One-way moisture-permeable and reverse osmosis-preventing multi-layer composite sanitary material and preparation method thereof

Abstract

The application discloses a one-way moisture-conducting anti-reverse osmosis multilayer composite sanitary material and a preparation method thereof, and relates to the technical field of sanitary materials; the preparation steps are as follows: fiber raw materials are opened and carded to obtain three layers of fiber webs, the three layers of fiber webs are cross-laid, water-jet reinforced, and dried, a hydrophobic antibacterial finishing agent is sprayed on the side of the surface layer of the three layers of fiber webs away from the middle layer, a hydrophilic antibacterial finishing agent is sprayed on the side of the inner layer of the three layers of fiber webs away from the middle layer, and after solidification and drying, the multilayer composite sanitary material is obtained through hot rolling; the fiber raw materials are polylactic acid fibers and regenerated cellulose fibers; the weight ratio of the polylactic acid fibers to the regenerated cellulose fibers in the surface layer is (80-90):(10-20), the weight ratio of the polylactic acid fibers to the regenerated cellulose fibers in the middle layer is (40-50):(50-60), and the inner layer is single regenerated cellulose fibers.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of sanitary materials, in particular to a one-way moisture-conducting and anti-back-permeation multi-layer composite sanitary material and a preparation method thereof. BACKGROUND

[0002] At present, traditional sanitary materials cannot simultaneously achieve rapid moisture conduction and anti-back-permeation functions in actual application, which easily leads to damp and hot, and causes bacterial breeding and allergy problems. Spunlace nonwoven fabric becomes an ideal substrate due to its high fiber entanglement degree, softness and other characteristics. With the continuous growth of the global health product market, the driving of domestic policy and the upgrading of consumer ability, the demand for high-performance and green materials has surged, and the demand for moisture-conducting and anti-permeation materials in the fields of medical care, personal care and sanitary products has increased year by year. Domestic and foreign enterprises have begun to explore new processes and technologies to develop new materials with the characteristics of anti-back-permeation, softness, air permeability and environmental friendliness. Therefore, it is of practical significance to develop an integrated multi-layer one-way moisture-conducting and anti-back-permeation composite sanitary material. SUMMARY

[0003] The purpose of the present application is to provide a one-way moisture-conducting and anti-back-permeation multi-layer composite sanitary material and a preparation method thereof to solve the problems in the prior art.

[0004] To achieve the above-mentioned purpose, the present application provides the following technical solutions:

[0005] A preparation method of a one-way moisture-conducting and anti-back-permeation multi-layer composite sanitary material, comprising the following preparation steps: opening and carding fiber raw materials to obtain three layers of fiber webs, cross-laying and then water jetting and reinforcing, and drying and hot rolling to obtain a multi-layer composite sanitary material; the fiber raw materials are polylactic acid fibers and regenerated cellulose fibers; the three layers of fiber webs are used as a surface layer with a weight ratio of polylactic acid fibers to regenerated cellulose fibers of (80-90):(10-20), a middle layer with a weight ratio of polylactic acid fibers to regenerated cellulose fibers of (40-50):(50-60), and a single layer of regenerated cellulose fibers as an inner layer.

[0006] Preferably, a hydrophobic and antibacterial finishing agent is sprayed on the side of the surface layer of the three layers of fiber webs away from the middle layer; the preparation steps of the hydrophobic and antibacterial finishing agent are as follows:

[0007] Step 1: Dissolve chitosan in acetic acid solution, add anhydrous ethanol, stir and add vanillin-containing ethanol solution dropwise, after the dropwise addition is completed, heat to 60-65℃ and reflux for 20h, after cooling, adjust the pH of the solution to 7.0, then filter and wash, and then disperse in alkali solution, add 2,3-epoxypropyltrimethylammonium chloride, stir at 50-70℃ for 4-6h, pour into anhydrous ethanol, settle and filter, then stir in hydrochloric acid ethanol solution for 20-24h, add deionized water, pour into acetone, precipitate and filter to obtain quaternary ammonium salt chitosan I;

[0008] Step 2: Dissolve the quaternary ammonium salt chitosan I in acetic acid solution, drop 3-isocyanate propyl trimethoxysilane in N,N-dimethylacetamide solution, after constant temperature stirring at 40℃ for 12h, dialysis and drying to obtain silane modified quaternary ammonium salt chitosan;

[0009] Step 3: Dissolve zinc acetate in anhydrous methanol and ultrasonic dispersion, 2-methyl imidazole and hinokitiol are ultrasonic dispersed in anhydrous methanol, then mix and stir for 24h, centrifugal washing and drying to obtain hydrophobic antibacterial particles; put the silane modified quaternary ammonium salt chitosan prepared in step 2 in ethanol water solution, add hydrophobic antibacterial particles and stir to disperse to obtain hydrophobic antibacterial finishing agent;

[0010] Preferably, the mass ratio of chitosan, vanillin and 2,3-epoxy propyl trimethyl ammonium chloride in step 1 is 1:(2-4):(0.4-0.7);

[0011] Preferably, the mass ratio of quaternary ammonium salt chitosan I and 3-isocyanate propyl trimethoxysilane in step 2 is 1:(0.6-2);

[0012] Preferably, the mass ratio of zinc acetate, 2-methyl imidazole and hinokitiol in step 3 is 1:3:(0.03-0.08); the dosage ratio of silane modified quaternary ammonium salt chitosan and hydrophobic antibacterial particles is 1:(0.05-0.1);

[0013] Preferably, the spraying amount of hydrophobic antibacterial finishing agent is 0.4-0.6g / m 2 ; after spraying, solidify at 80℃ for 2-3h;

[0014] Preferably, the inner layer of the three-layer fiber web is sprayed with hydrophobic antibacterial finishing agent away from the middle layer; the preparation steps of the hydrophobic antibacterial finishing agent are as follows: dissolve chitosan in acetic acid solution, add anhydrous ethanol, stir and drop vanillin ethanol solution, after dropping, heat to 60-65℃ and reflux for 20h, after cooling, adjust the solution pH to 7.0, filter and wash, then put in alkali solution and stir to disperse, add 2,3-epoxy propyl trimethyl ammonium chloride, stir at 50-90℃ for 18-24h, pour into anhydrous ethanol to settle and filter, put in hydrochloric acid ethanol solution and stir for 20-24h, then add deionized water, pour into acetone to precipitate and filter, to obtain quaternary ammonium salt chitosan II; take quaternary ammonium salt chitosan II and put in deionized water, adjust the pH to 4.0, then add sodium periodate, stir in dark for 1-8h, add ethylene glycol to terminate the reaction, after 2h, filter the solid by adding sodium chloride and anhydrous ethanol, dialysis and drying to obtain aldehyde quaternary ammonium salt chitosan; take aldehyde quaternary ammonium salt chitosan, use acetic acid as solvent and stir to obtain hydrophobic antibacterial finishing agent;

[0015] Preferably, the mass ratio of chitosan, vanillin and 2,3-epoxypropyl trimethyl ammonium chloride is 1:(2-4):(1.4-2.5); the mass ratio of quaternary ammonium salt chitosan II and sodium periodate is 1:(0.2-0.3); the concentration of aldehyde-modified quaternary ammonium salt chitosan in the hydrophilic antibacterial finishing agent is 1-3%;

[0016] Preferably, the spraying amount of the hydrophilic antibacterial finishing agent is 0.5-0.6g / m 2 ; after spraying, curing at 80℃ for 2-3h;

[0017] Preferably, the fiber web surface density is 120-150g / m 2 ; the water jet reinforcement water pressure is 3-8MPa; the hot rolling temperature is 150-170℃, and the hot rolling roller speed is 10-12m / min;

[0018] A one-way wetting and anti-reverse osmosis multi-layer composite sanitary material is prepared by the above preparation method.

[0019] Compared with the prior art, the present application has the following advantages:

[0020] 1. The present application adopts a green and environmentally friendly bio-based raw material system, replaces traditional petroleum-based raw materials with biodegradable polylactic acid and regenerated cellulose fibers, and designs a three-layer gradient according to the fiber ratio to form a hydrophobic-transition-hydrophilic liquid conducting structure composite, utilizes capillary effect and wettability difference to provide a structural basis for one-way wetting; combined with water jet reinforcement and hot rolling process, an integrated multi-layer structure is constructed to further improve the anti-reverse osmosis strength of the sanitary material.

[0021] 2. The present application performs hydrophobic antibacterial finishing on the surface layer of the composite fiber web and hydrophilic antibacterial finishing on the inner layer; by adjusting the reaction time and the ratio of the reaction raw materials, two modified chitosans with different quaternary ammonium salt substitution degrees are designed to further regulate the antibacterial performance and hydrophilic performance of chitosan; the silicon-oxygen bond is introduced into the quaternary ammonium salt chitosan in the hydrophobic antibacterial finishing agent to improve the hydrophobicity and interfacial adhesion, achieving hydrophobic-antibacterial balance; the hydrophobic antibacterial finishing agent also includes hydrophobic antibacterial particles, which load natural antibacterial agent-thujol on metal organic frameworks, effectively adjusting the release of Zn 2+ ions and embedded thujol, and together with the silane-modified quaternary ammonium salt chitosan, improving the antibacterial durability; the hydrophilic antibacterial finishing agent is modified by aldehyde modification of quaternary ammonium salt chitosan, retaining the antibacterial performance of quaternary ammonium salt while forming a hemiacetal chemical bond with the hydroxyl groups on the regenerated cellulose in the inner layer through aldehyde groups, enhancing the bonding force between the finishing agent and the non-woven material, further improving the hydrophilic performance of the inner layer, and achieving rapid wetting; thus, the interface gradient of the hydrophobic barrier and the hydrophilic channel formed by the surface layer hydrophobic antibacterial finishing agent and the inner layer hydrophilic antibacterial finishing agent makes the liquid realize one-way wetting and anti-reverse osmosis under the joint action of the surface layer hydrophobicity repulsion and the inner layer hydrophilicity attraction. DETAILED DESCRIPTION

[0022] All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present application without creative labor fall within the scope of protection of the present application.

[0023] In the experiment, the polylactic acid fiber has a length of 38 mm and a fineness of 1.33D, and is purchased from Haining Xinneng Textile;

[0024] The regenerated cellulose fiber (regenerated viscose fiber) has a length of 38 mm and a fineness of 1.33D, and is purchased from Xingda Chemical Fiber;

[0025] The chitosan is purchased from the National Pharmaceutical Group, has a degree of deacetylation of 80-95%, and has a National Pharmaceutical code 69047438;

[0026] The preparation steps of the quaternary ammonium salt chitosan I are as follows: 5 g of chitosan is dissolved in 500 mL of an acetic acid solution with a concentration of 10%, 100 mL of anhydrous ethanol is added for stirring, and 50 mL of an ethanol solution containing 14.17 g of vanillin is added dropwise. After the dropwise addition is completed, the temperature is raised to 60 DEG C for refluxing for 20 h. After cooling, the solution pH is adjusted to 7.0, and then the solution is filtered and washed. The solution is then dispersed in 100 mL of a 0.5% sodium hydroxide solution for stirring. 2.42 g of 2,3-epoxypropyltrimethylammonium chloride is added, and stirring is performed at 70 DEG C for 5 h. The solution is then poured into anhydrous ethanol for sedimentation and filtration. The solution is then stirred in 100 mL of a 0.25 g / mL hydrochloric acid ethanol solution for 24 h. Deionized water is then added to dissolve the solution. The solution is then poured into acetone for precipitation and filtration, and the quaternary ammonium salt chitosan I is obtained.

[0027] The preparation steps of the quaternary ammonium salt chitosan II are as follows: 5 g of chitosan is dissolved in 500 mL of an acetic acid solution with a concentration of 10%, 100 mL of anhydrous ethanol is added for stirring, and 50 mL of an ethanol solution containing 14.17 g of vanillin is added dropwise. After the dropwise addition is completed, the temperature is raised to 60 DEG C for refluxing for 20 h. After cooling, the solution pH is adjusted to 7.0, and then the solution is filtered and washed. The solution is then dispersed in 500 mL of a 0.5% sodium hydroxide solution for stirring. 12.09 g of 2,3-epoxypropyltrimethylammonium chloride is added, and stirring is performed at 80 DEG C for 24 h. The solution is then poured into anhydrous ethanol for sedimentation and filtration. The solution is then stirred in 500 mL of a 0.25 g / mL hydrochloric acid ethanol solution for 24 h. Deionized water is then added, and the solution is poured into acetone for precipitation and filtration, and the quaternary ammonium salt chitosan II is obtained.

[0028] Embodiment 1: The present embodiment provides a preparation method of a one-way moisture-conducting anti-reverse osmosis multi-layer composite sanitary material, and the specific steps are as follows:

[0029] Step 1: The polylactic acid fiber and the regenerated cellulose fiber are opened and carded to obtain polylactic acid fibers and regenerated cellulose fibers with a surface density of 120 g / m 2a three-layer fiber web, cross-laid and hydroentangled at a water pressure of 5 MPa and dried at 80°C for 40 min; wherein the three-layer fiber web has a top layer of polylactic acid fiber and regenerated cellulose fiber in a weight ratio of 80:20, a middle layer of polylactic acid fiber and regenerated cellulose fiber in a weight ratio of 40:60, and a single layer of regenerated cellulose fiber as an inner layer;

[0030] Step 2: 5 g of quaternary ammonium salt chitosan I was dissolved in 500 mL of 10% acetic acid solution, and 50 mL of N,N-dimethylacetamide solution containing 6.50 g of 3-isocyanate propyl trimethoxysilane was added dropwise. After constant temperature stirring at 40°C for 12 h, dialysis and drying were performed to obtain silane-modified quaternary ammonium salt chitosan. 1 g of zinc acetate was dissolved in 100 mL of anhydrous methanol and ultrasonically dispersed, 3 g of 2-methyl imidazole and 0.03 g of thujyl alcohol were placed in 100 mL of anhydrous methanol and ultrasonically dispersed, and then the two were mixed and stirred for 24 h. After centrifugal washing and drying, hydrophobic antibacterial particles were obtained. 5 g of silane-modified quaternary ammonium salt chitosan was placed in 500 mL of an ethanol aqueous solvent and stirred, and then 0.25 g of the hydrophobic antibacterial particles was added and stirred and dispersed. The particles were sprayed on the side of the top layer of the three-layer fiber web away from the middle layer at a spraying amount of 0.5 g / m 2 , and after spraying was completed, solidification was performed at 80°C for 2 h.

[0031] Step 3: 5 g of quaternary ammonium salt chitosan II was placed in 50 mL of 10% acetic acid solution, and 1 g of sodium periodate was added. After stirring in the dark for 6 h, the reaction was terminated by adding 100 mL of ethylene glycol. After 2 h, 10 g of sodium chloride and 1 L of anhydrous ethanol were added to filter out the solid. Dialysis and drying were performed to obtain aldehyde-modified quaternary ammonium salt chitosan. 5 g of the aldehyde-modified quaternary ammonium salt chitosan was stirred in 10% acetic acid solution as a solvent to obtain a 1% hydrophilic antibacterial finishing agent. The agent was sprayed on the side of the inner layer of the three-layer fiber web away from the middle layer at a spraying amount of 0.6 g / m 2 , and after spraying was completed, solidification was performed at 80°C for 3 h. After solidification was completed, hot rolling was performed at a roller speed of 12 m / min and a temperature of 165°C to obtain a multi-layer composite sanitary material with a thickness of 0.3 mm.

[0032] Example 2: A preparation method of a one-way wet guide anti-reverse osmosis multi-layer composite sanitary material is provided in this example, and the specific steps are as follows:

[0033] Step 1: polylactic acid fiber and regenerated cellulose fiber were opened and carded to obtain a three-layer fiber web with an area density of 120 g / m 2 , cross-laid and hydroentangled at a water pressure of 6 MPa and dried at 80°C for 40 min; wherein the three-layer fiber web has a top layer of polylactic acid fiber and regenerated cellulose fiber in a weight ratio of 80:20, a middle layer of polylactic acid fiber and regenerated cellulose fiber in a weight ratio of 40:60, and a single layer of regenerated cellulose fiber as an inner layer;

[0034] Step 2: 5 g of quaternary ammonium salt chitosan I was dissolved in 500 mL of 10% acetic acid solution, 50 mL of N,N-dimethylacetamide solution containing 7.90 g of 3-isocyanate propyl trimethoxysilane was added dropwise, and after constant temperature stirring at 40℃ for 12 h, dialysis and drying were performed to obtain silane modified quaternary ammonium salt chitosan; 1 g of zinc acetate was dissolved in 100 mL of anhydrous methanol and ultrasonically dispersed, 3 g of 2-methyl imidazole and 0.05 g of thujyl alcohol were placed in 100 mL of anhydrous methanol and ultrasonically dispersed, then the two were mixed and stirred for 24 h, centrifuged, washed and dried to obtain hydrophobic antibacterial particles; 5 g of silane modified quaternary ammonium salt chitosan was placed in 500 mL of an ethanol aqueous solvent and stirred, then 0.30 g of hydrophobic antibacterial particles was added and stirred and dispersed, and sprayed on the surface layer of the three-layer fiber web away from the middle layer side, with a spraying amount of 0.5 g / m 2 , and after spraying, solidification was performed at 80℃ for 2 h;

[0035] Step 3: 5 g of quaternary ammonium salt chitosan II was placed in 50 mL of 10% acetic acid solution, 1 g of sodium periodate was added, and stirring was performed in the dark for 6 h, then 100 mL of ethylene glycol was added to terminate the reaction, 10 g of sodium chloride and 1 L of anhydrous ethanol were added after 2 h, the solid was filtered out, dialysis and drying were performed to obtain aldehyde-modified quaternary ammonium salt chitosan; 5 g of aldehyde-modified quaternary ammonium salt chitosan was stirred with 10% acetic acid solution as a solvent to obtain a 2% hydrophilic antibacterial finishing agent, which was sprayed on the inner layer of the three-layer fiber web away from the middle layer side, with a spraying amount of 0.6 g / m 2 , and after spraying, solidification was performed at 80℃ for 3 h; after solidification, hot rolling was performed at a roller speed of 12 m / min and a temperature of 165℃ to obtain a multi-layer composite sanitary material with a thickness of 0.3 mm.

[0036] Example 3: The present embodiment provides a preparation method of a one-way wet guide anti-reverse osmosis multi-layer composite sanitary material, and the specific steps are as follows:

[0037] Step 1: polylactic acid fibers and regenerated cellulose fibers were opened and carded to obtain three-layer fiber webs with a surface density of 120 g / m 2 , respectively, and after cross-laying, water jet reinforcement was performed at a water pressure of 8 MPa and drying was performed at 80℃ for 40 min; wherein the three-layer fiber web was taken as the surface layer with a proportion of polylactic acid fibers and regenerated cellulose fibers of 80:20, as the middle layer with a proportion of polylactic acid fibers and regenerated cellulose fibers of 40:60, and as the inner layer with single regenerated cellulose fibers;

[0038] Step 2: 5 g of quaternary ammonium salt chitosan I was dissolved in 500 mL of 10% acetic acid solution, and 50 mL of N,N-dimethylacetamide solution containing 9.23 g of 3-isocyanate propyl trimethoxysilane was added dropwise. After constant temperature stirring at 40℃ for 12 h, dialysis and drying were performed to obtain silane modified quaternary ammonium salt chitosan. 1 g of zinc acetate was dissolved in 100 mL of anhydrous methanol and ultrasonically dispersed, 3 g of 2-methyl imidazole and 0.08 g of cypressol were placed in 100 mL of anhydrous methanol and ultrasonically dispersed, and then the two were mixed and stirred for 24 h. After centrifugal washing and drying, hydrophobic antibacterial particles were obtained. 5 g of silane modified quaternary ammonium salt chitosan was placed in 500 mL of an ethanol aqueous solvent and stirred, and then 0.40 g of hydrophobic antibacterial particles was added and stirred and dispersed. Spraying was performed on the surface layer of the three-layer fiber web away from the middle layer at a spraying amount of 0.5 g / m 2 , and after spraying was completed, solidification was performed at 80℃ for 2 h.

[0039] Step 3: 5 g of quaternary ammonium salt chitosan II was placed in 50 mL of 10% acetic acid solution, and 1 g of sodium periodate was added. Stirring was performed in the dark for 6 h, and then 100 mL of ethylene glycol was added to terminate the reaction. After 2 h, 10 g of sodium chloride and 1 L of anhydrous ethanol were added to filter out the solid. Dialysis and drying were performed to obtain aldehyde-modified quaternary ammonium salt chitosan. 5 g of aldehyde-modified quaternary ammonium salt chitosan was stirred in 10% acetic acid solution to obtain a hydrophilic antibacterial finishing agent with a concentration of 3%. Spraying was performed on the inner layer of the three-layer fiber web away from the middle layer at a spraying amount of 0.6 g / m 2 , and after spraying was completed, solidification was performed at 80℃ for 3 h. After solidification was completed, hot rolling was performed at a roller speed of 12 m / min and a temperature of 165℃ to obtain a multi-layer composite sanitary material with a thickness of 0.3 mm.

[0040] Comparative Example 1: As a control experiment of Example 3, no hydrophobic antibacterial particles were added in Step 2. The specific steps are as follows:

[0041] Step 1: Polylactic acid fibers and regenerated cellulose fibers were opened and carded to obtain three-layer fiber webs with a face density of 120 g / m 2 . Cross-laying was performed, and water jet reinforcement was performed at a water pressure of 8 MPa, and then drying was performed at 80℃ for 40 min. The three-layer fiber web was taken as the surface layer, the middle layer, and the inner layer, and the weight ratio of polylactic acid fibers to regenerated cellulose fibers was 80:20, 40:60, and 100%, respectively.

[0042] Step 2: 5 g of quaternary ammonium salt chitosan I was dissolved in 500 mL of 10% acetic acid solution, and 50 mL of N,N-dimethylacetamide solution containing 9.23 g of 3-isocyanate propyl trimethoxysilane was added dropwise. After constant temperature stirring at 40℃ for 12 h, dialysis and drying were performed to obtain silane modified quaternary ammonium salt chitosan. 5 g of silane modified quaternary ammonium salt chitosan was dispersed by stirring in 500 mL of ethanol aqueous solvent, and was sprayed on the surface layer of the three-layer fiber web away from the middle layer side, with a spraying amount of 0.5 g / m 2 After spraying, it was cured at 80℃ for 2 h;

[0043] Step 3: 5 g of quaternary ammonium salt chitosan II was placed in 50 mL of 10% acetic acid solution, and 1 g of sodium periodate was added. After stirring in the dark for 6 h, 100 mL of ethylene glycol was added to terminate the reaction. After 2 h, 10 g of sodium chloride and 1 L of anhydrous ethanol were added to filter out the solid. Dialysis and drying were performed to obtain aldehyde-modified quaternary ammonium salt chitosan. 5 g of aldehyde-modified quaternary ammonium salt chitosan was stirred in 10% acetic acid solution to obtain a hydrophilic antibacterial finishing agent with a concentration of 3%. The agent was sprayed on the inner layer of the three-layer fiber web away from the middle layer side, with a spraying amount of 0.6 g / m 2 After spraying, it was cured at 80℃ for 3 h. After curing, hot rolling was performed at a roller speed of 12 m / min and a temperature of 165℃ to obtain a multi-layer composite sanitary material with a thickness of 0.3 mm.

[0044] Comparative Example 2: As a control experiment of Example 3, no spraying of hydrophilic antibacterial finishing agent on the inner layer was performed. The specific steps are as follows:

[0045] Step 1: Polylactic acid fibers and regenerated cellulose fibers were opened and carded to obtain three-layer fiber webs with a surface density of 120 g / m 2 After cross-laying, water jet reinforcement was performed at a water pressure of 8 MPa, and drying was performed at 80℃ for 40 min. Among them, the three-layer fiber web had a portion ratio of polylactic acid fibers and regenerated cellulose fibers of 80:20 as the surface layer, a portion ratio of polylactic acid fibers and regenerated cellulose fibers of 40:60 as the middle layer, and single regenerated cellulose fibers as the inner layer.

[0046] Step 2: 5 g of quaternary ammonium salt chitosan I was dissolved in 500 mL of 10% acetic acid solution, and 50 mL of N,N-dimethylacetamide solution containing 9.23 g of 3-isocyanate propyl trimethoxysilane was added dropwise. After constant temperature stirring at 40°C for 12 h, dialysis and drying were performed to obtain silane modified quaternary ammonium salt chitosan. 1 g of zinc acetate was dissolved in 100 mL of anhydrous methanol and ultrasonically dispersed, 3 g of 2-methyl imidazole and 0.08 g of cypressol were placed in 100 mL of anhydrous methanol and ultrasonically dispersed, and then the two were mixed and stirred for 24 h. After centrifugal washing and drying, hydrophobic antibacterial particles were obtained. 5 g of silane modified quaternary ammonium salt chitosan was placed in 500 mL of an ethanol aqueous solvent and stirred, and then 0.40 g of hydrophobic antibacterial particles was added and stirred and dispersed. Spraying was performed on the surface layer of the three-layer fiber web away from the middle layer, and the spraying amount was 0.5 g / m 2 After spraying was completed, curing was performed at 80°C for 2 h.

[0047] Step 3: After curing was completed, hot rolling was performed at a roller speed of 12 m / min and a temperature of 165°C to obtain a multi-layer composite sanitary material with a thickness of 0.3 mm.

[0048] Detection test

[0049] Liquid penetration time: According to GB / T 24218.13, the multi-layer composite materials prepared in Examples 1-3 and Comparative Examples 1-2 were cut to obtain samples with a size of 100 mm x 100 mm. The samples were placed on the base plate of a liquid penetration instrument, ten standard water absorption filter papers were placed under the bottom layer of the sample, the distance between the tip of the liquid funnel and the sample was adjusted to 30 mm, 5 mL of artificial urine (0.9% sodium chloride solution) was taken with a dropper and added to the liquid funnel, and when the artificial urine contacted the penetration disc, the liquid was conductive, the electrodes were connected, and the electronic timer started timing. When the liquid completely penetrated into the sample and the standard water absorption filter paper, there was no liquid conduction in the penetration disc, at which time the electrodes were disconnected and stopped in time, and the penetration time was obtained. Each sample was tested five times, and the average value was taken. The data are recorded in Table 1.

[0050] Reverse wet amount: According to the standard GB / T 24218.14, the sample was tested three times repeatedly according to the liquid penetration time test method. A 1.2 kg block was placed on the sample and the standard water absorption filter paper, ten water absorption filter papers were placed on the surface of the sample, and the block was placed on the water absorption filter paper for 2 min. After being removed, the mass of the water absorption filter paper was weighed again, the difference in mass was calculated, and the data are recorded in Table 1.

[0051] Antibacterial durability: According to FZ / T 73023, the antibacterial performance of the sample was measured after 50 times of washing, and the data are recorded in Table 1.

[0052] Table 1

[0053]

[0054] Conclusion: From the above data, it can be seen that Example 3 has more excellent anti-back penetration and antibacterial properties than the other examples; Comparative Example 1, as a control experiment of Example 3, does not add hydrophobic antibacterial particles during surface finishing, which has an impact on liquid penetration time, reverse wetting amount and antibacterial properties; Comparative Example 2 does not perform inner layer hydrophilic antibacterial finishing agent spraying, the liquid penetration time is prolonged, the reverse wetting amount is significantly increased, and the antibacterial properties are obviously decreased.

[0055] Finally, it should be noted that the above only describes the preferred embodiments of the present application and is not intended to limit the present application. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent replacements to some technical features. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application shall be included in the protection scope of the present application.

Claims

1. A method for producing a one-way moisture conducting, anti- reverse osmosis multilayer composite sanitary material, characterized by, The preparation steps include: opening and carding the fiber raw material to obtain three layers of fiber webs, respectively, cross-laying, water jetting and reinforcing, and drying, and hot rolling after drying to obtain a multi-layer composite sanitary material; the fiber raw material is polylactic acid fiber and regenerated cellulose fiber; the three layers of fiber webs are polylactic acid fiber and regenerated cellulose fiber in a proportion of (80-90):(10-20) as the surface layer, polylactic acid fiber and regenerated cellulose fiber in a proportion of (40-50):(50-60) as the middle layer, and single regenerated cellulose fiber as the inner layer; A hydrophobic antibacterial finishing agent is sprayed on the surface layer of the three layers of fiber webs away from the middle layer; the preparation steps of the hydrophobic antibacterial finishing agent are: Step 1: Dissolve chitosan in acetic acid solution, add anhydrous ethanol and stir, and then add vanillin-containing ethanol solution dropwise, heat to 60-65 DEG C to reflux for 20 hours after dropwise addition is completed, adjust the solution pH to 7.0 after cooling, and then filter and wash, and then disperse in alkali solution, add 2, 3-epoxypropyltrimethylammonium chloride, stir at 50-70 DEG C for 4-6 hours, pour into anhydrous ethanol, settle and filter, disperse in hydrochloric acid ethanol solution for 20-24 hours, add deionized water, pour into acetone, precipitate and filter to obtain quaternary ammonium salt chitosan I; Step 2: Dissolve quaternary ammonium salt chitosan I in acetic acid solution, add 3-isocyanate propyl trimethoxysilane-containing N, N-dimethylacetamide solution dropwise, and stir at 40 DEG C for 12 hours, then dialyze and dry to obtain silane-modified quaternary ammonium salt chitosan; Step 3: ultrasonic dispersion of zinc acetate in anhydrous methanol, 2-methyl imidazole and thujyl alcohol are ultrasonic dispersed in anhydrous methanol, then the two are mixed and stirred for 24 hours, centrifuged, washed and dried to obtain hydrophobic antibacterial particles; the silane-modified quaternary ammonium salt chitosan prepared in step 2 is stirred in an ethanol aqueous solvent and hydrophobic antibacterial particles are added, and then stirred and dispersed to obtain a hydrophobic antibacterial finishing agent; The mass ratio of chitosan, vanillin and 2, 3-epoxypropyltrimethylammonium chloride in step 1 is 1:(2-4):(0.4-0.7); the mass ratio of quaternary ammonium salt chitosan I and 3-isocyanate propyl trimethoxysilane in step 2 is 1:(0.6-2); The mass ratio of zinc acetate, 2-methyl imidazole and thujyl alcohol in step 3 is 1:3:(0.03-0.08); the amount ratio of silane-modified quaternary ammonium salt chitosan and hydrophobic antibacterial particles is 1:(0.05-0.1); The inner layer of the three-layer fiber web is sprayed with a hydrophilic antibacterial finishing agent away from the middle layer; the hydrophilic antibacterial finishing agent is prepared by the following steps: dissolving chitosan in acetic acid solution, adding anhydrous ethanol and stirring, and then adding vanillin-containing ethanol solution dropwise; after the dropwise addition is completed, the temperature is raised to 60-65℃ and refluxed for 20h; after cooling, the solution pH is adjusted to 7.0, then filtered and washed, and then dispersed in alkali solution; 2,3-epoxypropyltrimethylammonium chloride is added, and stirred at 50-90℃ for 18-24h; then poured into anhydrous ethanol for sedimentation and filtration; then stirred in hydrochloric acid ethanol solution for 20-24h, then added deionized water, poured into acetone for precipitation and filtration, to obtain quaternary ammonium salt chitosan II; quaternary ammonium salt chitosan II is placed in deionized water, the pH is adjusted to 4.0, then sodium periodate is added, stirred in the dark for 1-8h, then added ethylene glycol to terminate the reaction, 2h later, added sodium chloride and anhydrous ethanol to filter out the solid, then dialyzed and dried to obtain aldehyde-modified quaternary ammonium salt chitosan; the aldehyde-modified quaternary ammonium salt chitosan is stirred with acetic acid as the solvent to obtain the hydrophilic antibacterial finishing agent. The mass ratio of chitosan, vanillin and 2,3-epoxypropyltrimethylammonium chloride in the preparation step of the hydrophilic antibacterial finishing agent is 1:(2-4):(1.4-2.5); the mass ratio of quaternary ammonium salt chitosan II and sodium periodate is 1:(0.2-0.3); the concentration of aldehyde-modified quaternary ammonium salt chitosan in the hydrophilic antibacterial finishing agent is 1-3%.

2. The method for preparing a unidirectional moisture-wicking, anti-backflow multilayer composite sanitary material according to claim 1, characterized in that, The spraying amount of the hydrophobic antibacterial finishing agent is 0.4-0.6 g / m 2 ; and after the spraying is completed, curing is performed at 80°C for 2-3 h.

3. The method for preparing a unidirectional moisture-wicking, anti-backflow multilayer composite sanitary material according to claim 1, characterized in that, The spraying amount of the hydrophilic antibacterial finishing agent is 0.5-0.6 g / m 2 ; and after the spraying is completed, curing is performed at 80°C for 2-3 h.

4. The method for preparing a unidirectional moisture-wicking, anti-backflow multilayer composite sanitary material according to claim 1, characterized in that, The fiber web surface density is 120-150 g / m 2 The water pressure for water jet reinforcement is 3-8 MPa; the hot rolling temperature is 150-170℃, and the hot rolling roller speed is 10-12 m / min.

5. A one-way moisture conducting, anti- reverse osmosis multilayer composite sanitary material, characterized by, Prepared by the preparation method of any one of claims 1-4.

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