Preparation method of degradable disinfection wet tissue

Abstract

The invention discloses a degradable disinfection wet tissue and a preparation method thereof, and the method comprises the following steps: dissolving PBST in a mixed solvent composed of dichloromethane and N, N-dimethylformamide according to a mass ratio of 7: 3 to prepare a spinning solution with PBST mass fraction of 5%-10%, then adding tetra-n-butylammonium chloride to make the mass ratio of PBST to tetra-n-butylammonium chloride be 4: 1-16: 1, and stirring to obtain a spinning solution; stirring until the mixture is completely dissolved to form a uniform and stable spinning solution; the spinning solution is subjected to spinning through a solution electrostatic spinning process, the spinning voltage is 20-30 kV, the solution supply speed is 0.5-1.5 mL / h, the spinning distance is fixed to be 15 cm, the rotating speed of a receiving roller is 90 r / min, the spinning environment temperature is 21 DEG C, and PBST superfine nanofiber non-woven fabric is obtained; and cutting the obtained PBST superfine nanofiber non-woven fabric into the size and shape required by the wet tissue, immersing the cut PBST superfine nanofiber non-woven fabric into a disinfectant, and then packaging the soaked PBST superfine nanofiber non-woven fabric. The disinfection wet tissue prepared by the method is environment-friendly, has high sterilization rate on various common germs, and is mild and non-irritant to skin.

Description

Technical Field

[0001] The present invention relates to the technical field of preparation of disinfectant wet wipes, and in particular to a method for preparing degradable disinfectant wet wipes. Background Art

[0002] As a convenient and quick-use cleaning product, wet wipes have become an indispensable part of daily life and medical care. Their development can be roughly divided into the following stages: The wet wipes concept began to take root in the Chinese market from the late 1980s to the early 1990s. However, due to their relatively high price, market demand was primarily concentrated in economically developed regions and among high-income individuals. Their use was also limited, primarily for emergency cleaning during travel or special occasions. With rising living standards and shifting consumer attitudes, people's demand for personal hygiene and cleanliness has gradually increased, and the wet wipes market has slowly taken off.

[0003] Entering the 21st century, the wet wipes industry entered a golden period of rapid development. On the one hand, a stable supply of raw materials and continuous advancements in production technology have gradually reduced the production cost of wet wipes, making them more affordable and further expanding the consumer base. On the other hand, consumers are increasingly concerned about hygiene and health, and wet wipes have become widely popular because they provide a more thorough cleansing effect than ordinary dry paper towels. The frequency of wet wipe use has increased significantly in the healthcare, maternity and baby, and travel sectors. According to market research firms, the size of China's wet wipes market has continued to expand at a double-digit annual rate over the past decade, and the product range has also become increasingly diverse, evolving from simple cleansing wipes to wipes with multiple functions such as disinfection, moisturization, and soothing, meeting the needs of different consumer groups.

[0004] However, traditional wet wipes technology also presents some significant challenges. For example, traditional wet wipes often use non-degradable raw materials, such as polyester, which are difficult to decompose in the natural environment and can easily contribute to "white pollution." Statistics show that the amount of waste generated globally each year from discarded wet wipes can take hundreds of years to fully degrade in landfills or the natural environment, posing a long-term potential threat to soil, water bodies, and ecosystems. Furthermore, traditional wet wipes struggle to strike the ideal balance between disinfection effectiveness and skin gentleness. To achieve a strong disinfecting effect, many wet wipes contain a large amount of chemicals, such as alcohol, fragrances, and preservatives. While these ingredients are effective in killing bacteria and viruses, they can also be irritating to the skin, leading to adverse reactions such as dryness and allergies. For those with sensitive skin, using these wipes can cause serious skin problems, such as contact dermatitis. These issues have limited the further development and application of traditional wet wipes.

[0005] In recent years, the industry has begun exploring and applying new technologies and materials to address the problems of traditional wet wipes. For example, some companies have begun using biodegradable materials, such as polylactic acid (PLA) fibers, to make wet wipe substrates. This material not only has good flexibility and water absorption, but also can be completely decomposed into carbon dioxide and water by microorganisms in the natural environment, without causing environmental pollution. In terms of the selection of disinfectant ingredients, researchers are also working hard to find more gentle and effective natural antimicrobial agents to replace traditional chemical disinfectants. For example, plant extract antimicrobial agents are gradually gaining attention. This type of antimicrobial agent generally has good biocompatibility and low skin irritation, while also providing a certain antibacterial effect. In addition, there have been some improvements and innovations in the production process of wet wipes, such as by optimizing the impregnation process of wet wipes to improve the uniform distribution of disinfectant, thereby reducing the use of chemical ingredients and reducing the risk of skin irritation while ensuring the disinfection effect.

[0006] However, these improvement measures still face some challenges in practical application. First, the cost of biodegradable materials is relatively high, which may lead to an increase in product prices, thereby affecting consumers' willingness to buy. Second, the antibacterial effect of natural antimicrobial agents is relatively weak, and further research and development of more efficient natural antimicrobial ingredients are needed to meet the disinfection requirements of wet wipes. Finally, during the production and use of wet wipes, how to ensure their stability and microbial safety during the shelf life is also one of the problems that need to be solved. Therefore, the future development of the wet wipes industry requires comprehensive consideration of multiple aspects such as material research and development, process innovation and cost control to achieve environmentally friendly, efficient and safe wet wipes products. Summary of the Invention

[0007] The present invention provides a method for preparing a degradable disinfectant wet wipe, so as to solve the technical problems that the existing disinfectant wet wipe is not environmentally friendly and cannot simultaneously meet the requirements of high sterilization rate against multiple common pathogens and mildness and non-irritation to the skin.

[0008] In order to solve the above technical problems, the present invention provides the following technical solutions:

[0009] The present invention provides a method for preparing a degradable disinfectant wet wipe, comprising:

[0010] The wet wipes are based on a poly (butylene terephthalate-co-succinate) (PBST) ultrafine nanofiber nonwoven fabric. The PBST ultrafine nanofiber nonwoven fabric is prepared as follows: PBST is dissolved in a mixed solvent consisting of dichloromethane and N,N-dimethylformamide in a mass ratio of 7:3 to prepare a spinning solution with a PBST mass fraction of 5% to 10%, tetra-n-butylammonium chloride is added to make the mass ratio of PBST to tetra-n-butylammonium chloride 4:1-16:1, and stirred until complete. The PBST ultrafine nanofiber non-woven fabric is obtained by completely dissolving the PBST into a uniform and stable spinning solution; the spinning solution is spun through a solution electrospinning process, with a spinning voltage of 20 kV to 30 kV, a liquid supply rate of 0.5 mL / h to 1.5 mL / h, a spinning distance fixed at 15 cm, a receiving roller speed of 90 r / min, and a spinning environment temperature of 21°C, thereby obtaining the PBST ultrafine nanofiber non-woven fabric; the obtained PBST ultrafine nanofiber non-woven fabric is cut into the size and shape required for the wet wipes, immersed in a disinfectant, and then packaged.

[0011] Furthermore, the PBST has a rigid aromatic ring structure and can be hydrolyzed into oligomers or monomers under the action of moisture and microorganisms, thereby achieving biodegradation;

[0012] The synthesis steps of the PBST are as follows: first, terephthalic acid, 1,4-butanediol, and succinic acid are precisely mixed according to a molar ratio of 1:(1.2-1.5):(0.8-1.2); the mixed ingredients are added to an esterification reaction kettle, and under nitrogen protection, the mixture is heated to 220°C-240°C at a heating rate of 5°C / min-10°C / min to carry out an esterification reaction. The esterification reaction time is 2 hours-4 hours, and the acid value at the end point of the esterification reaction is controlled to be 0.05 mgKOH / g-0.15 mgKOH / g;

[0013] After the esterification reaction is completed, the reaction material is transferred to a polycondensation reaction kettle and heated to 250°C-260°C at a heating rate of 10°C / min-15°C / min under a vacuum degree of -0.09MPa--0.1MPa for a polycondensation reaction. The polycondensation reaction time is 3h-5h. Small molecular by-products are continuously removed during the polycondensation reaction. The intrinsic viscosity at the reaction end point is controlled at 0.6dL / g-1.2dL / g;

[0014] The obtained PBST polymer melt is cut into particles by an underwater pelletizer to obtain PBST polymer particles.

[0015] Furthermore, the mixed solvent system of dichloromethane and N,N-dimethylformamide is composed of a mass ratio of 7:3, dichloromethane is used as the main solvent, the purity reaches more than 99.5%, the boiling point is 39.7 ° C, and the density is 1.3256 g / cm 3, can quickly dissolve PBST.

[0016] Furthermore, the amount of tetra-n-butylammonium chloride added is controlled to be 1 / 4-1 / 16 of the mass of PBST;

[0017] When adding tetra-n-butylammonium chloride, first slowly add the tetra-n-butylammonium chloride solid powder into the evenly stirred PBST / mixed solvent solution, control the stirring speed at 400 r / min-600 r / min, control the temperature at 25°C ± 2°C, and stir for 2 h-4 h to fully dissolve the tetra-n-butylammonium chloride and evenly disperse it in the spinning solution.

[0018] Furthermore, the spinning voltage is selected from a high-voltage DC power supply of 20kV-30kV, and the voltage stability is controlled within ±1%;

[0019] The liquid supply speed is precisely controlled by a peristaltic pump between 0.5mL / h and 1.5mL / h, and the stability of the liquid supply speed is controlled within ±2%;

[0020] The spinning distance is fixed at 15 cm, and the allowable error range is ±0.5 cm;

[0021] The receiving roller speed is set to 90r / min, and the speed fluctuation range is controlled within ±2r / min;

[0022] The spinning environment temperature is strictly controlled at 21℃±1℃.

[0023] Furthermore, the disinfectant formula contains the following components in mass percentage: 0.1%-1% of a quaternary ammonium antibacterial agent, wherein the quaternary ammonium antibacterial agent is alkylbenzalkonium chloride, the alkyl carbon chain length of which is C12-C18, and the ratio of C12, C14 and C18 is 1:1:3.

[0024] Furthermore, when the PBST ultrafine nanofiber non-woven fabric is immersed in disinfectant, a specific dipping process is adopted to ensure that the non-woven fabric can fully absorb the disinfectant, and the absorption amount is accurately controlled to 2-4 times the weight of the non-woven fabric;

[0025] The specific dipping process is as follows: first, the cut PBST ultrafine nanofiber nonwoven fabric is placed in the dipping tank, and the stacking thickness of the nonwoven fabric in the tank does not exceed 5 cm; then, the prepared disinfectant is slowly injected into the dipping tank through a metering pump at a flow rate of 0.5L / min-1.5L / min, and the ultrasonic device is turned on at the same time, the ultrasonic frequency is set to 20kHz-40kHz, the power is controlled at 100W-300W, and the ultrasonic treatment time is 10min-30min; during the ultrasonic treatment process, the temperature in the dipping tank is controlled at 25℃±2℃; when the amount of disinfectant injected reaches 2-4 times the weight of the nonwoven fabric, the injection is stopped and the ultrasonic treatment is continued for 5min-10min; next, the dipping tank is immersed in the disinfectant. The impregnated non-woven fabric is taken out of the impregnation tank and gently squeezed by the squeezing roller to squeeze out the excess disinfectant in the non-woven fabric, so that the liquid content of the non-woven fabric is accurately controlled between 2-4 times, the pressure of the squeezing roller is controlled at 0.1MPa-0.3MPa, and the squeezing speed is 1m / min-3m / min; the extruded non-woven fabric needs to be vacuum dried at a drying temperature of 30℃-50℃, a vacuum degree of -0.09MPa--0.1MPa, and a drying time of 1h-3h to remove excess moisture and solvent in the non-woven fabric; the humidity of the dried wet wipes is controlled at 70%-85%, and real-time monitoring and feedback control are carried out by a humidity sensor; finally, the dried wet wipes are flattened to make their surface flat and wrinkle-free.

[0026] Furthermore, the wet wipes must undergo flatness correction before packaging, and a hot roller pressing device is used to adjust the flatness of the wet wipes. The hot roller temperature is controlled at 40°C-60°C, the pressure is 0.05MPa-0.15MPa, and the rolling speed is 5m / min-10m / min; microbial limit testing is carried out in accordance with relevant standards to ensure that the total number of bacterial colonies per gram of wet wipes does not exceed 200CFU, the total number of molds and yeasts does not exceed 100CFU, and coliform bacteria, Staphylococcus aureus and Pseudomonas aeruginosa shall not be detected.

[0027] Furthermore, the packaging material of the wet wipes is a degradable composite film with good air permeability and sealing properties;

[0028] The composite film is formed by compounding an inner layer of polylactic acid film and an outer layer of modified PBST film through a three-layer co-extrusion process.

[0029] Furthermore, after use, the wet wipes can be completely biodegraded under the action of microorganisms in the soil, water or compost conditions in the natural environment, and eventually decomposed into harmless substances such as carbon dioxide, water and inorganic salts.

[0030] The beneficial effects brought about by the technical solution provided by the present invention include at least:

[0031] The disinfectant wipes of the present invention are made of PBST ultrafine nanofiber non-woven fabric, which has excellent biodegradability and can be completely degraded into harmless substances under soil, water or compost conditions in the natural environment, effectively solving the "white pollution" problem caused by traditional wet wipes and being environmentally friendly.

[0032] The preparation process of the disinfectant wipes of the present invention precisely controls the preparation of the PBST solution, electrospinning parameters, and the composition and absorption amount of the disinfectant, ensuring that the wipes not only have excellent physical properties, such as appropriate thickness, strength, and air permeability, but also have excellent disinfection effects, a high sterilization rate against a variety of common pathogens, and are mild and non-irritating to the skin.

[0033] The disinfectant wipes of the present invention undergo strict processes such as flatness correction, microbial limit detection, disinfection effect verification and stability testing before packaging, which ensures the stability and reliability of product quality, meets the disinfection needs of different scenarios such as medical, household and personal care, and has significant social benefits and market application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0035] Figure 1 The present invention provides a flow chart of a method for preparing degradable disinfectant wipes. DETAILED DESCRIPTION

[0036] To make the objectives, technical solutions and advantages of the present invention more clear, the embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.

[0037] This embodiment provides a method for preparing a biodegradable disinfectant wipe. Figure 1 The flowchart of the preparation method of the degradable disinfectant wipes provided by an embodiment of the present invention is shown.

[0038] The wet wipes use poly (butylene terephthalate-co-succinate) (PBST) ultrafine nanofiber non-woven fabric as a base material. The preparation steps of the PBST ultrafine nanofiber non-woven fabric are as follows: dissolving PBST in a mixed solvent consisting of dichloromethane and N,N-dimethylformamide in a mass ratio of 7:3 to prepare a spinning solution with a PBST mass fraction of 5%-10%, then adding tetra-n-butylammonium chloride to make the mass ratio of PBST to tetra-n-butylammonium chloride 4:1-16:1, stirring until the PBST is completely dissolved to form a uniform and stable spinning solution; passing the spinning solution through a solution static filtration. The electrospinning process is used for spinning, with a spinning voltage of 20kV-30kV, a liquid supply rate of 0.5mL / h-1.5mL / h, a spinning distance fixed at 15cm, a receiving roller speed of 90r / min, and a spinning environment temperature of 21°C to obtain a PBST ultrafine nanofiber non-woven fabric; the obtained PBST ultrafine nanofiber non-woven fabric is cut into the size and shape required for wet wipes; and the cut PBST ultrafine nanofiber non-woven fabric is immersed in a disinfectant to allow the non-woven fabric to fully absorb the disinfectant, the absorption amount being 2-4 times the weight of the non-woven fabric, and then packaged.

[0039] Specifically, the PBST has a rigid aromatic ring structure, good thermal stability, mechanical properties and processability, and can be hydrolyzed into oligomers or monomers under the action of moisture and microorganisms to achieve biodegradation.

[0040] During the synthesis process of PBST, the purity of the raw monomer is controlled at above 99%, the polymerization reaction temperature is set at 220°C-260°C, the reaction time is 4h-8h, and the vacuum degree is maintained at -0.09MPa--0.1MPa. After esterification, polycondensation and other reaction steps, PBST polymer particles that meet the requirements are obtained.

[0041] Specifically:

[0042] First, terephthalic acid, 1,4-butanediol, and succinic acid are precisely mixed in a molar ratio of 1:(1.2-1.5):(0.8-1.2). These ingredients are added to an esterification reactor. Under nitrogen, the reaction is heated to 220-240°C at a heating rate of 5-10°C / min. The esterification reaction lasts 2-4 hours, and the acid value at the end of the esterification reaction is controlled between 0.05mgKOH / g and 0.15mgKOH / g. After the esterification reaction is completed, the reaction materials are transferred to a polycondensation reactor and heated to 250°C-260°C at a heating rate of 10°C / min-15°C / min under a vacuum degree of -0.09MPa--0.1MPa for a polycondensation reaction. The polycondensation reaction time is 3h-5h. Small molecule by-products are continuously removed during the polycondensation reaction, and the intrinsic viscosity at the end of the reaction is controlled at 0.6dL / g-1.2dL / g. Finally, the obtained PBST polymer melt is cut into granules by an underwater pelletizer to obtain PBST polymer particles. The drying loss of the particles is controlled within 0.3%, the ash content is controlled within 0.1%, the melting point is 100°C-120°C, the glass transition temperature is 40°C-60°C, and the density is 1.2g / cm 3 -1.35g / cm 3 Its mechanical properties are tensile strength 30MPa-50MPa and elongation at break 300%-500%.

[0043] Precise control of these parameters ensures the spinnability and stability of the PBST polymer during the spinning process, as well as the physical properties and biodegradability of the final wet wipe substrate. Furthermore, during the synthesis of PBST, reaction conditions are strictly controlled to avoid the introduction of chemicals harmful to the human body, thus ensuring the biocompatibility and safety of the wet wipe substrate.

[0044] Specifically, a mixed solvent system consisting of dichloromethane and N,N-dimethylformamide in a mass ratio of 7:3 can effectively improve the dissolution effect and spinning performance of PBST.

[0045] Dichloromethane is used as the main solvent, with a purity of more than 99.5%, a boiling point of 39.7°C, and a density of 1.3256 g / cm 3 , has good solubility, dissolves PBST quickly and has good dissolution effect. The purity of N,N-dimethylformamide also reaches more than 99.5%, the boiling point is 153℃, and the density is 0.944g / cm 3 , which has a high dielectric constant of 36.7, and can improve the conductivity and charge density of the spinning solution in the electric field.

[0046] To prepare the spinning solution, first add PBST polymer particles to dichloromethane. Stir at a speed of 300-500 rpm and a temperature of 25°C ± 2°C for 0.5-1 hour to initially dissolve the PBST in the dichloromethane. Then, add N,N-dimethylformamide and continue stirring for 1-2 hours to completely dissolve the PBST, forming a uniform, transparent spinning solution. Throughout the dissolution process, strictly control the stirring speed and temperature to avoid localized overheating of the solution, the formation of bubbles, and degradation of the PBST molecular chains due to excessive stirring speed or high temperature.

[0047] To ensure the uniformity of the solution, the solution is turned upside down and stirred every 15-30 minutes during the stirring process to ensure that the PBST is fully dispersed and dissolved in the mixed solvent. The container used for dissolution is made of corrosion-resistant glass, and the container is strictly cleaned and dried before dissolution to ensure that there is no interference from impurities and moisture. The dissolved spinning solution needs to be filtered through a 10μm-20μm filter to remove tiny particle impurities in the solution to prevent clogging of the nozzle during the spinning process, ensuring the continuity of spinning and the quality of the fiber. The PBST spinning solution prepared by the above steps has suitable viscosity and fluidity. Its viscosity is controlled at 15mPa·s-40mPa·s, the surface tension is controlled at 25mN / m-35mN / m, and the conductivity is controlled at 10μS / cm-100μS / cm, which can meet the process requirements of electrospinning.

[0048] Specifically, the added tetra-n-butylammonium chloride is a quaternary ammonium organic salt, and its function in the spinning solution is mainly reflected in that it can significantly increase the conductivity of the polymer spinning solution.

[0049] Tetra-n-butylammonium chloride has a purity exceeding 95%, exhibits excellent solubility in dichloromethane and N,N-dimethylformamide, and exhibits no precipitation. The addition amount is precisely controlled to be 1 / 4-1 / 16 of the mass of PBST. When adding tetra-n-butylammonium chloride, the solid powder is slowly added to the well-stirred PBST / mixed solvent solution at a stirring speed of 400-600 rpm and a temperature of 25°C ± 2°C for 2-4 hours to ensure that the tetra-n-butylammonium chloride is fully dissolved and evenly dispersed in the spinning solution. During this process, the addition of tetra-n-butylammonium chloride disrupts the stable charge distribution in the spinning solution, increasing the number of free charges in the solution and significantly improving the conductivity of the spinning solution.

[0050] As the amount of tetra-n-butylammonium chloride added increases, the conductivity of the spinning solution first increases rapidly. When the amount of tetra-n-butylammonium chloride added reaches 1 / 4 of the mass of PBST, the conductivity can be increased to 3-5 times that of the solution without tetra-n-butylammonium chloride added.

[0051] Further increasing the amount of tetra-n-butylammonium chloride added, the conductivity will still increase, but the increase will gradually decrease.

[0052] At the same time, the average diameter of the nanofibers first decreases rapidly with the increase in the amount of tetrabutylammonium chloride added, and then gradually stabilizes. When the amount of tetrabutylammonium chloride added is 1 / 4 of the mass of PBST, the average fiber diameter can be reduced to 1 / 3-1 / 2 of the value when no tetrabutylammonium chloride is added.

[0053] In addition, the addition of tetra-n-butylammonium chloride can also improve the rheological properties of the spinning solution, reduce the viscoelasticity of the solution, make the jet of the solution more stable during the spinning process, reduce the occurrence of fiber breakage and capillary action, and thus improve the quality and continuity of the fiber.

[0054] By precisely controlling the amount of tetra-n-butylammonium chloride added, the conductivity and rheological properties of the spinning solution can be effectively adjusted, thereby achieving precise control of the diameter and morphology of PBST nanofibers.

[0055] Specifically, the solution electrospinning process parameters have an important influence on the morphology and properties of PBST nanofibers. The specific parameters are as follows:

[0056] The spinning voltage is a 20kV-30kV high-voltage DC power supply, with voltage stability controlled within ±1%. The liquid supply rate is precisely controlled by a peristaltic pump between 0.5mL / h and 1.5mL / h, with a stability within ±2%.

[0057] The spinning distance is fixed at 15 cm, with an allowable error of ±0.5 cm. The receiving roller speed is set at 90 rpm, with a speed fluctuation range of ±2 rpm. The spinning environment temperature is strictly controlled at 21°C ±1°C.

[0058] By precisely controlling the above electrospinning process parameters, ultrafine PBST nanofiber nonwoven fabrics that meet the requirements of wet wipes substrates can be prepared.

[0059] The average fiber diameter can reach 65nm-223.2nm, the standard deviation of the fiber diameter is controlled within 15nm-30nm, and the distribution uniformity between the fibers reaches more than 90%.

[0060] The thickness of the non-woven fabric is controlled at 0.1mm-0.3mm, the breaking strength in the longitudinal and transverse directions reaches 10N / 5cm and 8N / 5cm respectively, and the elongation in the longitudinal and transverse directions reaches 300% and 250% respectively. The air permeability is controlled at 500mm / s-1500mm / s, and the moisture permeability is controlled at 3000g / m 2 24h-8000g / m 224h, weight controlled at 30g / m 2 -80g / m 2 .

[0061] Specifically, the disinfectant formula contains the following components in mass percentage: 0.1%-1% of a quaternary ammonium antibacterial agent, wherein the quaternary ammonium antibacterial agent is alkylbenzalkonium chloride, whose alkyl carbon chain length is C12-C18, and the ratio of C12, C14 and C18 is 1:1:3, and 0.5%-2% of a plant extract.

[0062] The plant extract is a golden grass extract, and its preparation method is as follows: weigh a crushed golden grass sample, decoct it with 7-8 times the amount of purified water for 3 hours, filter it, concentrate it under reduced pressure to a relative density of 1.15-1.2 at room temperature, and extract it with ethyl acetate to obtain the golden grass extract.

[0063] 0.05%-0.15% organic acid buffer, a mixture of citric acid and potassium dihydrogen phosphate in a mass ratio of 3:1-5:1. The balance is deionized water. The order of adding the components to the deionized water is as follows: first add the alkylbenzalkonium chloride to the deionized water, stirring at a speed of 300-500 rpm and a temperature of 25°C ± 2°C, and stir until completely dissolved.

[0064] Then add the golden grass extract and continue stirring for 1-2 hours to evenly disperse the golden grass extract in the solution. Finally, slowly add the mixture of citric acid and potassium dihydrogen phosphate while stirring to adjust the pH value of the solution to 5.0-6.5, and stir for 0.5-1 hour to fully mix the components.

[0065] Throughout the preparation process, the amount and order of each component are strictly controlled to ensure the uniformity and stability of the disinfectant. Furthermore, the prepared disinfectant must be filtered through a 0.22μm filter membrane to remove tiny particles and microorganisms in the solution, ensuring clarity and sterility.

[0066] Specifically, when PBST ultrafine nanofiber non-woven fabric is immersed in disinfectant, a specific dipping process is used to ensure that the non-woven fabric can fully absorb the disinfectant, and the absorption amount is precisely controlled to be 2-4 times the weight of the non-woven fabric. The specific dipping process is as follows:

[0067] First, the cut PBST ultrafine nanofiber nonwoven fabric is placed in an immersion tank, and the stacking thickness of the nonwoven fabric in the tank does not exceed 5 cm.

[0068] Then, the prepared disinfectant is slowly injected into the immersion tank through a metering pump at a flow rate of 0.5L / min-1.5L / min. At the same time, the ultrasonic device is turned on, the ultrasonic frequency is set to 20kHz-40kHz, the power is controlled at 100W-300W, and the ultrasonic treatment time is 10min-30min.

[0069] During the ultrasonic treatment, the temperature in the immersion tank was controlled at 25°C ± 2°C. When the amount of disinfectant injected reached 2-4 times the weight of the non-woven fabric, the injection was stopped and the ultrasonic treatment was continued for 5-10 minutes.

[0070] Next, the impregnated non-woven fabric is removed from the impregnation tank and gently squeezed through a squeeze roller to squeeze out excess disinfectant from the non-woven fabric. The liquid content of the non-woven fabric is precisely controlled between 2-4 times. The pressure of the squeeze roller is controlled at 0.1MPa-0.3MPa, and the squeezing speed is 1m / min-3m / min. The extruded non-woven fabric is then vacuum dried at a temperature of 30℃-50℃, a vacuum degree of -0.09MPa--0.1MPa, and a drying time of 1h-3h to remove excess moisture and solvent from the non-woven fabric, preventing dripping and microbial growth after the wipes are packaged.

[0071] The humidity of the dried wipes is controlled at 70%-85%, and real-time monitoring and feedback control are carried out through humidity sensors.

[0072] Finally, smooth the dried wipes to make their surface smooth and wrinkle-free.

[0073] Specifically, the wet wipes need to undergo flatness correction before packaging, and a hot roller pressing device is used to adjust the flatness of the wet wipes. The hot roller temperature is controlled at 40°C-60°C, the pressure is 0.05MPa-0.15MPa, and the roller pressing speed is 5m / min-10m / min.

[0074] Microbial limit testing is carried out in accordance with relevant standards to ensure that the total bacterial colony count in each gram of wet wipes does not exceed 200 CFU, the total number of molds and yeasts does not exceed 100 CFU, and coliform bacteria, Staphylococcus aureus and Pseudomonas aeruginosa shall not be detected.

[0075] The disinfection effect is verified by using a quantitative sterilization test method to ensure that the sterilization rate of the wet wipes against Staphylococcus aureus, Escherichia coli and Candida albicans reaches more than 99.9%, and the action time does not exceed 5 minutes.

[0076] The skin irritation test is carried out in accordance with the skin irritation test method in the "Technical Specifications for Safety of Cosmetics" to ensure that the skin irritation score of the wipes is less than 1.0.

[0077] The stability test places the packaged wet wipes in a constant temperature box at 40℃±2℃ for 30 days for accelerated aging. The wipes are taken out regularly to test their disinfection effect, microbial limits and physical properties to ensure that the performance indicators of the wet wipes meet the requirements within the shelf life.

[0078] Specifically, the packaging material of the wet wipes is a degradable composite film with good air permeability and sealing properties.

[0079] The composite film is made of an inner layer of polylactic acid film and an outer layer of modified PBST film through a three-layer co-extrusion process. The inner layer of polylactic acid film is in direct contact with the wet wipes and has a thickness of 10μm-20μm. The thickness of the outer layer of modified PBST film is 30μm-50μm. The modification method is to add 5%-10% by mass of nano-titanium dioxide and 2%-5% of bamboo fiber powder to PBST, and make it through a melt blending extrusion process.

[0080] The middle layer is the bonding layer, which uses 1%-3% maleic anhydride grafted polypropylene as the bonding agent. The inner and outer layers are composited together through the melt extrusion coating process. The thickness of the bonding layer is controlled at 5μm-10μm. The air permeability of the composite film is controlled at 500g / m 2 24h-1500g / m 2 24h, moisture permeability controlled at 3000g / m 2 24h-8000g / m 2 ·24h, oxygen transmission rate is controlled at 50cm 3 / m 2 24h-200cm 3 / m 2 ·24h, water vapor transmission rate is controlled at 500g / m 2 24h-1500g / m 2 ·24h.

[0081] The composite film's rubbing resistance reaches above level 5, its puncture resistance exceeds 10N, its tensile strength exceeds 15MPa in the longitudinal direction and 12MPa in the transverse direction, and its elongation at break exceeds 300% in the longitudinal direction and 250% in the transverse direction. During the packaging process, a combination of continuous and intermittent heat sealing is used, with a controlled temperature of 120°C to 150°C, a pressure of 0.2MPa to 0.5MPa, and a sealing time of 0.5s to 2s.

[0082] Specifically, after use, the wet wipes can be completely biodegraded under the action of microorganisms in the soil, water or compost conditions of the natural environment, and eventually decomposed into harmless substances such as carbon dioxide, water and inorganic salts.

[0083] In the soil environment, PBST ultrafine nanofiber nonwovens undergo hydrolysis under the combined action of microorganisms, water, and oxygen, generating small molecular oligomers and monomers. These small molecules can be metabolized and degraded by soil microorganisms. In the water environment, PBST fibers undergo hydrolysis under the action of hydrolytic enzymes, and microorganisms in the water can also accelerate its degradation process.

[0084] Under composting conditions, PBST fibers can be rapidly decomposed by microorganisms in the compost in a high-temperature, high-humidity, and oxygen-rich environment. Ingredients in disinfectants, such as quaternary ammonium salt antimicrobials, plant extracts, and organic acid buffers, can also be decomposed or converted into harmless substances by microorganisms in the natural environment.

[0085] The polylactic acid and modified PBST film in the packaging material are also completely biodegradable.

[0086] Furthermore, it should be noted that the present invention may be provided as a method, apparatus, or computer program product. Thus, embodiments of the present invention may take the form of entirely hardware embodiments, entirely software embodiments, or embodiments combining software and hardware aspects. Furthermore, embodiments of the present invention may take the form of a computer program product embodied on one or more computer-usable storage media containing computer-usable program code.

[0087] The embodiments of the present invention are described with reference to the flowcharts and / or block diagrams of the methods, terminal devices (systems), and computer program products according to the embodiments of the present invention. It should be understood that each process and / or block in the flowchart and / or block diagram, as well as the combination of the processes and / or blocks in the flowchart and / or block diagram, can be implemented by computer program instructions. These computer program instructions can be provided to a processor of a general-purpose computer, an embedded processor, or other programmable data processing terminal device to generate a machine, so that the instructions executed by the processor of the computer or other programmable data processing terminal device generate instructions for implementing the process in the flowchart and / or block diagram. Figure 1 a process or multiple processes and / or boxes Figure 1 A device that provides the functions specified in a block or multiple blocks.

[0088] These computer program instructions may also be stored in a computer readable memory that can direct a computer or other programmable data processing terminal device to operate in a specific manner, so that the instructions stored in the computer readable memory produce a manufactured product including an instruction device, which implements the process Figure 1 a process or multiple processes and / or boxes Figure 1These computer program instructions can also be loaded onto a computer or other programmable data processing terminal device, so that a series of operation steps are executed on the computer or other programmable terminal device to produce a computer-implemented process, thereby providing instructions for implementing the process in the process. Figure 1 a process or multiple processes and / or boxes Figure 1 A step that specifies a function in one or more boxes.

[0089] It should also be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. The terms "comprises," "includes," or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article, or terminal device that includes a series of elements includes not only those elements, but also other elements not explicitly listed, or elements inherent to such process, method, article, or terminal device. In the absence of further restrictions, an element defined by the phrase "comprises a ..." does not exclude the presence of additional identical elements in the process, method, article, or terminal device that includes the element.

[0090] Finally, it should be noted that the above is a preferred embodiment of the present invention. It should be noted that although the preferred embodiment of the present invention has been described, it is clear that those skilled in the art, once they understand the basic inventive concept of the present invention, can make various improvements and modifications without departing from the principles of the present invention. Such improvements and modifications should also be considered as within the scope of protection of the present invention. Therefore, the appended claims are intended to be interpreted as including the preferred embodiment and all changes and modifications that fall within the scope of the embodiments of the present invention.

Claims

1. A method for preparing a degradable disinfectant wet wipe, characterized in that: include: The wet wipes are based on a poly (butylene terephthalate-co-succinate) (PBST) ultrafine nanofiber nonwoven fabric. The PBST ultrafine nanofiber nonwoven fabric is prepared as follows: PBST is dissolved in a mixed solvent consisting of dichloromethane and N,N-dimethylformamide in a mass ratio of 7:3 to prepare a spinning solution with a PBST mass fraction of 5% to 10%, tetra-n-butylammonium chloride is added to make the mass ratio of PBST to tetra-n-butylammonium chloride 4:1-16:1, and stirred until complete. The PBST ultrafine nanofiber non-woven fabric is obtained by completely dissolving the PBST into a uniform and stable spinning solution; the spinning solution is spun through a solution electrospinning process, with a spinning voltage of 20 kV to 30 kV, a liquid supply rate of 0.5 mL / h to 1.5 mL / h, a spinning distance fixed at 15 cm, a receiving roller speed of 90 r / min, and a spinning environment temperature of 21°C, thereby obtaining the PBST ultrafine nanofiber non-woven fabric; the obtained PBST ultrafine nanofiber non-woven fabric is cut into the size and shape required for the wet wipes, immersed in a disinfectant, and then packaged.

2. The method for preparing a degradable disinfectant wet wipe according to claim 1, wherein: The PBST has a rigid aromatic ring structure and can be hydrolyzed into oligomers or monomers under the action of moisture and microorganisms to achieve biodegradation; During the synthesis of PBST, the purity of the raw monomer is controlled at above 99%, the polymerization reaction temperature is set at 220° C.-260° C., the reaction time is 4 h-8 h, and the vacuum degree is maintained at -0.09 MPa--0.1 MPa. After esterification, polycondensation and other reaction steps, PBST polymer particles that meet the requirements are obtained; The synthesis steps of the PBST are as follows: first, terephthalic acid, 1,4-butanediol, and succinic acid are precisely mixed according to a molar ratio of 1:(1.2-1.5):(0.8-1.2); the mixed ingredients are added to an esterification reaction kettle, and under nitrogen protection, the mixture is heated to 220°C-240°C at a heating rate of 5°C / min-10°C / min to carry out an esterification reaction. The esterification reaction time is 2 hours-4 hours, and the acid value at the end point of the esterification reaction is controlled to be 0.05 mgKOH / g-0.15 mgKOH / g; After the esterification reaction is completed, the reaction material is transferred to a polycondensation reaction kettle and heated to 250°C-260°C at a heating rate of 10°C / min-15°C / min under a vacuum degree of -0.09MPa--0.1MPa for a polycondensation reaction. The polycondensation reaction time is 3h-5h. Small molecular by-products are continuously removed during the polycondensation reaction. The intrinsic viscosity at the reaction end point is controlled at 0.6dL / g-1.2dL / g; The obtained PBST polymer melt is cut into granules by an underwater pelletizer to obtain PBST polymer particles. The drying loss of the particles is controlled within 0.3%, the ash content is controlled within 0.1%, the melting point is 100°C-120°C, the glass transition temperature is 40°C-60°C, and the density is 1.2g / cm 3 -1.35g / cm 3 Its mechanical properties are tensile strength 30MPa-50MPa and elongation at break 300%-500%.

3. The method for preparing a degradable disinfectant wet wipe according to claim 1, wherein: The mixed solvent system of dichloromethane and N,N-dimethylformamide is composed of a mass ratio of 7:3, and dichloromethane is used as the main solvent, with a purity of more than 99.5%, a boiling point of 39.7°C, and a density of 1.3256 g / cm 3 , can quickly dissolve PBST; When preparing the spinning solution, first add PBST polymer particles into dichloromethane, control the stirring speed at 300r / min-500r / min, control the temperature at 25℃±2℃, and stir for 0.5h-1h to allow the PBST to initially dissolve in dichloromethane; Then add N,N-dimethylformamide and continue stirring for 1-2 hours to completely dissolve PBST and form a uniform and transparent spinning solution; During the entire dissolution process, strictly control the stirring speed and temperature to avoid local overheating of the solution, bubble generation, and degradation of the PBST molecular chain due to excessive stirring speed or high temperature. To ensure the uniformity of the solution, turn the solution upside down every 15-30 minutes during the stirring process to ensure that PBST is fully dispersed and dissolved in the mixed solvent. The container used for dissolution is made of corrosion-resistant glass, and is strictly cleaned and dried before dissolution to ensure that there is no interference from impurities and moisture; The dissolved spinning solution is filtered through a 10μm-20μm filter to remove tiny particles of impurities in the solution, prevent the nozzle from being blocked during the spinning process, and ensure the continuity of spinning and the quality of the fiber; The obtained PBST spinning solution has suitable viscosity and fluidity. Its viscosity is controlled at 15mPa·s-40mPa·s, its surface tension is controlled at 25mN / m-35mN / m, and its conductivity is controlled at 10μS / cm-100μS / cm, which can meet the process requirements of electrospinning.

4. The method for preparing a degradable disinfectant wet wipe according to claim 1, wherein: The amount of tetra-n-butylammonium chloride added is controlled to be 1 / 4-1 / 16 of the mass of PBST; When adding tetra-n-butylammonium chloride, first slowly add the tetra-n-butylammonium chloride solid powder into the evenly stirred PBST / mixed solvent solution, control the stirring speed at 400 r / min-600 r / min, control the temperature at 25°C ± 2°C, and stir for 2 h-4 h to fully dissolve the tetra-n-butylammonium chloride and evenly disperse it in the spinning solution.

5. The method for preparing a degradable disinfectant wet wipe according to claim 1, wherein: The spinning voltage is a high-voltage DC power supply of 20kV-30kV, and the voltage stability is controlled within ±1%; The liquid supply speed is precisely controlled by a peristaltic pump between 0.5mL / h and 1.5mL / h, and the stability of the liquid supply speed is controlled within ±2%; The spinning distance is fixed at 15 cm, and the allowable error range is ±0.5 cm; The receiving roller speed is set to 90r / min, and the speed fluctuation range is controlled within ±2r / min; The spinning environment temperature is strictly controlled at 21℃±1℃; By controlling the above-mentioned electrospinning process parameters, an ultrafine PBST nanofiber non-woven fabric that meets the requirements of wet wipes substrate is prepared. The average fiber diameter is 65nm-223.2nm, the standard deviation of the fiber diameter is controlled at 15nm-30nm, the distribution uniformity between the fibers reaches more than 90%, the thickness of the non-woven fabric is controlled at 0.1mm-0.3mm, the breaking strength in the longitudinal and transverse directions reaches more than 10N / 5cm and 8N / 5cm respectively, the elongation in the longitudinal and transverse directions reaches more than 300% and 250% respectively, the air permeability is controlled at 500mm / s-1500mm / s, and the moisture permeability is controlled at 3000g / m 2 24h-8000g / m 2 24h, weight controlled at 30g / m 2 -80g / m 2 .

6. The method for preparing a degradable disinfectant wet wipe according to claim 1, wherein: The disinfectant formula comprises the following components in percentage by mass: 0.1%-1% of a quaternary ammonium antibacterial agent, wherein the quaternary ammonium antibacterial agent is an alkylbenzalkonium chloride, the alkyl carbon chain length of which is C12-C18, and the ratio of C12, C14 and C18 is 1:1:3; The plant extract is 0.5%-2%, and the plant extract is a golden grass extract. The preparation method is as follows: weighing a crushed golden grass sample, decocting it with 7-8 times the amount of purified water for 3 hours, filtering, concentrating under reduced pressure to a relative density of 1.15-1.2 at room temperature, extracting with ethyl acetate to obtain the golden grass extract, and an organic acid buffer of 0.05%-0.15%, wherein the organic acid buffer is a mixture of citric acid and potassium dihydrogen phosphate in a mass ratio of 3:1-5:1, and the balance is deionized water. The components are The order of addition to the deionized water is as follows: first add alkylbenzalkonium chloride to deionized water, control the stirring speed at 300r / min-500r / min, control the temperature at 25℃±2℃, stir until completely dissolved, then add the golden grass extract, continue stirring for 1h-2h, so that the golden grass extract is evenly dispersed in the solution, and finally slowly add the mixture of citric acid and potassium dihydrogen phosphate while stirring, adjust the pH value of the solution to 5.0-6.5, and stir for 0.5h-1h to fully mix the components; The prepared disinfectant solution needs to be filtered through a 0.22μm filter membrane to remove tiny particulate impurities and microorganisms in the solution to ensure the clarity and sterility of the disinfectant solution.

7. The method for preparing a degradable disinfectant wet wipe according to claim 1, wherein: When the PBST ultrafine nanofiber non-woven fabric is immersed in the disinfectant, a specific dipping process is adopted to ensure that the non-woven fabric can fully absorb the disinfectant, and the absorption amount is accurately controlled to 2-4 times the weight of the non-woven fabric; The specific dipping process is as follows: first, the cut PBST ultrafine nanofiber nonwoven fabric is placed in the dipping tank, and the stacking thickness of the nonwoven fabric in the tank does not exceed 5 cm; then, the prepared disinfectant is slowly injected into the dipping tank through a metering pump at a flow rate of 0.5L / min-1.5L / min, and the ultrasonic device is turned on at the same time, the ultrasonic frequency is set to 20kHz-40kHz, the power is controlled at 100W-300W, and the ultrasonic treatment time is 10min-30min; during the ultrasonic treatment process, the temperature in the dipping tank is controlled at 25℃±2℃; when the amount of disinfectant injected reaches 2-4 times the weight of the nonwoven fabric, the injection is stopped and the ultrasonic treatment is continued for 5min-10min; next, the dipping tank is immersed in the disinfectant. The impregnated non-woven fabric is taken out of the impregnation tank and gently squeezed by the squeezing roller to squeeze out the excess disinfectant in the non-woven fabric, so that the liquid content of the non-woven fabric is accurately controlled between 2-4 times, the pressure of the squeezing roller is controlled at 0.1MPa-0.3MPa, and the squeezing speed is 1m / min-3m / min; the extruded non-woven fabric needs to be vacuum dried at a drying temperature of 30℃-50℃, a vacuum degree of -0.09MPa--0.1MPa, and a drying time of 1h-3h to remove excess moisture and solvent in the non-woven fabric; the humidity of the dried wet wipes is controlled at 70%-85%, and real-time monitoring and feedback control are carried out by a humidity sensor; finally, the dried wet wipes are flattened to make their surface flat and wrinkle-free.

8. The method for preparing a degradable disinfectant wet wipe according to claim 1, wherein: The wet wipes are also required to undergo flatness correction before packaging, and a hot roller pressing device is used to adjust the flatness of the wet wipes. The hot roller temperature is controlled at 40°C-60°C, the pressure is 0.05MPa-0.15MPa, and the rolling speed is 5m / min-10m / min; the microbial limit test is carried out in accordance with relevant standards to ensure that the total bacterial colony count per gram of wet wipes does not exceed 200CFU, the total mold and yeast count does not exceed 100CFU, and coliform bacteria, Staphylococcus aureus and Pseudomonas aeruginosa are not detected; The disinfection effect is verified by using a quantitative bactericidal test method to ensure that the bactericidal rate of the wipes against Staphylococcus aureus, Escherichia coli and Candida albicans reaches more than 99.9%, and the action time does not exceed 5 minutes; The stability test places the packaged wet wipes in a constant temperature box at 40℃±2℃ for 30 days for accelerated aging. The wipes are taken out regularly to test their disinfection effect, microbial limits and physical properties to ensure that the performance indicators of the wet wipes meet the requirements within the shelf life.

9. The method for preparing a degradable disinfectant wet wipe according to claim 1, wherein: The packaging material of the wet wipes is a degradable composite film with good air permeability and sealing properties; The composite film is made of an inner layer of polylactic acid film and an outer layer of modified PBST film through a three-layer co-extrusion process. The inner polylactic acid film is in direct contact with the wet wipes and has a thickness of 10-20 μm. The outer modified PBST film has a thickness of 30-50 μm. The modification method is to add 5%-10% by mass of nano-titanium dioxide and 2%-5% of bamboo fiber powder to PBST, and then produce the modified film through melt blending and extrusion process. The middle layer is the bonding layer, which uses 1%-3% maleic anhydride grafted polypropylene as the bonding agent. The inner and outer layers are composited together through the melt extrusion coating process. The thickness of the bonding layer is controlled at 5μm-10μm; the air permeability of the composite film is controlled at 500g / m 2 24h-1500g / m 2 24h, moisture permeability controlled at 3000g / m 2 24h-8000g / m 2 ·24h, oxygen transmission rate is controlled at 50cm 3 / m 2 24h-200cm 3 / m 2 ·24h, water vapor transmission rate is controlled at 500g / m 2 24h-1500g / m 2 24 hours; The composite film has a rubbing resistance of more than level 5, a puncture resistance of more than 10N, a tensile strength of more than 15MPa in the longitudinal direction and more than 12MPa in the transverse direction, and an elongation at break of more than 300% in the longitudinal direction and more than 250% in the transverse direction. During the packaging process, a combination of continuous heat sealing and intermittent heat sealing is adopted, the heat sealing temperature is controlled at 120℃-150℃, the heat sealing pressure is 0.2MPa-0.5MPa, and the heat sealing time is 0.5s-2s.

10. The method for preparing a degradable disinfectant wet wipe according to claim 1, wherein: After use, the wet wipes can be completely biodegraded under the action of microorganisms in the soil, water or compost conditions of the natural environment, and eventually decomposed into harmless substances such as carbon dioxide, water and inorganic salts.

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