Preparation process of long-acting composite disinfectant for livestock farm

Abstract

The invention provides a preparation process of a long-acting composite disinfectant for a livestock farm, and belongs to the technical field of disinfectant preparation. The preparation process comprises the following steps: preparing dihydrodemethyleneberberine; preparation of titanium dioxide-dihydrodemethyleneberberine at calcium phosphate; preparing a composite antibacterial nano emulsion; preparing an organosilicon quaternary ammonium salt antibacterial agent; and preparing the composite disinfectant. The composite disinfectant prepared by compounding the titanium dioxide-dihydrodemethyleneberberine calcium phosphate, the composite antibacterial nano-emulsion and the organosilicon quaternary ammonium salt antibacterial agent does not contain mercury and contains arsenic; therefore, the composite disinfectant overcomes the defect of short-term effect, reduces the risk of drug resistance, and also gives consideration to environmental protection and biological safety.

Description

Technical Field

[0001] The invention relates to the technical field of disinfectant preparation, and in particular to a preparation process of a long-acting composite disinfectant for farms. Background Art

[0002] With the booming development of the global aquaculture industry, the scale of farms is expanding and the density of aquaculture is increasing. Whether it is poultry farming, livestock farming or aquaculture, many poultry, livestock and aquatic animals live in a relatively concentrated space, creating extremely favorable conditions for the spread of diseases. According to industry statistics, the economic losses of aquaculture caused by the outbreak of epidemics have been increasing year by year in recent years, which not only threatens the vital interests of farmers, but also has an impact on the stability of the entire food supply chain such as meat and eggs.

[0003] Traditional disinfectants are widely used in daily sanitation maintenance of farms, but they generally have the defect of short disinfection time. Take the commonly used chlorine-containing disinfectants as an example. In the high humidity, high temperature and complex organic pollution environment of farms, the effective ingredients are very easy to volatilize and decompose, and it is difficult to maintain the disinfection effect continuously. This forces farmers to apply the medicine frequently, which greatly increases the manpower and material costs; and the long-term single use of traditional disinfectants, such as quaternary ammonium salt disinfectants, makes the pathogenic microorganisms in the farms gradually develop drug resistance; at the same time, some chemically synthesized disinfectants will release irritating odors or harmful gases when they play a disinfection role. For example, the volatile gas of peracetic acid disinfectant will not only irritate the respiratory mucosa of poultry and livestock, but also cause stress reactions such as coughing and wheezing, affecting the growth and development of poultry and livestock. Long-term exposure to such an environment may also damage the respiratory health of farmers. Moreover, if used improperly, some strong oxidizing disinfectants also have the risk of chemically reacting with feed, veterinary drugs, etc. to produce toxic byproducts, further threatening the biological safety of farms.

[0004] From an environmental perspective, the frequent and large-scale use of traditional disinfectants will cause their residual components to enter the surrounding soil and water environment through rainwater erosion, sewage discharge and other channels. For example, some disinfectants containing mercury and arsenic will accumulate in the soil for a long time, causing heavy metal pollution in the soil, affecting the structure of soil microbial communities, and thus destroying the surrounding ecological balance; the residual disinfectants discharged into the water will inhibit or even poison the growth and reproduction of aquatic organisms, causing aquatic ecosystem disorders. In addition, with the growing demand of consumers for green and antibiotic-free aquaculture products, farms are in urgent need of seeking more environmentally friendly, safer and sustainable sanitation and disinfection solutions to adapt to market development trends and ensure the long-term healthy development of the aquaculture industry.

[0005] Therefore, we proposed a preparation process for a long-acting composite disinfectant for farms that can overcome the disadvantages of short-term effectiveness, reduce the risk of drug resistance, and take into account environmental protection and biosafety. Summary of the invention

[0006] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a preparation process of a long-acting composite disinfectant for farms.

[0007] A preparation process of a long-acting composite disinfectant for farms comprises the following steps: S1: Preparation of dihydrodesmethyleneberberine An intermediate product is prepared by reacting berberine, xylene, trifluoromethanesulfonic acid and hydrogen chloride solution, and then dihydrodesmethylene berberine is prepared by the intermediate product; S2: Preparation of titanium dioxide-dihydrodemethylberberine@calcium phosphate A dihydrodesmethoxy berberine methanol solution is prepared by using dihydrodesmethoxy berberine and methanol, a titanium solution is prepared by using tetrabutyl titanate and methanol, and then titanium dioxide-dihydrodesmethoxy berberine is prepared by reacting after mixing, and finally titanium dioxide-dihydrodesmethoxy berberine is incubated in a sugar-free DMEM medium, and a calcium chloride solution is added to obtain titanium dioxide-dihydrodesmethoxy berberine@calcium phosphate; S3: Preparation of composite antibacterial nanoemulsion A mixed solution of whey protein solution and dextran sulfate is used as an aqueous phase and then mixed with an oil phase containing thymol and Zanthoxylum essential oil to prepare a composite antibacterial nanoemulsion; S4: Preparation of organosilicon quaternary ammonium salt antibacterial agent Dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride is prepared by using γ-chloropropyltrimethoxysilane and N,N-dimethyloctadecylamine, and then isopropanol and glacial acetic acid are added to prepare an organosilicon quaternary ammonium salt antibacterial agent; S5: Preparation of compound disinfectant Deionized water is mixed with graphene oxide, α-olefin sulfonate and sodium citrate, and then a composite antibacterial nanoemulsion, titanium dioxide-dihydrodemethacrylic berberine@calcium phosphate, an organosilicon quaternary ammonium salt antibacterial agent and glutaraldehyde-decylmethylammonium bromide solution are added and mixed evenly to obtain a composite disinfectant.

[0008] Furthermore, the preparation of dihydrodesmethylene berberine in step S1 specifically comprises the following steps: S1.1: Add 2-3 parts by weight of berberine to 10-12 parts by weight of xylene, stir and mix at room temperature for 10-20 minutes, then add 1.5-2 parts by weight of trifluoromethanesulfonic acid, continue mechanical stirring for 20-30 minutes, then add 2-3 parts by weight of 1M hydrogen chloride solution at 0-1°C, filter after complete precipitation, then wash with water and petroleum ether 2-3 times in sequence, and finally recrystallize with ethanol to obtain an intermediate product; S1.2: Add 2-3 parts by weight of the intermediate product to 30-40 parts by weight of methanol, stir mechanically at room temperature for 10-20 minutes, then add 1-2 parts by weight of potassium carbonate, continue mechanical stirring for 20-30 minutes, then add 1-2 parts by weight of 5-8% sodium hydroxide solution and 0.3-0.5 parts by weight of sodium borohydride, continue stirring for 2-3 hours, and obtain a solid product after the reaction is completed. Then add 100-200 parts by weight of deionized water, dissolve it, extract it with ethyl acetate for 2-3 times, and finally distill and dry it under reduced pressure to obtain dihydrodesmethoxy berberine.

[0009] Furthermore, the structure of the intermediate product in step S1.1 is .

[0010] Further, the structure of dihydrodemethyberberine in step S1.2 is .

[0011] Furthermore, step S2 of preparing titanium dioxide-dihydrodemethyberberine@calcium phosphate specifically comprises the following steps: S2.1: 2-3 parts by weight of dihydrodemethylated berberine are added to 10-20 parts by weight of methanol, followed by ultrasonic treatment for 20-30 minutes to obtain a dihydrodemethylated berberine methanol solution, 2-3 parts by weight of tetrabutyl titanate are dissolved and dispersed in 20-30 parts by weight of methanol, and then 0.5-1 parts by weight of acetylacetone are added, and the mixture is stirred to obtain a titanium solution; S2.2: The dihydrodemethyberberine methanol solution and the titanium solution are mixed and transferred to a microwave reactor. The temperature of the microwave reactor is set to 180-200°C. The mixture is heated for reaction for 10-12 hours. After the reaction is completed, the mixture is naturally cooled to room temperature and then centrifuged to obtain a precipitate. The precipitate is washed with deionized water and anhydrous ethanol for 2-3 times, and then vacuum dried in a vacuum oven at 60-70°C for 8-10 hours to obtain titanium dioxide-dihydrodemethyberberine. S2.3: Disperse 1-2 parts by weight of titanium dioxide-dihydrodesmethoxy berberine in 20-30 parts by weight of sugar-free DMEM culture medium, seal and incubate in an incubator at 37°C for 12-13 hours, then add 2-3 parts by weight of calcium chloride solution, continue incubation for 22-23 hours, and finally centrifuge at 1000-2000 r / min for 5-10 minutes to obtain a solid precipitate, wash with deionized water and anhydrous ethanol 2-3 times, and then vacuum dry in a vacuum oven at 60-70°C for 8-10 hours to obtain titanium dioxide-dihydrodesmethoxy berberine @ calcium phosphate.

[0012] Furthermore, step S2 of preparing titanium dioxide-dihydrodemethyberberine@calcium phosphate specifically comprises the following steps: S2.1: 2-3 parts by weight of dihydrodemethylated berberine are added to 10-20 parts by weight of methanol, followed by ultrasonic treatment for 20-30 minutes to obtain a dihydrodemethylated berberine methanol solution, 2-3 parts by weight of tetrabutyl titanate are dissolved and dispersed in 20-30 parts by weight of methanol, and then 0.5-1 parts by weight of acetylacetone are added, and the mixture is stirred to obtain a titanium solution; S2.2: The dihydrodemethyberberine methanol solution and the titanium solution are mixed and transferred to a microwave reactor. The temperature of the microwave reactor is set to 180-200°C. The mixture is heated for reaction for 10-12 hours. After the reaction is completed, the mixture is naturally cooled to room temperature and then centrifuged to obtain a precipitate. The precipitate is washed with deionized water and anhydrous ethanol for 2-3 times, and then vacuum dried in a vacuum oven at 60-70°C for 8-10 hours to obtain titanium dioxide-dihydrodemethyberberine. S2.3: Disperse 1-2 parts by weight of titanium dioxide-dihydrodesmethoxy berberine in 20-30 parts by weight of sugar-free DMEM culture medium, seal and incubate in an incubator at 37°C for 12-13 hours, then add 2-3 parts by weight of calcium chloride solution, continue incubation for 22-23 hours, and finally centrifuge at 1000-2000 r / min for 5-10 minutes to obtain a solid precipitate, wash with deionized water and anhydrous ethanol 2-3 times, and then vacuum dry in a vacuum oven at 60-70°C for 8-10 hours to obtain titanium dioxide-dihydrodesmethoxy berberine @ calcium phosphate.

[0013] Furthermore, step S4 of preparing the organosilicon quaternary ammonium salt antibacterial agent specifically comprises the following steps: S4.1: 3-5 parts by weight of γ-chloropropyltrimethoxysilane and 5-8 parts by weight of N,N-dimethyloctadecylamine are mixed, and then 0.2-0.5 parts by weight of potassium iodide catalyst and 2-3 parts by weight of a mixed solvent of methanol and dimethyl sulfoxide are added, and then heated and stirred to 70-75° C. by a magnetic stirrer, and reacted at a constant temperature for 45-50 hours to obtain dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride; S4.2: Add 8-10 parts by weight of dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride and 5-8 parts by weight of isopropanol to 50-80 parts by weight of deionized water, stir and mix in a magnetic stirrer for 1-2 minutes, then add 2-3 parts by weight of glacial acetic acid, continue stirring for 2-3 hours, and obtain an organosilicon quaternary ammonium salt antibacterial agent.

[0014] Furthermore, step S5 of preparing the composite disinfectant specifically comprises the following steps: S5.1: 100-120 parts by weight of deionized water and 0.01-0.02 parts by weight of graphene oxide are mixed, and then 0.1-0.2 parts by weight of α-olefin sulfonate and 2-3 parts by weight of sodium citrate are added, followed by ultrasonic dispersion at 100-120 W and 50-60 KHz for 3-4 hours to obtain a mixed dispersion; S5.2: Add 15-18 parts by weight of composite antibacterial nanoemulsion and 13-14 parts by weight of titanium dioxide-dihydrodemethyl berberine @ calcium phosphate to the mixed dispersion, stir continuously at a speed of 5000-6000 r / min for 1-2 hours, add 20-30 parts by weight of organosilicon quaternary ammonium salt antibacterial agent and 5-8 parts by weight of glutaraldehyde-decylmethyl ammonium bromide solution after mixing evenly, stir and mix at a speed of 200-300 r / min for 1-2 hours to obtain a composite disinfectant.

[0015] Furthermore, the glutaraldehyde-decylmethylammonium bromide solution in step S5.2 is specifically prepared by adding 50-60 parts by weight of glutaraldehyde and 50-60 parts by weight of decanylmethylammonium bromide to 500-530 parts by weight of 70% ethanol solution, stirring evenly to fully dissolve the glutaraldehyde-decylmethylammonium bromide solution.

[0016] Compared with the prior art, the present invention has at least the following beneficial effects: 1. The present invention adopts titanium dioxide-dihydrodemethyberberine@calcium phosphate, composite antibacterial nanoemulsion and organosilicon quaternary ammonium salt antibacterial agent to prepare a composite disinfectant, which can act on different targets of bacteria from multiple angles, thereby achieving broad-spectrum antibacterial activity and reducing the risk of drug resistance. The sustained-release effect and the silyl propyl group in the organosilicon quaternary ammonium salt antibacterial agent can achieve long-term antibacterial effect. The composite disinfectant does not contain mercury or arsenic-containing disinfectants. Therefore, the composite disinfectant overcomes the disadvantages of short-term effect and reduces the risk of drug resistance while taking into account environmental protection and biosafety.

[0017] 2. The tetrabutyl titanate of the present invention undergoes a hydrolysis reaction in a methanol solvent to generate titanium dioxide. The dihydrodemethoxy berberine molecule contains multiple hydroxyl groups and aromatic ring structures. These groups can interact with the hydroxyl groups or oxygen vacancies on the surface of the titanium dioxide, such as hydrogen bonding, π-π stacking, etc., so that the dihydrodemethoxy berberine is fixed on the surface of the titanium dioxide to form a stable complex. During the incubation process, the phosphate ions in the culture medium react with the subsequently added calcium chloride to generate calcium phosphate that is wrapped on the surface of the titanium dioxide-dihydrodemethoxy berberine complex. The prepared titanium dioxide-dihydrodemethoxy berberine@phosphorus Calcium phosphate has dual light / pH response. Under the acidic conditions of bacterial infection, the calcium phosphate shell will slowly decompose to release titanium dioxide-dihydrodemethylberberine. At the same time, after exposure to sunlight, the photodynamic effect of titanium dioxide-dihydrodemethylberberine@calcium phosphate can produce a large amount of singlet oxygen to kill bacteria. Singlet oxygen has extremely strong oxidizing properties and can directly destroy important biological macromolecules such as bacterial cell membranes, proteins, and nucleic acids, quickly killing bacteria. It can achieve point-to-point release through pH response and combine with the singlet oxygen generated by photodynamics for efficient sterilization. The two mechanisms work synergistically to significantly improve the antibacterial effect.

[0018] 3. Dextran sulfate in the present invention is a polyanionic polysaccharide. After being compounded with whey protein, a stable emulsified system is formed through electrostatic interaction, which realizes the embedding of thymol and prickly ash essential oil, thereby achieving a slow release effect. This avoids direct exposure of thymol and prickly ash essential oil to the environment, reduces volatilization, oxidation or degradation caused by factors such as light, air, and temperature changes, ensures that the content of the active ingredient of the disinfectant is stable during storage and transportation, and extends the shelf life of the product. Thymol is lipophilic and can easily penetrate the cell membrane of bacteria. The phenolic hydroxyl group in its molecular structure can interact with components such as phospholipids on the cell membrane to change the fluidity and integrity of the cell membrane. When thymol is embedded in the cell membrane in large quantities, the cell membrane will be damaged, the ion balance in the cell will be broken, and important cell contents such as potassium ions will be lost. Zanthoxylum bungeanum essential oil contains a variety of chemical components, such as limonene, thymol, citronellol, etc. These components have synergistic antibacterial effects. Different components can act on different targets of bacteria, and the two cooperate with each other to exert a synergistic antibacterial effect. The slow release mechanism enables thymol and Zanthoxylum bungeanum essential oil to continue to exert a synergistic antibacterial effect for a long time. After large-scale use of disinfectants in farms, the continuously released active ingredients can continuously inhibit and kill newly grown or residual bacteria, fungi and other pathogens, avoiding secondary pollution and infection risks caused by short action time of disinfectants and rapid rebound of pathogens, providing lasting hygiene protection for farms.

[0019] 4. The present invention adds an organosilicon quaternary ammonium salt antibacterial agent to the composite disinfectant. The quaternary ammonium salt group in the organosilicon quaternary ammonium salt antibacterial agent has good antibacterial activity. The quaternary ammonium salt cation can be electrostatically attracted to the negatively charged part of the bacterial surface, such as cell wall, cell membrane, etc., and then closely combined with the bacterial surface through adsorption. Afterwards, the quaternary ammonium salt cation can destroy the structure and function of the bacterial cell membrane, resulting in increased permeability of the cell membrane, leakage of intracellular substances such as proteins and nucleic acids, and ultimately causing bacterial death. Dimethyloctadecyl [3-trimethoxysilylpropyl] ammonium chloride is a key intermediate. The long-chain octadecyl group makes it have strong hydrophobicity, which helps the antibacterial agent to better interact with the lipid membrane of the bacteria and enhance the adsorption and destructive ability of the bacteria. At the same time, the presence of the silicon propyl group can make the antibacterial agent better combined with the surface of the object, forming a lasting antibacterial protective film, which continuously exerts an antibacterial effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] The accompanying drawings, which are incorporated herein and constitute a part of the specification, illustrate embodiments of the invention and, together with the description, further serve to explain the principles of the invention and to enable those skilled in the relevant art to make and use the invention.

[0021] Figure 1 The present invention is a flow chart of the preparation process of a long-acting composite disinfectant for farms used in an embodiment of the present invention. DETAILED DESCRIPTION

[0022] The following is a detailed description of the preparation process of a long-acting composite disinfectant for farms provided by the present invention in conjunction with the accompanying drawings and specific embodiments. At the same time, it is explained here that in order to make the embodiments more detailed, the following embodiments are the best and preferred embodiments, and those skilled in the art may also adopt other alternatives to implement some known technologies; and the accompanying drawings are only for a more specific description of the embodiments, and are not intended to specifically limit the present invention.

[0023] The structure of the intermediate product is: ; The structure of dihydrodesmethyleneberberine is: .

[0024] Example 1 A preparation process of a long-acting composite disinfectant for farms, such as Figure 1 As shown, the following steps are included: S1: Preparation of dihydrodesmethyleneberberine S1.1: Add 2 parts by weight of berberine to 10 parts by weight of xylene, stir and mix at room temperature for 10 minutes, then add 1.5 parts by weight of trifluoromethanesulfonic acid, continue mechanical stirring for 20 minutes, then add 2 parts by weight of 1M hydrogen chloride solution at 0°C, filter after complete precipitation, then wash twice with water and petroleum ether in sequence, and finally recrystallize with ethanol to obtain an intermediate product; S1.2: Add 2 parts by weight of the intermediate product to 30 parts by weight of methanol, stir mechanically at room temperature for 10 minutes, then add 1 part by weight of potassium carbonate, continue to stir mechanically for 20 minutes, then add 1 part by weight of 5% sodium hydroxide solution and 0.3 parts by weight of sodium borohydride, continue to stir for 2 hours, and obtain a solid product after the reaction is completed. Then add 100 parts by weight of deionized water, dissolve it, extract it with ethyl acetate twice, and finally distill and dry it under reduced pressure to obtain dihydrodesmethoxy berberine; S2: Preparation of titanium dioxide-dihydrodemethylberberine@calcium phosphate S2.1: 2 parts by weight of dihydrodemethylated berberine are added to 10 parts by weight of methanol, followed by ultrasonic treatment for 20 minutes to obtain a dihydrodemethylated berberine methanol solution, 2 parts by weight of tetrabutyl titanate are dissolved and dispersed in 20 parts by weight of methanol, and then 0.5 parts by weight of acetylacetone are added, and the mixture is stirred to obtain a titanium solution; S2.2: The dihydrodemethyberberine methanol solution and the titanium solution were mixed and transferred to a microwave reactor. The temperature of the microwave reactor was set to 180°C. The reaction was heated for 10 hours. After the reaction was completed, the mixture was naturally cooled to room temperature. The mixture was then centrifuged to obtain a precipitate. The precipitate was washed twice with deionized water and anhydrous ethanol. The precipitate was then vacuum dried in a vacuum oven at 60°C for 8 hours to obtain titanium dioxide-dihydrodemethyberberine. S2.3: Disperse 1 part by weight of titanium dioxide-dihydrodesmethoxy berberine in 20 parts by weight of sugar-free DMEM culture medium, seal and incubate in an incubator at 37°C for 12 hours, then add 2 parts by weight of calcium chloride solution, continue incubation for 22 hours, and finally centrifuge at 1000 r / min for 5 minutes to obtain a solid precipitate, wash twice with deionized water and anhydrous ethanol, and then vacuum dry in a vacuum oven at 60°C for 8 hours to obtain titanium dioxide-dihydrodesmethoxy berberine @ calcium phosphate; S3: Preparation of composite antibacterial nanoemulsion S3.1: 1 part by weight of whey protein is added to deionized water, and stirred to obtain a 1% (w / v) whey protein solution; 2 parts by weight of dextran sulfate are added to deionized water, and stirred to obtain a 2% (w / v) dextran sulfate solution; after mixing the whey protein solution and the dextran sulfate solution, the pH is adjusted to neutral, and then magnetic stirring is performed for 12 hours to obtain an emulsifier; S3.2: Dissolve 2 parts by weight of thymol and 2 parts by weight of Zanthoxylum bungeanum essential oil in 3 parts by weight of edible oil and stir at room temperature for 30 minutes to prepare an oil phase. Use an emulsifier as an aqueous phase, drop the aqueous phase into the oil phase, stir magnetically for 10 minutes to obtain an oil-water mixed solution, and use a high-speed homogenizer to homogenize at a speed of 100,000 r / min for 6 minutes to obtain a crude emulsion; S3.3: The crude emulsion was subjected to an ultrasonic cell disruptor, which was operated for 5 seconds, paused for 5 seconds, and circulated for 5 minutes. Then, a high-speed homogenizer was used to homogenize the crude emulsion at a speed of 10,000 r / min for 6 minutes to obtain a composite antibacterial nanoemulsion. S4: Preparation of organosilicon quaternary ammonium salt antibacterial agent S4.1: 3 parts by weight of γ-chloropropyltrimethoxysilane and 5 parts by weight of N,N-dimethyloctadecylamine were mixed, 0.2 parts by weight of potassium iodide catalyst and 2 parts by weight of a mixed solvent of methanol and dimethyl sulfoxide were added, and then heated and stirred to 70° C. by a magnetic stirrer, and reacted at a constant temperature for 45 hours to obtain dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride; S4.2: Add 8 parts by weight of dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride and 5 parts by weight of isopropanol to 50 parts by weight of deionized water, stir and mix in a magnetic stirrer for 1 min, then add 2 parts by weight of glacial acetic acid, continue stirring for 2 h, and obtain an organosilicon quaternary ammonium salt antibacterial agent; S5: Preparation of compound disinfectant S5.1: 100 parts by weight of deionized water and 0.01 parts by weight of graphene oxide are mixed, and then 0.1 parts by weight of α-olefin sulfonate and 2 parts by weight of sodium citrate are added, followed by ultrasonic dispersion at 100 W and 50 kHz for 3 h to obtain a mixed dispersion; S5.2: Add 15 parts by weight of the composite antibacterial nanoemulsion and 13 parts by weight of titanium dioxide-dihydrodemethacrylic berberine @ calcium phosphate to the mixed dispersion, stir continuously at a speed of 5000 r / min for 1 hour, and after mixing evenly, add 20 parts by weight of an organosilicon quaternary ammonium salt antibacterial agent and 5 parts by weight of glutaraldehyde-decylmethylammonium bromide solution, stir and mix at a speed of 200 r / min for 1 hour to obtain a composite disinfectant; The glutaraldehyde-decylmethylammonium bromide solution is specifically prepared by adding 50 parts by weight of glutaraldehyde and 50 parts by weight of decanylmethylammonium bromide into 500 parts by weight of 70% ethanol solution, and stirring evenly to fully dissolve the glutaraldehyde-decylmethylammonium bromide solution.

[0025] Example 2 A preparation process of a long-acting composite disinfectant for farms, such as Figure 1 As shown, the following steps are included: S1: Preparation of dihydrodesmethyleneberberine S1.1: Add 2 parts by weight of berberine to 10 parts by weight of xylene, stir and mix at room temperature for 20 minutes, then add 1.5 parts by weight of trifluoromethanesulfonic acid, continue mechanical stirring for 30 minutes, then add 2 parts by weight of 1M hydrogen chloride solution at 1°C, filter after complete precipitation, then wash with water and petroleum ether three times in sequence, and finally recrystallize with ethanol to obtain an intermediate product; S1.2: Add 2 parts by weight of the intermediate product to 30 parts by weight of methanol, stir mechanically at room temperature for 20 minutes, then add 1 part by weight of potassium carbonate, continue to stir mechanically for 30 minutes, then add 1 part by weight of 5% sodium hydroxide solution and 0.3 parts by weight of sodium borohydride, continue to stir for 3 hours, and obtain a solid product after the reaction is completed. Then add 100 parts by weight of deionized water, dissolve it, and use ethyl acetate 2-3 times, and finally distill and dry it under reduced pressure to obtain dihydrodemethyberberine; S2: Preparation of titanium dioxide-dihydrodemethylberberine@calcium phosphate S2.1: 2 parts by weight of dihydrodemethoxy berberine are added to 10 parts by weight of methanol, followed by ultrasonic treatment for 30 minutes to obtain a dihydrodemethoxy berberine methanol solution, 2 parts by weight of tetrabutyl titanate are dissolved and dispersed in 20 parts by weight of methanol, and then 0.5 parts by weight of acetylacetone are added, and the mixture is stirred to obtain a titanium solution; S2.2: The dihydrodemethylated berberine methanol solution and the titanium solution were mixed and transferred to a microwave reactor. The temperature of the microwave reactor was set to 200°C. The reaction was heated for 12 hours. After the reaction was completed, the mixture was naturally cooled to room temperature and then centrifuged to obtain a precipitate. The precipitate was washed with deionized water and anhydrous ethanol for 3 times, and then vacuum dried in a vacuum oven at 70°C for 10 hours to obtain titanium dioxide-dihydrodemethylated berberine. S2.3: Disperse 1 part by weight of titanium dioxide-dihydrodesmethoxy berberine in 20 parts by weight of sugar-free DMEM culture medium, seal and incubate in an incubator at 37°C for 13 hours, then add 2 parts by weight of calcium chloride solution, continue incubation for 23 hours, and finally centrifuge at 2000 r / min for 10 minutes to obtain a solid precipitate, wash it with deionized water and anhydrous ethanol for 3 times, and then vacuum dry it in a vacuum oven at 70°C for 10 hours to obtain titanium dioxide-dihydrodesmethoxy berberine @ calcium phosphate; S3: Preparation of composite antibacterial nanoemulsion S3.1: 1 part by weight of whey protein is added to deionized water, and stirred to obtain a 1% (w / v) whey protein solution; 2 parts by weight of dextran sulfate are added to deionized water, and stirred to obtain a 2% (w / v) dextran sulfate solution; after mixing the whey protein solution and the dextran sulfate solution, the pH is adjusted to neutral, and then magnetic stirring is performed for 14 hours to obtain an emulsifier; S3.2: Dissolve 2 parts by weight of thymol and 2 parts by weight of Zanthoxylum bungeanum essential oil in 3 parts by weight of edible oil and stir at room temperature for 40 minutes to prepare an oil phase. Use an emulsifier as an aqueous phase, drop the aqueous phase into the oil phase, stir magnetically for 20 minutes to obtain an oil-water mixed solution, and use a high-speed homogenizer to homogenize at a speed of 12000r / min for 8 minutes to obtain a crude emulsion; S3.3: The crude emulsion was subjected to an ultrasonic cell disruptor, working for 5 seconds, pausing for 5 seconds, and circulating for 6 minutes, and then homogenized using a high-speed homogenizer at a speed of 12000 r / min for 8 minutes to obtain a composite antibacterial nanoemulsion; S4: Preparation of organosilicon quaternary ammonium salt antibacterial agent S4.1: 3 parts by weight of γ-chloropropyltrimethoxysilane and 5 parts by weight of N,N-dimethyloctadecylamine were mixed, 0.2 parts by weight of potassium iodide catalyst and 2 parts by weight of a mixed solvent of methanol and dimethyl sulfoxide were added, and then heated and stirred to 75° C. by a magnetic stirrer, and reacted at a constant temperature for 50 hours to obtain dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride; S4.2: Add 8 parts by weight of dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride and 5 parts by weight of isopropanol to 50 parts by weight of deionized water, stir and mix in a magnetic stirrer for 2 minutes, then add 2 parts by weight of glacial acetic acid, and continue stirring for 3 hours to obtain an organosilicon quaternary ammonium salt antibacterial agent; S5: Preparation of compound disinfectant S5.1: 100 parts by weight of deionized water and 0.01 parts by weight of graphene oxide are mixed, and then 0.1 parts by weight of α-olefin sulfonate and 2 parts by weight of sodium citrate are added, followed by ultrasonic dispersion at 120 W, 60 kHz for 4 h to obtain a mixed dispersion; S5.2: Add 15 parts by weight of the composite antibacterial nanoemulsion and 13 parts by weight of titanium dioxide-dihydrodemethacrylic berberine @ calcium phosphate to the mixed dispersion, stir continuously at a speed of 6000 r / min for 2 hours, and after mixing evenly, add 20 parts by weight of an organosilicon quaternary ammonium salt antibacterial agent and 5 parts by weight of glutaraldehyde-decylmethylammonium bromide solution, stir and mix at a speed of 300 r / min for 2 hours to obtain a composite disinfectant; The glutaraldehyde-decylmethylammonium bromide solution is specifically prepared by adding 50 parts by weight of glutaraldehyde and 50 parts by weight of decanylmethylammonium bromide into 500 parts by weight of 70% ethanol solution, and stirring evenly to fully dissolve the glutaraldehyde-decylmethylammonium bromide solution.

[0026] Example 3 A preparation process of a long-acting composite disinfectant for farms, such as Figure 1 As shown, the following steps are included: S1: Preparation of dihydrodesmethyleneberberine S1.1: 3 parts by weight of berberine were added to 12 parts by weight of xylene, and the mixture was stirred at room temperature for 10 minutes, and then 1.5 parts by weight of trifluoromethanesulfonic acid was added, and mechanical stirring was continued for 20 minutes, and then 3 parts by weight of 1M hydrogen chloride solution was added at 0°C. After complete precipitation, the mixture was filtered, and then washed with water and petroleum ether twice in sequence, and finally recrystallized with ethanol to obtain an intermediate product; S1.2: 3 parts by weight of the intermediate product are added to 40 parts by weight of methanol, mechanically stirred at room temperature for 10 minutes, then 2 parts by weight of potassium carbonate are added, mechanical stirring is continued for 20 minutes, then 2 parts by weight of 8% sodium hydroxide solution and 0.5 parts by weight of sodium borohydride are added, and stirring is continued for 2 hours. After the reaction is completed, a solid product is obtained, and then 200 parts by weight of deionized water is added. After dissolution, it is extracted twice with ethyl acetate, and finally vacuum distilled and dried to obtain dihydrodesmethoxy berberine; S2: Preparation of titanium dioxide-dihydrodemethylberberine@calcium phosphate S2.1: 3 parts by weight of dihydrodemethylated berberine are added to 20 parts by weight of methanol, followed by ultrasonic treatment for 20 minutes to obtain a dihydrodemethylated berberine methanol solution, 3 parts by weight of tetrabutyl titanate are dissolved and dispersed in 30 parts by weight of methanol, and then 1 part by weight of acetylacetone is added, and the mixture is stirred to obtain a titanium solution; S2.2: The dihydrodemethyberberine methanol solution and the titanium solution were mixed and transferred to a microwave reactor. The temperature of the microwave reactor was set to 180°C. The reaction was heated for 10 hours. After the reaction was completed, the mixture was naturally cooled to room temperature. The mixture was then centrifuged to obtain a precipitate. The precipitate was washed twice with deionized water and anhydrous ethanol. The precipitate was then vacuum dried in a vacuum oven at 60°C for 8 hours to obtain titanium dioxide-dihydrodemethyberberine. S2.3: Disperse 2 parts by weight of titanium dioxide-dihydrodesmethoxy berberine in 30 parts by weight of sugar-free DMEM culture medium, seal and incubate in an incubator at 37°C for 12 hours, then add 3 parts by weight of calcium chloride solution, continue incubation for 22 hours, and finally centrifuge at 1000 r / min for 5 minutes to obtain a solid precipitate, wash twice with deionized water and anhydrous ethanol, and then vacuum dry in a vacuum oven at 60°C for 8 hours to obtain titanium dioxide-dihydrodesmethoxy berberine @ calcium phosphate; S3: Preparation of composite antibacterial nanoemulsion S3.1: 2 parts by weight of whey protein are added to deionized water, and stirred to obtain a 2% (w / v) whey protein solution; 3 parts by weight of dextran sulfate are added to deionized water, and stirred to obtain a 3% (w / v) dextran sulfate solution; after mixing the whey protein solution and the dextran sulfate solution, the pH is adjusted to neutral, and then magnetic stirring is performed for 12 hours to obtain an emulsifier; S3.2: 3 parts by weight of thymol and 3 parts by weight of Zanthoxylum bungeanum essential oil were dissolved in 5 parts by weight of edible oil and stirred at room temperature for 30 minutes to prepare an oil phase. The emulsifier was used as the water phase, and the water phase was added dropwise into the oil phase. The mixture was stirred magnetically for 10 minutes to obtain an oil-water mixed solution. The mixture was homogenized at a speed of 10,000 r / min for 6 minutes using a high-speed homogenizer to obtain a crude emulsion. S3.3: The crude emulsion was subjected to an ultrasonic cell disruptor, which was operated for 5 seconds, paused for 5 seconds, and circulated for 5 minutes. Then, a high-speed homogenizer was used to homogenize the crude emulsion at a speed of 10,000 r / min for 6 minutes to obtain a composite antibacterial nanoemulsion. S4: Preparation of organosilicon quaternary ammonium salt antibacterial agent S4.1: 5 parts by weight of γ-chloropropyltrimethoxysilane and 8 parts by weight of N,N-dimethyloctadecylamine were mixed, 0.5 parts by weight of potassium iodide catalyst and 3 parts by weight of a mixed solvent of methanol and dimethyl sulfoxide were added, and then heated and stirred to 70° C. by a magnetic stirrer, and reacted at a constant temperature for 45 hours to obtain dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride; S4.2: Add 10 parts by weight of dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride and 8 parts by weight of isopropanol to 80 parts by weight of deionized water, stir and mix in a magnetic stirrer for 1 min, then add 3 parts by weight of glacial acetic acid, continue stirring for 2 h, and obtain an organosilicon quaternary ammonium salt antibacterial agent; S5: Preparation of compound disinfectant S5.1: 120 parts by weight of deionized water and 0.02 parts by weight of graphene oxide are mixed, and then 0.2 parts by weight of α-olefin sulfonate and 3 parts by weight of sodium citrate are added, followed by ultrasonic dispersion at 100 W and 50 kHz for 3 h to obtain a mixed dispersion; S5.2: Add 18 parts by weight of the composite antibacterial nanoemulsion and 14 parts by weight of titanium dioxide-dihydrodemethacrylic berberine @ calcium phosphate to the mixed dispersion, stir continuously at a speed of 5000 r / min for 1 hour, and after mixing evenly, add 30 parts by weight of an organosilicon quaternary ammonium salt antibacterial agent and 8 parts by weight of glutaraldehyde-decylmethyl ammonium bromide solution, stir and mix at a speed of 200 r / min for 1 hour to obtain a composite disinfectant; The glutaraldehyde-decylmethylammonium bromide solution is specifically prepared by adding 60 parts by weight of glutaraldehyde and 60 parts by weight of decanylmethylammonium bromide into 530 parts by weight of 70% ethanol solution, and stirring evenly to fully dissolve the glutaraldehyde-decylmethylammonium bromide solution.

[0027] Comparative Example 1 Compared with Example 1, the difference of Comparative Example 1 is that Comparative Example 1 uses conventional glutaraldehyde benzalkonium bromide disinfectant, which is purchased from Luoyang Huizhong Veterinary Medicine Co., Ltd.

[0028] Comparative Example 2 Compared with Example 1, the difference of Comparative Example 2 is that the titanium dioxide-dihydrodemethacrylic berberine@calcium phosphate in steps S1-S2 and step S5.2 is removed in Comparative Example 2, and the remaining steps remain unchanged to prepare the composite disinfectant, which is recorded as Comparative Example 2.

[0029] Comparative Example 3 Compared with Example 1, the difference of Comparative Example 3 is that Comparative Example 3 removes step S2.3, replaces the titanium dioxide-dihydrodemethoxyberberine@calcium phosphate in step S5.2 with titanium dioxide-dihydrodemethoxyberberine, and prepares the composite disinfectant without changing the other steps, which is recorded as Comparative Example 3.

[0030] Comparative Example 4 Compared with Example 1, the difference of Comparative Example 4 is that Comparative Example 4 removes step S3, replaces the composite antibacterial nanoemulsion in step S5.2 with thymol and pepper essential oil, and prepares the composite disinfectant without changing the other steps, which is recorded as Comparative Example 4.

[0031] Comparative Example 5 Compared with Example 1, the difference of Comparative Example 5 is that, in Comparative Example 5, thymol in step S3.2 is removed, and the other steps remain unchanged to prepare the composite disinfectant, which is recorded as Comparative Example 5.

[0032] Comparative Example 6 Compared with Example 1, the difference of Comparative Example 6 is that, in Comparative Example 6, the Zanthoxylum essential oil in step S3.2 is removed, and the other steps remain unchanged to prepare the composite disinfectant, which is recorded as Comparative Example 6.

[0033] Comparative Example 7 Compared with Example 1, the difference of Comparative Example 7 is that the organosilicon quaternary ammonium salt antibacterial agent in step S4 and step S5.2 is removed in Comparative Example 7, and the remaining steps remain unchanged to prepare the composite disinfectant, which is recorded as Comparative Example 7.

[0034] Bactericidal effect experiment: Experimental design: Five pig pens were randomly selected in the farm, and an area of ​​0.5m×0.5m was marked out in each pig pen as the sampling site. At the same time, 3 sampling points with an area of ​​5cm×5cm were selected in each sampling site. The division standards of the sampling sites and sampling points in each pig pen were consistent. The five pig pens were disinfected with the disinfectants in Examples 1-3 and Comparative Examples 1-7, respectively. Each group of disinfectants was diluted with sterile water at a volume ratio of composite disinfectant: sterile water = 1:200 and then sprayed for disinfection. The amount of disinfectant sprayed in each pig pen was consistent. Finally, sampling was carried out before disinfection, 30 minutes after disinfection, and 10 days after disinfection.

[0035] Sampling method: Wet the sterile cotton swab with sterile water. No water should drip from the cotton swab. Then use the wet cotton swab to sample the 5cm×5cm sampling point in each pigpen. When sampling, wipe the wet cotton swab 5 times in the horizontal and vertical directions respectively, and rotate the cotton swab while sampling. After sampling, place the contaminated cotton swab of each sampling point in a centrifuge tube containing 5mL of sterile water, and centrifuge at 1000r / min for 1min. Elute the bacteria into sterile water, and combine the bacterial solution obtained by wiping three times for later use.

[0036] Calculation of sterilization rate: According to the relevant provisions of GB4789.2-2010 "National Food Safety Standard for Determination of Total Colonies in Food Microbiological Examination", when interacting with disinfectants, the concentration of bacterial solution must be ensured to be 1×10 7 -5×10 8 cfu / mL, therefore, before the experiment, the above-obtained bacterial solution needed to be diluted with sterile water to the above-mentioned concentration range, and then 100 μL of the diluted bacterial solution was aspirated with a pipette and spread on a Martin agar plate containing 10% serum. The bacterial solution for each pigpen was repeated 3 times and finally placed in a constant temperature incubator at 37°C for 24 hours. After the incubation, the number of bacteria on each plate was recorded, and the average number of bacteria in each pigpen was counted to calculate the bactericidal rate.

[0037] Sterilization rate = (average bacterial count before disinfection - average bacterial count after disinfection) / average bacterial count before disinfection × 100%. Please refer to Table 1 for the test results.

[0038] Table 1. Bactericidal effect test results

[0039] It can be seen from the data in Table 1 that the present invention can produce a synergistic effect through the compounding of the components, thereby achieving an excellent antibacterial effect. It can be seen from the data of the embodiment and the comparative example 1 that the composite disinfectant prepared in the embodiment has a better disinfection effect than the commercially available disinfectant in comparative example 1, and can maintain a long-lasting disinfection effect.

[0040] It can be seen from the data of Comparative Examples 2 and 3 that the titanium dioxide-dihydrodesmethylene berberine@calcium phosphate prepared by the present invention has a good antibacterial effect, and after being wrapped with calcium phosphate, it has a certain sustained-release effect, and can achieve a long-lasting antibacterial effect.

[0041] It can be seen from the data of Comparative Examples 4-6 that the composite antibacterial nanoemulsion prepared by the present invention can enable thymol and Zanthoxylum bungeanum essential oil to continuously exert a synergistic antibacterial effect for a long time through a slow release mechanism.

[0042] It can be seen from the data of Comparative Example 7 that adding an organosilicon quaternary ammonium salt antibacterial agent to the composite disinfectant can improve the bactericidal effect of the composite disinfectant and can continuously exert the antibacterial effect.

[0043] The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by a person of ordinary skill in the art without departing from the spirit and technical concept disclosed by the present invention shall still be covered by the claims of the present invention.

Claims

1. A preparation process of a long-acting composite disinfectant for farms, characterized in that: The steps include: S1: Preparation of dihydrodesmethyleneberberine An intermediate product is prepared by reacting berberine, xylene, trifluoromethanesulfonic acid and hydrogen chloride solution, and then dihydrodesmethylene berberine is prepared by the intermediate product; S2: Preparation of titanium dioxide-dihydrodemethylberberine@calcium phosphate A dihydrodesmethoxy berberine methanol solution is prepared by using dihydrodesmethoxy berberine and methanol, a titanium solution is prepared by using tetrabutyl titanate and methanol, and then titanium dioxide-dihydrodesmethoxy berberine is prepared by reacting after mixing, and finally titanium dioxide-dihydrodesmethoxy berberine is incubated in a sugar-free DMEM medium, and a calcium chloride solution is added to obtain titanium dioxide-dihydrodesmethoxy berberine@calcium phosphate; S3: Preparation of composite antibacterial nanoemulsion A mixed solution of whey protein solution and dextran sulfate is used as an aqueous phase and then mixed with an oil phase containing thymol and Zanthoxylum essential oil to prepare a composite antibacterial nanoemulsion; S4: Preparation of organosilicon quaternary ammonium salt antibacterial agent Dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride is prepared by using γ-chloropropyltrimethoxysilane and N,N-dimethyloctadecylamine, and then isopropanol and glacial acetic acid are added to prepare an organosilicon quaternary ammonium salt antibacterial agent; S5: Preparation of compound disinfectant Deionized water is mixed with graphene oxide, α-olefin sulfonate and sodium citrate, and then a composite antibacterial nanoemulsion, titanium dioxide-dihydrodemethacrylic berberine@calcium phosphate, an organosilicon quaternary ammonium salt antibacterial agent and glutaraldehyde-decylmethylammonium bromide solution are added and mixed evenly to obtain a composite disinfectant.

2. The preparation process of a long-acting composite disinfectant for farms according to claim 1, characterized in that: Step S1: Preparation of dihydrodesmethylene berberine, specifically comprising the following steps: S1.1: Add 2-3 parts by weight of berberine to 10-12 parts by weight of xylene, stir and mix at room temperature for 10-20 minutes, then add 1.5-2 parts by weight of trifluoromethanesulfonic acid, continue mechanical stirring for 20-30 minutes, then add 2-3 parts by weight of 1M hydrogen chloride solution at 0-1°C, filter after complete precipitation, then wash with water and petroleum ether 2-3 times in sequence, and finally recrystallize with ethanol to obtain an intermediate product; S1.2: Add 2-3 parts by weight of the intermediate product to 30-40 parts by weight of methanol, stir mechanically at room temperature for 10-20 minutes, then add 1-2 parts by weight of potassium carbonate, continue mechanical stirring for 20-30 minutes, then add 1-2 parts by weight of 5-8% sodium hydroxide solution and 0.3-0.5 parts by weight of sodium borohydride, continue stirring for 2-3 hours, and obtain a solid product after the reaction is completed. Then add 100-200 parts by weight of deionized water, dissolve it, extract it with ethyl acetate for 2-3 times, and finally distill and dry it under reduced pressure to obtain dihydrodesmethoxy berberine.

3. The preparation process of a long-acting composite disinfectant for farms according to claim 2, characterized in that: The structure of the intermediate product in step S1.1 is .

4. The preparation process of a long-acting composite disinfectant for farms according to claim 2, characterized in that: The structure of dihydrodemethyberberine in step S1.2 is .

5. The preparation process of a long-acting composite disinfectant for farms according to claim 2, characterized in that: Step S2: Preparation of titanium dioxide-dihydrodemethyberberine@calcium phosphate, specifically comprising the following steps: S2.1: 2-3 parts by weight of dihydrodemethylated berberine are added to 10-20 parts by weight of methanol, followed by ultrasonic treatment for 20-30 minutes to obtain a dihydrodemethylated berberine methanol solution, 2-3 parts by weight of tetrabutyl titanate are dissolved and dispersed in 20-30 parts by weight of methanol, and then 0.5-1 parts by weight of acetylacetone are added, and the mixture is stirred to obtain a titanium solution; S2.2: The dihydrodemethyberberine methanol solution and the titanium solution are mixed and transferred to a microwave reactor. The temperature of the microwave reactor is set to 180-200°C. The mixture is heated for reaction for 10-12 hours. After the reaction is completed, the mixture is naturally cooled to room temperature and then centrifuged to obtain a precipitate. The precipitate is washed with deionized water and anhydrous ethanol for 2-3 times, and then vacuum dried in a vacuum oven at 60-70°C for 8-10 hours to obtain titanium dioxide-dihydrodemethyberberine. S2.3: Disperse 1-2 parts by weight of titanium dioxide-dihydrodesmethoxy berberine in 20-30 parts by weight of sugar-free DMEM culture medium, seal and incubate in an incubator at 37°C for 12-13 hours, then add 2-3 parts by weight of calcium chloride solution, continue incubation for 22-23 hours, and finally centrifuge at 1000-2000 r / min for 5-10 minutes to obtain a solid precipitate, wash with deionized water and anhydrous ethanol 2-3 times, and then vacuum dry in a vacuum oven at 60-70°C for 8-10 hours to obtain titanium dioxide-dihydrodesmethoxy berberine @ calcium phosphate.

6. The preparation process of a long-acting composite disinfectant for farms according to claim 5, characterized in that: Step S3: Preparation of composite antibacterial nanoemulsion, specifically comprising the following steps: S3.1: 1-2 parts by weight of whey protein are added to deionized water, and stirred to obtain a 1-2% (w / v) whey protein solution; 2-3 parts by weight of dextran sulfate are added to deionized water, and stirred to obtain a 2-3% (w / v) dextran sulfate solution; after mixing the whey protein solution and the dextran sulfate solution, the pH is adjusted to neutral, and then magnetic stirring is performed for 12-14 hours to obtain an emulsifier; S3.2: Dissolve 2-3 parts by weight of thymol and 2-3 parts by weight of prickly ash essential oil in 3-5 parts by weight of edible oil and stir at room temperature for 30-40 minutes to prepare an oil phase. Use an emulsifier as an aqueous phase, add the aqueous phase dropwise into the oil phase, stir magnetically for 10-20 minutes to obtain an oil-water mixed solution, and use a high-speed homogenizer to homogenize at a speed of 10000-12000 r / min for 6-8 minutes to obtain a crude emulsion; S3.3: The crude emulsion is subjected to an ultrasonic cell disruptor, which is operated for 5 seconds, paused for 5 seconds, and circulated for 5-6 minutes. The crude emulsion is then homogenized at a speed of 10,000-12,000 r / min for 6-8 minutes to obtain a composite antibacterial nanoemulsion.

7. The preparation process of a long-acting composite disinfectant for farms according to claim 6, characterized in that: Step S4 is the preparation of the organosilicon quaternary ammonium salt antibacterial agent, which specifically comprises the following steps: S4.1: 3-5 parts by weight of γ-chloropropyltrimethoxysilane and 5-8 parts by weight of N,N-dimethyloctadecylamine are mixed, and then 0.2-0.5 parts by weight of potassium iodide catalyst and 2-3 parts by weight of a mixed solvent of methanol and dimethyl sulfoxide are added, and then heated and stirred to 70-75° C. by a magnetic stirrer, and reacted at a constant temperature for 45-50 hours to obtain dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride; S4.2: Add 8-10 parts by weight of dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride and 5-8 parts by weight of isopropanol to 50-80 parts by weight of deionized water, stir and mix in a magnetic stirrer for 1-2 minutes, then add 2-3 parts by weight of glacial acetic acid, continue stirring for 2-3 hours, and obtain an organosilicon quaternary ammonium salt antibacterial agent.

8. The preparation process of a long-acting composite disinfectant for farms according to claim 7, characterized in that: Step S5: Preparation of the composite disinfectant, specifically comprising the following steps: S5.1: 100-120 parts by weight of deionized water and 0.01-0.02 parts by weight of graphene oxide are mixed, and then 0.1-0.2 parts by weight of α-olefin sulfonate and 2-3 parts by weight of sodium citrate are added, followed by ultrasonic dispersion at 100-120 W and 50-60 KHz for 3-4 hours to obtain a mixed dispersion; S5.2: Add 15-18 parts by weight of composite antibacterial nanoemulsion and 13-14 parts by weight of titanium dioxide-dihydrodemethyl berberine @ calcium phosphate to the mixed dispersion, stir continuously at a speed of 5000-6000 r / min for 1-2 hours, add 20-30 parts by weight of organosilicon quaternary ammonium salt antibacterial agent and 5-8 parts by weight of glutaraldehyde-decylmethyl ammonium bromide solution after mixing evenly, stir and mix at a speed of 200-300 r / min for 1-2 hours to obtain a composite disinfectant.

9. The preparation process of a long-acting composite disinfectant for farms according to claim 8, characterized in that: The glutaraldehyde-decylmethylammonium bromide solution in step S5.2 is specifically prepared by adding 50-60 parts by weight of glutaraldehyde and 50-60 parts by weight of decanylmethylammonium bromide into 500-530 parts by weight of 70% ethanol solution, stirring evenly to fully dissolve the glutaraldehyde-decylmethylammonium bromide solution.

Images