CN112352789A - Preparation method of silver chloride ion symbiotic disinfection concentrated solution - Google Patents

Preparation method of silver chloride ion symbiotic disinfection concentrated solution Download PDF

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CN112352789A
CN112352789A CN202011296507.8A CN202011296507A CN112352789A CN 112352789 A CN112352789 A CN 112352789A CN 202011296507 A CN202011296507 A CN 202011296507A CN 112352789 A CN112352789 A CN 112352789A
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silver
disinfection
complex
symbiotic
solution
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张春明
冉伟
李章鹏
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Shanghai Juzhi New Material Technology Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16Heavy metals; Compounds thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/26Biocides, 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
    • A01N25/28Microcapsules or nanocapsules
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N33/00Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
    • A01N33/02Amines; Quaternary ammonium compounds
    • A01N33/12Quaternary ammonium compounds
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N47/00Biocides, 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
    • A01N47/40Biocides, 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
    • A01N47/42Biocides, 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
    • A01N47/44Guanidine; Derivatives thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds

Abstract

A preparation method of silver chloride ion symbiotic disinfection concentrated solution comprises the steps of firstly dissolving a silver compound in deionized water to prepare a solution, adding an iminoamber complex surfactant to form a mixed solution, dropwise adding an alkaline regulator to adjust the pH value to 8-10, continuously stirring to form a stable complex silver ion compound, inducing the iminoamber complex surfactant to self-assemble to form a vesicle structure by the stable complex silver ion compound and the excessive iminoamber complex surfactant in a special combination mode under the alkaline constant temperature condition, coordinately coating complex silver ions in the vesicle to form a stable core-shell structure, finally compounding the core-shell complex silver ion solution with a chlorine-containing disinfectant, adding a humectant and a defoaming agent, and stirring to be colorless and transparent to obtain the silver chloride ion symbiotic disinfection concentrated solution. The invention solves the problem of symbiosis of chloride ions and silver ions by using the complexing agent, and solves the problem of quick sterilization and disinfection of the silver ions through the silver-chlorine synergistic effect.

Description

Preparation method of silver chloride ion symbiotic disinfection concentrated solution
Technical Field
The invention belongs to the technical field of silver ion sterilization and disinfection, and particularly relates to a preparation method of a silver chloride ion symbiotic disinfection concentrated solution.
Background
In ancient times, silver products were recognized to have antibacterial and antiseptic effects, and were used in real life. At present, nano silver is widely applied to various aspects such as baby products, hand sanitizer, food packaging, medical dressing and the like. The research reports of the nano silver particles on the antibacterial action at home and abroad are more, and the nano silver has lasting and efficient effect of resisting environmental pathogenic bacteria in the clinical urology surgery, gynecology, orthopedic surgery, dermatology and burn and scald surgical treatment. The nano silver has the advantages that the nano silver has extremely high antibacterial activity and does not generate drug resistance, and the nano silver has incomparable advantages compared with the traditional inorganic antibacterial agent.
Although the antibacterial activity of nano silver is widely acknowledged, the nano silver has long sterilization duration, but the rapid sterilization and disinfection of low-concentration nano silver in a very short time still has problems. In order to solve the problem that the use amount of silver can be reduced by quickly sterilizing and disinfecting silver ions, the chlorine-containing organic bactericide is compounded with the silver ions, and the problem of quickly sterilizing and disinfecting the silver ions is solved through the silver-chlorine synergistic effect.
As is known, silver ions and chloride ions cannot coexist in a solution, so that white silver chloride precipitates are easily generated, and in order to solve the coexistence problem of the silver ions and the chloride ions, the vesicles are used for coordinating and coating the silver ions to form a protective film with a core-shell structure, so that the vesicles of the silver ions and the chloride ions are independent and can coexist, and the content of effective substances can be reduced under the condition that the sterilization and disinfection capacity is not changed due to the silver-chlorine synergistic effect. The silver chloride ion symbiotic disinfection concentrated solution is diluted for use, and can kill common bacteria, fungi and viruses within 1 minute.
Disclosure of Invention
The invention provides a preparation method of silver chloride ion symbiotic disinfection concentrated solution, which comprises the following specific steps: (1) preparing a stable vesicle silver ion solution: weighing silver compound powder with a certain mass, adding the silver compound powder into deionized water, stirring until the silver compound powder is completely dissolved, then adding iminoamber complex type surfactant with a certain mass to form a mixed solution, dropwise adding an alkaline regulator to adjust the pH value of the solution to 8-10, continuously stirring for a certain time to form a stable silver ion complex, inducing the iminoamber complex type surfactant to self-assemble to form a vesicle structure by using a special combination mode under the alkaline constant temperature condition through the stable complex silver ion compound and the excessive iminoamber complex type surfactant, and coating the complex silver ions in the vesicle to form a stable core-shell structure;
(2) preparing a silver chloride ion symbiotic disinfection concentrated solution: adding a chlorine-containing disinfectant into the mixture obtained in the step (1) to prepare a disinfection concentrated solution, adding a humectant and a defoaming agent, and stirring at a constant temperature until the mixture is colorless and transparent to obtain the disinfectant.
Preferably, the slurry in the step (1) is prepared according to a ratio, wherein the slurry is prepared according to a ratio of 1-5% (w/w) of a silver compound, and the silver compound is one or a combination of silver acetate, silver nitrate and silver oxide.
Preferably, the proportion of the aminosuccinic complex type surface active ingredient added in the step (1) is 3 to 15% (w/w), and the iminosuccinic complex type surfactant is one or a combination of iminodisuccinic acid, tetrasodium iminodisuccinate, N' -disuccinimidyl carbonate, 9-fluorenylmethyl-N-succinimide carbonate and N-benzylsuccinimide carbonate.
Preferably, the alkaline regulator in the step (1) is one or a combination of triethanolamine and amp95, the pH of the solution is regulated to 8-10 by using the alkaline regulator, the temperature is regulated to 30-50 ℃, and the stirring speed is 100-.
Preferably, the chlorine-containing disinfectant in the step (2) is a chlorine-containing quaternary ammonium salt (one or a combination of benzalkonium chloride, benzethonium chloride and didodecyldimethylammonium chloride) or a chlorine-containing double-arc salt (one or a combination of polymethylene biguanide hydrochloride, chitosan biguanide hydrochloride and 1, 6-bis (N1-p-chlorophenyl-N5-biguanidino) hexane diacetate), and the concentration of the chlorine-containing disinfectant is 1-5% (w/w).
Preferably, the mixture ratio in the step (4) is 1-5% (w/w) of a humectant and 0.1-0.5% (w/w) of a defoaming agent, wherein the humectant is one or a combination of glycerol, xylitol and sorbitol. Wherein the defoaming agent is one or the combination of BYK011, BYK024, BYK025 and BYK 028.
Compared with the prior art, the silver chloride ion symbiotic disinfection concentrated solution prepared by the method has the following beneficial effects:
(1) silver ions and chloride ions can produce silver chloride precipitates in a solution and cannot coexist, and the silver ions are coated by utilizing a vesicular core-shell structure to avoid direct contact with the chloride ions;
(2) the silver ions and the chlorine-containing organic antibacterial agent are compounded, so that the sterilization rate can be greatly improved, the problem of rapid sterilization and disinfection of the silver ions is solved through the silver-chlorine synergistic effect, and the use concentrations of silver and chlorine can be reduced;
(3) the silver chloride ion symbiotic disinfection concentrated solution can kill common bacteria, fungi and viruses within 1 minute when diluted for use.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic structural diagram of a product according to an embodiment of the present invention
FIG. 2 is a TEM image of the product of example two of the present invention
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The first embodiment is as follows:
preparing a stable vesicle silver ion solution: weighing 10g of silver nitrate powder, adding the silver nitrate powder into 939g of ionized water, and stirring until the silver nitrate powder is completely dissolved. Then 30g of iminodisuccinic acid was added to form a mixture. And dropwise adding triethanolamine to adjust the pH value of the solution to 8, stirring for 1h at the constant temperature of 30 ℃ and the stirring speed of 100r/min to form a stable silver ion complex, inducing self-assembly of the iminosuccinic complex type surfactant to form a vesicle structure by the stable complex silver ion compound and excessive iminodisuccinic acid in a special combination mode under the condition of alkaline constant temperature, and coating the complex silver ions in the vesicle to form a stable core-shell structure.
Preparing a silver chloride ion symbiotic disinfection concentrated solution: adding 10g of benzalkonium chloride into the solution, compounding to obtain a disinfection concentrated solution, adding 10g of glycerol and 1g of defoaming agent BYK011, and stirring until the solution is colorless and transparent.
Example two:
preparing a stable vesicle silver ion solution: weighing 15g of silver acetate powder, adding the silver acetate powder into 900g of deionized water, stirring until the silver acetate powder is completely dissolved, then adding 45g of tetrasodium iminodisuccinate to form a mixed solution, dropwise adding amp95 to adjust the pH value of the solution to 8.5, stirring at the constant temperature of 35 ℃ and the stirring speed of 200r/min for 1h to form a stable silver ion complex, inducing self-assembly of the iminosuccinic complex surfactant to form a vesicle structure by the stable complex silver ion compound and excessive tetrasodium iminodisuccinate in a special combination mode under the alkaline constant temperature condition, and coating the complex silver ions in the vesicle to form the stable core-shell structure.
Preparing a silver chloride ion symbiotic disinfection concentrated solution: adding 15g of polymethylene biguanide hydrochloride into the solution, compounding to obtain a disinfection concentrated solution, adding 15g of xylitol and 1.5g of defoamer BYK024, and stirring to obtain a colorless transparent state.
Example three:
preparing a stable vesicle silver ion solution: weighing 25g of silver oxide powder, adding the silver oxide powder into 850g of deionized water, stirring until the silver oxide powder is completely dissolved, then adding 75g of iminodisuccinic acid to form a mixed solution, dropwise adding triethanolamine to adjust the pH value of the solution to 9, stirring at the constant temperature of 40 ℃ and the stirring speed of 300r/min for 1h to form a stable silver ion complex, inducing self-assembly of the iminosuccinic complex surfactant to form a vesicle structure by using a stable complex silver ion compound and excessive N, N' -disuccinimidyl carbonate in a special combination mode under the alkaline constant temperature condition, and coating the complex silver ions in the vesicle to form the stable core-shell structure.
Preparing a silver chloride ion symbiotic disinfection concentrated solution: adding 25g benzethonium chloride into the solution, compounding to obtain a disinfection concentrated solution, adding 25g sorbitol and 2.5g defoamer BYK025, and stirring to obtain the disinfectant.
Example four:
preparing a stable vesicle silver ion solution: weighing 40g of silver nitrate powder, adding the silver nitrate powder into 756g of deionized water, stirring until the silver nitrate powder is completely dissolved, then adding 120g of tetrasodium iminodisuccinate to form a mixed solution, dropwise adding amp95 to adjust the pH value of the solution to 9.5, stirring at a constant temperature of 40 ℃ and a stirring speed of 400r/min for 1h to form a stable silver ion complex, inducing self-assembly of the iminosuccinic complex surfactant to form a vesicle structure by the stable complex silver ion compound and the excessive iminosuccinic complex surfactant in a special combination mode under an alkaline constant temperature condition, and coating the complex silver ions in the vesicle to form the stable core-shell structure.
Preparing a silver chloride ion symbiotic disinfection concentrated solution: and adding 40g of chitosan biguanide hydrochloride into the solution to prepare a disinfection concentrated solution. Adding 40g of glycerol and 1g of defoaming agent BYK028, and stirring until the mixture is colorless and transparent.
Example five:
preparing a stable vesicle silver ion solution: 50g of silver acetate powder is weighed and added into 695g of deionized water, and stirred until the silver acetate powder is completely dissolved. Then 150g of iminodisuccinic acid was added to form a mixture. And dropwise adding triethanolamine to adjust the pH value of the solution to 10, and stirring at the constant temperature of 50 ℃ and the stirring speed of 500r/min for 1h to form a stable silver ion complex. Meanwhile, the stable complex silver ion compound and the excessive iminosuccinic complex surfactant induce the self-assembly of the iminosuccinic complex surfactant to form a vesicle structure in a special combination mode under the alkaline constant temperature condition, and the complex silver ions are coated in the vesicle to form a stable core-shell structure.
Preparing a silver chloride ion symbiotic disinfection concentrated solution: 50g of didecyl dimethyl ammonium chloride is added into the solution to be compounded to prepare the disinfection concentrated solution. Adding 50g of xylitol and 5g of defoaming agent BYK011, and stirring until the mixture is colorless and transparent.
TABLE 1 comparison of the Disinfection efficiency of E.coli, S.aureus, P.aeruginosa and C.albicans in 1min for dilutions of the products of examples one, two, three, four and five to a silver content of 20ppm
Figure BDA0002785577780000051

Claims (6)

1. A preparation method of silver chloride ion symbiotic disinfection concentrated solution is characterized by comprising the following specific steps:
(1) preparing a stable vesicle silver ion solution: weighing silver compound powder with a certain mass, adding the silver compound powder into deionized water, stirring until the silver compound powder is completely dissolved, then adding iminoamber complex type surfactant with a certain mass to form a mixed solution, dropwise adding an alkaline regulator to adjust the pH value of the solution to 8-10, continuously stirring for a certain time to form a stable silver ion complex, inducing the iminoamber complex type surfactant to self-assemble to form a vesicle structure by using a special coordination and combination mode through a stable complex silver ion compound and excessive iminoamber complex type surfactant under an alkaline constant temperature condition, and coating the complex silver ions in the vesicle to form a stable core-shell structure;
(2) preparing a silver chloride ion symbiotic disinfection concentrated solution: adding a chlorine-containing disinfectant into the mixture obtained in the step (1) to prepare a disinfection concentrated solution, adding a humectant and a defoaming agent, and stirring at a constant temperature until the mixture is colorless and transparent, wherein the concentrated solution can be diluted for use.
2. The method for preparing a silver chloride ion symbiotic disinfection concentrate according to claim 1, wherein the silver compound in step (1) is added in a proportion of 3-15% (w/w) in the concentrate, and the silver compound is one or a combination of silver acetate, silver nitrate and silver oxide.
3. The method for preparing silver chloride ion symbiotic disinfectant concentrate according to claim 1, wherein the proportion of the aminosuccinic type complexing surfactant added to the concentrate in the step (1) is 3-15% (w/w), and the iminosuccinic type complexing surfactant is one or a combination of iminodisuccinic acid, tetrasodium iminodisuccinate, N' -disuccinimidyl carbonate, 9-fluorenylmethyl-N-succinimide carbonate and N-benzylsuccinimide carbonate.
4. The method for preparing silver chloride ion symbiotic disinfection concentrate as claimed in claim 1, wherein the alkaline regulator in step (1) is one or a combination of triethanolamine and AMP95, the pH of the solution is adjusted to 8-10 by using the alkaline regulator, the temperature is adjusted to 30-50 ℃, and the stirring speed is 100-500 r/min.
5. The method for preparing a silver chloride ion symbiotic disinfectant concentrated solution according to claim 1, wherein the chlorine-containing disinfectant in the step (2) is a chlorine-containing quaternary ammonium salt (one or a combination of benzalkonium chloride, benzethonium chloride and didodecyldimethylammonium chloride) or a chlorine-containing double-arc salt (one or a combination of polymethylene biguanide hydrochloride, chitosan biguanide hydrochloride and 1, 6-bis (N1-p-chlorophenyl-N5-biguanidino) hexane diacetate), and the concentration solution contains 1-5% (w/w) of the chlorine-containing disinfectant.
6. The preparation method of the silver chloride ion symbiotic disinfection concentrate as claimed in claim 1, wherein the ratio in step (2) is 1-5% (w/w) of humectant and 0.1-0.5% of defoaming agent, wherein the humectant is one or a combination of glycerin, xylitol and sorbitol, and the defoaming agent is one or a combination of BYK011, BYK024, BYK025 and BYK 028.
CN202011296507.8A 2020-11-18 2020-11-18 Preparation method of silver chloride ion symbiotic disinfection concentrated solution Pending CN112352789A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1356042A (en) * 2001-09-01 2002-07-03 宁夏宏奇实业发展有限公司 Broad-spectrum composite antibacterial agent
CN101319460A (en) * 2008-05-22 2008-12-10 福建鑫华股份有限公司 Production method of durable combined antimicrobial non-woven fabric material
CN101946310A (en) * 2008-02-15 2011-01-12 狮王株式会社 Cleaning composition and method for cleaning substrate for electronic device
CN102021613A (en) * 2009-09-17 2011-04-20 肖特太阳能控股公司 Electrolyte composition
CN102271691A (en) * 2008-12-05 2011-12-07 克劳罗克斯公司 Natural silver disinfectant compositions
CN102579317A (en) * 2011-01-07 2012-07-18 北京因科瑞斯医药科技有限公司 Cantharidin vesicles and preparation thereof and preparation methods of cantharidin vesicles and preparation thereof
CN105934507A (en) * 2014-01-29 2016-09-07 荷兰联合利华有限公司 Aqueous composition containing oligodynamic metal
CN111493073A (en) * 2020-05-28 2020-08-07 李学军 Surface disinfection film covering agent and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1356042A (en) * 2001-09-01 2002-07-03 宁夏宏奇实业发展有限公司 Broad-spectrum composite antibacterial agent
CN101946310A (en) * 2008-02-15 2011-01-12 狮王株式会社 Cleaning composition and method for cleaning substrate for electronic device
CN101319460A (en) * 2008-05-22 2008-12-10 福建鑫华股份有限公司 Production method of durable combined antimicrobial non-woven fabric material
CN102271691A (en) * 2008-12-05 2011-12-07 克劳罗克斯公司 Natural silver disinfectant compositions
CN102021613A (en) * 2009-09-17 2011-04-20 肖特太阳能控股公司 Electrolyte composition
CN102579317A (en) * 2011-01-07 2012-07-18 北京因科瑞斯医药科技有限公司 Cantharidin vesicles and preparation thereof and preparation methods of cantharidin vesicles and preparation thereof
CN105934507A (en) * 2014-01-29 2016-09-07 荷兰联合利华有限公司 Aqueous composition containing oligodynamic metal
CN111493073A (en) * 2020-05-28 2020-08-07 李学军 Surface disinfection film covering agent and preparation method thereof

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