine Substances 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 235000019426 modified starch Nutrition 0.000 claims description 2
- 150000002978 peroxides Chemical class 0.000 claims description 2
- 229920005749 polyurethane resin Polymers 0.000 claims description 2
- 239000007771 core particle Substances 0.000 claims 6
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 claims 2
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 description 20
- 230000001954 sterilising effect Effects 0.000 description 17
- 238000004659 sterilization and disinfection Methods 0.000 description 13
- 239000000463 material Substances 0.000 description 11
- 239000007787 solid Substances 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- 239000012266 salt solution Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 229920002635 polyurethane Polymers 0.000 description 4
- 239000004814 polyurethane Substances 0.000 description 4
- 230000003115 biocidal effect Effects 0.000 description 3
- 230000001877 deodorizing effect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000013095 identification testing Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000000159 acid neutralizing agent Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000003361 porogen Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005563 spheronization Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000003206 sterilizing agent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
- 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
- A01N25/26—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 in coated particulate form
-
- 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
- A01N55/00—Biocides, pest repellants or attractants, or plant growth regulators, containing organic compounds containing elements other than carbon, hydrogen, halogen, oxygen, nitrogen and sulfur
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P3/00—Fungicides
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Environmental Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Medicinal Preparation (AREA)
Abstract
An antibacterial slow-release granule and a preparation method thereof, wherein the antibacterial slow-release granule comprises an antibacterial inner core, and the antibacterial inner core comprises the following raw materials: antibacterial agent, forming pore-forming agent, adsorbent and adhesive. The slow-release antibacterial agent has long-acting slow-release characteristic, and can maintain long-time antibacterial effect in environments such as liquid. The antibacterial slow-release particles do not change the particle volume in the slow-release process, and only release the antibacterial agent.
Description
Technical Field
The invention relates to the technical field of antibiosis, in particular to antibiosis slow-release particles and a preparation method thereof.
Background
Along with the increasing importance of people on daily life health, epidemic prevention has become an indispensable part of people's life, and the significance of antibiosis and sterilization is particularly important. Antibacterial agents have been found everywhere in life, but the long-acting property and deodorizing property and antibacterial effect of the existing antibacterial agents are poor, and a solution is needed.
Disclosure of Invention
According to a first aspect, in an embodiment, there is provided an antimicrobial slow release granule comprising an antimicrobial core comprising the following materials:
antibacterial agent, forming pore-forming agent, adsorbent and adhesive.
According to a second aspect, in an embodiment, there is provided a method for preparing the antibacterial sustained-release particles of any one of the first aspects, comprising:
The preparation method comprises the steps of (1) mixing raw materials and water according to the formula amount to prepare a granular antibacterial inner core;
and the coating step comprises the steps of soaking the antibacterial inner core at least once in a polyvinyl alcohol solution and at least once in a resin solution, so that at least part of the surface of the antibacterial inner core is coated with at least one coating layer, and the antibacterial slow-release particles are obtained.
According to the antibacterial slow-release particles and the preparation method thereof, the slow-release antibacterial agent has long-acting slow-release characteristics, and can maintain long-time antibacterial efficacy in environments such as liquid.
In one embodiment, the antimicrobial slow release particles do not change particle volume during the slow release process, releasing only the antimicrobial agent.
Drawings
FIG. 1 is a photograph of the solution obtained after 1 day of sustained release as measured by a quaternary ammonium salt test paper;
FIG. 2 is a photograph of the solution obtained after 2 days of sustained release as measured by a quaternary ammonium salt test paper;
FIG. 3 is a photograph of the solution obtained after 3 days of sustained release as measured by a quaternary ammonium salt test paper;
FIG. 4 is a photograph of the solution obtained after 5 days of sustained release as measured by a quaternary ammonium salt test paper;
FIG. 5 is a diagram of the antibacterial sustained-release particles prepared in example 1;
FIG. 6 is a diagram of the antibacterial sustained-release granule obtained in comparative example 1.
Detailed Description
The application will be described in further detail below with reference to the drawings by means of specific embodiments. In the following embodiments, numerous specific details are set forth in order to provide a better understanding of the present application. However, one skilled in the art will readily recognize that some of the features may be omitted in various situations, or replaced by other materials, methods. In some instances, related operations of the present application have not been shown or described in the specification in order to avoid obscuring the core portions of the present application, and may be unnecessary to persons skilled in the art from a detailed description of the related operations, which may be presented in the description and general knowledge of one skilled in the art.
Furthermore, the described features, operations, or characteristics of the description may be combined in any suitable manner in various embodiments. Also, various steps or acts in the method descriptions may be interchanged or modified in a manner apparent to those of ordinary skill in the art. Thus, the various orders in the description and drawings are for clarity of description of only certain embodiments, and are not meant to be required orders unless otherwise indicated.
The numbering of the components itself, e.g. "first", "second", etc., is used herein merely to distinguish between the described objects and does not have any sequential or technical meaning.
According to a first aspect, in an embodiment, there is provided an antimicrobial slow release granule comprising an antimicrobial core comprising the following materials:
antibacterial agent, forming pore-forming agent, adsorbent and adhesive.
The antibacterial agent has antibacterial effect.
The forming pore-forming agent plays a role in forming and pore-forming.
The adsorbent mainly plays an adsorption role.
The adhesive mainly plays a role in adhesion.
In one embodiment, the antimicrobial core comprises the following materials by mass:
2-8 parts of antibacterial agent, 30-50 parts of forming pore-forming agent, 10-15 parts of adsorbent and 1-5 parts of adhesive.
In one embodiment, the antimicrobial agent includes, but is not limited to, at least one of quaternary ammonium based antimicrobial agents, organoguanidine based antimicrobial agents, metal ion based antimicrobial agents, chlorine based antimicrobial agents, peroxide based antimicrobial agents, iodine based antimicrobial agents, phenolic based antimicrobial agents, ethylene oxide based antimicrobial agents. The antibacterial agent suitable for the present invention is not limited and may be any antibacterial agent.
In one embodiment, the quaternary ammonium salt comprises a silicone quaternary ammonium salt.
In one embodiment, the quaternary ammonium salt includes, but is not limited to, at least one of a di-long alkyl quaternary ammonium salt, a mono-long alkyl quaternary ammonium salt.
In one embodiment, the bis-long chain alkyl quaternary ammonium salt includes, but is not limited to, at least one of methyl bis-behenyl [3- (dimethoxysilyl) propyl ] ammonium chloride (also known as methyl bis-behenyl [3- (diethoxysilyl) propyl ] ammonium chloride), methyl bis-octadecyl [3- (dimethoxysilyl) propyl ] ammonium chloride (also known as methyl bis-octadecyl [3- (diethoxysilyl) propyl ] ammonium chloride), methyl bis-hexadecyl [3- (dimethoxysilyl) propyl ] ammonium chloride, methyl bis-tetradecyl [3- (dimethoxysilyl) propyl ] ammonium chloride, methyl bis-dodecyl [3- (dimethoxysilyl) propyl ] ammonium chloride.
In one embodiment, the mono-long alkyl quaternary ammonium salt includes, but is not limited to, at least one of methyl dodecyl [3- (dimethoxy silicon based) propyl ] ammonium chloride, methyl tetradecyl [3- (dimethoxy silicon based) propyl ] ammonium chloride, methyl dodecyl [3- (diethoxy silicon based) propyl ] ammonium chloride.
In one embodiment, slow release particles are typically prepared using a solution containing an antimicrobial agent, typically comprising a quaternary ammonium salt and a solvent, as a starting material. Solvents include, but are not limited to, water.
In one embodiment, the mass concentration of quaternary ammonium salt in the antimicrobial agent is 40% and the remainder of the antimicrobial agent is typically solvent water. Antibacterial agents are commercially available and formulated to the desired concentration.
In one embodiment, the raw materials used to make the antimicrobial core include:
5 to 20 parts of solution containing an antibacterial agent, 30 to 50 parts of forming pore-forming agent, 10 to 15 parts of adsorbent and 1 to 5 parts of adhesive.
In one embodiment, the shaped porogen includes, but is not limited to, microcrystalline cellulose (CAS number 9004-34-6).
In one embodiment, the adsorbent includes, but is not limited to, at least one of starch, modified starch.
In one embodiment, the binder includes, but is not limited to, cellulose.
In one embodiment, the cellulose includes, but is not limited to, at least one of hydroxymethyl cellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose.
In one embodiment, the antimicrobial sustained release particles further comprise a coating layer coating at least a portion of the surface of the antimicrobial core.
In one embodiment, the coating completely encapsulates the antimicrobial core.
In one embodiment, the material of the coating layer includes, but is not limited to, at least one of polyvinyl alcohol, resin, polyethylene glycol.
In one embodiment, the average molecular weight of the polyvinyl alcohol may be 15 to 20 tens of thousands.
In one embodiment, the surface of the antimicrobial core is coated with at least one coating layer.
In one embodiment, the surface of the antimicrobial core is coated with 2-10 coating layers.
In one embodiment, each coating layer comprises a polyvinyl alcohol layer and a resin layer.
In one embodiment, the thickness of each polyvinyl alcohol layer, resin layer, is independently 100nm to 100 μm, preferably 100nm to 2 μm.
In one embodiment, the polyvinyl alcohol layer and the resin layer are sequentially laminated in a direction away from the antibacterial core.
In one embodiment, the resin layer and the polyvinyl alcohol layer are sequentially laminated in a direction away from the antibacterial core.
In one embodiment, the resin layer contains at least one of polyurethane resin, acrylic resin, silicone resin, and modified resin.
In one embodiment, the antimicrobial slow-release particles have a diameter of 0.1 to 30mm, including but not limited to 0.1mm、0.1mm、0.2mm、0.3mm、0.4mm、0.5mm、0.6mm、0.7mm、0.8mm、0.9mm、1mm、2mm、3mm、4mm、5mm、6mm、7mm、8mm、9mm、10mm、20mm、30mm.
According to a second aspect, in an embodiment, there is provided a method for preparing the antibacterial sustained-release particles of any one of the first aspects, comprising:
The preparation method comprises the steps of (1) mixing raw materials and water according to the formula amount to prepare a granular antibacterial inner core;
The coating step comprises the steps of soaking the antibacterial inner core at least once in a polyvinyl alcohol solution and at least once in a resin solution, so that at least part of the surface of the antibacterial inner core is coated with at least one coating layer, and the antibacterial slow-release particles are obtained.
In one embodiment, in the core preparation step, the amounts of the respective raw materials for preparing the antibacterial core and water by mass are as follows:
5 to 20 parts of solution containing an antibacterial agent, 30 to 50 parts of forming pore-forming agent, 10 to 15 parts of adsorbent, 1 to 5 parts of adhesive and 2 to 8 parts of water. Water is the solvent.
In one embodiment, the antimicrobial agent is present in the solution at a concentration of 40% by mass, the balance being solvent water. Antibacterial agents can be purchased commercially and formulated to the desired concentration.
In one embodiment, in the coating step, the antimicrobial core is subjected to at least one soak dry, each soak dry comprising:
the antibacterial inner core is soaked into a solution containing polyvinyl alcohol, then taken out, dried to remove the solvent, then soaked into a solution containing resin, and dried again to remove the solvent.
In one embodiment, the coating step is cycled through 5 to 10 soak dries. Too little soaking times can lead to too fast release of the antimicrobial without long-lasting effect; too many times of soaking can cause slow release of the antibacterial agent, lower effective concentration and poor antibacterial effect.
In one embodiment, the coating step is performed for a period of time ranging from 5 to 10 minutes per soak. The soaking time is positively correlated with the thickness of the coating layer, and the longer the soaking time is, the larger the thickness of the coating layer is.
In one embodiment, the temperature of each drying step is 60 to 150 ℃, preferably 100 to 150 ℃, more preferably 100 to 130 ℃, more preferably 120 ℃.
In one embodiment, the coating step is performed for a period of 3 to 5 minutes per drying. Too short a time may result in failure to dry, too long a time may be unnecessary, and drying may be performed for a certain time.
In one embodiment, in the coating step, the resin solution used to form the resin layer may be an aqueous polyurethane emulsion.
In one embodiment, the coating step, the resin solution used to form the resin layer may have a solids content of 10 to 40%.
In one embodiment, the coating step, the aqueous polyvinyl alcohol solution used to form the polyvinyl alcohol layer may have a solids content of 1 to 5%.
Example 1
The preparation process of the antibacterial sustained-release particles of the embodiment is as follows:
mixing materials, extruding strips, centrifuging, rolling, drying, screening and coating.
Specifically, the organosilicon quaternary ammonium salt and the starch are premixed according to the formula amount, and then other components are sequentially added into a mixer to be uniformly mixed; then adding the materials into an extruder, extruding the materials into strips, granulating the strips by a centrifugal spheronization technology, drying the granules at 80 ℃ for 1 to 2 hours, and sieving the granules to obtain the granules with the particle size range of 8mm.
In this example, the antibacterial sustained-release particles were prepared from the following raw materials in mass: 15 parts of organosilicon quaternary ammonium salt solution, 40 parts of microcrystalline cellulose, 12 parts of starch, 2 parts of cellulose and 5 parts of water. In the organosilicon quaternary ammonium salt solution, the mass ratio of the organosilicon quaternary ammonium salt is 40 percent, and the balance is solvent water. The composition of the silicone quaternary ammonium salt solution is the same as in this example.
Coating:
the coating material includes a resin emulsion for forming a resin layer and an aqueous polyvinyl alcohol solution for forming a polyvinyl alcohol (PVA) layer. Resin emulsion: an aqueous polyurethane emulsion with a solid content of 30%. The solids content of the aqueous polyvinyl alcohol solution was 2%.
The prepared particles are soaked in PVA (average molecular weight of 15 ten thousand) aqueous solution for 5 to 10 minutes, taken out, dried for 3 to 5 minutes at 120 ℃, then soaked in resin emulsion for 2 to 10 minutes, taken out, dried for 3 to 5 minutes at 120 ℃, and the soaking and drying are repeated for 5 times, so that the final antibacterial slow-release particles are obtained. The granules have coating layers formed of PVA and resin alternately, 5 coating layers each having one PVA layer and one resin layer. The thickness of each PVA layer, resin layer, was independently about 250nm.
Antibacterial effect test experiment
① Quaternary ammonium salt concentration test and bactericidal effect test
The experimental contents are as follows:
1 antibacterial slow-release particle with the diameter of about 8mm is taken and placed in 100mL of deionized water, and after being placed for sampling for different time, the concentration of the antibacterial slow-release particle is tested by using quaternary ammonium salt test paper.
The sterilization experiment is performed by referring to the national standard GB/T38502-2020 sterilizing effect test method of sterilizing agent laboratory.
Neutralization agent identification test:
The sterilization rate detection method comprises the following steps: reference is made to the quantitative identification test of the suspensions of "sterilizing technical Specification" (2002 edition) 2.1.1.5.5 of the Ministry of health of China.
Test strain: coli 8099.
The detection method comprises the following steps: quantitative sterilization test of 2.1.1.7.4 suspension by reference to the "sterilizing technical Specification (2002 edition) of the Ministry of health of China
The test results are shown in tables 1 and 2.
TABLE 1
As can be seen from Table 1, after 1 day of slow release, the concentration of the quaternary ammonium salt was as high as 50ppm, and the sterilization rate was as high as 90%. After 7 days, the concentration of the quaternary ammonium salt is maintained to be more than 500ppm, and the sterilization rate is as high as 99.999 percent. The antibacterial slow-release particles have excellent long-acting antibacterial effect.
FIG. 1 is a photograph of the resulting solution after 1 day of sustained release as measured by a quaternary ammonium salt test paper.
FIG. 2 is a photograph of the resulting solution after 2 days of sustained release as measured by a quaternary ammonium salt test paper.
FIG. 3 is a photograph of the resulting solution after 3 days of sustained release as measured by a quaternary ammonium salt test paper.
FIG. 4 is a photograph of the resulting solution after 5 days of sustained release as measured by a quaternary ammonium salt test paper.
TABLE 2
As can be seen from Table 2, the concentration of quaternary ammonium salt in the solution after 6 months is still up to more than 500ppm, and the sterilization rate is up to 99.999%. The antibacterial slow-release particles have excellent long-acting antibacterial effect, and the antibacterial effect can be maintained for more than 6 months.
② Testing of concentration and sterilization rate of quaternary ammonium salt after water change
The experimental contents are as follows: taking 1 antibacterial slow-release particle with the diameter of about 8mm, placing the antibacterial slow-release particle in 100mL of deionized water, emptying the solution after placing the antibacterial slow-release particle in 100mL of deionized water for 7 days (higher concentration and 99.999% sterilization rate are achieved in seven days), adding 100mL of deionized water again, placing the antibacterial slow-release particle for sampling in different time periods, and testing the concentration of the antibacterial slow-release particle by using quaternary ammonium salt test paper. The results are shown in tables 3 and 4.
TABLE 3 Table 3
| Time of slow release | For 1 day | For 2 days | For 3 days | For 5 days | For 7 days |
| Quaternary ammonium salt test paper (ppm) | 50 | 100～250 | 250～500 | ＞500 | ＞500 |
| Sterilization rate | 90％ | 99％ | 99.999％ | 99.999％ | 99.999％ |
As can be seen from Table 3, the solution was emptied after 7 days and then re-added with water, and the concentration of quaternary ammonium salt in the solution after 1 day was still as high as 50ppm, and the sterilization rate was as high as 90%. After 7 days, the concentration of the quaternary ammonium salt is maintained to be more than 500ppm, and the sterilization rate is as high as 99.999 percent.
TABLE 4 Table 4
As can be seen from Table 4, the concentration of quaternary ammonium salt in the solution after 6 months is still up to more than 500ppm, and the sterilization rate is up to 99.999%. The antibacterial slow-release particles have excellent long-acting antibacterial effect, and the antibacterial effect can be maintained for more than 6 months.
The sustained release particles prepared in this example are shown in fig. 5.
Comparative example 1
The antibacterial slow-release granule is prepared from the following raw materials in mass: 15 parts of organosilicon quaternary ammonium salt solution, 40 parts of microcrystalline cellulose, 2 parts of starch, 2 parts of cellulose and 5 parts of water.
Coating:
the coating material includes a resin emulsion for forming a resin layer and an aqueous polyvinyl alcohol solution for forming a polyvinyl alcohol (PVA) layer. Resin emulsion: an aqueous polyurethane emulsion with a solid content of 30%. The solids content of the aqueous polyvinyl alcohol solution was 2%.
The prepared particles are soaked in PVA (average molecular weight of 15 ten thousand) aqueous solution for 5 to 10 minutes, taken out, dried for 3 to 5 minutes at 120 ℃, then soaked in resin emulsion for 2 to 10 minutes, taken out, dried for 3 to 5 minutes at 120 ℃, and the soaking and drying are repeated for 5 times.
As shown in FIG. 6, particle B is a physical image of the antibacterial sustained-release particles prepared in the comparative example, and the obtained particles are instantly dispersed in water.
Comparative example 2
The antibacterial slow-release granule is prepared from the following raw materials in mass: 15 parts of organosilicon quaternary ammonium salt solution, 40 parts of microcrystalline cellulose, 12 parts of starch, 2 parts of cellulose and 5 parts of water.
Coating:
the coating material includes a resin emulsion for forming a resin layer and an aqueous polyvinyl alcohol solution for forming a polyvinyl alcohol (PVA) layer. Resin emulsion: an aqueous polyurethane emulsion with a solid content of 30%. The solids content of the aqueous polyvinyl alcohol solution was 2%.
The prepared particles are soaked in PVA (average molecular weight of 15 ten thousand) aqueous solution for 5 to 10 minutes, taken out, dried for 3 to 5 minutes at 120 ℃, then soaked in resin emulsion for 2 to 10 minutes, taken out, dried for 3 to 5 minutes at 120 ℃, and the soaking and drying are repeated for 15 times.
TABLE 5
| Time of slow release | For 1 day | For 2 days | For 3 days | For 5 days | For 7 days |
| Quaternary ammonium salt test paper (ppm) | 0 | 0～10 | 0～10 | 0～10 | 10～50 |
As can be seen from table 5, the too thick coating layer resulted in extremely slow release of the antimicrobial agent and poor antimicrobial effect.
The sustained-release particles prepared in this comparative example were similar in appearance to fig. 5, but were extremely slow in release of the antibacterial agent due to the excessively thick coating layer, and were inferior in antibacterial effect.
In one embodiment, the invention provides a preparation method of the antibacterial slow-release particles with low cost and simple process, the slow-release particles can be put in liquid to achieve the effects of long-acting slow release and continuous antibacterial, the slow release period of a single slow-release particle can reach half a year or more, and the slow-release particle has the long-acting deodorizing effect, has a wide application range, can be used in a coverage way in daily life, medical treatment or other fields, and is nontoxic and harmless to people and pets.
In some embodiments, the antibacterial slow-release particles of the invention are mainly used in the fields of environmental cleaning and industry, and realize long-acting antibacterial effect on liquid such as waste liquid.
The existing antibacterial agent is almost disposable, and is used in a spraying or diluting mode, new antibacterial agent is needed to be added repeatedly or diluted again after the antibacterial agent is used up, and in one embodiment, the antibacterial slow-release particles can be slowly released in a long-acting mode, the antibacterial slow-release particles can be only needed to be added once for more than half a year in service life, the sterilizing effect is not reduced, and meanwhile the deodorizing effect is achieved.
In one embodiment, the antibacterial slow-release particles provided by the invention are low in preparation and use cost, simple in preparation process, nontoxic and harmless.
The foregoing description of the invention has been presented for purposes of illustration and description, and is not intended to be limiting. Several simple deductions, modifications or substitutions may also be made by a person skilled in the art to which the invention pertains, based on the idea of the invention.
Claims (7)
1. The antibacterial slow-release granule is characterized by comprising an antibacterial inner core, wherein the antibacterial inner core is prepared from the following raw materials: 2-8 parts of an antibacterial agent, 30-50 parts of a forming pore-forming agent, 10-15 parts of an adsorbent and 1-5 parts of an adhesive;
The antibacterial agent is at least one of quaternary ammonium salt antibacterial agent, organic guanidine antibacterial agent, metal ion antibacterial agent, chlorine antibacterial agent, peroxide antibacterial agent, iodine antibacterial agent, phenol antibacterial agent and ethylene oxide antibacterial agent; the forming pore-forming agent comprises microcrystalline cellulose; the adsorbent comprises at least one of starch and modified starch; the adhesive is cellulose;
The antibacterial slow-release particles further comprise a coating layer coated on the surface of the antibacterial inner core, and the coating layer completely coats the antibacterial inner core;
The coating layer comprises a polyvinyl alcohol layer and a resin layer; the surface of the antibacterial inner core is coated with 5 coating layers; each coating layer comprises a polyvinyl alcohol layer and a resin layer; the resin layer is at least one of polyurethane resin, acrylic resin, organic silicon resin and modified resin;
The coating layer is prepared by the following steps of firstly soaking the prepared antibacterial inner core particles in a polyvinyl alcohol aqueous solution with the average molecular weight of 15 ten thousand, taking out the antibacterial inner core particles after soaking for 5-10 min, drying for 3-5 min at 60-150 ℃, then taking out the antibacterial inner core particles after soaking for 2-10 min in a resin emulsion, drying for 3-5 min at 60-150 ℃, and repeating the soaking and drying for 5 times to obtain the final antibacterial slow-release particles.
2. The antimicrobial slow release granule of claim 1, wherein the quaternary ammonium salt comprises a silicone quaternary ammonium salt.
3. The antimicrobial slow-release granule of claim 1, wherein the quaternary ammonium salt comprises at least one of a di-long alkyl quaternary ammonium salt, a mono-long alkyl quaternary ammonium salt.
4. An antimicrobial slow release granule according to claim 3, wherein the bis-long chain alkyl quaternary ammonium salt comprises at least one of methyl bis-behenyl [3- (dimethoxysilyl) propyl ] ammonium chloride, methyl bis-octadecyl [3- (dimethoxysilyl) propyl ] ammonium chloride, methyl bis-hexadecyl [3- (dimethoxysilyl) propyl ] ammonium chloride, methyl bis-tetradecyl [3- (dimethoxysilyl) propyl ] ammonium chloride, methyl bis-dodecyl [3- (dimethoxysilyl) propyl ] ammonium chloride;
Or, the mono-long chain alkyl quaternary ammonium salt comprises at least one of methyl dodecyl [3- (dimethoxy silicon base) propyl ] ammonium chloride, methyl tetradecyl [3- (dimethoxy silicon base) propyl ] ammonium chloride and methyl dodecyl [3- (diethoxy silicon base) propyl ] ammonium chloride.
5. The antimicrobial slow-release granule of claim 1, wherein the cellulose comprises at least one of hydroxymethyl cellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose.
6. The method for preparing the antibacterial sustained-release particles according to any one of claims 1 to 5, comprising:
The preparation method comprises the steps of (1) mixing raw materials and water according to the formula amount to prepare a granular antibacterial inner core;
And a coating step, namely firstly soaking the prepared antibacterial inner core particles in a polyvinyl alcohol aqueous solution with the average molecular weight of 15 ten thousand, taking out the antibacterial inner core particles after soaking for 5-10 min, drying for 3-5 min at 60-150 ℃, then taking out the antibacterial inner core particles after soaking for 2-10 min in a resin emulsion, drying for 3-5 min at 60-150 ℃, and repeating the soaking and drying for 5 times to obtain the final antibacterial slow-release particles.
7. The method of producing an antibacterial core according to claim 6, wherein in the core producing step, the amounts of the respective raw materials for producing the antibacterial core and water by mass are as follows:
5-20 parts of a solution containing an antibacterial agent, 30-50 parts of a forming pore-forming agent, 10-15 parts of an adsorbent, 1-5 parts of an adhesive and 2-8 parts of water.
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| CN1444852A (en) * | 2002-06-17 | 2003-10-01 | 龙膺厚 | Granulated strong action disinfectant |
| CN105412132A (en) * | 2014-09-12 | 2016-03-23 | 中牧实业股份有限公司黄冈动物药品厂 | Compound invermectin slow-release granules and preparation method thereof |
| CN109319913A (en) * | 2018-10-11 | 2019-02-12 | 仲恺农业工程学院 | A kind of slow-release oxone and preparation method thereof |
| CN109601533A (en) * | 2019-01-29 | 2019-04-12 | 刘宏波 | Sustained and controlled release pesticide granules and preparation method thereof |
| CN110452056A (en) * | 2019-09-11 | 2019-11-15 | 句容市后白镇农业服务中心 | A kind of coated release-controlled Synergistic type herbicide fertilizer granules of multilayer and its preparation and method of administration |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1444852A (en) * | 2002-06-17 | 2003-10-01 | 龙膺厚 | Granulated strong action disinfectant |
| CN105412132A (en) * | 2014-09-12 | 2016-03-23 | 中牧实业股份有限公司黄冈动物药品厂 | Compound invermectin slow-release granules and preparation method thereof |
| CN109319913A (en) * | 2018-10-11 | 2019-02-12 | 仲恺农业工程学院 | A kind of slow-release oxone and preparation method thereof |
| CN109601533A (en) * | 2019-01-29 | 2019-04-12 | 刘宏波 | Sustained and controlled release pesticide granules and preparation method thereof |
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