Nanometer oxygen disinfectant and preparation method thereof

Abstract

The invention discloses a nanometer oxygen disinfectant and a preparation method thereof, and belongs to the technical field of disinfectants. The active component of the nano oxygen disinfectant is hydrogen peroxide co-complexed by povidone and quaternary ammonium salt. Hydrogen peroxide is selected as a disinfection substance, povidone and quaternary ammonium salt are co-complexed with hydrogen peroxide to improve the stability of hydrogen peroxide in the disinfectant, and addition of quaternary ammonium salt not only stabilizes hydrogen peroxide, but also can cooperate with hydrogen peroxide for sterilization. The nano disinfectant provided by the invention not only is stable in property, but also has strong sterilization capability, the preparation process is simple, the required raw materials are cheap, and the nano disinfectant has wide popularization and application prospects.

Description

Technical Field

[0001] The invention belongs to the technical field of disinfectants, and specifically relates to a nano oxygen disinfectant and a preparation method thereof. Background Art

[0002] Hydrogen peroxide is a strong oxidant. Its aqueous solution is commonly known as hydrogen peroxide and is a colorless and transparent liquid. Because it has four atoms covalently bonded into a non-polar HOOH structure, the chemical properties of hydrogen peroxide solution are very active and it is easy to decompose into oxygen and water. It has no residual toxicity and will not cause secondary pollution to the environment. Therefore, it is called the cleanest disinfectant.

[0003] The disinfection mechanism of hydrogen peroxide mainly includes the hydrogen peroxide molecule itself, as well as the free hydroxyl groups and active derivatives produced after its decomposition. It directly acts on the bacterial cell membrane, destroying its permeability barrier, causing the contents of the cell to leak out and killing the bacteria; it reacts with the proteins and nucleic acids of microorganisms, destroying their structures and causing death.

[0004] The disinfection effect of hydrogen peroxide disinfectant alone is not ideal and its stability is poor. How to overcome this defect and obtain a strong and stable hydrogen peroxide disinfectant is a new research direction in this field. Summary of the invention

[0005] The object of the present invention is to provide a nano oxygen disinfectant and a preparation method thereof. By co-complexing hydrogen peroxide with polyvidone and quaternary ammonium salt, not only the disinfection effect of hydrogen peroxide is enhanced, but also the stability of the hydrogen peroxide disinfectant is improved, thereby obtaining a strong and stable nano oxygen disinfectant.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] One of the technical solutions of the present invention is to provide a nano oxygen disinfectant, the active ingredient of which is hydrogen peroxide co-complexed with polyvidone and quaternary ammonium salt.

[0008] The invention utilizes polyvidone and quaternary ammonium salt to jointly complex hydrogen peroxide to obtain a stable nano oxygen disinfectant. Hydrogen peroxide in the disinfectant is first complexed with polyvidone. Hydrogen peroxide separated from hydrogen peroxide complexed with polyvidone is captured by the quaternary ammonium salt during storage. The hydrogen peroxide captured by the quaternary ammonium salt is further transferred to the polyvidone to form hydrogen peroxide complexed with polyvidone, so that hydrogen peroxide is kept stable in the disinfectant system, and the stability of the prepared nano oxygen disinfectant is greatly improved. In addition, the quaternary ammonium salt can also cooperate with hydrogen peroxide to sterilize, so as to obtain a potent nano oxygen disinfectant.

[0009] Preferably, the nano oxygen disinfectant is an aqueous solution of hydrogen peroxide co-complexed with povidone and a quaternary ammonium salt.

[0010] Preferably, the usage ratio of povidone, quaternary ammonium salt cation and hydrogen peroxide in the hydrogen peroxide co-complexed with povidone and quaternary ammonium salt is 300-400 kg: 1.3-1.5 mol: 0.008-0.012 mol.

[0011] Preferably, the povidone includes povidone K30 and / or povidone K90.

[0012] Preferably, the quaternary ammonium salt comprises benzalkonium chloride and / or benzalkonium bromide.

[0013] The second technical solution of the present invention is to provide a method for preparing the above-mentioned nano oxygen disinfectant, comprising the following steps: mixing hydrogen peroxide, quaternary ammonium salt and povidone with water, and obtaining the nano oxygen disinfectant after complexation.

[0014] Preferably, the complexation is carried out under closed conditions.

[0015] Closed complexation can reduce the volatilization loss of hydrogen peroxide.

[0016] Preferably, the complexing temperature is 10-30°C.

[0017] Since hydrogen peroxide will decompose above 30°C, the complexation temperature is controlled below 30°C. If the temperature is too low, the complexation speed is slow, which is not conducive to production. Therefore, the complexation is selected at room temperature (10-30°C).

[0018] Preferably, the complexing time is 12 to 16 hours.

[0019] Preferably, the complexing process is stirred once every 15 to 30 minutes, each stirring lasts for 30 to 60 seconds, and the stirring speed is 75 to 100 rpm.

[0020] The third technical solution of the present invention is to provide an application of the above-mentioned nano oxygen disinfectant in the disinfection of the external environment.

[0021] Preferably, the concentration of hydrogen peroxide in the nano oxygen disinfectant is 3 to 6 wt.%.

[0022] The beneficial technical effects of the present invention are as follows:

[0023] The present invention selects hydrogen peroxide as a disinfectant, and utilizes polyvidone and quaternary ammonium salt to co-complex hydrogen peroxide to improve the stability of hydrogen peroxide in the disinfectant. The addition of quaternary ammonium salt not only stabilizes hydrogen peroxide, but also can cooperate with hydrogen peroxide in sterilization.

[0024] The nano disinfectant provided by the present invention is not only stable in nature, but also has a strong bactericidal ability, and the preparation process is simple, the required raw materials are cheap, and it has broad prospects for promotion and application. DETAILED DESCRIPTION

[0025] Now, various exemplary embodiments of the present invention are described in detail, and this detailed description should not be considered as a limitation of the present invention, but should be understood as a more detailed description of certain aspects, characteristics and embodiments of the present invention. It should be understood that the terms described in the present invention are only for describing specific embodiments and are not used to limit the present invention.

[0026] In addition, for the numerical range in the present invention, it is understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. The intermediate value in any stated value or stated range, and each smaller range between any other stated value or intermediate value in the range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded in the scope.

[0027] Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which the invention pertains. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein may also be used in the practice or testing of the present invention.

[0028] The words “include,” “including,” “have,” “contain,” etc. used in this document are open-ended terms, meaning including but not limited to.

[0029] Example 1

[0030] Preparation of Nano Oxygen Disinfectant:

[0031] Add 330g of povidone K30, 47.6g (1.4mol) of hydrogen peroxide, 3.84g (0.01mol) of benzalkonium bromide and 619mL of water into the reactor, seal the reactor, stir evenly at 100rpm, and then complex at room temperature (10-30°C) for 14h. Stir once every 30min during the complexation process, and each stirring lasts for 1min to obtain a nano oxygen disinfectant.

[0032] Comparative Example 1

[0033] Preparation of Nano Oxygen Disinfectant:

[0034] After adding 330g of povidone K30, 47.6g (1.4mol) of hydrogen peroxide and 623mL of water into the reactor, the reactor was sealed and stirred evenly at 100rpm. Then, the complex was carried out at room temperature (10-30°C) for 14h. During the complexation process, the solution was stirred once every 30min, and each stirring lasted for 1min to obtain a nano oxygen disinfectant.

[0035] The bactericidal effects of the nano oxygen disinfectants prepared in Example 1 and Comparative Example 1 were tested:

[0036] According to the method specified in Appendix C3.1 and C3.2 of GB 15979-2002 "Hygiene Standard for Disposable Sanitary Products", the bactericidal effects of the nano oxygen disinfectant prepared in Example 1 and Comparative Example 1 on Staphylococcus aureus (ATCC 6538), Escherichia coli (8099) and Candida albicans (ATCC 10231) were determined. The specific results are shown in Table 1.

[0037] Table 1 Bactericidal effect of nano oxygen disinfectant

[0038]

[0039] Note: Each group of negative controls showed sterile growth.

[0040] The results in Table 1 show that the nano oxygen disinfectant prepared in Example 1 is significantly more effective than the nano oxygen disinfectant prepared in Comparative Example 1, and the bactericidal rates against Staphylococcus aureus, Escherichia coli and Candida albicans are in line with the standard requirements of GB 15979-2002 "Hygiene Standards for Disposable Sanitary Products".

[0041] The stability of the nano oxygen disinfectant prepared in Example 1 and Comparative Example 1 was tested:

[0042] The nano oxygen disinfectants prepared in Example 1 and Comparative Example 1 were sealed and placed in a stable test box at 40°C for 2 months, and then taken out to test their bactericidal effects. The bactericidal effects of the nano oxygen disinfectants prepared in Example 1 and Comparative Example 1 on Staphylococcus aureus (ATCC 6538), Escherichia coli (8099) and Candida albicans (ATCC 10231) after high temperature acceleration were measured according to the methods specified in Appendix C3.1 and C3.2 of GB 15979-2002 "Sanitary Standards for Disposable Sanitary Products". The specific results are shown in Table 2.

[0043] Table 2 Bactericidal effect of nano oxygen disinfectant after high temperature acceleration

[0044]

[0045] Note: Each group of negative controls showed sterile growth.

[0046] It can be seen from Table 2 that the nano oxygen disinfectant prepared in Example 1 still has a strong bactericidal effect on the sterilization rates of Staphylococcus aureus, Escherichia coli and Candida albicans after high temperature acceleration, and meets the standard requirements of GB 15979-2002 "Sanitary Standards for Disposable Sanitary Products", indicating that the nano oxygen disinfectant prepared in Example 1 has good stability. The nano oxygen disinfectant prepared in Comparative Example 1 in which quaternary ammonium salt is omitted has a significantly lower bactericidal ability after high temperature acceleration, indicating that its stability is poor.

[0047] The irritation of the nano oxygen disinfectant prepared in Test Example 1 to the skin:

[0048] The test is based on 2.3.3 Skin irritation test in the Technical Specifications for Disinfection (2002 edition).

[0049] Animal preparation: New Zealand rabbits were pre-raised in the laboratory animal room for 3 days to adapt to the environment. 24 hours before exposure, the hair on both sides of the spine of the New Zealand rabbits was removed with electric clippers without damaging the skin. The area of ​​the hair removal should not be less than 3cm×3cm on both sides.

[0050] Infection method: Using the self-comparison method on the left and right sides of the same body, drop 0.5mL of nano oxygen disinfectant on a two-layer sterile gauze with an area of ​​2.5cm×2.5cm, and then apply the sterile gauze to the intact hairless skin on the left side, then cover it with a layer of non-irritating cellophane, and then fix it with a non-irritating adhesive tape. Sodium chloride injection was given to the right skin in the same way as the negative control group. The application time was 4h. After the application, gently wash the infected area with warm water and wipe off the residual water stains with absorbent paper.

[0051] Symptom observation: observe the local skin reaction 1h, 24h, and 48h after removing the test substance, and score according to the scoring criteria of Table 2-11 skin irritation reaction in 2.3.3 of "Technical Specifications for Disinfection" (2002 Edition), and judge according to Table 2-12 skin irritation intensity classification. The specific scoring results are shown in Table 3.

[0052] Table 3 Scoring results of a complete skin irritation test

[0053]

[0054] The results in Table 3 show that the nano oxygen disinfectant prepared by the present invention has a non-irritating irritation intensity to the intact skin of New Zealand rabbits, which meets the requirements of the Technical Specification for Disinfection (2002 Edition).

[0055] Synergistic effect of quaternary ammonium salt and hydrogen peroxide in the nano oxygen disinfectant prepared in Example 1:

[0056] The synergistic effect was demonstrated by comparing the quaternary ammonium salt-hydrogen peroxide disinfection with the quaternary ammonium salt disinfection under the same conditions, with the killing rate of Escherichia coli (the initial Escherichia coli concentration was 8×10 8 CFU / mL, the disinfection time of quaternary ammonium salt alone is 5 minutes, the disinfection time of quaternary ammonium salt-hydrogen peroxide is 5+5 minutes, the initial concentration of quaternary ammonium salt (benzalkonium bromide) is 1 mg / L, and the initial concentration of hydrogen peroxide is 30 mg / L); the synergistic effect is represented by the first-order Chick-Watson dynamic model:

[0057]

[0058] When calculating the K value of quaternary ammonium salt-hydrogen peroxide disinfection, in the above formula, N0 is the concentration of Escherichia coli after quaternary ammonium salt disinfection and before hydrogen peroxide disinfection (CFU / mL); N is the concentration of Escherichia coli after hydrogen peroxide disinfection (CFU / mL); K is the first-order rate constant (L·mg -1 ·min); t Hydrogen peroxide disinfection time (min); C i is the concentration of hydrogen peroxide before hydrogen peroxide disinfection (mg / L); C f It is the concentration of hydrogen peroxide after hydrogen peroxide disinfection (mg / L).

[0059] When calculating the K value of quaternary ammonium salt disinfection, in the above formula, N0 is the concentration of Escherichia coli before quaternary ammonium salt disinfection (CFU / mL); N is the concentration of Escherichia coli after quaternary ammonium salt disinfection (CFU / mL); K is the first-order rate constant (L·mg -1 ·min); tQuaternary ammonium salt disinfection time (min); C i is the concentration of quaternary ammonium salt before disinfection (mg / L); C f It is the concentration of quaternary ammonium salt after quaternary ammonium salt disinfection (mg / L).

[0060] Comparing the K values ​​of quaternary ammonium salt-hydrogen peroxide disinfection and quaternary ammonium salt disinfection, K1 and K2 are the K values ​​of quaternary ammonium salt disinfection alone and quaternary ammonium salt-hydrogen peroxide disinfection respectively. After calculation, K2-K1>0, indicating that quaternary ammonium salt and hydrogen peroxide have a synergistic disinfection effect.

[0061] The embodiments described above are only descriptions of the preferred modes of the present invention, and are not intended to limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should all fall within the protection scope determined by the claims of the present invention.

Claims

1. A nano oxygen disinfectant, characterized in that: The active ingredient is hydrogen peroxide co-complexed with povidone and quaternary ammonium salt.

2. The nano oxygen disinfectant according to claim 1, characterized in that The nano oxygen disinfectant is an aqueous solution of hydrogen peroxide co-complexed with polyvidone and quaternary ammonium salt.

3. The nano oxygen disinfectant according to claim 1, characterized in that The dosage ratio of the polyvidone, the quaternary ammonium salt cation and the hydrogen peroxide in the hydrogen peroxide co-complexed with the polyvidone and the quaternary ammonium salt is 300-400 g: 1.3-1.5 mol: 0.008-0.012 mol.

4. The nano oxygen disinfectant according to claim 1, characterized in that The povidone includes povidone K30 and / or povidone K90; and / or the quaternary ammonium salt includes benzalkonium chloride and / or benzalkonium bromide.

5. A method for preparing the nano oxygen disinfectant according to any one of claims 1 to 4, characterized in that: The method comprises the following steps: mixing hydrogen peroxide, quaternary ammonium salt and polyvidone with water, and obtaining the nano oxygen disinfectant after complexation.

6. The method for preparing the nano oxygen disinfectant according to claim 5, characterized in that: The complexation is carried out under closed conditions.

7. The method for preparing the nano oxygen disinfectant according to claim 5, characterized in that: The complexing temperature is 10-30°C.

8. The method for preparing the nano oxygen disinfectant according to claim 5, characterized in that: The complexing time is 12 to 16 hours.

9. The method for preparing the nano oxygen disinfectant according to claim 5, characterized in that: The complexing process is stirred once every 15 to 30 minutes, each stirring lasts for 30 to 60 seconds, and the stirring speed is 75 to 100 rpm.

10. Use of the nano oxygen disinfectant according to any one of claims 1 to 4 in disinfecting an external environment.

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