A fungicide

By rationally formulating a non-resistant bactericide and using a variety of formulation components and preparation processes, the impact of drug resistance and water mineralization of quaternary ammonium bactericides after long-term use is solved, achieving efficient and safe bactericidal effect.

CN112400873BActive Publication Date: 2025-05-02BEIJING KANGSHENGLUN BIOTECHNOLOGY CO LTD
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Patent Information

Application Number
CN202010930649.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2020-09-07
Publication Date
2025-05-02
Estimated Expiration
2040-09-07

AI Technical Summary

Technical Problem

Existing quaternary ammonium salt bactericides are prone to lead to microbial resistance after long-term use, and the bactericidal effect is reduced when the mineralization degree of water is high, and the prior art has failed to effectively solve these problems.

Method used

By reasonably formulating a non-resistant bactericide, including purified water, hexamethylenetetramine, Tween 80, benzalkonium bromide, bisoctadecyldimethylamine chloride, dodecyldimethylamine oxide, Jimmy quaternary ammonium salt, bisdecyldimethylammonium bromide and isopropanol, the preparation method of stirring and aging steps is adopted to form a bactericide with high-efficiency bactericidal effect.

Benefits of technology

It has achieved efficient sterilization, avoided the drug resistance problem caused by the use of simple quaternary ammonium salts, and maintained a good sterilization effect under different water mineralization conditions, low toxicity of the product, and strong circulating sterilization and disinfection ability.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention relates to bactericides that utilize mild quaternary ammonium salts, with Gimichi quaternary ammonium salt as the main component. Taking advantage of the properties of ionic compounds, it is readily soluble in water but insoluble in nonpolar solvents, exhibiting stable chemical properties. Furthermore, it incorporates hexamethylenetetramine, benzalkonium bromide, Tween 80, and dioctadecyl dimethylammonium chloride and didecyl dimethylammonium bromide to form a core structure. This allows the cations in the bactericide to adsorb negatively charged bacteria through electrostatic forces, hydrogen bonds, and hydrophobic interactions between surfactant molecules and protein molecules. The bacteria aggregate on the cell wall, creating a compartmentalization effect, thus achieving highly efficient bacterial killing without inducing drug resistance.
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Description

Technical Field

[0001] The invention relates to a fungicide, in particular to a fungicide without drug resistance, and belongs to the field of fungicides. Background Art

[0002] Bactericides are in demand in all areas of production and life. For example, in life, bacteria will grow on the surface of furniture and clothing. Moisture-prone places such as kitchens and toilets are also suitable places for bacteria to grow. This is especially true for families with pets, as pets generally carry a large number of bacteria.

[0003] Hospitals also need to kill or control bacteria in the environment, media, and treatment equipment, and the requirements for bactericides and antibacterial agents are relatively high. In addition, in special environments such as clean rooms, animal model institutes, and key laboratories, it is also necessary to thoroughly disinfect the skin and clothing of personnel to reduce the spread of pathogens, and at this time, very high requirements are placed on the safety of disinfectants.

[0004] The pharmaceutical and food industries have very strict control over bacteria and microorganisms. Once the bacteria and microorganisms exceed the microbial control standards, it means that the quality of food and medicine is threatened, which not only threatens the lives of consumers, but also brings huge economic losses and legal liabilities to manufacturers. Due to the particularity of these two fields, people work in the workshop for a long time and the amount of wastewater discharged is also relatively large. How to ensure the safety of people using disinfectants and the compliance of wastewater discharge has faced huge challenges so far. In addition, manufacturers also need to frequently change different types of disinfectants to solve the problem of drug resistance of disinfectants that has been plaguing manufacturers.

[0005] In the agricultural field, there is also a strong demand for fungicides, such as sterilization of the environment for raising animals and slaughtering animals. In the forestry field, in order to ensure the normal and vigorous growth of plants, it is also necessary to disinfect fungi and bacteria during the growth process of plants.

[0006] At present, conventional disinfectants and bactericides are classified into bactericides, high-efficiency disinfectants, medium-efficiency disinfectants, and low-efficiency disinfectants according to their levels from high to low. Bactericides can kill all microorganisms to meet the sterilization requirements, but their composition must include formaldehyde, glutaraldehyde (or aldehyde substance OPA, such as US Patent US2009 / 0203645A1), ethylene oxide, peracetic acid, hydrogen peroxide, chlorine dioxide, chlorine, copper sulfate, quicklime, and ethanol.

[0007] Quaternary ammonium salt fungicides are low-efficiency disinfectants. They generally have low bactericidal concentrations, few side effects, are non-irritating, non-toxic, meet the technical requirements for fungicides in this field (such as patents CN101473832A, CN101642449A, CN1593150A), and are not easily affected by changes in pH values, so they have received widespread attention. Quaternary ammonium salt fungicides have derived seven generations of products. After the second generation of derivatives was derived based on the first generation of fungicides benzalkonium chloride / bromide; the third generation fungicides used double long-chain quaternary ammonium salts (DDAC); and the fourth generation fungicides were composites of the first and third generations; the fifth generation fungicides considered gemini quaternary ammonium salts to improve the bactericidal effect; the sixth generation followed the fifth generation's idea to find polyquaternary ammonium salts with denser groups; the seventh generation fungicides were inspired by the fourth generation design on the basis of the previous generations, and the third and sixth generations were composited.

[0008] However, the long-term use of quaternary ammonium salts easily leads to drug resistance. Although many novel quaternary ammonium salts can be derived by changing the structure of hydrophobic groups, hydrophilic groups and counterions on the one hand, the problem is that the molecular structure design cycle is long and the initial research cost is high. Although Chinese patent CN101279219A agrees that some microorganisms develop drug resistance to bactericides, it does not fundamentally avoid the starting point of molecular structure improvement. On the other hand, the prior art also does not take into account the mineralization problem of water. This is because the bactericidal effect of bactericides can be reduced when the mineralization of water is higher. Patent CN106035361A uses sterilized water, does not pay attention to the mineralization of water, and its killing logarithm does not specifically provide a numerical value greater than 5, and its bactericidal specific effect is unknown. If the mild performance of existing quaternary ammonium salt bactericides is utilized, on the basis of the molecular structure of quaternary ammonium salts that does not need to be designed and improved, the purpose of efficient sterilization is achieved by matching suitable bactericide components, which is a problem that has not been solved in the current prior art. Summary of the invention

[0009] The invention provides a quaternary ammonium salt bactericide capable of achieving efficient sterilization.

[0010] In order to solve the above technical problems, the present invention is achieved through the following technical solutions:

[0011] A non-resistant fungicide, comprising the following components in parts by weight:

[0012] 35-45 parts of purified water

[0013] 35-40 parts of hexamethylenetetramine

[0014] Tween 80 2.5-3 parts

[0015] Benzalkonium bromide 11-15 parts

[0016] 2.5-3 parts of dioctadecyl dimethyl ammonium chloride

[0017] 1.5-3 parts of dodecyl dimethyl amine oxide

[0018] 5-10 parts of Jimiqi quaternary ammonium salt

[0019] 1-1.5 parts of didecyl dimethyl ammonium bromide

[0020] 1.5-4 parts of isopropyl alcohol.

[0021] Preferably, the following components are included in parts by weight:

[0022] 40 parts of purified water

[0023] 35 parts of hexamethylenetetramine

[0024] Tween 80 2.5 parts

[0025] Benzalkonium bromide 12 parts

[0026] 2.5 parts of dioctadecyl dimethyl ammonium chloride

[0027] 2 parts of dodecyl dimethyl amine oxide

[0028] 6 parts of Jimmie quaternary ammonium salt

[0029] 1 part of didecyl dimethyl ammonium bromide

[0030] 2 parts of isopropyl alcohol.

[0031] Also disclosed is a method for preparing the above bactericide, comprising the following steps:

[0032] (1) Pour 35-45 parts of purified water into a container and stir for 1-10 minutes; add 35-40 parts of hexamethylenetetramine and stir for 8-11 minutes;

[0033] (2) adding 2.5-3 parts of Tween 80 to the solution after stirring in step (1), and stirring for 8-11 minutes;

[0034] (3) adding 11-15 parts of benzalkonium bromide to the solution after stirring in step (2), and stirring for 18-23 minutes;

[0035] (4) adding 2.5-3 parts of dioctadecyl dimethyl ammonium chloride to the solution after stirring in step (3), and stirring for 13-18 minutes;

[0036] (5) adding 1.5-3 parts of dodecyl dimethyl amine oxide to the solution after stirring in step (4), and stirring for 3-8 minutes;

[0037] (6) adding 5-10 parts of Jimic quaternary ammonium salt to the solution after stirring in step (5), and stirring for 8-11 minutes;

[0038] (7) adding 1-1.5 parts of didecyldimethylammonium bromide to the solution after stirring in step (6), and stirring for 8-11 minutes;

[0039] (8) adding 1.5-4 parts of isopropanol to the solution after stirring in step (7), and stirring for 8-11 minutes;

[0040] (9) Continue stirring for 3-4 hours.

[0041] Preferably, an aging step is further included, and the aging time is 70-75 hours.

[0042] The temperature during preparation is room temperature, which is 20-25°C.

[0043] The shear stirring time of purified water is 1-10min.

[0044] The shear stirring speed of purified water is 300-500 rpm.

[0045] When the above sterilizing agents are used, they are usually diluted with purified water to a sterilizing agent concentration of 1-5% (V / V).

[0046] The above technical solution of the present invention has the following advantages compared with the prior art:

[0047] 1. The bactericide of the present invention adopts a quaternary ammonium salt with mild properties, with Jimiqi quaternary ammonium salt as the main component, and cooperates with benzalkonium bromide, dioctadecyl dimethyl ammonium chloride, dodecyl dimethyl amine oxide, and didecyl dimethyl ammonium bromide to avoid the bacterial resistance produced by the simple use of quaternary ammonium salt. Quaternary ammonium salt is soluble in water and insoluble in non-polar solvents due to the properties of ionic compounds, and has stable chemical properties. Therefore, on this basis, in combination with hexamethylenetetramine, benzalkonium bromide, Tween 80, dioctadecyl dimethyl amine oxide, didecyl dimethyl ammonium bromide to form a core structure, so that the cation in the bactericide can absorb negatively charged bacteria through electrostatic force, hydrogen bond force and hydrophobic combination between surfactant molecules and protein molecules, gather on the cell wall, produce chamber resistance effect, and cause bacterial growth to be inhibited and die; at the same time, its hydrophobic alkyl group can also act on the hydrophilic group of bacteria to change the permeability of the membrane, and then lyse occurs, destroying the cell structure, causing the dissolution and death of the cell. Simply put, it changes the permeability of the cell membrane, causing the cytoplasm to leak out, hindering respiration or denaturing proteases.

[0048] The new compound components can effectively reduce the surface tension of water, significantly increase the viscosity of the aqueous solution, and also have the functions of scale inhibition and pH adjustment; the product is more conducive to its hydrophobic base penetrating into the lipid layer of bacterial cells and the hydrophilic base penetrating into the protein layer, resulting in enzyme inactivity and protein denaturation. The most important thing is that it can change the molecular structure of quaternary ammonium salt from symmetric to extremely asymmetric structural characteristics, which can catalyze the rapid increase of its positive charge density, making it easier for surfactants to adsorb on the bacterial surface, changing the permeability of bacterial cell walls and causing them to rupture, achieving the effect of highly efficient bacterial killing.

[0049] The bactericide described in the present application does not undergo chemical reactions during the sterilization process, and the structure and properties of the product itself do not change after the sterilization effect is achieved. Therefore, the bactericide has a strong cyclic sterilization ability, a long service life, and low toxicity.

[0050] 2. The most important thing about the preparation method of the bactericide of the present invention is that the purified water added to the main active component must be stirred in advance. This process is particularly critical. By subjecting the purified water to a separate shearing and stirring treatment at room temperature, the purified water is fully preactivated. Under the preferred conditions: shear speed 300-500 rpm, room temperature 20-25°C, 1-10min, the volume of water droplets can be reduced, the density of water droplet particles can be increased, the surface tension of water molecules can be reduced, the specific surface area of ​​water can be increased, and thus the solubility of purified water to solute molecules can be increased, and the interaction between molecules can be accelerated.

[0051] At the same time, the fusion and coating effects between the components can be fully exerted, so that the prepared bactericidal agent has a bactericidal effect different from other quaternary ammonium salt mild disinfectants. DETAILED DESCRIPTION

[0052] In order to better reflect the actual selected amount and the study of drug resistance, a comparative test was carried out before using the examples, and each strain was repeatedly carried out on strains from the same test batch, and the amount of medicine applied each time was controlled so that the bactericidal effect was less than 100%, and the bactericidal result was within the range of continued cultivation and reproduction, and after sterilization, it was applied in sufficient amount for the examples to test its drug resistance.

[0053] Comparative Example 1

[0054] A fungicide is prepared by the following method: (1) injecting 45 kg of purified water into a container and stirring for 10 minutes; adding 40 kg of hexamethylenetetramine thereto and stirring for 11 minutes;

[0055] (2) adding 3 kg of Tween 80 to the solution after stirring in step (1) and stirring for 11 minutes;

[0056] (3) adding 15 kg of benzalkonium bromide to the solution after stirring in step (2), and stirring for 23 min;

[0057] (4) adding 3 kg of dioctadecyl dimethyl ammonium chloride to the solution after stirring in step (3), and stirring for 18 min;

[0058] (5) adding 3 kg of dodecyl dimethyl amine oxide to the solution after stirring in step (4) and stirring for 8 min;

[0059] (6) adding 3 kg of didecyl dimethyl ammonium bromide to the solution after stirring in step (5), and stirring for 11 minutes;

[0060] (7) adding 4 kg of isopropanol to the solution after stirring in step (6) and stirring for 11 min;

[0061] (8) Continue stirring at room temperature for 4 h.

[0062] The following bactericide composition is obtained:

[0063] 45 parts of purified water

[0064] 40 parts of hexamethylenetetramine

[0065] Tween 80 3 parts

[0066] 15 parts of benzalkonium bromide

[0067] 3 parts of dioctadecyl dimethyl ammonium chloride

[0068] 3 parts of dodecyl dimethyl amine oxide

[0069] 3 parts of didecyl dimethyl ammonium bromide

[0070] 4 parts of isopropyl alcohol.

[0071] Comparative Example 2

[0072] A fungicide is prepared by the following method: (1) injecting 45 kg of purified water into a container, stirring for 10 min, adding 40 kg of hexamethylenetetramine thereto, and stirring for 11 min;

[0073] (2) adding 3 kg of Tween 80 to the solution after stirring in step (1) and stirring for 11 minutes;

[0074] (3) adding 15 kg of benzalkonium bromide to the solution after stirring in step (2), and stirring for 23 min;

[0075] (4) adding 3 kg of dioctadecyl dimethyl ammonium chloride to the solution after stirring in step (3), and stirring for 18 min;

[0076] (5) adding 3 kg of dodecyl dimethyl amine oxide to the solution after stirring in step (4) and stirring for 8 min;

[0077] (6) adding 10 kg of Jimmie quaternary ammonium salt to the solution after stirring in step (5) and stirring for 11 min;

[0078] (7) adding 3 kg of didecyl dimethyl ammonium bromide to the solution after stirring in step (6) and stirring for 11 minutes;

[0079] (8) Add 4 kg of isopropanol to the solution after stirring in step (7) and stir for 11 minutes;

[0080] (9) Continue stirring at room temperature for 4 h.

[0081] The following bactericide composition is obtained:

[0082] 45 parts of purified water

[0083] 40 parts of hexamethylenetetramine

[0084] Tween 80 3 parts

[0085] 15 parts of benzalkonium bromide

[0086] 3 parts of dioctadecyl dimethyl ammonium chloride

[0087] 3 parts of dodecyl dimethyl amine oxide

[0088] 10 parts of Jimiqi quaternary ammonium salt

[0089] 3 parts of didecyl dimethyl ammonium bromide

[0090] 4 parts of isopropyl alcohol.

[0091] Comparative Example 3

[0092] A fungicide is prepared by the following method: (1) injecting 45 kg of purified water into a container and stirring for 10 minutes; adding 40 kg of hexamethylenetetramine, 3 kg of Tween 80, 15 kg of benzalkonium bromide, 3 kg of dioctadecyldimethylammonium chloride, 3 kg of dodecyldimethylamine oxide, 10 kg of gimmick quaternary ammonium salt, 3 kg of didecyldimethylammonium bromide, and 4 kg of isopropanol, and stirring at room temperature for 4 hours.

[0093] The following bactericide composition is obtained:

[0094] 45 parts of purified water

[0095] 40 parts of hexamethylenetetramine

[0096] Tween 80 3 parts

[0097] 15 parts of benzalkonium bromide

[0098] 3 parts of dioctadecyl dimethyl ammonium chloride

[0099] 3 parts of dodecyl dimethyl amine oxide

[0100] 10 parts of Jimiqi quaternary ammonium salt

[0101] 3 parts of didecyl dimethyl ammonium bromide

[0102] 4 parts of isopropyl alcohol.

[0103] Comparative Example 4

[0104] A fungicide is prepared by the following method: (1) injecting 45 kg of purified water into a container and stirring for 10 minutes; adding 40 kg of hexamethylenetetramine thereto and stirring for 11 minutes;

[0105] (2) adding 3 kg of Tween 80 to the solution after stirring in step (1) and stirring for 11 minutes;

[0106] (3) adding 15 kg of benzalkonium bromide to the solution after stirring in step (2), and stirring for 23 min;

[0107] (4) adding 3 kg of hexadecyl dimethyl ammonium chloride to the solution after stirring in step (3), and stirring for 18 min;

[0108] (5) adding 3 kg of dodecyl dimethyl amine oxide to the solution after stirring in step (4) and stirring for 8 min;

[0109] (6) adding 10 kg of Jimmie quaternary ammonium salt to the solution after stirring in step (5) and stirring for 11 min;

[0110] (7) adding 3 kg of didecyl dimethyl ammonium bromide to the solution after stirring in step (6) and stirring for 11 minutes;

[0111] (8) Add 4 kg of isopropanol to the solution after stirring in step (7) and stir for 11 minutes;

[0112] (9) Continue stirring at room temperature for 4 h.

[0113] The following bactericide composition is obtained:

[0114] 45 parts of purified water

[0115] 40 parts of hexamethylenetetramine

[0116] Tween 80 3 parts

[0117] 15 parts of benzalkonium bromide

[0118] 3 parts of hexadecyl dimethyl ammonium chloride

[0119] 3 parts of dodecyl dimethyl amine oxide

[0120] 10 parts of Jimiqi quaternary ammonium salt

[0121] 3 parts of didecyl dimethyl ammonium bromide

[0122] 4 parts of isopropyl alcohol.

[0123] Comparative Example 5

[0124] A fungicide is prepared by the following method: (1) injecting 45 kg of purified water into a container and stirring for 10 minutes; adding 40 kg of hexamethylenetetramine thereto and stirring for 11 minutes;

[0125] (2) adding 3 kg of Tween 80 to the solution after stirring in step (1) and stirring for 11 minutes;

[0126] (3) adding 15 kg of benzalkonium bromide to the solution after stirring in step (2), and stirring for 23 min;

[0127] (4) adding 3 kg of dioctadecyl dimethyl ammonium chloride to the solution after stirring in step (3), and stirring for 18 min;

[0128] (5) adding 3 kg of dodecyl dimethyl ammonium bromide to the solution after stirring in step (4) and stirring for 8 min;

[0129] (6) adding 10 kg of Jimmie quaternary ammonium salt to the solution after stirring in step (5) and stirring for 11 min;

[0130] (7) adding 3 kg of didecyl dimethyl ammonium bromide to the solution after stirring in step (6) and stirring for 11 minutes;

[0131] (8) Add 4 kg of isopropanol to the solution after stirring in step (7) and stir for 11 minutes;

[0132] (9) Continue stirring at room temperature for 4 h.

[0133] The following bactericide composition is obtained:

[0134] 45 parts of purified water

[0135] 40 parts of hexamethylenetetramine

[0136] Tween 80 3 parts

[0137] 15 parts of benzalkonium bromide

[0138] 3 parts of dioctadecyl dimethyl ammonium chloride

[0139] 3 parts of dodecyl dimethyl ammonium bromide

[0140] 10 parts of Jimiqi quaternary ammonium salt

[0141] 3 parts of didecyl dimethyl ammonium bromide

[0142] 4 parts of isopropyl alcohol.

[0143] Example 1

[0144] A fungicide is prepared by the following method: (1) injecting 35 kg of purified water into a container and stirring for 5 minutes; adding 30 kg of hexamethylenetetramine thereto and stirring for 8 minutes;

[0145] (2) adding 2.5 kg of Tween 80 to the solution after stirring in step (1) and stirring for 8 min;

[0146] (3) adding 11 kg of benzalkonium bromide to the solution after stirring in step (2), and stirring for 18 min;

[0147] (4) adding 2.5 kg of dioctadecyl dimethyl ammonium chloride to the solution after stirring in step (3), and stirring for 13 min;

[0148] (5) adding 1.5 kg of dodecyl dimethyl amine oxide to the solution after stirring in step (4) and stirring for 3 min;

[0149] (6) adding 5 kg of Jimmie quaternary ammonium salt to the solution after stirring in step (5) and stirring for 8 min;

[0150] (7) adding 1 kg of didecyl dimethyl ammonium bromide to the solution after stirring in step (6) and stirring for 8 min;

[0151] (8) adding 1.5 kg of isopropanol to the solution after stirring in step (7) and stirring for 8 min;

[0152] (9) Continue stirring at room temperature for 3 h.

[0153] The following bactericide composition is obtained:

[0154] 35 parts of purified water

[0155] 30 parts of hexamethylenetetramine

[0156] Tween 80 2.5 parts

[0157] Benzalkonium bromide 11 parts

[0158] 2.5 parts of dioctadecyl dimethyl ammonium chloride

[0159] 1.5 parts of dodecyl dimethyl amine oxide

[0160] 5 parts of Jimmie quaternary ammonium salt

[0161] 1 part of didecyl dimethyl ammonium bromide

[0162] 1.5 parts of isopropyl alcohol.

[0163] Example 2

[0164] A fungicide is prepared by the following method: (1) injecting 45 kg of purified water into a container and stirring for 10 minutes; adding 40 kg of hexamethylenetetramine thereto and stirring for 11 minutes;

[0165] (2) adding 3 kg of Tween 80 to the solution after stirring in step (1) and stirring for 11 minutes;

[0166] (3) adding 15 kg of benzalkonium bromide to the solution after stirring in step (2), and stirring for 23 min;

[0167] (4) adding 3 kg of dioctadecyl dimethyl ammonium chloride to the solution after stirring in step (3), and stirring for 18 min;

[0168] (5) adding 3 kg of dodecyl dimethyl amine oxide to the solution after stirring in step (4) and stirring for 8 min;

[0169] (6) adding 10 kg of Jimmie quaternary ammonium salt to the solution after stirring in step (5) and stirring for 11 min;

[0170] (7) adding 3 kg of didecyl dimethyl ammonium bromide to the solution after stirring in step (6) and stirring for 11 minutes;

[0171] (8) Add 4 kg of isopropanol to the solution after stirring in step (7) and stir for 11 minutes;

[0172] (9) Continue stirring at room temperature for 4 h.

[0173] The following bactericide composition is obtained:

[0174] 45 parts of purified water

[0175] 40 parts of hexamethylenetetramine

[0176] Tween 80 3 parts

[0177] 15 parts of benzalkonium bromide

[0178] 3 parts of dioctadecyl dimethyl ammonium chloride

[0179] 3 parts of dodecyl dimethyl amine oxide

[0180] 10 parts of Jimiqi quaternary ammonium salt

[0181] 3 parts of didecyl dimethyl ammonium bromide

[0182] 4 parts of isopropyl alcohol.

[0183] Example 3

[0184] A fungicide is prepared by the following method: (1) injecting 40 kg of purified water into a container and stirring for 1 min; adding 37 kg of hexamethylenetetramine thereto and stirring for 10 min;

[0185] (2) adding 2 kg of Tween 80 to the solution after stirring in step (1) and stirring for 10 min;

[0186] (3) adding 12 kg of benzalkonium bromide to the solution after stirring in step (2), and stirring for 20 min;

[0187] (4) adding 2.5 kg of dioctadecyl dimethyl ammonium chloride to the solution after stirring in step (3), and stirring for 15 min;

[0188] (5) adding 2 kg of dodecyl dimethyl amine oxide to the solution after stirring in step (4) and stirring for 5 min;

[0189] (6) adding 6 kg of Jimmie quaternary ammonium salt to the solution after stirring in step (5) and stirring for 10 min;

[0190] (7) adding 1 kg of didecyl dimethyl ammonium bromide to the solution after stirring in step (6), and stirring for 10 min;

[0191] (8) adding 2 kg of isopropanol to the solution after stirring in step (7) and stirring for 10 min;

[0192] (9) Continue stirring at room temperature for 3 h.

[0193] The following bactericide composition is obtained:

[0194] 40 parts of purified water

[0195] 37 parts of hexamethylenetetramine

[0196] Tween 80 2 parts

[0197] Benzalkonium bromide 12 parts

[0198] 2.5 parts of dioctadecyl dimethyl ammonium chloride

[0199] 2 parts of dodecyl dimethyl amine oxide

[0200] 6 parts of Jimmie quaternary ammonium salt

[0201] 1 part of didecyl dimethyl ammonium bromide

[0202] 2 parts of isopropyl alcohol.

[0203] Example 4

[0204] A fungicide is prepared by the following method: (1) injecting 40 kg of purified water into a container and stirring for 10 minutes; adding 37 kg of hexamethylenetetramine thereto and stirring for 10 minutes;

[0205] (2) adding 2 kg of Tween 80 to the solution after stirring in step (1) and stirring for 10 min;

[0206] (3) adding 12 kg of benzalkonium bromide to the solution after stirring in step (2), and stirring for 20 min;

[0207] (4) adding 2.5 kg of dioctadecyl dimethyl ammonium chloride to the solution after stirring in step (3), and stirring for 15 min;

[0208] (5) adding 2 kg of dodecyl dimethyl amine oxide to the solution after stirring in step (4) and stirring for 5 min;

[0209] (6) adding 6 kg of Jimmie quaternary ammonium salt to the solution after stirring in step (5) and stirring for 10 min;

[0210] (7) adding 1 kg of didecyl dimethyl ammonium bromide to the solution after stirring in step (6), and stirring for 10 min;

[0211] (8) adding 2 kg of isopropanol to the solution after stirring in step (7) and stirring for 10 min;

[0212] (9) Continue stirring at room temperature for 3 h;

[0213] (10) Aging step, the aging time is 70 h.

[0214] The following bactericide composition is obtained:

[0215] 40 parts of purified water

[0216] 37 parts of hexamethylenetetramine

[0217] Tween 80 2 parts

[0218] Benzalkonium bromide 12 parts

[0219] 2.5 parts of dioctadecyl dimethyl ammonium chloride

[0220] 2 parts of dodecyl dimethyl amine oxide

[0221] 6 parts of Jimmie quaternary ammonium salt

[0222] 1 part of didecyl dimethyl ammonium bromide

[0223] 2 parts of isopropyl alcohol.

[0224] Example 5

[0225] A fungicide is prepared by the following method: (1) injecting 40 kg of purified water into a container and stirring for 10 minutes; adding 37 kg of hexamethylenetetramine thereto and stirring for 11 minutes;

[0226] (2) adding 2 kg of Tween 80 to the solution after stirring in step (1) and stirring for 10 min;

[0227] (3) adding 12 kg of benzalkonium bromide to the solution after stirring in step (2), and stirring for 20 min;

[0228] (4) adding 2.5 kg of dioctadecyl dimethyl ammonium chloride to the solution after stirring in step (3), and stirring for 18 min;

[0229] (5) adding 2 kg of dodecyl dimethyl amine oxide to the solution after stirring in step (4) and stirring for 8 min;

[0230] (6) adding 6 kg of Jimmie quaternary ammonium salt to the solution after stirring in step (5) and stirring for 11 min;

[0231] (7) adding 1 kg of didecyl dimethyl ammonium bromide to the solution after stirring in step (6), and stirring for 11 minutes;

[0232] (8) adding 2 kg of isopropanol to the solution after stirring in step (7) and stirring for 10 min;

[0233] (9) Continue stirring at room temperature for 3 h;

[0234] (10) Aging step, the aging time is 70 hours.

[0235] The following bactericide composition is obtained:

[0236] 40 parts of purified water

[0237] 37 parts of hexamethylenetetramine

[0238] Tween 80 2 parts

[0239] Benzalkonium bromide 12 parts

[0240] 2.5 parts of dioctadecyl dimethyl ammonium chloride

[0241] 2 parts of dodecyl dimethyl amine oxide

[0242] 6 parts of Jimmie quaternary ammonium salt

[0243] 1 part of didecyl dimethyl ammonium bromide

[0244] 2 parts of isopropyl alcohol.

[0245] When the sterilizing agents in the above examples 1-5 and comparative examples 1-5 are prepared, the temperature is room temperature, which is 20-25°C.

[0246] When the sterilizing agents in the above-mentioned Examples 1-5 and Comparative Examples 1-5 are used, they are usually diluted with purified water to a sterilizing agent concentration of 1-5% (V / V).

[0247] Example 6

[0248] A fungicide is prepared by the following method: (1) injecting 40 kg of purified water into a container and stirring for 10 minutes; adding 35 kg of hexamethylenetetramine thereto and stirring for 10 minutes;

[0249] (2) adding 2 kg of Tween 80 to the solution after stirring in step (1) and stirring for 10 min;

[0250] (3) adding 12 kg of benzalkonium bromide to the solution after stirring in step (2), and stirring for 20 min;

[0251] (4) adding 2.5 kg of dioctadecyl dimethyl ammonium chloride to the solution after stirring in step (3), and stirring for 15 min;

[0252] (5) adding 2 kg of dodecyl dimethyl amine oxide to the solution after stirring in step (4) and stirring for 5 min;

[0253] (6) adding 6 kg of Jimmie quaternary ammonium salt to the solution after stirring in step (5) and stirring for 10 min;

[0254] (7) adding 1 kg of didecyl dimethyl ammonium bromide to the solution after stirring in step (6), and stirring for 10 min;

[0255] (8) adding 2 kg of isopropanol to the solution after stirring in step (7) and stirring for 10 min;

[0256] (9) Continue stirring at room temperature for 3 h;

[0257] (10) Aging step, the aging time is 70 hours.

[0258] The following bactericide composition is obtained:

[0259] 40 parts of purified water

[0260] 35 parts of hexamethylenetetramine

[0261] Tween 80 2 parts

[0262] Benzalkonium bromide 12 parts

[0263] 2.5 parts of dioctadecyl dimethyl ammonium chloride

[0264] 2 parts of dodecyl dimethyl amine oxide

[0265] 6 parts of Jimmie quaternary ammonium salt

[0266] 1 part of didecyl dimethyl ammonium bromide

[0267] 2 parts of isopropyl alcohol.

[0268] Test Case

[0269] The bactericide of the present invention was subjected to physical and chemical tests, corrosion tests, toxicity tests and stability tests. The specific data are shown in Table 1:

[0270] Table 1 Fungicide safety test data table

[0271]

[0272]

[0273] It can be seen from the above data that the fungicide described in the present invention is non-corrosive, non-irritating, non-toxic and harmless to the human body.

[0274] The present invention also carries out effect test on the bactericide in the above-mentioned embodiment and comparative example, and carries out according to the method and standard of "Technical Specification for Disinfection" (2002 edition of Ministry of Health), and the test of killing Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa needs to dilute the bactericide in the above-mentioned embodiment and comparative example to the use concentration of 1% (V / V), and act for 5 minutes; the test of killing Candida albicans and Aspergillus niger needs to dilute the bactericide in the above-mentioned embodiment and comparative example to the use concentration of 3% (V / V), and act for 5 minutes; the test of killing Bacillus subtilis black variant needs to dilute the bactericide in the above-mentioned embodiment and comparative example to the use concentration of 5% (V / V), and act for 30 minutes. Purified water is used for dilution. Specific data are shown in Tables 2 and 3.

[0275] Table 2 Comparative Examples 1-5 Bactericide Disinfection Effect Test Data Table

[0276]

[0277]

[0278] Table 3 Test data of disinfection effect of bactericide in Examples 1-6

[0279]

[0280] It can be seen from Table 3 above that in Examples 1-5, the bactericide can kill common bacteria as well as pathogenic molds and spore-forming fungi, achieving the disinfection effect of a high-efficiency disinfectant. Particularly note that in Examples 3-5, the influence of the control of stirring time and aging time on the bactericidal effect was studied separately. The results showed that the influence of the pre-stirring activation of water was higher than the influence of the aging time. The proportion of each component was increased in proportion, and the bactericidal effect decreased overall.

[0281] The present invention also compares and analyzes the pre-shear stirring activation process of purified water in the above embodiment, selects benzalkonium bromide which is sparingly soluble in water for testing, and adopts the hanging drop method to determine the concentration of benzalkonium bromide and calculate the solubility according to the method and standard of "Technical Specification for Disinfection" (Ministry of Health 2002 edition), as shown in Table 4.

[0282] Table 4 Example 1-5 Benzalkonium Bromide Solubility

[0283]

[0284] As can be seen from Table 4 above, in Examples 1-5, the solubility of benzalkonium bromide was above 95% when the stirring shearing time was from 1 to 10 min, and the best time was 10 min. This shows that in the production process, sufficient pre-activation of purified water can increase the solubility of purified water for solute molecules, accelerate the interaction between the molecules of each component, and improve the overall bactericidal effect.

[0285] From the above data, it can be seen that in the comparison between the comparative example and the embodiment, although the embodiment is carried out after the comparative example is cultured and the proportion of each reagent is reduced, the bactericidal effect is significantly improved.

[0286] In order to reflect the characteristic that the bactericide of the present invention has no drug resistance, the disinfectant is used to verify the disinfection effect of the surface and air disinfection of the powder injection workshop of a pharmaceutical enterprise. In this powder injection workshop, powder injection medicines are normally produced according to the production plan of the enterprise. After each shift of powder injection production, the disinfectant of Example 1 of the present invention is used alone for routine disinfection at a concentration of 1%, and other types of disinfectants are not replaced or used alternately.

[0287] According to the methods and standards of the Technical Specifications for Disinfection (2002 edition of the Ministry of Health), nutrient agar, sandcastle agar medium, and malt extract agar were used to culture Staphylococcus aureus, Escherichia coli, Staphylococcus albus, Pseudomonas aeruginosa, and Bacillus subtilis var. niger spores on surfaces and in the air, and Candida albicans and Aspergillus niger were used respectively. Among them, Pseudomonas aeruginosa and Bacillus subtilis var. niger spores represent drug-resistant bacteria.

[0288] The use of the above disinfectant has been recorded for up to 3 years. From all production and disinfection records, the bacterial culture results of samples taken at a certain time point in late June and mid-December each year before work the next day and before personnel entered are randomly selected, as shown in Table 5.

[0289] Table 53 Bacterial culture results after surface disinfection (colony count / dish)

[0290]

[0291]

[0292] Table 6 3-year air disinfection floating bacteria / settled bacteria culture results (colonies / dish)

[0293]

[0294] The results of Tables 5 and 6 above show that long-term (3 years) use of the disinfectant of the present invention without alternation or replacement of other types of disinfectants can completely continuously meet or exceed the national standards for the powder injection workshop of the pharmaceutical company with the strictest microbial control standards. The spores of Pseudomonas aeruginosa and Bacillus subtilis var. niger, which often show drug resistance, were not detected; the common pathogenic fungi, Candida albicans and Aspergillus niger, all met the standards. This shows that the bactericide of the present invention has no drug resistance.

[0295] Although the present invention has been described in detail through the above-mentioned specific embodiments, those skilled in the art should understand that any changes in form and detail made on this basis that do not exceed the scope of protection of the claims shall fall within the scope of protection of the present invention.

Claims

1. A non-resistance fungicide, characterized in that: The composition comprises the following components in parts by weight: 35-45 parts of purified water Hexamethylenetetramine 35-40 parts Tween 80 2.5-3 parts Benzalkonium bromide 11-15 parts 2.5-3 parts of dioctadecyl dimethyl ammonium chloride 1.5-3 parts of dodecyl dimethyl amine oxide 5-10 parts of Jimiqi quaternary ammonium salt 1-1.5 parts of didecyl dimethyl ammonium bromide 1.5-4 parts of isopropyl alcohol; The bactericide is prepared by the following steps: (1) Pour 35-45 parts of purified water into a container and stir for 1-10 minutes; add 35-40 parts of hexamethylenetetramine and stir for 8-11 minutes; (2) Add 2.5-3 parts of Tween 80 to the solution after stirring in step (1) and stir for 8-11 minutes; (3) adding 11-15 parts of benzalkonium bromide to the solution after stirring in step (2), and stirring for 18-23 minutes; (4) adding 2.5-3 parts of dioctadecyl dimethyl ammonium chloride to the solution after stirring in step (3), and stirring for 13-18 minutes; (5) adding 1.5-3 parts of dodecyl dimethyl amine oxide to the solution after stirring in step (4) and stirring for 3-8 minutes; (6) Add 5-10 parts of Jimic quaternary ammonium salt to the solution after stirring in step (5), and stir for 8-11 minutes; (7) adding 1-1.5 parts of didecyldimethylammonium bromide to the solution after stirring in step (6) and stirring for 8-11 minutes; (8) Add 1.5-4 parts of isopropanol to the solution after stirring in step (7) and stir for 8-11 minutes; (9) Continue stirring for 3-4 hours.

2. The non-resistance fungicide according to claim 1, characterized in that: The composition comprises the following components in parts by weight: 40 parts of purified water 35 parts of hexamethylenetetramine Tween 80 2.5 parts Benzalkonium bromide 12 parts 2.5 parts of dioctadecyl dimethyl ammonium chloride 2 parts of dodecyl dimethyl amine oxide 6 parts of Jimmie quaternary ammonium salt 1 part of didecyl dimethyl ammonium bromide 2 parts of isopropyl alcohol.

3. The non-resistance fungicide according to claim 1, characterized in that: The following components are included by weight: 40 parts of purified water 37 parts of hexamethylenetetramine Tween 80 2 parts Benzalkonium bromide 12 parts 2.5 parts of dioctadecyl dimethyl ammonium chloride 2 parts of dodecyl dimethyl amine oxide 6 parts of Jimmie quaternary ammonium salt 1 part of didecyl dimethyl ammonium bromide 2 parts of isopropyl alcohol.

4. The non-resistance fungicide according to claim 1, characterized in that: After step (9), an aging step is also included, and the aging time is 70-75 hours.

5. The non-resistance fungicide according to claim 1 or 4, characterized in that: The temperature during preparation is room temperature.

6. The non-resistance fungicide according to claim 1 or 4, characterized in that: The room temperature is 20-25°C.

7. The non-resistance fungicide according to claim 1 or 4, characterized in that: The shear stirring time of purified water is 1-10min.

8. The non-resistance fungicide according to claim 1 or 4, characterized in that: The shear stirring speed of purified water is 300-500 rpm.

Citation Information

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