A broad-spectrum, high-efficiency and long-lasting chlorine oxyacid system disinfectant and a preparation method thereof

Abstract

The present application relates to the technical field of disinfectant, and discloses a broad-spectrum, efficient and persistent chlorine oxyacid system disinfectant, which is composed of core material A, high-performance modified surface active coating material B and buffer coating layer D; compared with the prior art, the present application effectively solves the core problems of poor stability, insufficient persistence and limited disinfection efficiency of traditional solid disinfectants, and has stronger and more obvious three-dimensional and stereoscopic sterilization effect through oxidation sterilization, chlorination sterilization and acidification (cation adsorption and penetration) sterilization. The present application does not need to add complex auxiliary components, has simple and easy-to-control preparation process, is suitable for large-scale production, and has flexible dilution ratio when used, and is suitable for various scenes. The disinfectant of the present application realizes overall improvement in broad-spectrum, efficiency, persistence and stability, provides a more reliable disinfection solution for the fields of medical health, food processing, environmental cleaning and the like, and has significant practical value and market prospect.

Description

Technical Field

[0001] This invention relates to the field of disinfectant technology, specifically to a broad-spectrum, highly efficient, and long-lasting chloroxylic acid system disinfectant and its preparation method. Background Technology

[0002] Solid disinfectants are a key product formulation in fields such as medical and health care, food processing, and environmental cleaning, and their application scenarios are constantly expanding, leading to continuous growth in market demand. Currently, solid disinfectants on the market mainly include inorganic, organic, and compound products. Among them, inorganic compound disinfectants with potassium persulfate and chlorine dioxide as core components have become the mainstream choice in the market due to their broad bactericidal range and rapid effectiveness.

[0003] However, existing solid disinfectants still face many unresolved problems. On one hand, the core disinfectant components of traditional disinfectants are easily decomposed by moisture and oxygen in the environment, leading to the loss of effective ingredients during storage, insufficient product stability, and consequently affecting the reliability of disinfection effects. On the other hand, ordinary disinfectants lack a reasonable structural design; the disinfectant components are rapidly released after dissolving in water, resulting in short-lived action, poor persistence, and potential environmental residues due to excessively high local concentrations, or incomplete sterilization due to uneven concentrations. Furthermore, conventional disinfectants use a single component, making it difficult to comprehensively kill various microorganisms such as bacteria, fungi, and viruses. The surface-active ingredients are also ineffective, failing to effectively assist the disinfectant components in acting on microorganisms, further reducing disinfection efficiency.

[0004] To meet the comprehensive needs of disinfectants in practical applications for broad-spectrum, high-efficiency, long-lasting and stable properties, it is urgent to develop a new type of powder disinfectant with better performance to adapt to disinfection needs in different scenarios and promote the development of the disinfectant powder industry towards high efficiency and stability. Summary of the Invention

[0005] To address the problems in the prior art, this invention provides a broad-spectrum, highly efficient, and long-lasting chloroxylic acid system disinfectant and its preparation method.

[0006] The technical solution adopted by this invention to solve its technical problem is: This invention provides a broad-spectrum, highly efficient, and long-lasting chloroxylic acid system disinfectant, which consists of a core material A, a high-performance modified surfactant coating material B, and a buffer coating layer D. The core material A is prepared by mixing potassium persulfate, sodium percarbonate, chlorine dioxide, and sodium chloride in a mass ratio of 2-3:2-3:1-1.5:5-6. The high-performance modified surfactant coating material B is a coconut oil-based alkyl glycoside-polyoxyethylene-polyoxypropylene block copolymer graft copolymer, and its mass accounts for 2-3% of the total mass of the core material A; As a further technical solution, the high-performance modified surfactant coating material B is dispersed in deionized water to prepare a dispersion with a mass concentration of 10-12%. Then, it is coated onto the surface of the core material A through a two-fluid atomizing spray device to form a composite material C. The spraying pressure is 0.4-0.6 MPa, the atomized particle size is 50-100 μm, the rotation speed of the turntable stirring device is 35-45 r / min, the spraying time is 2-3 min, and the stirring is continued for 3-4 min. The coating thickness is 3-5 μm. The buffer coating layer D is prepared by mixing sodium citrate and boric acid at a mass ratio of 2-3:1 for 10-15 minutes. It is then sprayed at a rate of 5-10 mL / min onto the surface of the composite material C under stirring at 40-60 r / min for 15-20 minutes to form a coating layer with a thickness of 6-10 μm. Its mass accounts for 0.5-1% of the total mass of the core material A. The core material A is specifically prepared by screening potassium persulfate, sodium percarbonate, chlorine dioxide, and sodium chloride through a 100-120 mesh standard sieve, taking the sieve residue, vacuum drying it, and then mixing it at the mass ratio for 15-20 minutes before dispensing it for later use.

[0007] As a further technical solution, the vacuum drying is performed by vacuum drying at 25℃ and -0.08~-0.09MPa for 4-6 hours until the moisture content is below 0.5%.

[0008] As a further technical solution, the high-performance modified surface-active coating material B is prepared by the following method: coconut oil-based alkyl glycosides and polyoxyethylene-polyoxypropylene block copolymers are mixed at a mass ratio of 3-5:1. An initiator accounting for 0.8%-1.2% of the total mass of the mixture is added. The solid content of the system is adjusted to 30%-40% using deionized water. Under inert gas protection, a free radical polymerization reaction is carried out at 60-70℃ for 3-4 hours. After the reaction, γ-aminopropyltriethoxysilane accounting for 1%-2% of the mass of the mixture is added. The mixture is stirred at 80-100 r / min and crosslinked at 50-55℃ for 1-1.5 hours. The temperature is then adjusted to 35℃±2℃ to obtain the final product.

[0009] As a further technical solution, the number average molecular weight of the polyoxyethylene-polyoxypropylene block copolymer is 2000-5000, and the polyoxyethylene segment accounts for 40%-60%.

[0010] As a further technical solution, the initiator is ammonium persulfate.

[0011] As a further technical solution, the inert gas is nitrogen.

[0012] As a further technical solution, the powder disinfectant is diluted with water at a mass ratio of 1:200-400 when used.

[0013] Another aspect of the present invention provides a method for preparing a broad-spectrum, highly efficient, and long-lasting powder disinfectant, comprising the following steps: Preparation of core material A: To be used; Preparation of high-performance modified surfactant coating material B: to be used; Preparation of composite material C: The above core material A is transported to a rotary evaporator and stirred at 35-45 r / min. The above high-performance modified surface active coating material B is sprayed into deionized water at a pressure of 0.4-0.6 MPa using a dual-fluid atomizing nozzle to prepare a dispersion with a mass concentration of 10-12% and an atomized particle size of 50-100 μm. After spraying for 2 min, stirring is continued for 3 min to form composite material C with a coating thickness of 3-8 μm. Preparation of buffer coating layer D: to be used; Preparation of finished product: The composite material C is put into a rotary stirrer and stirred at 40-60 r / min. At the same time, the buffer coating layer D is sprayed at a uniform rate of 5-10 mL / min. Stir for 15-20 min to form a coating layer with a thickness of 5-10 μm. After drying at 60℃ for 4 h, the finished product is obtained. The buffer coating layer D needs to be mixed with deionized water to prepare a dispersion with a mass fraction of 12-14% for spraying.

[0014] As a further technical solution, the gas-liquid ratio of the atomizing nozzle is 5-8:1.

[0015] The beneficial effects of this invention are: 1. The core material A in this invention is a combination of potassium persulfate, sodium percarbonate, chlorine dioxide, and sodium chloride in a specific mass ratio. The four components work synergistically, providing a material basis for broad-spectrum sterilization. Potassium persulfate and sodium percarbonate, as strong oxidizing components, can rapidly release active oxygen, while chlorine dioxide can generate active chlorine. The combination of these three broadens the sterilization range, effectively targeting various microorganisms such as bacteria, fungi, and viruses. The addition of sodium chloride not only regulates the osmotic pressure of the system but also promotes the release and reaction of active ingredients, increasing the sterilization rate.

[0016] 2. High-performance modified surfactant coating material B is prepared through a specific process. Its grafted structure of cocoyl alkyl glycoside and polyoxyethylene-polyoxypropylene block copolymer endows it with excellent amphiphilic properties. This material is coated onto the surface of the core material A through a two-fluid atomization spray, forming a uniform coating layer. This reduces the contact between the core component and the external environment, lowers the decomposition rate, and promotes the dispersion of the core material during dissolution, avoiding excessively high or low local concentrations. The buffer coating layer D is composed of sodium citrate and boric acid in a specific ratio. Its coating effect further isolates the core material from the influence of moisture and oxygen. At the same time, the buffer system formed by sodium citrate and boric acid provides a stable environment for subsequent disinfection reactions.

[0017] 3. The disinfectant of this invention employs a layered coating structure, forming a unique stepwise dissolution mechanism. When used, after dilution with water at a ratio of 1:200-400 (by mass), the outermost buffer coating layer D dissolves first, rapidly creating a weakly acidic environment in the action area. This environment provides suitable conditions for the disinfection reaction of the core component A, preventing fluctuations in environmental pH from affecting the efficiency of the active ingredients. Subsequently, the second layer, the high-performance modified surfactant coating material B, dissolves. Its cocoyl alkyl glycoside component rapidly adsorbs and kills bacteria, viruses, and other targets, effectively locking onto the target microorganisms and creating conditions for the core disinfectant components to act, preventing microbial escape. Finally, the core component A dissolves, and the components react steadily and continuously to generate highly active oxygen and chlorine, achieving precise and efficient killing of microorganisms based on the locked target.

[0018] 4. Compared with existing technologies, this invention effectively solves the core problems of poor stability, insufficient duration of action, and limited disinfection efficiency of traditional powder disinfectants. It requires no additional complex auxiliary ingredients, has a simple and easily controllable preparation process, is suitable for large-scale production, and offers flexible dilution ratios for various applications. Through comprehensive synergy in material selection, structural design, and process optimization, the disinfectant of this invention achieves a comprehensive improvement in broad-spectrum activity, high efficiency, durability, and stability, providing a more reliable disinfection solution for fields such as medical and health care, food processing, and environmental sanitation, demonstrating significant practical value and market potential. Detailed Implementation

[0019] The technical solutions in the embodiments of the present invention will be clearly and completely described below. 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 skilled in the art without creative effort are within the scope of protection of the present invention.

[0020] This invention provides a broad-spectrum, highly efficient, and long-lasting chloroxylic acid system disinfectant and its preparation method. The solid disinfectant consists of a core material A, a high-performance modified surfactant coating material B, and a buffer coating layer D. The preparation method includes the steps of preparing the core material A, preparing the high-performance modified surfactant coating material B, preparing the composite material C, preparing the buffer coating layer D, and preparing the finished product.

[0021] The present invention does not impose any special restrictions on the source of the potassium persulfate, sodium percarbonate, chlorine dioxide, sodium chloride, cocoyl alkyl glycoside, polyoxyethylene-polyoxypropylene block copolymer, ammonium persulfate, γ-aminopropyltriethoxysilane, sodium citrate, and boric acid, and any commercially available products well known to those skilled in the art can be used.

[0022] Cocoyl alkyl glycoside has a molecular weight of 320 g / mol; In this invention, the number average molecular weight of the polyoxyethylene-polyoxypropylene block copolymer is 2000-5000, and the polyoxyethylene segment accounts for 40%-60%.

[0023] Preparation of core material A: Potassium persulfate, sodium percarbonate, chlorine dioxide, and sodium chloride are screened through a 100-120 mesh standard sieve. The material remaining on the sieve is vacuum dried at 25℃ and -0.08~-0.09MPa for 4-6 hours until the moisture content is below 0.5%. Then, it is mixed at a mass ratio of 2-3:2-3:1-1.5:5-6 for 15-20 minutes and packaged for later use to obtain core material A.

[0024] Preparation of high-performance modified surfactant coating material B: A mixture of coconut oil-based alkyl glycosides and polyoxyethylene-polyoxypropylene block copolymers was prepared at a mass ratio of 3-5:1. Ammonium persulfate initiator (0.8%-1.2% by mass) was added to the mixture. The solid content of the mixture was adjusted to 30%-40% using deionized water. Under nitrogen protection, a free radical polymerization reaction was carried out at 60-70℃ for 3-4 hours. After the reaction, γ-aminopropyltriethoxysilane (1%-2% by mass) was added to the mixture. The mixture was stirred at 80-100 r / min and crosslinked at 50-55℃ for 1-1.5 hours. The temperature was then adjusted to 35℃±2℃ to obtain high-performance modified surface-active coating material B.

[0025] The mass of the high-performance modified surfactant coating material B accounts for 2-3% of the total mass of the core material A.

[0026] Preparation of composite material C: The core material A is transported to a rotary evaporator and stirred at 35-45 r / min. The high-performance modified surfactant coating material B is dispersed in deionized water and sprayed at a pressure of 0.4-0.6 MPa using a dual-fluid atomizing nozzle to prepare a dispersion with a mass concentration of 10-12%. The gas-liquid ratio of the atomizing nozzle is 5-8:1, and the atomized particle size is 50-100 μm. After spraying for 2-3 min, stirring is continued for 3-4 min to form a composite material C with a coating thickness of 3-5 μm.

[0027] Preparation of buffer coating layer D: Sodium citrate and boric acid are mixed at a mass ratio of 2-3:1 for 10-15 minutes to obtain a buffer coating layer D. The mass of the buffer coating layer D accounts for 0.5-1% of the total mass of the core material A.

[0028] Finished product preparation: The composite material C is put into a rotary mixer and stirred at 40-60 r / min. At the same time, the buffer coating layer D is sprayed at a uniform rate of 5-10 mL / min. After stirring for 15-20 min, a coating layer with a thickness of 6-10 μm is formed. After drying at 60℃ for 4 h, the powder disinfectant product is obtained. The buffer coating layer D needs to be mixed with deionized water to prepare a dispersion with a mass fraction of 12-14% for spraying.

[0029] The chloroxygenated disinfectant of this invention is mainly composed of three synergistic disinfection mechanisms: oxidation, chlorination, and acidification, consisting of strong oxidants such as potassium persulfate (PMS) and sodium percarbonate (SPC), chlorides, inorganic acids, and slow-release surfactants.

[0030] After chloroxygenated acid disinfectant is diluted with water to form a disinfectant solution, its three major disinfection components quickly activate the sterilization and disinfection mode. First, positively charged micelles formed by the inorganic acid and slow-release surfactant electrostatically adsorb and encapsulate target microorganisms and surrounding organic particulate matter. The H2O2 released by the SPC also begins to oxidize and consume these interfering substances, ensuring the targeted oxidation and sterilization efficiency of active oxygen and active chlorine against the target microorganisms and reducing the ineffective consumption of the oxidant. Furthermore, the buffer system formed by the inorganic acid continuously provides a slightly acidic environment, helping active oxygen and active chlorine to clear interfering substances and immobilize target microorganisms for rapid sterilization.

[0031] Strong oxidants PMS and SPC react with water to produce reactive oxygen species, and react with chlorides to produce reactive chlorine and hypochlorous acid. Under acidic conditions, hypochlorous acid, a neutral molecule with strong oxidizing properties, can easily penetrate the negatively charged cell membranes of microorganisms, entering the cell to disrupt its structure and metabolism, thus achieving highly efficient disinfection. Reactive oxygen species and reactive chlorine rapidly oxidize and chlorinate pathogens, interfering with their DNA and RNA synthesis, causing protein coagulation and denaturation, thereby interfering with the activity of their enzyme systems, affecting their metabolism, increasing cell membrane permeability, causing enzyme and nutrient loss, and ultimately killing the pathogens. Through these three methods, a three-dimensional disinfection process is achieved, rapidly and thoroughly eliminating the target microorganisms.

[0032] To further illustrate the present invention, the following detailed description is provided through the examples and comparative examples.

[0033] Example 1: A method for preparing a broad-spectrum, highly efficient, and long-lasting chloroxylic acid disinfectant includes the following steps: Preparation of core material A: Potassium persulfate, sodium percarbonate, chlorine dioxide, and sodium chloride are screened through a 100-mesh standard sieve. The material on the sieve is taken and vacuum dried at 25℃ and -0.08MPa for 4 hours until the moisture content is less than 0.5%. Then, it is mixed by stirring at a mass ratio of 2:2:1:5 for 15 minutes and packaged for later use.

[0034] Preparation of high-performance modified surfactant coating material B: A mixture of coconut oil-based alkyl glycosides and polyoxyethylene-polyoxypropylene block copolymer (number-average molecular weight 2000, polyoxyethylene segment content 40%) was prepared at a mass ratio of 3:1. Ammonium persulfate initiator (0.8% by mass) was added. The solid content of the system was adjusted to 30% using deionized water. Under nitrogen protection, a free radical polymerization reaction was carried out at 60℃ for 3 hours. After the reaction, γ-aminopropyltriethoxysilane (1% by mass) was added, and the mixture was stirred at 80 r / min for 1 hour at 50℃ for crosslinking modification. The temperature was then adjusted to 33℃ to obtain high-performance modified surfactant coating material B. This material accounts for 2% of the total mass of the core material A.

[0035] Preparation of composite material C: The core material A is transported to a rotary evaporator and stirred at 35 r / min. High-performance modified surface-active coating material B is dispersed in deionized water and sprayed at a pressure of 0.4 MPa using a dual-fluid atomizing nozzle. After preparing a dispersion with a mass concentration of 10%, the gas-liquid ratio of the atomizing nozzle is 5:1 and the atomized particle size is 50 μm. After spraying for 2 min, stirring is continued for 3 min to form composite material C with a coating thickness of 3 μm.

[0036] Preparation of buffer coating layer D: Sodium citrate and boric acid were mixed at a mass ratio of 2:1 for 10 minutes to obtain buffer coating layer D. The mass of this material accounts for 0.5% of the total mass of the core material A.

[0037] Preparation of the finished product: The composite material C is added to a rotary mixer and stirred at 40 r / min. Simultaneously, the buffer coating layer D is sprayed at a uniform rate of 5 mL / min. The mixture is stirred for 15 min to form a 6 μm thick coating layer. After drying at 60℃ for 4 h, the powder disinfectant is obtained. The buffer coating layer D needs to be mixed with deionized water to prepare a 12% (w / w) dispersion for spraying. When using, it should be diluted with water at a mass ratio of 1:200.

[0038] Example 2: A method for preparing a broad-spectrum, highly efficient, and long-lasting chloroxylic acid disinfectant includes the following steps: Preparation of core material A: Potassium persulfate, sodium percarbonate, chlorine dioxide and sodium chloride are screened through a 100-mesh standard sieve. The material on the sieve is taken and vacuum dried at 25℃ and -0.085MPa for 5h until the moisture content is less than 0.5%. Then, it is mixed by stirring at a mass ratio of 3:3:1.5:6 for 15min and packaged for later use.

[0039] Preparation of high-performance modified surfactant coating material B: A mixture of coconut oil-based alkyl glycosides and polyoxyethylene-polyoxypropylene block copolymer (number-average molecular weight 3500, polyoxyethylene segment content 50%) was prepared at a mass ratio of 4:1. Ammonium persulfate initiator (1.0% by mass) was added. The solid content of the system was adjusted to 35% using deionized water. Under nitrogen protection, a free radical polymerization reaction was carried out at 65℃ for 3.5 h. After the reaction, γ-aminopropyltriethoxysilane (1.5% by mass) was added, and the mixture was stirred at 90 r / min for 1.2 h at 52℃ for crosslinking modification. The temperature was then adjusted to 35℃ to obtain high-performance modified surfactant coating material B. This material accounts for 2.5% of the total mass of the core material A.

[0040] Preparation of composite material C: The core material A is transported to a rotary evaporator and stirred at 40 r / min. High-performance modified surface-active coating material B is dispersed in deionized water and sprayed at a pressure of 0.5 MPa using a dual-fluid atomizing nozzle to prepare a dispersion with a mass concentration of 10%. The gas-liquid ratio of the atomizing nozzle is 6.5:1 and the atomized particle size is 75 μm. After spraying for 2 min, stirring is continued for 3 min to form composite material C with a coating thickness of 4 μm.

[0041] Preparation of buffer coating layer D: Sodium citrate and boric acid were mixed at a mass ratio of 2:1 for 10 minutes to obtain buffer coating layer D. This material accounts for 0.7% of the total mass of the core material A.

[0042] Preparation of the finished product: The composite material C is added to a rotary mixer and stirred at 50 r / min. Simultaneously, the buffer coating layer D is sprayed at a uniform rate of 7.5 mL / min. Stirring is continued for 17 min to form an 8 μm thick coating layer. After drying at 60℃ for 4 h, the powder disinfectant is obtained. The buffer coating layer D needs to be mixed with deionized water to prepare a 12% (w / w) dispersion for spraying. When using, dilute with water at a ratio of 1:300 (w / w).

[0043] Example 3: A method for preparing a broad-spectrum, highly efficient, and long-lasting chloroxylic acid disinfectant includes the following steps: Preparation of core material A: Potassium persulfate, sodium percarbonate, chlorine dioxide and sodium chloride are screened through a 100-mesh standard sieve. The material on the sieve is taken and vacuum dried at 25℃ and -0.09MPa for 6 hours until the moisture content is less than 0.5%. Then, it is mixed by stirring at a mass ratio of 2:2:1:5 for 15 minutes and packaged for later use.

[0044] Preparation of high-performance modified surfactant coating material B: A mixture of cocoyl alkyl glycoside and polyoxyethylene-polyoxypropylene block copolymer (number average molecular weight 5000, polyoxyethylene segment content 60%) was prepared at a mass ratio of 5:1. Ammonium persulfate initiator (1.2% by mass) was added. The solid content of the system was adjusted to 40% using deionized water. Under nitrogen protection, a free radical polymerization reaction was carried out at 70℃ for 4 hours. After the reaction, γ-aminopropyltriethoxysilane (2% by mass) was added, and the mixture was stirred at 100 r / min for 1.5 hours for crosslinking modification at 55℃. The temperature was then adjusted to 37℃ to obtain high-performance modified surfactant coating material B. This material accounts for 3% of the total mass of the core material A.

[0045] Preparation of composite material C: The core material A is transported to a rotary evaporator and stirred at 45 r / min. High-performance modified surface-active coating material B is dispersed in deionized water and sprayed at a pressure of 0.6 MPa using a dual-fluid atomizing nozzle. After preparing a dispersion with a mass concentration of 10%, the gas-liquid ratio of the atomizing nozzle is 8:1 and the atomized particle size is 100 μm. After spraying for 2 min, stirring is continued for 3 min to form composite material C with a coating thickness of 5 μm.

[0046] Preparation of buffer coating layer D: Sodium citrate and boric acid were mixed at a mass ratio of 2:1 for 10 minutes to obtain buffer coating layer D. This material accounts for 0.6% of the total mass of the core material A.

[0047] Preparation of the finished product: The composite material C is added to a rotary mixer and stirred at 60 r / min. Simultaneously, the buffer coating layer D is sprayed at a uniform rate of 10 mL / min. The mixture is stirred for 20 min to form a 10 μm thick coating layer. After drying at 60℃ for 4 h, the powder disinfectant is obtained. The buffer coating layer D needs to be mixed with deionized water to prepare a 12% (w / w) dispersion for spraying. When using, it should be diluted with water at a mass ratio of 1:400.

[0048] Comparative Example 1: The preparation method of Example 2 is adopted, except that: the high-performance modified surface-active coating material B is not added, and the core material A and the buffer coating layer D are directly mixed and coated in the corresponding proportion.

[0049] Specifically: A method for preparing a broad-spectrum, highly efficient, and long-lasting chloroxylic acid disinfectant includes the following steps: Preparation of core material A: Potassium persulfate, sodium percarbonate, chlorine dioxide and sodium chloride are screened through a 100-mesh standard sieve. The material on the sieve is taken and vacuum dried at 25℃ and -0.085MPa for 5h until the moisture content is less than 0.5%. Then, it is mixed by stirring at a mass ratio of 3:3:1.5:6 for 15min and packaged for later use.

[0050] Preparation of coating material B: water.

[0051] Preparation of composite material C: The core material A is transported to a rotary evaporator and stirred at 40 r / min. Clean water is sprayed at a pressure of 0.5 MPa using a dual-fluid atomizing nozzle with a gas-liquid ratio of 6.5:1 and an atomized particle size of 75 μm. After spraying for 2 min, stirring is continued for 3 min to form composite material C with a coating thickness of 4 μm.

[0052] Preparation of buffer coating layer D: Sodium citrate and boric acid were mixed at a mass ratio of 2:1 for 10 minutes to obtain buffer coating layer D. This material accounts for 0.7% of the total mass of the core material A.

[0053] Preparation of finished product: The composite material C is put into a rotary stirrer and stirred at 50 r / min. At the same time, the buffer coating layer D is sprayed at a uniform rate of 7.5 mL / min. After stirring for 17 min, a coating layer with a thickness of 8 μm is formed. After drying at 60℃ for 4 h, the powder disinfectant product is obtained. The buffer coating layer D needs to be mixed with deionized water to prepare a dispersion with a mass fraction of 12% for spraying.

[0054] Dilute with water at a ratio of 1:300 by weight before use.

[0055] Comparative Example 2: The preparation method of Example 2 is used, except that the buffer coating layer D is not added; the finished product is prepared solely from the core material A and the high-performance modified surfactant coating material B. The specific steps are as follows: A method for preparing a broad-spectrum, highly efficient, and long-lasting chloroxylic acid disinfectant includes the following steps: Preparation of core material A: Potassium persulfate, sodium percarbonate, chlorine dioxide and sodium chloride are screened through a 100-mesh standard sieve. The material on the sieve is taken and vacuum dried at 25℃ and -0.085MPa for 5h until the moisture content is less than 0.5%. Then, it is mixed by stirring at a mass ratio of 3:3:1.5:6 for 15min and packaged for later use.

[0056] Preparation of high-performance modified surfactant coating material B: A mixture of coconut oil-based alkyl glycosides and polyoxyethylene-polyoxypropylene block copolymer (number-average molecular weight 3500, polyoxyethylene segment content 50%) was prepared at a mass ratio of 4:1. Ammonium persulfate initiator (1.0% by mass) was added. The solid content of the system was adjusted to 35% using deionized water. Under nitrogen protection, a free radical polymerization reaction was carried out at 65℃ for 3.5 h. After the reaction, γ-aminopropyltriethoxysilane (1.5% by mass) was added, and the mixture was stirred at 90 r / min for 1.2 h at 52℃ for crosslinking modification. The temperature was then adjusted to 35℃ to obtain high-performance modified surfactant coating material B. This material accounts for 2.5% of the total mass of the core material A.

[0057] Preparation of composite material C: The core material A is transported to a rotary evaporator and stirred at 40 r / min. High-performance modified surface-active coating material B is dispersed in deionized water and sprayed at a pressure of 0.5 MPa using a dual-fluid atomizing nozzle to prepare a dispersion with a mass concentration of 10%. The gas-liquid ratio of the atomizing nozzle is 6.5:1 and the atomized particle size is 75 μm. After spraying for 2 min, stirring is continued for 3 min to form composite material C with a coating thickness of 4 μm.

[0058] Preparation of finished product: The composite material C is put into a rotary mixer and stirred at 50 r / min. At the same time, water is sprayed at a uniform rate of 7.5 mL / min. After stirring for 17 min, it is dried at 60℃ for 4 h to obtain the powder disinfectant product.

[0059] Dilute with water at a ratio of 1:300 by weight before use.

[0060] Comparative Example 3: The preparation method of Example 2 was used, except that the crosslinking modification step was not performed in the preparation of the high-performance modified surface-active coating material B; the remaining steps were the same as in Example 2. The specific steps are as follows: A method for preparing a broad-spectrum, highly efficient, and long-lasting chloroxylic acid disinfectant includes the following steps: Preparation of core material A: Potassium persulfate, sodium percarbonate, chlorine dioxide and sodium chloride are screened through a 100-mesh standard sieve. The material on the sieve is taken and vacuum dried at 25℃ and -0.085MPa for 5h until the moisture content is less than 0.5%. Then, it is mixed by stirring at a mass ratio of 3:3:1.5:6 for 15min and packaged for later use.

[0061] Preparation of coating material B: Hydroxypropyl methylcellulose, a conventional material, is used. This material accounts for 2.5% of the total mass of core material A.

[0062] Preparation of composite material C: The core material A is transported to a rotary evaporator and stirred at 40 r / min. Hydroxypropyl methylcellulose is sprayed at a pressure of 0.5 MPa using a dual-fluid atomizing nozzle with a gas-liquid ratio of 6.5:1 and an atomized particle size of 75 μm. After spraying for 2 min, stirring is continued for 3 min to form composite material C with a coating thickness of 4 μm.

[0063] Preparation of buffer coating layer D: Sodium citrate and boric acid were mixed at a mass ratio of 2:1 for 10 minutes to obtain buffer coating layer D. This material accounts for 0.7% of the total mass of the core material A.

[0064] Preparation of the finished product: The composite material C is added to a rotary mixer and stirred at 50 r / min. Simultaneously, the buffer coating layer D is sprayed at a uniform rate of 7.5 mL / min. Stirring is continued for 17 min to form an 8 μm thick coating layer. After drying at 60℃ for 4 h, the powder disinfectant is obtained. The buffer coating layer D needs to be mixed with deionized water to prepare a 12% (w / w) dispersion for spraying. When using, dilute with water at a ratio of 1:300 (w / w).

[0065] Dilute with water at a ratio of 1:300 by weight before use.

[0066] test: Experiment 1: Sterilization effect test; Common pathogenic bacteria were selected: Escherichia coli, Staphylococcus aureus, and Candida albicans, and concentrations of 1×10⁻⁶ were prepared respectively. 6 CFU / mL bacterial suspension.

[0067] Take the powdered disinfectant from each of the embodiments and comparative examples, and dilute it with water according to the prescribed dilution ratio to obtain a disinfection solution.

[0068] Mix 1 mL of bacterial suspension with 9 mL of disinfectant solution, incubate at 25°C for 10 min, and then count colonies using the pour plate method to calculate the sterilization rate. Sterilization rate = (number of colonies in control group - number of colonies in experimental group) / number of colonies in control group × 100%.

[0069] Each experiment had 3 parallel samples, and the average value was taken as the final result.

[0070] The test results are as follows: Table 1 As can be seen from Table 1, the powder disinfectants of Examples 1-3 all showed excellent bactericidal effects against Escherichia coli, Staphylococcus aureus, and Candida albicans, with a bactericidal rate of over 99%, indicating that the technical solution of the present invention can effectively achieve broad-spectrum and efficient bactericidal effects.

[0071] Experiment 2: Disinfection persistence test; The surface of the ceramic tile was selected as the test carrier. The carrier was cut into small pieces of 5cm×5cm and sterilized before use.

[0072] Take the powdered disinfectant from each of the embodiments and comparative examples, and dilute it with water according to the prescribed dilution ratio to obtain a disinfection solution.

[0073] Apply the disinfectant solution evenly to the entire surface of the tile using a sterile cotton swab. After air drying, apply 1 mL of the 1×10⁻⁶ solution to the tile surface at 0h, 24h, 48h, and 72h. 6After incubating a CFU / mL Escherichia coli suspension for 10 minutes, samples were taken using the swabbing method to count the colonies and calculate the sterilization rate.

[0074] Each experiment had 3 parallel samples, and the average value was taken as the final result.

[0075] The test results are as follows: Table 2 As shown in Table 2, the powder disinfectants in Examples 1-3 maintained a high sterilization rate of over 98% within 72 hours, demonstrating good disinfection persistence. This is because the dual protective effect of the high-performance modified surfactant coating material B and the buffer coating layer D delayed the release and decomposition of the disinfectant components in the core material A, allowing the disinfection effect to last for a longer period of time.

[0076] Experiment 3: Stability Test; After sealing and packaging the powder disinfectants of each embodiment and comparative example, they were stored in a constant temperature and humidity chamber at 40°C and 75% relative humidity for 3 months.

[0077] The content of the active ingredients (total content of potassium persulfate, sodium percarbonate, and chlorine dioxide) of the disinfectant was measured before and after storage, and the retention rate of the active ingredients was calculated. Active ingredient retention rate = (active ingredient content after storage / active ingredient content before storage) × 100%.

[0078] Meanwhile, after storage, the samples were diluted with water according to their respective dilution ratios, and the bactericidal rate against Escherichia coli was tested to assess the impact of stability on the bactericidal effect.

[0079] Each experiment had 3 parallel samples, and the average value was taken as the final result.

[0080] The test results are as follows: Table 3 As shown in Table 3, after 3 months of storage under high temperature and high humidity conditions, the powder disinfectants of Examples 1-3 all maintained an effective component retention rate of over 95%, and the bactericidal rate against Escherichia coli remained above 99% after storage, indicating that the technical solution of the present invention can effectively improve the stability of the disinfectant. This is due to the dual protection of the high-performance modified surfactant coating material B and the buffer coating layer D, which reduces the contact between the effective components and the external environment and lowers their decomposition rate.

[0081] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A broad-spectrum, highly efficient, and long-lasting chloroxylic acid system disinfectant, characterized in that, It consists of core material A, high-performance modified surfactant coating material B, and buffer coating layer D; The core material A is prepared by mixing potassium persulfate, sodium percarbonate, chlorine dioxide, and sodium chloride in a mass ratio of 2-3:2-3:1-1.5:5-6. The high-performance modified surfactant coating material B is a coconut oil-alkyl glycoside-polyoxyethylene-polyoxypropylene block copolymer graft copolymer, and its mass accounts for 2-3% of the total mass of the core material A.

2. The broad-spectrum, highly efficient, and long-lasting solid disinfectant according to claim 1, characterized in that, The high-performance modified surfactant coating material B is dispersed in deionized water and prepared into a dispersion with a mass concentration of 10%. Then, it is coated onto the surface of the core material A through a two-fluid atomizing spray device to form a composite material C. The spraying pressure is 0.4-0.6 MPa, the atomized particle size is 50-100 μm, the rotation speed of the turntable stirring device is 35-45 r / min, the spraying time is 2-3 min, and the stirring is continued for 3-4 min. The coating thickness is 3-5 μm. The buffer coating layer D is prepared by mixing sodium citrate and boric acid at a mass ratio of 2-3:1 for 10-15 minutes. It is then sprayed at a rate of 5-10 mL / min onto the surface of the composite material C under stirring at 40-60 r / min for 15-20 minutes to form a coating layer with a thickness of 6-10 μm. Its mass accounts for 0.5-1% of the total mass of the core material A. The buffer coating layer D needs to be mixed with deionized water to prepare a dispersion with a mass fraction of 12-14% for spraying. The core material A is as follows: potassium persulfate, sodium percarbonate, chlorine dioxide, and sodium chloride are screened through a 100-120 mesh standard sieve. The material on the sieve is collected, vacuum dried, and then mixed for 15-20 minutes according to the mass ratio. It is then packaged for later use.

3. The broad-spectrum, highly efficient, and long-lasting solid disinfectant according to claim 2, characterized in that, The vacuum drying process involves vacuum drying at 25℃ and -0.08 to -0.09 MPa for 4-6 hours until the moisture content is below 0.5%.

4. The broad-spectrum, highly efficient, and long-lasting solid disinfectant according to claim 1, characterized in that, The high-performance modified surface-active coating material B is prepared by the following method: coconut oil-based alkyl glycosides and polyoxyethylene-polyoxypropylene block copolymers are mixed at a mass ratio of 3-5:

1. An initiator accounting for 0.8%-1.2% of the total mass of the mixture is added. The solid content of the system is adjusted to 30%-40% using deionized water. Under inert gas protection, a free radical polymerization reaction is carried out at 60-70℃ for 3-4 hours. After the reaction, γ-aminopropyltriethoxysilane accounting for 1%-2% of the mass of the mixture is added. The mixture is stirred at 80-100 r / min and crosslinked at 50-55℃ for 1-1.5 hours. The temperature is then adjusted to 35℃±2℃ to obtain the final product.

5. The broad-spectrum, highly efficient, and long-lasting solid disinfectant according to claim 4, characterized in that, The polyoxyethylene-polyoxypropylene block copolymer has a number average molecular weight of 2000-5000 and a polyoxyethylene segment content of 40%-60%.

6. The broad-spectrum, highly efficient, and long-lasting solid disinfectant according to claim 4, characterized in that, The initiator is ammonium persulfate.

7. The broad-spectrum, highly efficient, and long-lasting solid disinfectant according to claim 4, characterized in that, The inert gas is nitrogen.

8. The broad-spectrum, highly efficient, and long-lasting solid disinfectant according to claim 1, characterized in that, The solid disinfectant should be diluted with water at a mass ratio of 1:200-400 when used.

9. A method for preparing a broad-spectrum, highly efficient, and long-lasting solid disinfectant as described in any one of claims 1-8, characterized in that, Includes the following steps: Preparation of core material A: To be used; Preparation of high-performance modified surfactant coating material B: to be used; Preparation of composite material C: The above core material A is transported to a rotary evaporator and stirred at 35-45 r / min. The above high-performance modified surface active coating material B is sprayed into deionized water at a pressure of 0.4-0.6 MPa using a dual-fluid atomizing nozzle to prepare a dispersion with a mass concentration of 10-12% and an atomized particle size of 50-100 μm. After spraying for 2 min, stirring is continued for 3 min to form composite material C with a coating thickness of 3-8 μm. Preparation of buffer coating layer D: to be used; Preparation of finished product: The composite material C is put into a rotary stirrer and stirred at 40-60 r / min. At the same time, the buffer coating layer D is sprayed at a uniform rate of 5-10 mL / min. Stir for 15-20 min to form a coating layer with a thickness of 5-10 μm. After drying at 60℃ for 4 h, the finished product is obtained. The buffer coating layer D needs to be mixed with deionized water to prepare a dispersion with a mass fraction of 12-14% for spraying.

10. The preparation method according to claim 9, characterized in that, The atomizing nozzle has a gas-liquid ratio of 5-8:1.

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