Disinfectant and preparation method thereof

Abstract

The invention relates to a disinfectant and a preparation method thereof, and belongs to the technical field of disinfectants, the disinfectant is prepared from a sodium hypochlorite solution, an alkaline regulator, surface-modified nano calcium carbonate, a stabilizer, a surfactant and purified water, the alkaline regulator is at least one of sodium hydroxide and potassium hydroxide, and the surface-modified nano calcium carbonate is at least one of sodium hydroxide and potassium hydroxide. A modification method of the surface modified nano calcium carbonate comprises the following steps: firstly, nano calcium carbonate is subjected to epoxy grafting of 3-glycidyl ether oxypropyl trimethoxy silane, then hydroxyl-epoxy addition of polyethylene glycol is performed, and the stabilizer comprises sodium sulfamate and sodium cyclohexyl sulfamate. The surface active agent comprises sodium dodecyl benzene sulfonate and nekal, the conductivity of the purified water is 10-50 us / cm, the disinfectant is good in stability, the effective chlorine content is reduced slowly, the sterilization speed is high, and the disinfection effect is improved.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of disinfectant, and particularly relates to a disinfectant and a preparation method thereof. BACKGROUND

[0002] Sodium hypochlorite, chemical formula NaClO, is a common and widely used chlorine-containing inorganic salt, which is easy to dissolve in water, can release hypochlorous acid with strong oxidizing property in water, and has broad-spectrum bactericidal, bleaching and decontamination capacity. At present, the common 84 disinfectant is a chlorine-containing disinfectant taking sodium hypochlorite as the main effective component. The 84 disinfectant is widely used in various fields such as family, medical treatment, food and breeding due to the advantages of low price and simple operation. However, the existing 84 disinfectant still has some deficiencies. Firstly, sodium hypochlorite itself is not stable and is easy to decompose under the influence of light, temperature and storage conditions, thereby causing the effective chlorine content of the 84 disinfectant to decrease, limiting the shelf life of the product and hindering the use. Generally, the storage period is only a few months. In addition, the bactericidal effect of the 84 disinfectant often needs a certain contact time to fully appear. In many occasions such as sudden health incidents and daily high-frequency disinfection, faster bactericidal speed undoubtedly helps to reduce the risk of pathogen transmission, reduce cross infection and enhance the protection effect. How to further improve the bactericidal speed of the 84 disinfectant has become a hot research direction. SUMMARY

[0003] In view of the problems in the prior art, the purpose of the present application is to provide a disinfectant and a preparation method thereof.

[0004] The purpose of the present application is achieved by the following technical solutions. In a first aspect, the present application provides a disinfectant prepared from 60-65 parts by weight of sodium hypochlorite solution, 0.3 parts by weight of alkaline regulator, 1-1.2 parts by weight of surface modified nano calcium carbonate, 3-3.5 parts by weight of stabilizer, 0.4 parts by weight of surfactant and 28-36 parts by weight of purified water.

[0005] As a preferred technical solution of the present application, the alkaline regulator is at least one of sodium hydroxide and potassium hydroxide.

[0006] As a preferred technical solution of the present application, the surface modified nano calcium carbonate is prepared by the following steps: Step A: under nitrogen protection, nano calcium carbonate and 3-glycidyl ether oxypropyl trimethoxysilane are added to toluene, heated under reflux, constant temperature stirring, centrifugation, discarding the supernatant, washing, drying, and obtaining component A; Step B: Under nitrogen protection, component A, polyethylene glycol and tetrabutylammonium bromide are added into dimethyl sulfoxide, heated at reflux, constant temperature stirring, centrifugation, discarding supernatant, washing, drying.

[0007] Preferably, the mass ratio of the nano calcium carbonate, the 3-glycidyloxypropyltrimethoxysilane and the toluene in step A is 5-7.2:2.5:260-290.

[0008] Preferably, the heating in step A refers to heating at a rate of 2-6℃ / min to 90-100℃.

[0009] Preferably, the stirring time in step A is 18-24h.

[0010] Preferably, the centrifugation speed in step A is 7500-12500r / min.

[0011] Preferably, the centrifugation time in step A is 10-15min.

[0012] Preferably, the washing in step A refers to alternating washing 2-3 times with ether and ethanol in turn.

[0013] Preferably, the drying temperature in step A is 45-50℃.

[0014] Preferably, the drying time in step A is 2-4h.

[0015] Preferably, the mass ratio of component A, polyethylene glycol and dimethyl sulfoxide in step B is 4-5.5:8-10:250-300; the molar ratio of polyethylene glycol and tetrabutylammonium bromide is 1-1.5:0.1.

[0016] Preferably, the molecular weight of polyethylene glycol in step B is 4000, 6000 or 8000.

[0017] Preferably, the heating in step B refers to heating at a rate of 2-6℃ / min to 70-85℃.

[0018] Preferably, the stirring time in step B is 6-7h.

[0019] Preferably, the centrifugation speed in step B is 7500-12500r / min.

[0020] Preferably, the centrifugation time in step B is 10-15min.

[0021] Preferably, the washing in step B refers to alternating washing 2-3 times with ethanol and deionized water in turn.

[0022] Preferably, the drying temperature in step B is 80-85°C.

[0023] Preferably, the drying time in step B is 8-10 hours.

[0024] As a preferred embodiment of the present invention, the stabilizer comprises 4-6 parts by weight of sodium aminosulfonate and 2-3 parts by weight of sodium cyclohexylaminosulfonate.

[0025] As a preferred embodiment of the present invention, the surfactant comprises 2-3 parts by weight of sodium dodecylbenzenesulfonate and 1.5 parts by weight of sodium dibutylnaphthalenesulfonate.

[0026] As a preferred embodiment of the present invention, the conductivity of the purified water is 10-50 μS / cm.

[0027] Secondly, the present invention provides a method for preparing a disinfectant, the method comprising the following steps: At room temperature and in the dark, add surface-modified nano-calcium carbonate, stabilizer and surfactant to the purified water, stir for 10-30 minutes, add sodium hypochlorite solution, stir for 30-60 minutes, then add alkalinity regulator, and stir for 10-15 minutes.

[0028] The beneficial effects of this invention are: 1. This invention utilizes surface-modified nano-calcium carbonate and stabilizers to stabilize sodium hypochlorite, thereby extending the shelf life of the prepared disinfectant and slowing the decline in effective chlorine content, thus improving its practicality. On one hand, the surface-modified nano-calcium carbonate is first epoxy-grafted onto 3-glycidyl etheroxypropyltrimethoxysilane, followed by hydroxyl-epoxy addition to polyethylene glycol. The surface-modified polyethylene glycol contains a large number of ether groups, which can form hydrogen bonds with water molecules, reducing the amount of free water in the system, thereby reducing the probability of molecular collisions with sodium hypochlorite and enhancing stability. This differs from the method used with polyethylene glycol. By directly introducing the surface modification of this invention, the ether groups "polymerize" with each other without forming a free state, resulting in stronger intermolecular forces and better interaction with water molecules. At the same time, this invention selects nano-calcium carbonate as the matrix for surface modification, which is stable in an alkaline environment and has low cost, making it highly feasible. On the other hand, the stabilizers include sodium aminosulfonate and sodium cyclohexylaminosulfonate. Many technologies have already used sodium aminosulfonate to stabilize sodium hypochlorite. Based on this, this invention combines an appropriate amount of sodium cyclohexylaminosulfonate, which further synergistically inhibits molecular collisions and reduces the decomposition rate of sodium hypochlorite through steric hindrance of the ring structure.

[0029] 2. This invention utilizes surfactants to enhance the disinfection effect of the prepared disinfectant solution. The surfactants include sodium dodecylbenzenesulfonate and sodium dibutylnaphthalenesulfonate, which are amphiphilic and can quickly wet and penetrate the surface of bacteria, assisting and promoting the penetration of disinfectant components and accelerating the sterilization speed.

[0030] 3. Through formula design, the present invention not only produces a disinfectant with good stability and a slow decline in effective chlorine content, but also improves its bactericidal and disinfection effects. At the same time, its usage method is no different from that of general 84 disinfectant, which can be used simply by diluting with water. Detailed Implementation

[0031] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0032] The sources of some of the raw materials used in the examples and comparative examples are as follows: Nano-calcium carbonate was purchased from Shanghai Yuanye Biotechnology Co., Ltd., product number S25402.

[0033] Sodium hypochlorite solution refers to sodium hypochlorite aqueous solution (mass fraction 10%), with a measured effective chlorine content of 9.3 wt%; the conductivity of purified water is 25.3 μS / cm.

[0034] Example 1 A disinfectant solution is prepared from 60 parts by weight of sodium hypochlorite solution, 0.3 parts by weight of alkalinity regulator, 1 part by weight of surface-modified nano-calcium carbonate, 3 parts by weight of stabilizer, 0.4 parts by weight of surfactant and 35.3 parts by weight of purified water.

[0035] The alkalinity regulator is sodium hydroxide.

[0036] The surface-modified nano-calcium carbonate is prepared through the following steps: Step A: Under nitrogen protection, nano-calcium carbonate and 3-glycidyl etheroxypropyltrimethoxysilane were added to toluene, heated under reflux, stirred at a constant temperature, centrifuged, the supernatant was discarded, washed, and dried to obtain component A; Step B: Under nitrogen protection, add component A, polyethylene glycol and tetrabutylammonium bromide to dimethyl sulfoxide, heat under reflux, stir at a constant temperature, centrifuge, discard the supernatant, wash and dry.

[0037] The mass ratio of the nano-calcium carbonate, the 3-glycidyl etheroxypropyltrimethoxysilane, and the toluene in step A is 5:2.5:260.

[0038] The heating mentioned in step A refers to heating to 90°C at a rate of 2°C / min.

[0039] The stirring time in step A is 18 hours.

[0040] The centrifugation speed in step A is 7500 r / min.

[0041] The centrifugation time in step A is 10 minutes.

[0042] The washing described in step A refers to washing twice, alternating between ether and ethanol.

[0043] The drying temperature in step A is 45°C.

[0044] The drying time in step A is 2 hours.

[0045] In step B, the mass ratio of component A, polyethylene glycol, and dimethyl sulfoxide is 4:8:250; the molar ratio of polyethylene glycol and tetrabutylammonium bromide is 1:0.1.

[0046] The polyethylene glycol mentioned in step B has a molecular weight of 4000.

[0047] The heating mentioned in step B refers to heating to 70°C at a rate of 2°C / min.

[0048] The stirring time in step B is 6 hours.

[0049] The centrifugation speed in step B is 7500 r / min.

[0050] The centrifugation time in step B is 10 minutes.

[0051] The washing described in step B refers to washing twice, alternating between ethanol and deionized water.

[0052] The drying temperature in step B is 80°C.

[0053] The drying time in step B is 8 hours.

[0054] The stabilizer comprises 4 parts by weight of sodium aminosulfonate and 2 parts by weight of sodium cyclohexylaminosulfonate.

[0055] The surfactant comprises 2 parts by weight of sodium dodecylbenzenesulfonate and 1.5 parts by weight of sodium dibutylnaphthalenesulfonate.

[0056] A method for preparing a disinfectant, the method comprising the following steps: At room temperature and in the dark, surface-modified nano-calcium carbonate, stabilizer and surfactant are added to purified water and stirred for 10 minutes. Sodium hypochlorite solution is added and stirred for 30 minutes. Then, alkalinity regulator is added and stirred for 10 minutes.

[0057] Example 2 A disinfectant solution is prepared from 63 parts by weight of sodium hypochlorite solution, 0.3 parts by weight of alkalinity regulator, 1.1 parts by weight of surface-modified nano-calcium carbonate, 3.2 parts by weight of stabilizer, 0.4 parts by weight of surfactant and 32 parts by weight of purified water.

[0058] The alkalinity regulator is sodium hydroxide.

[0059] The surface-modified nano-calcium carbonate is prepared through the following steps: Step A: Under nitrogen protection, nano-calcium carbonate and 3-glycidyl etheroxypropyltrimethoxysilane were added to toluene, heated under reflux, stirred at a constant temperature, centrifuged, the supernatant was discarded, washed, and dried to obtain component A; Step B: Under nitrogen protection, add component A, polyethylene glycol and tetrabutylammonium bromide to dimethyl sulfoxide, heat under reflux, stir at a constant temperature, centrifuge, discard the supernatant, wash and dry.

[0060] The mass ratio of the nano-calcium carbonate, the 3-glycidyl etheroxypropyltrimethoxysilane, and the toluene in step A is 6:2.5:280.

[0061] The heating mentioned in step A refers to heating to 96°C at a rate of 4°C / min.

[0062] The stirring time in step A is 20 hours.

[0063] The centrifugation speed in step A is 10000 r / min.

[0064] The centrifugation time in step A is 12 minutes.

[0065] The washing described in step A refers to washing twice, alternating between ether and ethanol.

[0066] The drying temperature in step A is 48°C.

[0067] The drying time in step A is 3 hours.

[0068] In step B, the mass ratio of component A, polyethylene glycol, and dimethyl sulfoxide is 5:9:270; the molar ratio of polyethylene glycol and tetrabutylammonium bromide is 1.2:0.1.

[0069] The polyethylene glycol mentioned in step B has a molecular weight of 6000.

[0070] The heating mentioned in step B refers to heating to 80°C at a rate of 4°C / min.

[0071] The stirring time in step B is 6.5 hours.

[0072] The centrifugation speed in step B is 10000 r / min.

[0073] The centrifugation time in step B is 14 minutes.

[0074] The washing described in step B refers to washing three times in sequence with alternating washes of ethanol and deionized water.

[0075] The drying temperature in step B is 82°C.

[0076] The drying time in step B is 9 hours.

[0077] The stabilizer comprises 5 parts by weight of sodium aminosulfonate and 2.2 parts by weight of sodium cyclohexylaminosulfonate.

[0078] The surfactant comprises 2.5 parts by weight of sodium dodecylbenzenesulfonate and 1.5 parts by weight of sodium dibutylnaphthalenesulfonate.

[0079] A method for preparing a disinfectant, the method comprising the following steps: At room temperature and in the dark, surface-modified nano-calcium carbonate, stabilizer and surfactant were added to the purified water and stirred for 20 minutes. Sodium hypochlorite solution was added and stirred for 45 minutes. Then an alkalinity regulator was added and stirred for 14 minutes.

[0080] Example 3 A disinfectant solution is prepared from 65 parts by weight of sodium hypochlorite solution, 0.3 parts by weight of alkalinity regulator, 1.2 parts by weight of surface-modified nano-calcium carbonate, 3.5 parts by weight of stabilizer, 0.4 parts by weight of surfactant and 29.6 parts by weight of purified water.

[0081] The alkalinity regulator is sodium hydroxide.

[0082] The surface-modified nano-calcium carbonate is prepared through the following steps: Step A: Under nitrogen protection, nano-calcium carbonate and 3-glycidyl etheroxypropyltrimethoxysilane were added to toluene, heated under reflux, stirred at a constant temperature, centrifuged, the supernatant was discarded, washed, and dried to obtain component A; Step B: Under nitrogen protection, add component A, polyethylene glycol and tetrabutylammonium bromide to dimethyl sulfoxide, heat under reflux, stir at a constant temperature, centrifuge, discard the supernatant, wash and dry.

[0083] The mass ratio of the nano-calcium carbonate, the 3-glycidyl etheroxypropyltrimethoxysilane, and the toluene in step A is 7.2:2.5:290.

[0084] The heating mentioned in step A refers to heating to 100°C at a rate of 6°C / min.

[0085] The stirring time in step A is 24 hours.

[0086] The centrifugation speed in step A is 12500 r / min.

[0087] The centrifugation time in step A is 15 minutes.

[0088] The washing described in step A refers to washing three times in sequence with alternating washes of ether and ethanol.

[0089] The drying temperature in step A is 50°C.

[0090] The drying time in step A is 4 hours.

[0091] In step B, the mass ratio of component A, polyethylene glycol, and dimethyl sulfoxide is 5.5:10:300; the molar ratio of polyethylene glycol and tetrabutylammonium bromide is 1.5:0.1.

[0092] The polyethylene glycol mentioned in step B has a molecular weight of 8000.

[0093] The heating mentioned in step B refers to heating to 85°C at a rate of 6°C / min.

[0094] The stirring time in step B is 7 hours.

[0095] The centrifugation speed in step B is 12500 r / min.

[0096] The centrifugation time in step B is 15 minutes.

[0097] The washing described in step B refers to washing three times in sequence with alternating washes of ethanol and deionized water.

[0098] The drying temperature in step B is 85°C.

[0099] The drying time in step B is 10 hours.

[0100] The stabilizer comprises 6 parts by weight of sodium aminosulfonate and 3 parts by weight of sodium cyclohexylaminosulfonate.

[0101] The surfactant comprises 3 parts by weight of sodium dodecylbenzenesulfonate and 1.5 parts by weight of sodium dibutylnaphthalenesulfonate.

[0102] A method for preparing a disinfectant, the method comprising the following steps: At room temperature and in the dark, surface-modified nano-calcium carbonate, stabilizer and surfactant were added to the purified water and stirred for 30 minutes. Sodium hypochlorite solution was added and stirred for 60 minutes. Then an alkalinity regulator was added and stirred for 15 minutes.

[0103] Comparative Example 1 Based on Example 2, the preparation method of surface-modified nano-calcium carbonate was changed to mix nano-calcium carbonate and polyethylene glycol, wherein the mass ratio of nano-calcium carbonate to polyethylene glycol was 5:9, the molecular weight of polyethylene glycol was 6000, and other parameters and settings remained the same.

[0104] Comparative Example 2 Based on Example 2, sodium aminosulfonate was replaced with an equal weight of sodium cyclohexylaminosulfonate, while other parameters and settings remained the same.

[0105] Comparative Example 3 Based on Example 2, sodium cyclohexylsulfamate was replaced with an equal weight of sodium aminosulfonate, while other parameters and settings remained the same.

[0106] Comparative Example 4 Based on Example 2, sodium dodecylbenzenesulfonate was replaced with an equal weight of sodium dibutylnaphthalenesulfonate, while other parameters and settings remained the same.

[0107] Comparative Example 5 Based on Example 2, sodium dibutylnaphthalene sulfonate was replaced with an equal weight of sodium dodecylbenzene sulfonate, while other parameters and settings remained the same.

[0108] Comparative Example 6 Based on Example 2, the surface-modified nano-calcium carbonate was replaced with an equal weight of stabilizer, while other parameters and settings remained the same.

[0109] Comparative Example 7 Based on Example 2, the stabilizer was changed to an equal weight of surface-modified nano-calcium carbonate, while other parameters and settings remained the same.

[0110] Stability test: According to standard GB / T 38499-2020, the stability of the disinfectant prepared in Example 2 and Comparative Examples 1-7 was tested. The test was accelerated (54℃, 14d). The effective chlorine content before and after the accelerated test was determined by chemical method, and the decrease rate was calculated. A decrease rate of less than or equal to 15% was considered qualified and could be regarded as reaching the 1-year validity period.

[0111] Table 1. Stability Tests As can be seen from the results in Table 1 above, the disinfectant prepared by the present invention has good stability and the effective chlorine content decreases slowly. Among them, after the composition and content of the surface-modified nano-calcium carbonate and stabilizer changed, the decrease rate increased to varying degrees and the stability deteriorated. Although the decrease rate also increased after the composition of the surfactant changed, the magnitude was not large and was still less than 15%.

[0112] Sterilization test: According to standard GB / T 38502-2020, the disinfectant solutions prepared in Example 2 and Comparative Examples 1-7 were subjected to bactericidal tests. The tests were quantitative suspension bactericidal tests, and the solutions were diluted with water to an effective chlorine content of 0.1 wt%. The test strains were Staphylococcus aureus and Aspergillus niger.

[0113] Table 2. Sterilization Test As can be seen from the results in Table 2 above, the disinfectant prepared by the present invention has a fast sterilization speed and a good disinfection effect. Among them, after the composition and content of the surface-modified nano-calcium carbonate and stabilizer changed, the kill log value was still qualified. However, after the composition of the surfactant changed, the sterilization speed decreased slightly and could not reach the qualified standard at 4 minutes.

[0114] In the description of this specification, the references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0115] The above description is merely an example and illustration of the concept of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described or use similar methods to replace them, as long as they do not deviate from the concept of the invention or exceed the scope defined in the claims, they should all fall within the protection scope of the present invention.

Claims

1. A disinfectant, characterized in that: The disinfectant is prepared from 60-65 parts by weight of sodium hypochlorite solution, 0.3 parts by weight of alkaline regulator, 1-1.2 parts by weight of surface-modified nano-calcium carbonate, 3-3.5 parts by weight of stabilizer, 0.4 parts by weight of surfactant and 28-36 parts by weight of purified water.

2. The disinfectant according to claim 1, characterized in that: The alkalinity regulator is at least one of sodium hydroxide and potassium hydroxide.

3. The disinfectant according to claim 1, characterized in that: The surface-modified nano-calcium carbonate is prepared through the following steps: Step A: Under nitrogen protection, nano-calcium carbonate and 3-glycidyl etheroxypropyltrimethoxysilane were added to toluene, heated under reflux, stirred at a constant temperature, centrifuged, the supernatant was discarded, washed, and dried to obtain component A; Step B: Under nitrogen protection, add component A, polyethylene glycol and tetrabutylammonium bromide to dimethyl sulfoxide, heat under reflux, stir at a constant temperature, centrifuge, discard the supernatant, wash and dry.

4. The disinfectant according to claim 3, characterized in that: The mass ratio of the nano-calcium carbonate, the 3-glycidyl etheroxypropyltrimethoxysilane, and the toluene in step A is 5-7.2:2.5:260-290.

5. The disinfectant according to claim 3, characterized in that: The heating mentioned in step A refers to heating to 90-100℃ at a rate of 2-6℃ / min.

6. The disinfectant according to claim 3, characterized in that: In step B, the mass ratio of component A, polyethylene glycol, and dimethyl sulfoxide is 4-5.5:8-10:250-300; the molar ratio of polyethylene glycol and tetrabutylammonium bromide is 1-1.5:0.

1.

7. The disinfectant according to claim 3, characterized in that: The polyethylene glycol mentioned in step B has a molecular weight of 4000, 6000, or 8000.

8. The disinfectant according to claim 1, characterized in that: The stabilizer comprises 4-6 parts by weight of sodium aminosulfonate and 2-3 parts by weight of sodium cyclohexylaminosulfonate.

9. The disinfectant according to claim 1, characterized in that: The surfactant comprises 2-3 parts by weight of sodium dodecylbenzenesulfonate and 1.5 parts by weight of sodium dibutylnaphthalenesulfonate.

10. A method for preparing a disinfectant solution as described in any one of claims 1-9, characterized in that: The preparation method includes the following steps: At room temperature and in the dark, add surface-modified nano-calcium carbonate, stabilizer and surfactant to the purified water, stir for 10-30 minutes, add sodium hypochlorite solution, stir for 30-60 minutes, then add alkalinity regulator, and stir for 10-15 minutes.

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