CN112042645A - Composite quaternary ammonium salt disinfectant - Google Patents

Composite quaternary ammonium salt disinfectant Download PDF

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CN112042645A
CN112042645A CN202010852691.3A CN202010852691A CN112042645A CN 112042645 A CN112042645 A CN 112042645A CN 202010852691 A CN202010852691 A CN 202010852691A CN 112042645 A CN112042645 A CN 112042645A
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quaternary ammonium
ammonium salt
disinfectant
ammonium chloride
compound
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邓旭东
尹大川
张连兵
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Northwestern Polytechnical University
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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
    • 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
    • A01N33/00Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
    • A01N33/02Amines; Quaternary ammonium compounds
    • A01N33/04Nitrogen directly attached to aliphatic or cycloaliphatic carbon atoms
    • 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
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/44Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids

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Abstract

The invention discloses a compound quaternary ammonium salt disinfectant, which comprises the following components: the volume of the compound quaternary ammonium salt disinfectant is 1000mL, 5-30 g of didecyl dimethyl ammonium chloride, 5-30 g of didodecyl dimethyl ammonium chloride, 10-50 g of benzalkonium chloride, 5-30 g of disodium edetate, 5-30 g of tetrasodium edetate, 0.1-10 g of polyvinyl amine, 30-120 mL of ethanol and the balance of water; the benzalkonium chloride is a compound of dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride and hexadecyl dimethyl benzyl ammonium chloride in a mass ratio of (2-6): 2.5-10): 1. The compound quaternary ammonium salt disinfectant has short time for killing viruses, bacteria and fungi, quick response, broad universality, no water pollution and environmental friendliness.

Description

Composite quaternary ammonium salt disinfectant
Technical Field
The invention belongs to the technical field of disinfectants, and particularly relates to a compound quaternary ammonium salt disinfectant.
Background
At present, the main components of disinfectants used for disinfecting the surfaces of air and various objects in public places, families and other places are alcohol and/or sodium hypochlorite, and the disinfectants are mainly used for killing pathogenic microorganisms such as viruses. However, alcohol is flammable and explosive, easily causes accidents such as fire disasters and the like, and is not suitable for large-area killing, and chlorine-containing disinfectants such as sodium hypochlorite have strong irritation and corrosivity, and are easy to generate toxic and harmful substances such as chlorine and the like to cause personnel injury if the disinfectant is not diluted or used properly.
The quaternary ammonium salt disinfectant is a disinfectant taking quaternary ammonium salt as a main component, and is mainly applied to the fields of sterilization, fungus, virus and the like at present due to the advantages of small irritation, no corrosiveness and the like. The existing commercial quaternary ammonium salt disinfectant product is generally a single-chain quaternary ammonium salt, or a double-chain quaternary ammonium salt, or a single-chain quaternary ammonium salt and a medium double-chain quaternary ammonium salt are compounded, wherein the single-chain quaternary ammonium salt can be used for killing bacteria and fungi, the double-chain quaternary ammonium salt can simultaneously kill bacteria, fungi and viruses, the killing effect of the existing commercial quaternary ammonium salt disinfectant on the viruses is mostly that the inactivation logarithm value is more than 3, the virus inactivation rate is more than 99.9%, the inactivation logarithm value specified in the disinfectant standard is not reached and is more than 4, and the virus inactivation rate is more than 99.99%, so that the defect of poor virus killing effect exists.
Disclosure of Invention
The invention aims to solve the technical problem of providing a compound quaternary ammonium salt disinfectant aiming at the defects of the prior art. The composite quaternary ammonium salt disinfectant takes double-chain quaternary ammonium salts of didodecyldimethylammonium chloride and didodecyldimethylammonium chloride, benzalkonium chloride, disodium edetate, tetrasodium edetate and a water-soluble high molecular compound polyvinyl amine as main components, and has short time for killing viruses, bacteria and fungi and quick response. The detection result shows that the compound quaternary ammonium salt disinfectant can effectively kill enveloped viruses (represented by influenza A virus H1N 1), bacteria (represented by staphylococcus aureus and Escherichia coli), fungi (represented by Candida albicans) and the like. The surface air and object disinfecting and killing device can meet the large-scale air and object surface disinfecting and killing requirements of public places such as airports, stations, subways and the like, and is also suitable for households, offices, vehicles, pets and the like.
In order to solve the technical problems, the invention adopts the technical scheme that: the compound quaternary ammonium salt disinfectant is characterized by comprising the following components: the volume of the compound quaternary ammonium salt disinfectant is 1000mL, 5-30 g of didecyl dimethyl ammonium chloride, 5-30 g of didodecyl dimethyl ammonium chloride, 10-50 g of benzalkonium chloride, 5-30 g of disodium edetate, 5-30 g of tetrasodium edetate, 0.1-10 g of polyvinyl amine, 30-120 mL of ethanol and the balance of water, wherein the volume of the water is the volume of the water for supplementing the compound quaternary ammonium salt disinfectant to 1000 mL;
the benzalkonium chloride is a compound of dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride and hexadecyl dimethyl benzyl ammonium chloride in a mass ratio of (2-6): 2.5-10): 1.
The compound quaternary ammonium salt disinfectant is characterized by comprising the following components: by taking the volume of the composite quaternary ammonium salt disinfectant as 1000mL, 15 g-18 g of didecyl dimethyl ammonium chloride, 12 g-15 g of didodecyl dimethyl ammonium chloride, 15 g-18 g of benzalkonium chloride, 22 g-28 g of disodium ethylenediamine tetraacetate, 25.2 g-27.2 g of tetrasodium ethylenediamine tetraacetate, 0.5 g-2.2 g of polyvinylamine, 57.175 mL-114.35 mL of ethanol, and the balance of water, wherein the volume of the water is the volume of water for supplementing the composite quaternary ammonium salt disinfectant to 1000 mL;
the benzalkonium chloride is a compound of dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride and hexadecyl dimethyl benzyl ammonium chloride in a mass ratio of (3-4.5): 4.5-7.5): 1.
The compound quaternary ammonium salt disinfectant is characterized in that the volume fraction of the ethanol is 75%.
The compound quaternary ammonium salt disinfectant is characterized in that the relative molecular mass of the polyvinylamine is 50000-80000.
The compound quaternary ammonium salt disinfectant is characterized in that the polyvinylamine is dialyzed, purified and dried, the dialysis medium for dialysis, purification and drying is water, and the dialysis time is 72 hours.
The compound quaternary ammonium salt disinfectant is characterized by being a neutral compound quaternary ammonium salt disinfectant.
Compared with the prior art, the invention has the following advantages:
1. the composite quaternary ammonium salt disinfectant takes the double-chain quaternary ammonium salts of the didecyl dimethyl ammonium chloride and the didodecyl dimethyl ammonium chloride, benzalkonium chloride, disodium edetate, tetrasodium edetate and the water-soluble macromolecular compound polyvinyl amine as main components, has short time for killing viruses, bacteria and fungi, takes effect quickly, has broad spectrum, does not cause water pollution and is environment-friendly.
2. The disinfectant meets the requirements of the specifications of disinfection technical specification 2002 edition, GB/T26369-. The detection result shows that the compound can effectively kill enveloped virus (represented by influenza A virus H1N 1), bacteria (represented by staphylococcus aureus and Escherichia coli), fungi (represented by Candida albicans) and the like, can meet the surface killing requirements of large-scale air and objects in public places such as airports, stations, subways and the like, and is also suitable for household use, office use, vehicles, pets and the like.
3. The benzalkonium chloride is a compound prepared by compounding dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride and hexadecyl dimethyl benzyl ammonium chloride according to the proportion of (3-4.5): (4.5-7.5): 1, and has better killing effect.
4. The ethanol is used for assisting the dissolution of the single-chain quaternary ammonium salt and the double-chain quaternary ammonium salt, the dissolution is rapid, the obtained compound quaternary ammonium salt disinfectant is completely dissolved, has no precipitate and no volatilization, has clear and transparent appearance, slightly takes alcohol smell, is colorless to extremely yellowish green, and still has no precipitate during long-time placement.
5. The disinfectant disclosed by the invention is added with disodium ethylene diamine tetraacetate and tetrasodium ethylene diamine tetraacetate, and is used as a safe additive component, so that the disinfection of microorganisms can be further promoted.
6. The water-soluble polymer compound polyvinylamine is added, is nontoxic to animal cells, can obviously inhibit growth and adhesion surfaces of escherichia coli and staphylococcus aureus, and is matched with the single-chain quaternary ammonium salt and the double-chain quaternary ammonium salt in a synergistic manner to kill viruses and bacteria.
7. The compound quaternary ammonium salt disinfectant is a neutral compound quaternary ammonium salt disinfectant, and cannot cause whitening, fading, corrosion or damage to the surface of a disinfectant due to oxidation or acid-base corrosion on the surface of the disinfectant.
8. The composite quaternary ammonium salt disinfectant has easily available raw materials, and the cost of 1L of the disinfectant is less than 10 yuan, so the cost is low; the compound quaternary ammonium salt disinfectant can be prepared by uniformly mixing the raw materials, the preparation method is simple, the disinfection and killing can be realized by spraying or smearing, the irritation to respiratory tracts, skins and the like in the use process is extremely low, the operation is easy, and the mass production is easy.
The technical solution of the present invention is further described in detail with reference to the following examples.
Detailed Description
Example 1
The 4L compound quaternary ammonium salt disinfectant prepared in the embodiment specifically comprises the following raw materials and a preparation method:
mixing 228.7mL of ethanol, 60g of didecyl dimethyl ammonium chloride, 48g of didodecyl dimethyl ammonium chloride, 72g of benzalkonium chloride, 88g of disodium ethylene diamine tetraacetate, 108.8g of tetrasodium ethylene diamine tetraacetate and 8.8g of polyvinyl amine, supplementing the mixture to 4000mL with water, shaking and stirring until the mixture is dissolved and mixed uniformly to obtain the compound quaternary ammonium salt disinfectant; the didecyl dimethyl ammonium chloride, the didodecyl dimethyl ammonium chloride and the benzalkonium chloride in the embodiment may be industrial products, such as 75g of 80% by mass industrial didecyl dimethyl ammonium chloride, 60g of 80% by mass industrial didodecyl dimethyl ammonium chloride and 90g of 80% by mass industrial benzalkonium chloride;
the benzalkonium chloride is a compound of dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride and hexadecyl dimethyl benzyl ammonium chloride in a mass ratio of 3:7.5: 1;
the volume fraction of the ethanol is 75%;
the relative molecular mass of the polyvinylamine is 60000, and the commercial name of the polyvinylamine is XeOREXTM RS 1100;
The polyvinylamine in the implementation is the polyvinylamine which is dialyzed, purified and dried, and the process of dialyzing, purifying and drying comprises the following steps: mixing the polyvinylamine and water to obtain a polyvinylamine aqueous solution with the mass percentage of 10%, placing the polyvinylamine aqueous solution in an MWCO8-14kd dialysis bag, carrying out dialysis treatment for 72h by using water as a dialysis medium, and carrying out freeze drying after the dialysis is finished to obtain the polyvinylamine which is subjected to dialysis, purification and drying.
Example 2
The 4L compound quaternary ammonium salt disinfectant prepared in the embodiment specifically comprises the following raw materials and a preparation method:
mixing 330.5mL of ethanol, 72g of didecyl dimethyl ammonium chloride, 60g of didodecyl dimethyl ammonium chloride, 60g of benzalkonium chloride, 112g of disodium ethylene diamine tetraacetate, 100.8g of tetrasodium ethylene diamine tetraacetate and 2g of polyvinyl amine, supplementing water to 4000mL, and oscillating and stirring until the materials are dissolved and mixed uniformly to obtain a compound quaternary ammonium salt disinfectant;
the benzalkonium chloride is a compound of dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride and hexadecyl dimethyl benzyl ammonium chloride in a mass ratio of 4.5:4.5: 1;
the volume fraction of the ethanol is 75%;
the relative molecular mass of the polyvinylamine is 60000, and the commercial name of the polyvinylamine is XeOREXTM RS 1100;
The polyvinylamine in the implementation is the polyvinylamine which is dialyzed, purified and dried, and the process of dialyzing, purifying and drying comprises the following steps: mixing the polyvinylamine and water to obtain a polyvinylamine aqueous solution with the mass percentage of 10%, placing the polyvinylamine aqueous solution in an MWCO8-14kd dialysis bag, carrying out dialysis treatment for 72h by using water as a dialysis medium, and carrying out freeze drying after the dialysis is finished to obtain the polyvinylamine which is subjected to dialysis, purification and drying.
Example 3
The 4L compound quaternary ammonium salt disinfectant prepared in the embodiment specifically comprises the following raw materials and a preparation method:
mixing 457.4mL of ethanol, 70g of didecyl dimethyl ammonium chloride, 55g of didodecyl dimethyl ammonium chloride, 55g of benzalkonium chloride, 92g of disodium ethylene diamine tetraacetate, 105.5g of tetrasodium ethylene diamine tetraacetate and 4.5g of polyvinyl amine, supplementing the mixture to 4000mL with water, shaking and stirring until the mixture is dissolved and mixed uniformly to obtain the compound quaternary ammonium salt disinfectant;
the benzalkonium chloride is a compound of dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride and hexadecyl dimethyl benzyl ammonium chloride in a mass ratio of 4.2:6.5: 1;
the volume fraction of the ethanol is 75%;
the relative molecular mass of the polyvinylamine is 60000, and the commercial name of the polyvinylamine is XeOREXTM RS 1100;
The polyvinylamine in the implementation is the polyvinylamine which is dialyzed, purified and dried, and the process of dialyzing, purifying and drying comprises the following steps: mixing the polyvinylamine and water to obtain a polyvinylamine aqueous solution with the mass percentage of 10%, placing the polyvinylamine aqueous solution in an MWCO8-14kd dialysis bag, carrying out dialysis treatment for 72h by using water as a dialysis medium, and carrying out freeze drying after the dialysis is finished to obtain the polyvinylamine which is subjected to dialysis, purification and drying.
Example 4
The 4L compound quaternary ammonium salt disinfectant prepared in the embodiment specifically comprises the following raw materials and a preparation method:
mixing 120mL of ethanol, 120g of didecyl dimethyl ammonium chloride, 120g of didodecyl dimethyl ammonium chloride, 200g of benzalkonium chloride, 120g of disodium ethylenediamine tetraacetic acid, 20g of tetrasodium ethylenediamine tetraacetic acid and 0.4g of polyvinyl amine, supplementing the mixture to 4000mL with water, shaking and stirring until the mixture is dissolved and mixed uniformly to obtain the compound quaternary ammonium salt disinfectant;
the benzalkonium chloride is a compound of dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride and hexadecyl dimethyl benzyl ammonium chloride in a mass ratio of 2:2.5: 1;
the volume fraction of the ethanol is 75%;
the relative molecular mass of the polyvinylamine is 50000, and the commercial name of the polyvinylamine is XeOREXTM RS 1100;
The polyvinylamine in the implementation is the polyvinylamine which is dialyzed, purified and dried, and the process of dialyzing, purifying and drying comprises the following steps: mixing the polyvinylamine and water to obtain a polyvinylamine aqueous solution with the mass percentage of 10%, placing the polyvinylamine aqueous solution in an MWCO8-14kd dialysis bag, carrying out dialysis treatment for 72h by using water as a dialysis medium, and carrying out freeze drying after the dialysis is finished to obtain the polyvinylamine which is subjected to dialysis, purification and drying.
Example 5
The 4L compound quaternary ammonium salt disinfectant prepared in the embodiment specifically comprises the following raw materials and a preparation method:
mixing 480mL of ethanol, 20g of didecyl dimethyl ammonium chloride, 20g of didodecyl dimethyl ammonium chloride, 40g of benzalkonium chloride, 20g of disodium ethylene diamine tetraacetate, 120g of tetrasodium ethylene diamine tetraacetate and 40g of polyvinyl amine, supplementing the mixture to 4000mL with water, shaking and stirring until the mixture is dissolved and mixed uniformly to obtain a compound quaternary ammonium salt disinfectant;
the benzalkonium chloride is a compound of dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride and hexadecyl dimethyl benzyl ammonium chloride in a mass ratio of 6:10: 1;
the volume fraction of the ethanol is 75%;
the relative molecular mass of the polyvinylamine is 80000, and the commercial name of the polyvinylamine is XELOREXTM RS 1100;
The polyvinylamine in the implementation is the polyvinylamine which is dialyzed, purified and dried, and the process of dialyzing, purifying and drying comprises the following steps: mixing the polyvinylamine and water to obtain a polyvinylamine aqueous solution with the mass percentage of 10%, placing the polyvinylamine aqueous solution in an MWCO8-14kd dialysis bag, carrying out dialysis treatment for 72h by using water as a dialysis medium, and carrying out freeze drying after the dialysis is finished to obtain the polyvinylamine which is subjected to dialysis, purification and drying.
And (3) killing test:
the disinfectant (stock solution) of examples 1 to 5 was subjected to an identification test of a physical removal method of residual disinfectant and a virus inactivation test with reference to "disinfection specification" 2002 edition-2.1.1.10.6 and "disinfection specification" 2002 edition-2.1.1.10.7, the detection mechanism was the analysis and detection center for microorganisms in Guangdong province, and the test results are shown in tables 1 and 2.
TABLE 1 identification test for physical removal of disinfectant residual disinfectant
Figure BDA0002645270370000071
Figure BDA0002645270370000081
TABLE 2 disinfectant Virus inactivation test
Figure BDA0002645270370000082
The disinfectants of the embodiments 1 to 5 are firstly diluted by 15 times by water (namely, the mass ratio of the disinfectants to the water is 1:14) by referring to the disinfection technical specification 2002 edition-2.1.1.10.6 and the disinfection technical specification 2002 edition-2.1.1.10.7, the 15 times of the dilutants are obtained to carry out the identification test and the virus inactivation test of the physical removal method of the residual disinfectants, the detection mechanism is the microbiological analysis and detection center of Guangdong province, and the test results are shown in tables 3 and 4.
TABLE 3 identification test for physical removal of residual disinfectant
Figure BDA0002645270370000091
TABLE 4H 1N1 Virus inactivation assay
Figure BDA0002645270370000092
Figure BDA0002645270370000101
From tables 1 to 4, the disinfectant of the invention acts on influenza A virus H1N1(A/PR/8/34) (MDCK cells) for 1 minute, the average inactivation log value is more than 4.58, and the virus inactivation rate is more than 99.99 percent; the 15-fold diluent of the disinfectant disclosed by the invention acts on influenza A virus H1N1(A/PR/8/34) (MDCK cells) for 10 minutes, the average inactivation log value is 3.67, and the virus inactivation rate is 99.98%.
Referring to the 'sterilization technical specification' 2002 edition, the disinfectants of the embodiments 1 to 5 are firstly diluted by 20 times by water (namely, the mass ratio of the disinfectants to the water is 1:19), the 20 times of the diluents are obtained to test the sterilization rate of staphylococcus aureus, escherichia coli and candida albicans, the test results are shown in table 5, and the detection mechanism is the analytical detection center of the research institute of microorganisms in shanxi province.
TABLE 5 Sterilization rates for Staphylococcus aureus, Escherichia coli, and Candida albicans
Figure BDA0002645270370000102
As can be seen from Table 5, the 20-fold diluent of the disinfectant disclosed by the invention acts on staphylococcus aureus (CGMCC 1.0089) for 10 minutes, the killing logarithm value is greater than 6.26, and the sterilization rate is greater than 99.9999%; acts on candida albicans (CGMCC 2.2086) for 10 minutes, the killing logarithm value is more than 6.56, and the sterilization rate is more than 99.9999 percent; acts on Escherichia coli (CGMCC (B)44102) for 10 minutes, and has a killing log value of 6.43 and a sterilization rate of 99.9999 percent.
The disinfectants of the embodiments 1 to 3 are detected by referring to the disinfection technical specification 2002 edition-2.2.1.4, 2.2.3, 2.2.4, 2.1.1.5, 2.1.1.7, 2.1.11.9, 2.1.2.10, GB 26369 and 2010 quaternary ammonium salt disinfectant sanitation standard appendix A and GB/T5174-2018 direct two-phase titration method for measuring the content of cationic active matters of surfactant detergent, and the detection mechanism is Guangdong Zhongke detection technical service company Limited.
The detection results are as follows:
testing the effective components: chloroform (analytically pure), isopropanol (analytically pure) and acidic mixed indicating liquid are used as reagents, sodium lauryl sulfate (sodium dodecyl sulfate) with the concentration of 0.004000mol/L is used as a standard titration solution, and 2 times of repeated tests are carried out according to the method A.1 and the method GB/T5174 and 2018, namely the direct two-phase titration method for measuring the content of the cationic active substance of the surfactant detergent, in the conditions that the detection environment temperature is 25.8 ℃ and the relative humidity is 69%, and the obtained results are shown in Table 6.
TABLE 6 content test results of effective components of disinfectant (stock solution)
Figure BDA0002645270370000111
According to the table 6, the determination result of the content of the effective component of the disinfectant of the present invention shows that the content of the chlorine type quaternary ammonium salt as the effective component in the disinfectant stock solution is 55.7 g/L.
And (3) pH value test: the pH (25 ℃) of a potassium hydrogen phthalate solution was 4.00, the pH (25 ℃) of a phosphate buffer solution was 6.86, and the pH (25 ℃) of a borate standard buffer solution was 9.18, and the pH was measured according to the measurement of pH 2.2.1.4 in "specification for disinfection (2002)" using an acidimeter model PHS-25 as an experimental device under the following conditions: the ambient temperature was 25.1 ℃ and the relative humidity was 60%. The number of test repetitions: the pH of the sample was measured directly (25 ℃)2 times. The results are shown in Table 7.
TABLE 7 disinfectant (stock solution) pH test results
Figure BDA0002645270370000121
According to Table 7, the disinfectant stock according to the invention has a pH (25 ℃) of 7.06.
And (3) stability testing: trichloromethane (analytically pure), isopropanol (analytically pure) and acid mixed indicating liquid are used as reagents, sodium lauryl sulfate (sodium dodecyl sulfate) with the concentration of 0.004000mol/L is used as a standard titration solution, the stability of a disinfection product is determined according to a method A.1 and a method GB/T5174 and 2018, namely a direct two-phase titration method for determining the content of a cationic active substance of a surfactant detergent, and a disinfection technical specification (2002 edition) 2.2.3 in GB 26369 2010 and a BSP-150 biochemical incubator is used as an experimental device, and the experiment is repeated for 2 times under the conditions that the environmental temperature is 27.8 ℃ and the relative humidity is 63 percent, and the obtained results are shown in tables 8 and 9.
TABLE 8 disinfectant (stock solution) content test results after 14 days storage
Figure BDA0002645270370000122
TABLE 9 disinfectant (stock solution) stability test results before and after storage
Figure BDA0002645270370000123
According to tables 8 and 9, the chlorine type quaternary ammonium salt content was 54.2g/L after the disinfectant stock solution was stored at 54 ℃ for 14 days. The content before the stability test is 55.7g/L, the reduction rate is 2.7 percent, and the requirement that the reduction rate of the content of the effective components in the disinfection technical specification (2002 edition) is less than or equal to 10 percent is met. The storage period of the disinfectant stock solution can be set as 1 year.
Metal corrosion test: the method comprises the steps of taking water sand paper with the granularity of 120, a wide-mouth reagent bottle, an electronic balance with the model of FA2004B, a stainless steel electric heating air blowing drying box with the model of LDO-101-1 and a vernier caliper with the model of Guangdong 0-150mm as material equipment, preparing a sample to be tested according to the mass ratio of 1:49 of the disinfectant to the metal corrosivity according to the determination of the disinfectant in the technical specification of disinfection (2002 edition) 2.2.4, and repeating the experiment for 3 times under the conditions that the environmental temperature is 25.4 ℃ and the relative humidity is 67%, wherein the experimental result is shown in Table 10.
TABLE 10 test results of degree of corrosion of metals
Figure BDA0002645270370000131
From Table 10, it is found that the test specimens are moderately corrosive to carbon steel, slightly corrosive to aluminum and copper, and substantially non-corrosive to stainless steel.
Killing tests of staphylococcus aureus and escherichia coli: staphylococcus aureus ATCC6538 and Escherichia coli 8099 are used as test strains, the generation number of the strains is 4, bacterial suspension is prepared by 0.03mol/LPBS, 3.9% D/E neutralization broth is used as a neutralizer, 3% bovine serum albumin is used as an organic interference substance, and the test is identified according to a neutralizer 2.1.1.5 in the technical Specification for disinfection (2002 edition); 2.1.1.7 bacteria quantitative kill test neutralizer identification test and kill performance test were carried out.
Preparation of bacterial suspension: selecting bacteria with a content of 1 × 108CFU/mL~5×108CFU/mL of bacterial suspension.
And (3) identification test of a neutralizer: the test bacterium is staphylococcus aureus. The test groups are: (1) the disinfectant comprises a disinfectant sample, a bacterial suspension, a disinfectant sample, a neutralizing agent, a disinfectant sample, a neutralizing agent, a bacterial suspension, a diluent, a neutralizing agent and a culture medium, wherein the disinfectant sample is prepared from a disinfectant stock solution and water according to a mass ratio of 1:49, the disinfectant is acted for 1min, and the test is repeated for 3 times.
And (3) testing the killing performance: according to the quantitative sterilization test of the suspension, a test solution is prepared from the disinfectant stock solution and water according to the mass ratio of 1:4, the action time is 5min, 10min and 15min, the test is repeated for 3 times, and the test environment temperature is as follows: 23.2 ℃, relative humidity: 50 percent. The results are shown in tables 11 and 12.
TABLE 11 neutralizing agent identification test results in Staphylococcus aureus and Escherichia coli killing test
Figure BDA0002645270370000141
TABLE 12 results of killing Staphylococcus aureus and Escherichia coli
Figure BDA0002645270370000142
According to tables 11 and 12, 3.9% D/E neutralization broth was used as neutralizer, disinfectant stock: the test solution is prepared from water according to the mass ratio of 1:49, the test solution acts for 10min, and the killing log values of the test solution to staphylococcus aureus are all more than 5.00, and the killing log values of the test solution to escherichia coli are all more than 5.00. Meets the requirements of disinfection technical specification (2002 edition).
Killing experiment of candida albicans: candida albicans ATCC 10231 is used as an experimental strain, the generation number of the strain is 4, a bacterial suspension is prepared by using PBS containing 0.03mol/L, 3.9% D/E neutralization broth is used as a neutralizer, and 3% bovine serum albumin is used as an organic interference substance. According to the specification of disinfection (2002 edition) 2.1.1.5 neutralizer identification test; 2.1.1.9 quantitative kill test of fungus neutralizer identification test and kill performance test are carried out.
Preparation of bacterial suspension: selecting bacteria with a content of 1 × 108CFU/mL~5×108CFU/mL bacterial suspension was subjected to neutralizer identification test.
And (3) identification test of a neutralizer: the test bacteria are Candida albicans. The test groups are: (1) the disinfectant comprises a disinfectant sample, a bacterial suspension, a disinfectant sample, a neutralizing agent, a disinfectant sample, a neutralizing agent, a bacterial suspension, a diluent, a neutralizing agent and a culture medium, wherein the disinfectant sample is prepared from a disinfectant stock solution and water according to a mass ratio of 1:49, the disinfectant is acted for 1min, and the test is repeated for 3 times.
And (3) testing the killing performance: according to the quantitative sterilization test of the suspension, the disinfectant stock solution and the water are prepared into a test solution according to the mass ratio of 1:49, the action time is 5min, 10min and 15min, and the test is repeated for 3 times. Test environment temperature: 23.2 ℃, relative humidity: 50 percent. The results are shown in tables 13 and 14.
TABLE 13 identification of neutralizing agent in Candida albicans killing test
Figure BDA0002645270370000151
Figure BDA0002645270370000161
TABLE 14 results on Candida albicans killing
Figure BDA0002645270370000162
Disinfectant stock according to tables 13 and 14, 3.9% D/E neutralization broth as neutralizing agent: the test solution is prepared from water according to the mass ratio of 1:49, the test solution acts for 10min, and the killing log values of the test solution to the candida albicans are all more than 4.00. Meets the requirements of disinfection technical specification (2002 edition).
And (3) field disinfection test: 3.9% D/E neutralization broth is taken as a neutralizer, 0.1% Tween 80PBS is taken as a control sampling solution, a wooden table is taken as a disinfection object, and other surface disinfection field identification tests are carried out according to the disinfection technical specification (2002 edition) 2.1.2.10 disinfectant, wherein
Positive control: a sterile cotton swab was wetted in a test tube containing 5mL of diluent, and a block was sampled by smearing and moving 8 times in each direction. After sampling, the sampling end of the cotton swab is cut into the original diluent test tube in a sterile operation mode, and the test tube is rapped 80 times to be used as a positive control group sample.
Test samples: the disinfectant stock solution and water are prepared into a test solution according to the mass ratio of 1:49, and the test solution is sprayed on the surface of an object for disinfection and acts for 10 min. After sterilization, the neutralizing agent was used instead of the diluent, and the sterilized block was smeared and sampled in the same manner as the positive control group to be used as a test group sample.
The number of the test pieces: 30 blocks. Test environment temperature: 24.0 ℃, relative humidity: 49 percent.
The results are shown in Table 15.
TABLE 15 results of in situ sterilization experiment on object surface
Figure BDA0002645270370000163
Figure BDA0002645270370000171
According to table 15, 3.9% D/E neutralization broth is used as a neutralizer, and a stock solution of disinfectant and water are prepared into a test solution according to a mass ratio of 1:49, and the test solution is subjected to 30 times of object surface field disinfection tests: spraying for 10min, and the killing log value of the natural bacteria on the surface of the object is more than 1.00. Meets the requirements of disinfection technical specification (2002 edition).
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.

Claims (6)

1. The compound quaternary ammonium salt disinfectant is characterized by comprising the following components: the volume of the compound quaternary ammonium salt disinfectant is 1000mL, 5-30 g of didecyl dimethyl ammonium chloride, 5-30 g of didodecyl dimethyl ammonium chloride, 10-50 g of benzalkonium chloride, 5-30 g of disodium edetate, 5-30 g of tetrasodium edetate, 0.1-10 g of polyvinyl amine, 30-120 mL of ethanol and the balance of water, wherein the volume of the water is the volume of the water for supplementing the compound quaternary ammonium salt disinfectant to 1000 mL;
the benzalkonium chloride is a compound of dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride and hexadecyl dimethyl benzyl ammonium chloride in a mass ratio of (2-6): 2.5-10): 1.
2. The compound quaternary ammonium salt disinfectant as claimed in claim 1, wherein the compound quaternary ammonium salt disinfectant comprises the following components: by taking the volume of the composite quaternary ammonium salt disinfectant as 1000mL, 15 g-18 g of didecyl dimethyl ammonium chloride, 12 g-15 g of didodecyl dimethyl ammonium chloride, 15 g-18 g of benzalkonium chloride, 22 g-28 g of disodium ethylenediamine tetraacetate, 25.2 g-27.2 g of tetrasodium ethylenediamine tetraacetate, 0.5 g-2.2 g of polyvinylamine, 57.175 mL-114.35 mL of ethanol, and the balance of water, wherein the volume of the water is the volume of water for supplementing the composite quaternary ammonium salt disinfectant to 1000 mL;
the benzalkonium chloride is a compound of dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride and hexadecyl dimethyl benzyl ammonium chloride in a mass ratio of (3-4.5): 4.5-7.5): 1.
3. The disinfectant with compound quaternary ammonium salt according to claim 1, wherein the volume fraction of ethanol is 75%.
4. The compound quaternary ammonium salt disinfectant as set forth in claim 1, wherein the relative molecular mass of the polyvinylamine is 50000-80000.
5. The compound quaternary ammonium salt disinfectant as claimed in claim 1, wherein the polyvinylamine is dialyzed, purified and dried, the dialysis medium for dialysis, purification and drying is water, and the dialysis time is 72 h.
6. The compound quaternary ammonium salt disinfectant as claimed in claim 1, wherein the compound quaternary ammonium salt disinfectant is a neutral compound quaternary ammonium salt disinfectant.
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CN112889820A (en) * 2021-01-22 2021-06-04 海韵一剑大卫生科技有限公司 Compound quaternary ammonium salt disinfectant and preparation method and use method thereof
CN114651819A (en) * 2022-03-10 2022-06-24 上海芜玮建晖生物科技有限公司 Organic disinfectant based on marine resources
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112618525A (en) * 2020-12-18 2021-04-09 上海海禾医疗科技有限公司 Disinfectant for quickly inactivating coronavirus
CN112640903A (en) * 2020-12-23 2021-04-13 北京瞬行生物科技有限公司 Composite quaternary ammonium salt disinfectant and preparation method thereof
WO2022135505A1 (en) * 2020-12-23 2022-06-30 北京瞬行生物科技有限公司 Composite quaternary ammonium salt disinfectant and preparation method therefor
CN112741087A (en) * 2021-01-05 2021-05-04 北京洛娃日化有限公司 Cold chain food disinfectant and preparation method thereof
CN112889820A (en) * 2021-01-22 2021-06-04 海韵一剑大卫生科技有限公司 Compound quaternary ammonium salt disinfectant and preparation method and use method thereof
WO2022171153A1 (en) * 2021-02-10 2022-08-18 北京普罗吉生物科技发展有限公司 Disinfectant
CN114651819A (en) * 2022-03-10 2022-06-24 上海芜玮建晖生物科技有限公司 Organic disinfectant based on marine resources

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