CN117481112A - Composite quaternary ammonium salt disinfectant and preparation method and application thereof - Google Patents
Composite quaternary ammonium salt disinfectant and preparation method and application thereof Download PDFInfo
- Publication number
- CN117481112A CN117481112A CN202311427224.6A CN202311427224A CN117481112A CN 117481112 A CN117481112 A CN 117481112A CN 202311427224 A CN202311427224 A CN 202311427224A CN 117481112 A CN117481112 A CN 117481112A
- Authority
- CN
- China
- Prior art keywords
- quaternary ammonium
- ammonium salt
- disinfectant
- salt disinfectant
- test
- 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
- 239000000645 desinfectant Substances 0.000 title claims abstract description 164
- 150000003242 quaternary ammonium salts Chemical class 0.000 title claims abstract description 125
- 239000002131 composite material Substances 0.000 title claims description 88
- 238000002360 preparation method Methods 0.000 title abstract description 11
- -1 compound quaternary ammonium salt Chemical class 0.000 claims abstract description 65
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 40
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000011780 sodium chloride Substances 0.000 claims abstract description 20
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 17
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 17
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 17
- 239000004094 surface-active agent Substances 0.000 claims abstract description 16
- 239000003906 humectant Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 12
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 26
- 239000000047 product Substances 0.000 claims description 23
- 238000004090 dissolution Methods 0.000 claims description 22
- 241000700605 Viruses Species 0.000 claims description 19
- 230000002147 killing effect Effects 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 241000894006 Bacteria Species 0.000 claims description 11
- 230000009471 action Effects 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004034 viscosity adjusting agent Substances 0.000 claims description 4
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims description 3
- 230000000249 desinfective effect Effects 0.000 claims description 3
- 230000000369 enteropathogenic effect Effects 0.000 claims description 3
- 125000000373 fatty alcohol group Chemical group 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 230000001717 pathogenic effect Effects 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 102220038387 rs587780404 Human genes 0.000 claims description 2
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 55
- 230000001954 sterilising effect Effects 0.000 abstract description 52
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 22
- 230000000694 effects Effects 0.000 abstract description 18
- 150000002191 fatty alcohols Chemical class 0.000 abstract description 7
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- 230000002195 synergetic effect Effects 0.000 abstract description 6
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- 238000006386 neutralization reaction Methods 0.000 description 13
- 230000003472 neutralizing effect Effects 0.000 description 13
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- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 238000010998 test method Methods 0.000 description 10
- HNDVDQJCIGZPNO-UHFFFAOYSA-N histidine Natural products OC(=O)C(N)CC1=CN=CN1 HNDVDQJCIGZPNO-UHFFFAOYSA-N 0.000 description 9
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- 229920001817 Agar Polymers 0.000 description 5
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 5
- 239000000159 acid neutralizing agent Substances 0.000 description 5
- 239000008272 agar Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 210000001185 bone marrow Anatomy 0.000 description 5
- 239000010962 carbon steel Substances 0.000 description 5
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- 229910052802 copper Inorganic materials 0.000 description 5
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- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 241000588724 Escherichia coli Species 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000012449 Kunming mouse Methods 0.000 description 4
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 description 4
- 239000005708 Sodium hypochlorite Substances 0.000 description 4
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- 239000011630 iodine Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
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- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 4
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- 239000012137 tryptone Substances 0.000 description 4
- 241000991587 Enterovirus C Species 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000010171 animal model Methods 0.000 description 3
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical group ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 3
- 230000007794 irritation Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 244000000010 microbial pathogen Species 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 208000035473 Communicable disease Diseases 0.000 description 2
- 244000208060 Lawsonia inermis Species 0.000 description 2
- 206010040914 Skin reaction Diseases 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- 238000007605 air drying Methods 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
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- 238000006065 biodegradation reaction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000872 buffer Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
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- 238000005520 cutting process Methods 0.000 description 2
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- 239000012153 distilled water Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 210000004209 hair Anatomy 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- 231100000989 no adverse effect Toxicity 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000001139 pH measurement Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
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- CPKVUHPKYQGHMW-UHFFFAOYSA-N 1-ethenylpyrrolidin-2-one;molecular iodine Chemical compound II.C=CN1CCCC1=O CPKVUHPKYQGHMW-UHFFFAOYSA-N 0.000 description 1
- 108091003079 Bovine Serum Albumin Proteins 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- CMSMOCZEIVJLDB-UHFFFAOYSA-N Cyclophosphamide Chemical compound ClCCN(CCCl)P1(=O)NCCCO1 CMSMOCZEIVJLDB-UHFFFAOYSA-N 0.000 description 1
- 239000006144 Dulbecco’s modified Eagle's medium Substances 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920000153 Povidone-iodine Polymers 0.000 description 1
- 102000004142 Trypsin Human genes 0.000 description 1
- 108090000631 Trypsin Proteins 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 238000011888 autopsy Methods 0.000 description 1
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- 239000003651 drinking water Substances 0.000 description 1
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- 230000001804 emulsifying effect Effects 0.000 description 1
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- 230000002496 gastric effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 210000002216 heart Anatomy 0.000 description 1
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- 230000005764 inhibitory process Effects 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
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- 230000002262 irrigation Effects 0.000 description 1
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- 231100000344 non-irritating Toxicity 0.000 description 1
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- 230000000474 nursing effect Effects 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 244000052769 pathogen Species 0.000 description 1
- 239000008363 phosphate buffer Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 description 1
- 229960001621 povidone-iodine Drugs 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
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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
- A01N25/02—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 liquids as carriers, diluents or solvents
-
- 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
- A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
- A01N31/02—Acyclic 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
- 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
- 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
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Environmental Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Toxicology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a compound quaternary ammonium salt disinfectant, and a preparation method and application thereof, and belongs to the technical field of disinfectant, wherein the compound quaternary ammonium salt disinfectant is prepared from the following raw materials in percentage by weight: 4% -5% of mixed surfactant, 0.4% -0.6% of humectant, 1% -2% of viscosity regulator, 1% -2% of pH regulator and the balance of water; the compound quaternary ammonium salt disinfectant takes effect together in a disinfectant liquid system by adopting 2 quaternary ammonium salt cationic surfactants, and the combination of the two surfactants can produce a synergistic antibacterial effect, so that the prepared compound quaternary ammonium salt disinfectant has excellent and durable antibacterial effect; meanwhile, in the compound quaternary ammonium salt disinfectant, the fatty alcohol polyoxyethylene ether, the sodium chloride, the sodium carbonate and the sodium bicarbonate have antibacterial performance and are uniformly dispersed in the disinfectant, so that the disinfectant is wide in antibacterial spectrum, mild, free of stimulation and good in stability, and a preservative is not required to be added; has the characteristics of strong sterilization performance, wide sterilization spectrum, mildness, no stimulation and the like.
Description
Technical Field
The invention belongs to the technical field of disinfectant, and particularly relates to a composite quaternary ammonium salt disinfectant, and a preparation method and application thereof.
Background
The venom is a preparation for killing pathogenic microorganisms on a transmission medium and making the pathogenic microorganisms reach harmless requirements. The disinfectant is different from antibiotics, and has the main effects of killing pathogenic microorganisms outside human bodies, cutting off the transmission path of infectious diseases and achieving the purpose of controlling the infectious diseases. There are a number of different main component disinfectants. The chlorine-containing disinfectant comprises the following components: the active ingredient of the disinfectant is hypochlorous acid or hypochlorite, and the disinfectant is widely applied to disinfection, cleaning, nursing and the like in various industries such as individuals, families, medical treatment, agriculture, livestock breeding industry and the like. However, sodium hypochlorite disinfectants suffer from a number of drawbacks: because hypochlorous acid in the solution has strong oxidizing property and bleaching capability, the hypochlorous acid can easily corrode skin, so that the sodium hypochlorite solution cannot be directly used in clinic; because the sodium hypochlorite is poor in stability and easy to decompose, great difficulty and loss are brought to aspects of production, storage, transportation, sales, use and the like; in order to improve the storage period of the sodium hypochlorite solution, the stabilizer and the like added into the product by manufacturers bring pollution to the environment, and the use is more limited. (2) The peroxyacetic acid disinfectant belongs to peroxide disinfectant, has strong oxidizing ability, can effectively kill various microorganisms, has the advantages of high speed, high efficiency, no residual harmful substances after decomposition and the like, and is widely applied to the fields of textile, papermaking, chemical industry, light industry, medicine, electronics, food, environmental protection, military industry and the like. However, the single-component peroxyacetic acid has low surface activity, and a high-concentration disinfectant is required to achieve the corresponding disinfection effect, however, the high-concentration disinfectant can corrode equipment, and as a strong-oxidizing substance, the peroxide cannot be stably stored for a long time, and the peroxide needs to be prepared at present and is greatly limited by time and space during use. (3) The iodine disinfectant is a preparation prepared by taking iodine as a main sterilization component, and has the function of sterilizing by precipitating protein through free iodine element, and can quickly kill pathogens such as bacteria, spores, viruses, bacteriophage, fungi and the like. But the following disadvantages are prevalent: low iodine concentration (between 0.1-1%) or causes insufficient efficacy; the stability is not good; skin irritation is great (such as iodine tincture using ethanol as solvent, iodized nipple infusion with ethanol content up to 45%; the price is relatively high, the production process conditions are relatively harsh (such as povidone iodine raw material), and the application is greatly limited.
The application research of the cationic surfactant in the field of disinfection is focused, and the quaternary ammonium salt serving as an important cationic surfactant has the advantages of good sterilization effect, low toxicity, small irritation, stable property, no bad smell and the like; meanwhile, the cationic surfactants have synergistic effect as bactericides after being compounded, and the bactericidal activity is stronger after a plurality of compounds are compounded, so that the research and development of the compound product is particularly important for preparing broad-spectrum antibacterial disinfectant; therefore, the patent aims to design the compound quaternary ammonium salt disinfectant with a strong sterilization effect so as to solve the problems of the existing disinfectant.
Disclosure of Invention
Aiming at the problems, the invention aims to provide the compound quaternary ammonium salt disinfectant, and the preparation method and application thereof, wherein the compound quaternary ammonium salt disinfectant has the characteristics of excellent sterilizing and bacteriostasis effects, mildness, no stimulation, no toxicity, no preservative, uniform dispersion in the disinfectant, synergistic antibacterial effect when being combined with a mixed surfactant, excellent and durable antibacterial effect, low production cost, simple preparation process, environmental protection and suitability for industrial production.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a composite quaternary ammonium salt disinfectant is prepared from the following raw materials in percentage by weight: 4% -5% of mixed surfactant, 0.4% -0.6% of humectant, 1% -2% of viscosity regulator, 1% -2% of pH regulator and the balance of water.
Preferably, the mixed surfactant is a mixture of alkyl dimethyl benzyl ammonium chloride and alkyl dimethyl ethyl benzyl ammonium chloride, and the mixing ratio of the alkyl dimethyl benzyl ammonium chloride to the alkyl dimethyl ethyl benzyl ammonium chloride is 1:1.
Preferably, C12:C14:C16:C18=5%: 60%:30%:5% in the alkyl dimethyl benzyl ammonium chloride; c12:c14=68% to 32% in alkyldimethylethylbenzyl ammonium chloride.
Preferably, the humectant is fatty alcohol polyoxyethylene ether, the viscosity regulator is sodium chloride, and the pH regulator is one of sodium carbonate or sodium bicarbonate.
Preferably, the pH value of the composite quaternary ammonium salt disinfectant is 10-11, and the color of the composite quaternary ammonium salt disinfectant is light blue viscous liquid without sediment.
A method for preparing composite quaternary ammonium salt disinfectant comprises
Step 1: adding water into a reaction kettle, heating to 40-80 ℃, adding alkyl dimethyl benzyl ammonium chloride and alkyl dimethyl ethyl benzyl ammonium chloride according to the proportion of 1:1, and stirring to assist dissolution until dissolution is complete;
step 2: when the temperature is cooled to room temperature, the humectant and the viscosity modifier are added in sequence and stirred until the humectant and the viscosity modifier are completely dissolved;
step 3: and after the dissolution is completed, adding a pH regulator into the reaction kettle, and uniformly stirring to ensure that the pH is 10-11, thus obtaining the finished product.
Preferably, in the step 1, if the production equipment cannot meet the heating requirement, adding sodium chloride and sodium carbonate into the reaction kettle, stirring and dissolving, and continuously feeding after standing for 12 hours; if the dissolution is still incomplete, the sodium chloride dosage is reduced.
The application of the composite quaternary ammonium salt disinfectant is that the composite quaternary ammonium salt disinfectant is used for killing pyogenic cocci, enteropathogenic bacteria, pathogenic yeasts and common bacteria infected in hospitals and can inactivate viruses.
Preferably, the composite quaternary ammonium salt disinfectant is used for disinfecting the surfaces of various hard objects such as hospitals, families, schools, air conditioners, toys for children and car seats.
Preferably, the application method of the composite quaternary ammonium salt disinfectant is that the product is directly wiped or sprayed on the surface of an object, and the action time is 10min.
The beneficial effects of the invention are as follows: the invention discloses a composite quaternary ammonium salt disinfectant, a preparation method and application thereof, and compared with the prior art, the invention has the following improvement:
1. the invention designs a composite quaternary ammonium salt disinfectant, which comprises 4-5% of mixed surfactant, 0.4-0.6% of humectant, 1-2% of viscosity regulator, 1-2% of pH regulator and the balance of water; when the compound quaternary ammonium salt disinfectant is used, 2 quaternary ammonium salt cationic surfactants (alkyl dimethyl benzyl ammonium chloride and alkyl dimethyl ethyl benzyl ammonium chloride) are adopted to jointly act in a disinfectant liquid system, and the combined use of the two surfactants can produce a synergistic antibacterial effect, so that the prepared compound quaternary ammonium salt disinfectant is excellent and durable in antibacterial effect;
2. meanwhile, in the compound quaternary ammonium salt disinfectant, the fatty alcohol polyoxyethylene ether, the sodium chloride, the sodium carbonate and the sodium bicarbonate have antibacterial performance and are uniformly dispersed in the disinfectant, so that the disinfectant is wide in antibacterial spectrum, mild, free of stimulation and good in stability, and a preservative is not required to be added; experiments prove that the pH of the composite quaternary ammonium salt disinfectant is 10-11, the viscosity is 17S, the composite quaternary ammonium salt disinfectant is light blue viscous liquid, no precipitation exists, the biological degradation degree of each surfactant in the raw materials is not lower than 90%, the total effective matters are not lower than 8%, and each technical index meets the national standard, and the composite quaternary ammonium salt disinfectant has the advantages of strong sterilization performance, wide sterilization spectrum, mildness, no stimulation and the like.
Detailed Description
In order to enable those skilled in the art to better understand the technical solution of the present invention, the technical solution of the present invention is further described below with reference to examples.
Example 1: a composite quaternary ammonium salt disinfectant comprises the following raw materials: 4% -5% of mixed surfactant, 0.4% -0.6% of humectant, 1% -2% of viscosity regulator, 1% -2% of pH regulator and the balance of water; the mixed surfactant is a mixture of alkyl dimethyl benzyl ammonium chloride and alkyl dimethyl ethyl benzyl ammonium chloride; the mixed surfactant comprises the following components in percentage by mass: 50% of alkyl dimethyl benzyl ammonium chloride: 50% of alkyl dimethyl ethyl benzyl ammonium chloride; the humectant is fatty alcohol polyoxyethylene ether; the viscosity regulator is sodium chloride; the pH regulator is one of sodium carbonate or sodium bicarbonate.
Preferably, in the composite quaternary ammonium salt disinfectant of the embodiment, a mixture of alkyl dimethyl benzyl ammonium chloride and alkyl dimethyl ethyl benzyl ammonium chloride is used as the cationic surfactant for washing; and the carbon chain length of the alkyl structure is generally C12-C18, and for alkyl dimethyl benzyl ammonium chloride, the preferred C12-C14-C16-C18 is 5 percent, 60 percent, 30 percent and 5 percent of alkyl dimethyl benzyl ammonium chloride; for alkyl dimethyl ethyl benzyl ammonium chloride, the preferred example uses alkyl dimethyl ethyl benzyl ammonium chloride with a C12:C14 of 68 percent to 32 percent; the alkyl dimethyl benzyl ammonium chloride and the alkyl dimethyl ethyl benzyl ammonium chloride are combined to generate synergistic antibacterial effect, and the sterilization effect of the antibacterial agent can be effectively enhanced by the mode.
Preferably, the fatty alcohol polyoxyethylene ether has a plurality of varieties due to the difference of the carbon number of fatty alcohol and the addition number of ethylene oxide, and the AEO7, AEO9 and AEO10 fatty alcohol polyoxyethylene ether are preferably adopted as the humectant in the embodiment, and the series has good wetting, emulsifying and decontamination performances and the like, has small irritation, has an antibacterial effect, is beneficial to reducing skin irritation and enhancing the antibacterial performance of the disinfectant, ensures that the surfactant component in the disinfectant is dispersed more uniformly, and ensures that the antibacterial effect is more durable.
Preferably, the pH of the composite quaternary ammonium salt disinfectant is 10-11, the composite quaternary ammonium salt disinfectant is light blue viscous liquid and has no sediment, the biodegradation degree of each surfactant in the raw materials is not lower than 90%, the total effective matters are not lower than 10%, the technical indexes of the composite quaternary ammonium salt disinfectant are in accordance with the national standard, and the composite quaternary ammonium salt disinfectant has relatively strong detergency and antibacterial effect. The embodiment does not need to add preservative, is mild, has no stimulation, and has good stability, safety and environmental protection.
The preparation process of the composite quaternary ammonium salt disinfectant comprises the following steps of
Step 1: adding water (usually deionized water) into a reaction kettle, preferably heating to 40-80 ℃, adding alkyl dimethyl benzyl ammonium chloride and alkyl dimethyl ethyl benzyl ammonium chloride, starting stirring, and stirring to assist dissolution until dissolution is complete;
step 2: when the temperature is cooled to room temperature, preferably, the humectant and the viscosity regulator are added in sequence and stirred until the humectant and the viscosity regulator are completely dissolved;
step 3: and after the dissolution is completed, adding a pH regulator into the reaction kettle, and uniformly stirring to ensure that the pH is 10-11, thus obtaining the finished product.
Preferably, in the preparation process of the composite quaternary ammonium salt disinfectant, if production equipment cannot meet the heating requirement, sodium chloride and sodium carbonate are recommended to be added, stirred and dissolved, and the mixture is continuously fed after being kept still for 12 hours; if the dissolution is still incomplete, the sodium chloride feeding amount can be properly reduced, so that the viscosity is only reduced, and the sterilization effect is not influenced.
Example 2: unlike example 1, in this example, a plurality of example experiments were used to verify the effect of the composite quaternary ammonium salt disinfectant described in example 1 above, and in this example, all parts by weight are given unless otherwise specified. In the following examples, the raw materials used were commercial products. The fatty alcohol polyoxyethylene ether is AEO9.
Example 1: adding 93.6kg of deionized water into a reaction kettle, heating to 40 ℃, adding 2kg of alkyl dimethyl benzyl ammonium chloride and 2kg of alkyl dimethyl ethyl benzyl ammonium chloride, and starting stirring until the mixture is completely dissolved; after the temperature is cooled to room temperature, 0.4kg of fatty alcohol-polyoxyethylene ether and 1kg of sodium chloride are sequentially added, and the mixture is stirred until the mixture is completely dissolved; after the dissolution is completed, adding 1kg of sodium carbonate into the reaction kettle, and uniformly stirring to ensure that the pH is 10-11, thus obtaining 100kg of finished products.
Example 2: 91.5kg of deionized water is added into a reaction kettle, 2.25kg of alkyl dimethyl benzyl ammonium chloride and 2.25kg of alkyl dimethyl ethyl benzyl ammonium chloride are added after the temperature is raised to 60 ℃, and stirring is started until the mixture is completely dissolved; after the temperature is cooled to room temperature, 0.5kg of fatty alcohol-polyoxyethylene ether and 1.5kg of sodium chloride are sequentially added, and the mixture is stirred until the mixture is completely dissolved; after the dissolution is completed, adding 1.5kg of sodium carbonate into the reaction kettle, and uniformly stirring to ensure that the pH is 10-11, thus obtaining 100kg of finished products.
Example 3: adding 90.4kg of deionized water into a reaction kettle, heating to 80 ℃, adding 2.5kg of alkyl dimethyl benzyl ammonium chloride and 2.5kg of alkyl dimethyl ethyl benzyl ammonium chloride, stirring until the mixture is completely dissolved, cooling to room temperature, sequentially adding 0.6kg of fatty alcohol polyoxyethylene ether and 2kg of sodium chloride, and stirring until the mixture is completely dissolved; after the dissolution is completed, adding 2kg of sodium carbonate into the reaction kettle, and uniformly stirring to ensure that the pH is 10-11, thus obtaining 100kg of finished products.
Comparative examples 1 and 2 dosage ratios refer to example 1, comparative examples 3 and 4 dosage ratios refer to example 2, and comparative examples 5 and 6 dosage ratios refer to example 3. The alkyl dimethyl ethyl benzyl ammonium chloride of comparative examples 1, 3 and 5 was replaced with alkyl dimethyl benzyl ammonium chloride in the same amount as the comparative examples; the alkyl dimethyl benzyl ammonium chloride of comparative examples 2, 4 and 6 was replaced by alkyl dimethyl ethyl benzyl ammonium chloride in the same amount as the comparative examples.
Comparative example 1: adding 93.6kg of deionized water into a reaction kettle, heating to 40 ℃, adding 4kg of alkyl dimethyl benzyl ammonium chloride, and starting stirring until the mixture is completely dissolved; after the temperature is cooled to room temperature, 0.4kg of fatty alcohol-polyoxyethylene ether and 1kg of sodium chloride are sequentially added, and the mixture is stirred until the mixture is completely dissolved; after the dissolution is completed, adding 1kg of sodium carbonate into the reaction kettle, and uniformly stirring to ensure that the pH is 10-11; thus, 100kg of a final product was obtained.
Comparative example 2: adding 93.6kg of deionized water into a reaction kettle, heating to 40 ℃, adding 4kg of alkyl dimethyl ethyl benzyl ammonium chloride, and starting stirring until the mixture is completely dissolved; after the temperature is cooled to room temperature, 0.4kg of fatty alcohol-polyoxyethylene ether and 1kg of sodium chloride are added in sequence, and the mixture is stirred until the mixture is completely dissolved. After the dissolution is completed, adding 1kg of sodium carbonate into the reaction kettle, and uniformly stirring to ensure that the pH is 10-11, thus obtaining 100kg of finished products.
Comparative example 3: 91.5kg of deionized water is added into a reaction kettle, after the temperature is raised to 60 ℃, 4.5kg of alkyl dimethyl benzyl ammonium chloride is added, and stirring is started until the mixture is completely dissolved; after the temperature is cooled to room temperature, 0.5kg of fatty alcohol-polyoxyethylene ether and 1.5kg of sodium chloride are sequentially added, and the mixture is stirred until the mixture is completely dissolved; after the dissolution is completed, adding 1.5kg of sodium carbonate into the reaction kettle, and uniformly stirring to ensure that the pH is 10-11, thus obtaining 100kg of finished products.
Comparative example 4: 91.5kg of deionized water is added into a reaction kettle, after the temperature is raised to 60 ℃, 4.5kg of alkyl dimethyl ethyl benzyl ammonium chloride is added, and stirring is started until complete dissolution is achieved; after the temperature is cooled to room temperature, 0.5kg of fatty alcohol-polyoxyethylene ether and 1.5kg of sodium chloride are sequentially added, and the mixture is stirred until the mixture is completely dissolved; after the dissolution is completed, adding 1.5kg of sodium carbonate into the reaction kettle, and uniformly stirring to ensure that the pH is 10-11, thus obtaining 100kg of finished products.
Comparative example 5: adding 90.4kg of deionized water into a reaction kettle, heating to 80 ℃, adding 5kg of alkyl dimethyl benzyl ammonium chloride, and starting stirring until the mixture is completely dissolved; after the temperature is cooled to room temperature, 0.6kg of fatty alcohol-polyoxyethylene ether and 2kg of sodium chloride are sequentially added, and the mixture is stirred until the mixture is completely dissolved; after the dissolution is completed, adding 2kg of sodium carbonate into the reaction kettle, and uniformly stirring to ensure that the pH is 10-11, thus obtaining 100kg of finished products.
Comparative example 6: adding 90.4kg of deionized water into a reaction kettle, heating to 80 ℃, adding 5kg of alkyl dimethyl ethyl benzyl ammonium chloride, and starting stirring until the mixture is completely dissolved; after the temperature is cooled to room temperature, 0.6kg of fatty alcohol-polyoxyethylene ether and 2kg of sodium chloride are sequentially added, and the mixture is stirred until the mixture is completely dissolved; after the dissolution is completed, adding 2kg of sodium carbonate into the reaction kettle, and uniformly stirring to ensure that the pH is 10-11, thus obtaining 100kg of finished products.
Examples 1 to 3 are composite quaternary ammonium salt disinfectant prepared by a normal process, comparative examples 1 to 6 are composite quaternary ammonium salt disinfectant added with single quaternary ammonium salt disinfectant, and antibacterial performance tests (antibacterial performance tests are performed according to WS/T650-2019 standard) are respectively performed, and the results are shown in Table 1;
table 1: examples and comparative examples antibacterial Property test Effect
As can be seen from Table 1, the sterilizing rates of the compound quaternary ammonium salt sterilizing liquid in examples 1-3 can reach more than 99% in 20 minutes; one quaternary ammonium salt disinfectant is singly used in comparative examples 1-6, and the sterilization rates of the quaternary ammonium salt disinfectant are respectively lower than those of examples 1-3, which shows that the combination of the two quaternary ammonium salt disinfectants can produce synergistic effect and enhance the antibacterial effect of the disinfectant.
From the above examples, the pH of the composite quaternary ammonium salt disinfectant disclosed in the embodiment 1 of the invention is 10-11, the viscosity is 17S, the disinfectant is light blue viscous liquid, no precipitate exists, the biodegradation degree of each surfactant in the raw materials is not lower than 90%, the total effective matters are not lower than 8%, and the technical indexes all meet the national standard. The composite quaternary ammonium salt disinfectant has the characteristics of strong sterilization performance, broad sterilization spectrum, mildness, no stimulation and the like.
Example 3: unlike the above examples, the above composite quaternary ammonium salt disinfectant was subjected to quaternary ammonium salt content measurement, pH measurement, stability test, metal corrosiveness measurement, staphylococcus aureus neutralizer identification test and suspension quantitative sterilization test, escherichia coli suspension quantitative sterilization test, pseudomonas aeruginosa suspension quantitative sterilization test, candida albicans neutralizer identification test and suspension quantitative sterilization test, poliovirus neutralizer identification test and suspension quantitative inactivation test, disinfection field test of a disinfectant on a general object surface, acute oral toxicity test, one-time complete skin irritation test and mouse bone marrow multi-dye red blood cell micronucleus test by using the present examples to verify whether the composite quaternary ammonium salt disinfectant meets enterprise and production standards.
Sampling: 20 bottles of 500 ml/bottle of the complex quaternary ammonium salt disinfectant as described in example 1 were taken, the date of production or lot number was 20210810, and sent to a detection service unit for the following experimental detection.
Experiment 1: quaternary ammonium salt content determination
1. And (3) equipment:
(1) Sample: the composite quaternary ammonium salt disinfectant (batch number is 20210810) contains quaternary ammonium salt as an active ingredient; (2) test apparatus: an electronic balance (model: ME204E, number: ZK-L-019) and a glass burette; (3) standard solution: the concentration of the tetraphenylboron sodium standard solution is 0.02000mo1/L (Beijing North Weijingsu technical institute);
2. method of
(1) The test basis is as follows: "sanitary requirements for quaternary ammonium salt disinfectants" GB/T26369-2020; (2) inspection environment: the temperature is 24 ℃ and the relative humidity is 45%;
3. results
The content of the quaternary ammonium salt of the effective component is 0.0796 percent (Table 2) through detection of the composite quaternary ammonium salt disinfectant
Table 2: determination result of quaternary ammonium salt content of disinfectant
4. Conclusion(s)
The effective component of the compound quaternary ammonium salt disinfectant has the quaternary ammonium salt content of 0.0796 percent and accords with the enterprise standard of Q/YD08-2021 of quaternary ammonium salt disinfectant.
Experiment 2: PH measurement
1. And (3) equipment:
(1) Sample: the composite quaternary ammonium salt disinfectant (batch number is 20210810) contains quaternary ammonium salt as an active ingredient; (2) test apparatus: PH meter (model: PHS-3C, number: ZK-L-013); (3) standard solution: phosphate buffer ph=6.86 (25 ℃), potassium hydrogen phthalate buffer ph=4.00 (25 ℃), borax buffer ph=9.18 (25 ℃);
2. method of
(1) The test basis is as follows: disinfection technical Specification (2002 edition); (2) inspection environment: the temperature is 24 ℃ and the relative humidity is 45%;
3. results
The pH value of the composite quaternary ammonium salt disinfectant is 10.33 (Table 3) after detection
Table 3: determination result of pH value of disinfectant containing quaternary ammonium salt for recovery of IZAON
4. Conclusion(s)
The pH value of the composite quaternary ammonium salt disinfectant is 10.33, and meets the requirements of the enterprise standard 'quaternary ammonium salt disinfectant' Q/YD08-2021.
Experiment 3: stability test
1. And (3) equipment:
(1) Sample: the composite quaternary ammonium salt disinfectant (batch number is 20210810) contains quaternary ammonium salt as an active ingredient; (2) test apparatus: constant temperature and humidity incubator (model: HWS-250, number: ZK-L-021);
2. method of
(1) The test basis is as follows: "disinfectant stability evaluation method" GB/T38499-2020; (2) inspection environment: the temperature is 23 ℃ and the relative humidity is 47%; (3) test conditions: the temperature is 54+/-1 ℃ and the time is 14d;
3. results
Experiments prove that the composite quaternary ammonium salt disinfectant is stored for 14 days in a constant temperature and humidity incubator at 54+/-1 ℃ and the content of the quaternary ammonium salt serving as an active ingredient is 0.0779%; the decrease rate of the content of the active ingredient was 2.1% as compared with 0.0796% before stabilization (Table 4)
Table 4: test result of content stability of quaternary ammonium salt in composite quaternary ammonium salt disinfectant
4. Conclusion(s)
The composite quaternary ammonium salt disinfectant is stored for 14 days in a constant temperature and humidity incubator at 54+/-1 ℃ and the content of the quaternary ammonium salt serving as an active ingredient is 0.0779%; compared with 0.0796% of the content before stabilization, the content reduction rate of the active ingredients is 2.1%, meets the requirements of GB/T38499-2020, and the storage and storage period of the product is 1 year.
Experiment 4: determination of metal corrosiveness
1. And (3) equipment:
(1) Sample: the composite quaternary ammonium salt disinfectant (batch number is 20210810) contains quaternary ammonium salt as an active ingredient; (2) test apparatus: electronic balance (model: ME204E, number: ZK-L-019) and electricA hot blast drying oven (model: GZX-9246MBE, number: ZK-L-017); (3) test sheet metal: stainless steel, carbon steel, copper, aluminum (round, 24.0mm diameter, 1.0mm thick, with a small hole of 2.0mm diameter, total surface area of about 9.8017 cm) 2 Finish degree 4-6, manufacturer: the laboratory equipment works in the city of gold altar).
2. Method of
(1) The test basis is as follows: "disinfectant stability evaluation method" GB/T38499-2020; (2) inspection environment: the temperature is 22-25 ℃ and the relative humidity is 42-47%;
3. results
The test proves that the corrosion rates (R) of the composite quaternary ammonium salt disinfectant on stainless steel, carbon steel, aluminum and copper are respectively 0.0016mm/a, 0.0859mm/a, 0.3592mm/a and 0.0142mm/a, and the corrosion rates are judged according to the corrosion grading standard: the disinfectant solution of the quaternary ammonium salt for the recovery of the Chinese patent is basically free from corrosion to stainless steel, carbon steel and copper are slightly corroded, and aluminum is moderately corroded (table 5);
table 5: corrosion test result of composite quaternary ammonium salt disinfectant
4. Conclusion(s)
The composite quaternary ammonium salt disinfectant is judged according to the corrosiveness grading standard that the disinfectant is basically non-corroding to stainless steel, slightly corroding to carbon steel and copper and moderately corroding to aluminum.
Experiment 5: staphylococcus aureus neutralizer identification assay and suspension quantitative sterilization assay
1. And (3) equipment:
(1) Sample: the composite quaternary ammonium salt disinfectant (batch number is 20210810) contains quaternary ammonium salt as an active ingredient; (2) Test strain staphylococcus aureus (ATCC 6538, provided by the national academy of medical science) passage 7; (3) organic interferents: 3.0% BSA; (4) neutralizing agent: D/E neutralization broth of 1.0% histidine; (5) culture medium: tryptone soy agar medium (TSA); (6) instrumentation: an electrothermal constant temperature incubator (model DHP-9272);
2. method of
(1) The test basis is as follows: the sterilizing effect test method of disinfectant laboratory GB/T38502-2020, 5.4.4 and 5.6.3; (2) neutralizer identification assay: the concentration of the sample is stock solution, and the test temperature is 20+/-1 ℃; (3) Quantitative sterilization test of suspension, wherein the concentration of a sample is stock solution, the action time is 5min, 10min and 15min respectively, and the test temperature is 20+/-1 ℃; (4) environmental conditions: the temperature is 23-25 ℃, the relative humidity is 55-58%, and the test is repeated for 3 times;
3. results
(1) A neutralizer identification test;
table 6: neutralization agent identification test results
(2) Test for killing staphylococcus aureus by composite quaternary ammonium salt disinfectant
Table 7: killing effect of disinfectant containing quaternary ammonium salt for killing staphylococcus aureus
4. Conclusion(s)
(1) The D/E neutralization broth neutralizing agent containing 1.0% histidine can neutralize the killing effect of the composite quaternary ammonium salt disinfectant stock solution on staphylococcus aureus, and the neutralizing agent and the neutralization product have no adverse effect on the growth and the culture medium of the tested bacteria, thereby meeting the requirements of GB/T38502-2020, the sterilizing effect test method of disinfectant laboratory;
(2) The sterilizing effect of the composite quaternary ammonium salt disinfectant stock solution is 10min, the killing logarithmic value of each test of staphylococcus aureus is more than or equal to 5.00, and the requirements of GB/T38502-2020 of sterilizing laboratory sterilizing effect test method are met.
Experiment 6: quantitative sterilization test of escherichia coli suspension
1. Equipment and method for manufacturing the same
(1) Sample: the composite quaternary ammonium salt disinfectant (batch number is 20210810) contains quaternary ammonium salt as an active ingredient; (2) test strain: coli (8099, proc. Natl. Acad. Sci. Of military medical science) 7 th generation; (3) organic interferents: 3.0% BSA; (4) neutralizing agent: D/E neutralization broth of 1.0% histidine; (5) culture medium: tryptone soy agar medium (TSA); (6) instrumentation: an electrothermal constant temperature incubator (model DHP-9272);
2. method of
(1) The test basis is as follows: the sterilizing effect test method of disinfectant laboratories GB/T38502-2020 item 5.6.3; (2) Quantitative sterilization test of suspension, wherein the concentration of a sample is stock solution, the action time is 5min, 10min and 15min respectively, and the test temperature is 20+/-1 ℃; (3) environmental conditions: the temperature is 23-24 ℃, the relative humidity is 57-58%, and the test is repeated for 3 times;
3. results
Table 8: killing effect of composite quaternary ammonium salt disinfectant on escherichia coli
Note that: the average colony number of the negative control group and the positive control group is 2.4X10 after sterile growth 7 CFU/mL；
4. Conclusion(s)
The sterilization effect of the composite quaternary ammonium salt disinfectant stock solution is 10min, the sterilization logarithmic value of each test of the escherichia coli is more than or equal to 5.00, and the requirements of GB/T38502-2020 of the sterilizing laboratory sterilizing effect test method are met.
Experiment 7: quantitative sterilization test for pseudomonas aeruginosa suspension
1. Equipment and method for manufacturing the same
(1) Sample: the composite quaternary ammonium salt disinfectant (batch number is 20210810) contains quaternary ammonium salt as an active ingredient; (2) test strain: pseudomonas aeruginosa (ATCC 15442, proc. Natl. Acad. Sci. Of military medical science) passage 7; (3) organic interferents: 3.0% BSA; (4) neutralizing agent: D/E neutralization broth of 1.0% histidine; (5) culture medium: tryptone soy agar medium (TSA); (6) instrumentation: an electrothermal constant temperature incubator (model DHP-9272);
2. method of
(1) The test basis is as follows: the sterilizing effect test method of disinfectant laboratories GB/T38502-2020 item 5.6.3; (2) quantitative sterilization test of suspension: the concentration of the sample is stock solution, the action time is 5min, 10min and 15min respectively, and the test temperature is 20+/-1 ℃; (3) environmental conditions: the temperature is 23-24 ℃, the relative humidity is 56-57%, and the test is repeated 3 times;
3. results
Table 9: killing effect of composite quaternary ammonium salt disinfectant on pseudomonas aeruginosa
Note that: the average colony number of the negative control group and the positive control group is 1.9X10 after sterile growth 7 CFU/mL；
4. Conclusion(s)
The sterilization effect of the composite quaternary ammonium salt disinfectant stock solution is 10min, the killing log value of each test of pseudomonas aeruginosa is more than or equal to 5.00, and the requirements of GB/T38502-2020 of disinfectant laboratory sterilizing effect test method are met.
Experiment 8: candida albicans neutralizer identification test and suspension quantitative sterilization test
1. Equipment and method for manufacturing the same
(1) Sample: the composite quaternary ammonium salt disinfectant (batch number is 20210810) contains quaternary ammonium salt as an active ingredient; (2) test strain: candida albicans (ATCC 10231, provided by the academy of primary military medical science) passage 7; (3) organic interferents: 3.0% BSA; (4) neutralizing agent: D/E neutralization broth of 1.0% histidine; (5) culture medium: sandcastle agar medium; (6) instrumentation: an electrothermal constant temperature incubator (model DHP-9272);
2. method of
(1) The test basis is as follows: the sterilizing effect test method of disinfectant laboratory GB/T38502-2020, 5.4.4 and 5.8.4; (2) The neutralizing agent identification test, wherein the concentration of a sample is stock solution, and the test temperature is 20+/-1 ℃; (3) Quantitative sterilization test of suspension, wherein the concentration of a sample is stock solution, the action time is 5min, 10min and 15min respectively, and the test temperature is 20+/-1 ℃; (4) The environmental conditions are that the temperature is 24 ℃ to 25 ℃ and the relative humidity is 55 to 58 percent, and the test is repeated for 3 times;
3. results
(1) Neutralization agent identification test
Table 10: neutralization agent identification test results
(2) Test for killing candida albicans by composite quaternary ammonium salt disinfectant
Table 11: killing effect of composite quaternary ammonium salt disinfectant on candida albicans
Note that: the average colony number of the negative control group and the positive control group is 1.8X10 after sterile growth 6 CFU/mL；
4. Conclusion(s)
(1) The D/E neutralization broth neutralizing agent containing 1.0% histidine can neutralize the killing effect of the original solution of the sterilizing solution of the quaternary ammonium salt of the recovery complex of the xiaone on candida albicans, and the neutralizing agent and the neutralization product have no adverse effect on the growth and the culture medium of the tested bacteria, thereby meeting the requirements of the sterilizing effect test method of disinfectant laboratory in GB/T38502-2020; (2) The sterilization effect of the composite quaternary ammonium salt disinfectant stock solution is 10min, the sterilization logarithmic value of each test of candida albicans is more than or equal to 4.00, and the requirements of GB/T38502-2020 of the sterilizing laboratory sterilizing effect test method are met.
Experiment 9: poliovirus neutralizer identification assay and suspension quantitative inactivation assay
1. And (3) equipment:
(1) Sample: the composite quaternary ammonium salt disinfectant (batch number is 20210810) contains quaternary ammonium salt as an active ingredient; (2) test strains: poliovirus (PV-I, vaccine strain; hereinafter PV-I virus); (3) the host cell is a Vero cell (ATCCCL-81); (4) DMEM medium, fetal bovine serum and 0.25% trypsin; (5) cell complete medium and cell maintenance medium; (6) neutralizing agent: D/E neutralization broth of 1.0% histidine; (7) cell culture flasks and 96-well plates; (8) carbon dioxide incubator (model: BPN-80 CH); (9) Inverted microscope (model: BM-37 XB) and centrifuge (model: RGL-160T); (10) other sterile equipment, etc.;
2. method of
(1) The test basis is as follows: 2.1.1.10 in the disinfection technical Specification (2002 edition) requires virus proliferation and virus titer measurement, and virus suspension is taken for neutralization agent identification test and virus inactivation test; (2) neutralizer identification assay: taking a composite quaternary ammonium salt disinfectant solution for direct use in a test, according to the rule of disinfection technical Specification (2002 edition), carrying out neutralizing agent identification test and result judgment in 6 groups by adopting a virus suspension quantitative test program in a residual disinfectant chemical neutralization method, wherein the test temperature is 20 ℃ plus or minus 1 ℃ and the action time is 1min, measuring the titer of each group of viruses and calculating the inactivation pair value after a sample is inoculated with cells, and repeating the test for 3 times; (3) virus inactivation assay: taking a composite quaternary ammonium salt disinfectant for direct use in a test, carrying out test operation by adopting a suspension quantitative inactivation test program according to the specification of the disinfection technical Specification (2002 edition), wherein the test temperature is 20+/-1 ℃, the action time is 5min, 10min and 15min respectively, inoculating 2 bottles into each dose group, inoculating 1ml into each bottle, culturing in a 37 ℃ and 5% carbon dioxide incubator, and calculating the virus titer inactivation logarithmic value; the test is repeated for 3 times, the inactivation logarithmic value of each test is more than or equal to 4.00, and the inactivation effect of the PV-I virus can be judged to reach the disinfection qualification requirement; the test is provided with a virus suspension positive control at the same time;
3. results
(1) Neutralization agent identification test results
Table 12: identification test result of composite quaternary ammonium salt disinfectant neutralizer
Note that: the numbers in the table are the average of 3 replicates;
(2) Results of the inactivation test on PV-I virus
Table 13: result of PV-I virus inactivation test by composite quaternary ammonium salt disinfectant
4. Conclusion(s)
(1) The D/E neutralization broth neutralizing agent containing 1.0% histidine can neutralize the residual effect of the complex quaternary ammonium salt disinfectant stock solution on the PV-I virus, and the neutralization product has no influence on the growth of Vero cells and the PV-I virus, thereby meeting the requirements specified in the disinfection technical Specification (2002 edition); (2) The disinfection effect of the composite quaternary ammonium salt disinfectant stock solution is that the PV-I virus inactivation logarithmic value is not less than 4.00 after 10 minutes, and meets the requirements specified in the disinfection technical Specification (2002 edition).
Experiment 10: sterilization field test of a sterilant on a surface of a general object
1. And (3) equipment:
(1) Sample: the composite quaternary ammonium salt disinfectant (batch number is 20210810) contains quaternary ammonium salt as an active ingredient; (2) test strain: natural bacteria; (3) neutralizing agent: D/E neutralization broth of 1.0% histidine; (4) culture medium: tryptone soy agar medium (TSA); (5) instrumentation: an electrothermal constant temperature incubator (model DHP-9272); (6) subject: a stainless steel table top; (7) specification plate: stainless steel material, a space of 5.0cm x 5.0cm is left in the center; (8) sterile swabs;
2. method of
(1) The test basis is as follows: 2.1.2.10 to the disinfection Specification (2002 edition); (2) Disinfection field test of disinfectants on general object surfaces: the concentration of the disinfectant is stock solution, the action time is 10min, and the number of test samples is 30; (3) environmental conditions: the temperature is 24 ℃ and the relative humidity is 56%;
3. results
Table 14: on-site test result of sterilizing stainless steel table top by composite quaternary ammonium salt sterilizing liquid
Note that: sterile growth of the negative control group;
4. conclusion(s)
The average killing logarithmic value of each test of the natural bacteria on 30 stainless steel table tops for 10min under the disinfection effect of the composite quaternary ammonium salt disinfectant stock solution is more than or equal to 1.00, and meets the requirements of disinfection technical Specification (2002 edition).
Experiment 11: acute oral toxicity test
1. And (3) equipment:
(1) Sample: composite quaternary ammonium salt disinfectant (batch number 20210810), liquid; (2) laboratory animals: SPF grade KM mice, animal pass number, supplied by Henan province laboratory animal center: no.41097521100036274; (3) animal feed: class C mouse feed provided by the experimental animal center in henna; (4) test environment: for barrier environment, use license number: SYXK (relaxation) 2017-0012;
2. method of
(1) The detection basis is as follows: disinfection technical Specification (2002 edition) 2.3.1; (2) contamination mode: oral contamination; (3) test operation steps: the dosage of the stomach of 20 animals (male and female halves) is 5000mg/kg body weight, and the animals are fasted overnight before stomach irrigation, so that drinking water is not limited; observing the poisoning performance and death time of the animal after the infection, performing autopsy on the dead animal and the dead animal at the expiration of the observation, and visually observing whether the viscera are abnormal or not, wherein the observation time is 14d;
3. results
The stomach was irrigated with a compound quaternary ammonium salt disinfectant (lot number 20210810) at a dosage of 5000mg/kg body weight for 14 days of continuous observation. Animals sacrificed at the end of the death and trial period were generally dissected and major organs such as liver, kidney, spleen, stomach, intestine, heart, lung, etc. were not visibly abnormal. According to the dosage, the acute oral toxicity test LD of the disinfectant of the quaternary ammonium salt of the XIAOEn rehabilitation to KM mice is known to be >5000mg/kg body weight, and the detailed data are shown in Table 15:
table 15: acute oral toxicity test result of composite quaternary ammonium salt disinfectant
4. Conclusion(s)
Compound quaternary ammonium salt disinfectant (batch number 20210810) KM mice acute oral toxicity test LD 50 >5000mg/kg body weight, according to the acute oral toxicity grading standard of the disinfection technical Specification (2002 edition), is practically nontoxic and meets the requirements of the disinfection technical Specification (2002 edition).
Experiment 12: one-time complete skin irritation test
1. And (3) equipment:
(1) Sample: composite quaternary ammonium salt disinfectant (batch number 20210810), liquid; (2) The number of the experimental animals is 3, and the number of the animal qualification number is No.42817300001543; (3) Animal feed, which is C-grade rabbit feed provided by Henan province laboratory animal center; (4) test environment: for a common environment, use license number: SYXK (relaxation) 2017-0012;
2. method of
(1) The detection basis is as follows: disinfection technical Specification (2002 edition) 2.3.3; (2) contamination mode: percutaneous contamination; (3) skin treatment mode: dehairing by using a pet trimmer; (4) test operation steps: removing hairs on two sides of the spine of the rabbit 24 hours before the test, and checking that the skin is intact, wherein the hair removal range is about 3cm multiplied by 3cm on the left and right; the next day, 0.5ml of the Xiaoenkang compound quaternary ammonium salt disinfectant is directly smeared on the skin at one side of the rabbit, the smearing area is 2.5cm multiplied by 2.5cm, then the rabbit is covered by oilpaper, and then the rabbit is fixed by using a non-irritating adhesive tape; distilled water was applied to the other side for comparison. The application time is 4 hours. After the test is finished, removing the residual test object by using warm water; local skin reactions were observed 1h, 24h, 48h after removal of the test subjects, respectively, and scored as required.
3. Results
After application and removal of the test subjects, the local skin reactions were observed over 1h, 24h and 48h and scored separately. The highest skin irritation index of the composite quaternary ammonium salt disinfectant (batch number 20210810) to rabbits is 0, and detailed data are shown in Table 16;
table 16: composite quaternary ammonium salt disinfectant (batch number 20210810) one-time complete skin irritation response score
Integral mean value 0min
4. Conclusion(s)
The highest skin irritation index of the compound quaternary ammonium salt disinfectant (the lot number is 20210810) to rabbits is 0, and the compound quaternary ammonium salt disinfectant belongs to no irritation according to the skin irritation intensity grading standard in the disinfection technical Specification (2002 edition), and meets the requirements of the disinfection technical Specification (2002 edition).
Experiment 13: mouse bone marrow multipotent erythrocyte micronucleus test
1. Equipment and method for manufacturing the same
(1) Sample: composite quaternary ammonium salt disinfectant (batch number 20210810), liquid; (2) Experimental animals SPF grade KM mice provided by Henan province experimental animal center, animal pass number: no.410975211100036274; (3) animal feed: class C mouse feed provided by the experimental animal center in henna; (4) test environment: for barrier environment, use license number: SYXK (relaxation) 2017-0012.
2. Method of
(1) The detection basis is as follows: 2.3.8.4 of the disinfection Specification (2002 edition); (2) experimental grouping: animals were randomly divided into 5 groups of 10 animals each, each male and female half according to body weight; the three dose groups of the test object are respectively 500mg/kg; (3) experimental operation steps: animal contamination adopts an oral gastric lavage 30h contamination method, namely, the two contamination intervals are 24h, and the materials are obtained 6h after the second contamination; animals were sacrificed by cervical whitening and sternum were removed. Stripping off muscles, wiping off blood stains, and cutting off the exposed bone marrow of the sternum; diluting the smear with calf serum, and air drying; fixing the dried smear in methanol for 5-10 min, dyeing with Giemsa for 10-15 min, washing with PBS with pH of 6.8, and air drying; the operation procedures of the positive control group and the negative control group are the same as those of the test group, the positive group adopts cyclophosphamide (40 mg/kg body weight), and the negative control group adopts distilled water; the area with uniform, complete and properly colored cell distribution was selected, and the number of micronucleated, multi-stained red blood cells (PCE) was counted under an oil microscope, with 2 or more micronuclei present in the PCE, still counting 1. In addition, PCE/NCE ratio should be observed as an indicator of cytotoxicity; 200 PCEs are typically counted, while the NCE seen with the counts indicates significant inhibition of bone marrow when PCB/NCE is less than 0.1, and the test should be re-performed with reduced doses of the test agent.
3. Results
The micronucleus rate of each dose group of the sample was not significantly different from that of the negative control group, whereas the difference was highly significant (P < 0.01) in the positive control group compared with the negative control group. Each set of PCE/NCE ratios is within the normal range.
Table 17: results of micronucleus test on mouse bone marrow cells with composite quaternary ammonium salt disinfectant (batch number 20210810)
4. Conclusion(s)
According to the disinfection technical Specification (2002 edition), the micronucleus test result of the mouse bone marrow multi-dye red blood cells of the composite quaternary ammonium salt disinfectant (batch No. 20210810) is negative, and meets the requirements of the disinfection technical Specification (2002 edition).
From the above verification, it can be seen that each component of the composite quaternary ammonium salt disinfectant designed in the embodiment 1 of the present invention can meet the production requirements of enterprises and national standards.
The application range, the application method and the notice are as follows:
1. the application range is as follows: the product can kill pyococcus, enteropathogenic bacteria, pathogenic yeast and common bacteria infected by hospital, and inactivate viruses, and is suitable for disinfecting surfaces of various hard objects such as hospital, family, school, air conditioner, children toy, car seat, etc.
2. The using method comprises the following steps: the product can be directly rubbed or sprayed on the surface of object for 10min.
3. Notice that: (1) The product is an external disinfectant, cannot be taken orally, and is stored in a place which is not easy to be touched by children; (2) The product has no corrosion to stainless steel basically, mild corrosion to carbon steel and copper, and moderate corrosion to aluminum; after sterilizing for a certain time, wiping or flushing the metal surface with clean water to remove residual disinfectant; (3) If the human body is carelessly contacted, clear water is used for continuous cleaning immediately, and if eyes are injured, medical treatment should be carried out early; the effective period is 24 months.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A composite quaternary ammonium salt disinfectant is characterized in that: the material is prepared from the following raw materials in percentage by weight: 4% -5% of mixed surfactant, 0.4% -0.6% of humectant, 1% -2% of viscosity regulator, 1% -2% of pH regulator and the balance of water.
2. The composite quaternary ammonium salt disinfectant as set forth in claim 1, wherein: the mixed surfactant is a mixture of alkyl dimethyl benzyl ammonium chloride and alkyl dimethyl ethyl benzyl ammonium chloride, and the mixing ratio of the alkyl dimethyl benzyl ammonium chloride to the alkyl dimethyl ethyl benzyl ammonium chloride is 1:1.
3. The composite quaternary ammonium salt disinfectant as set forth in claim 2, wherein: C12:C14:C16:C18=5%:60:30:5%; c12:c14=68% to 32% in alkyldimethylethylbenzyl ammonium chloride.
4. The composite quaternary ammonium salt disinfectant as set forth in claim 1, wherein: the humectant is fatty alcohol polyoxyethylene ether, the viscosity regulator is sodium chloride, and the pH regulator is one of sodium carbonate or sodium bicarbonate.
5. The composite quaternary ammonium salt disinfectant as set forth in claim 1, wherein: the pH value of the composite quaternary ammonium salt disinfectant is 10-11, and the color of the composite quaternary ammonium salt disinfectant is light blue viscous liquid without precipitate.
6. A method for preparing the composite quaternary ammonium salt disinfectant as set forth in claim 1, which is characterized in that: comprising
Step 1: adding water into a reaction kettle, heating to 40-80 ℃, adding alkyl dimethyl benzyl ammonium chloride and alkyl dimethyl ethyl benzyl ammonium chloride according to the proportion of 1:1, and stirring to assist dissolution until dissolution is complete;
step 2: when the temperature is cooled to room temperature, the humectant and the viscosity modifier are added in sequence and stirred until the humectant and the viscosity modifier are completely dissolved;
step 3: and after the dissolution is completed, adding a pH regulator into the reaction kettle, and uniformly stirring to ensure that the pH is 10-11, thus obtaining the finished product.
7. The method for preparing the composite quaternary ammonium salt disinfectant according to claim 6, which is characterized in that: in the step 1, if the production equipment cannot meet the heating requirement, adding sodium chloride and sodium carbonate into a reaction kettle, stirring and dissolving, and continuously feeding after standing for 12 hours; if the dissolution is still incomplete, the sodium chloride dosage is reduced.
8. Use of the composite quaternary ammonium salt disinfectant as set forth in claim 1, characterized in that: the compound quaternary ammonium salt disinfectant is used for killing pyogenic cocci, enteropathogenic bacteria, pathogenic yeasts and common bacteria infected by hospitals, and can inactivate viruses.
9. The use of a complex quaternary ammonium salt disinfectant according to claim 8, wherein: the composite quaternary ammonium salt disinfectant is used for disinfecting the surfaces of various hard objects such as hospitals, families, schools, air conditioners, toys for children and seats for automobiles.
10. The use of a complex quaternary ammonium salt disinfectant according to claim 8, wherein: the application method of the composite quaternary ammonium salt disinfectant is that the disinfectant is directly wiped or sprayed on the surface of an object, and the action time is 10min.
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