Bacteriostatic super absorbent resin for paper diapers and preparation method thereof
Through the preparation of modified bone meal and quaternary ammonization reaction, a highly absorbent resin with a quaternary ammonium salt network structure on the surface is constructed, which solves the problem of the lack of antibacterial properties and comfort in diaper applications, and achieves the improvement of high water absorption rate, antibacterial properties and softness.
Patent Information
- Application Number
- CN202510117649.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-24
- Publication Date
- 2025-04-18
AI Technical Summary
When used in diapers, existing high-absorbent resins lack antibacterial properties and comfort, making it difficult to meet the needs of the personal care field.
Through the preparation of modified bone meal, acrylamide, tert-butylaminoethyl methacrylate and N,N-methylenebisacrylamide are polymerized on the surface of the bone meal, and the tert-butylamino group is converted into quaternary ammonium salt through quaternary ammonization reaction to construct modified bone meal with a network structure on the surface, thereby improving the water absorption rate and antibacterial properties of the resin.
It significantly improves the water absorption rate, antibacterial properties and softness of the high-absorbent resin, and enhances the comfort and use effect of the diapers.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of polymer materials, and in particular relates to an antibacterial superabsorbent resin for diapers and a preparation method thereof. Background Art
[0002] Super absorbent resin is an important type of polymer material with super high water absorption and good water retention. It is widely used in agriculture, medical treatment, personal care and industry. In the field of personal care, especially in diaper applications, super absorbent resin is not only required to have super high water absorption and good water retention, but also to have certain antibacterial properties, that is, to meet the comfort and usability. Then, traditional super absorbent resins are usually made of hydrophilic monomers or polymers, such as acrylic acid, acrylamide, etc. Among them, cross-linked polyacrylic acid (salt) super absorbent resins are the most widely used.
[0003] For example, patent number CN 112552468 A discloses a super absorbent resin and a preparation method thereof, wherein an interpenetrating polymer is dissolved in deionized water, acrylic acid is added, and the mixture is neutralized to a pH value of 6-7; the temperature is lowered to 23±2°C; oxygen is isolated, a crosslinking agent and an initiator are added to initiate polymerization and the temperature is naturally raised to a constant temperature, and then the temperature is kept at 80-90°C for 2 hours to obtain a resin colloid, and the resin colloid is granulated, dried, crushed, and sieved to obtain resin particles; a surface crosslinking liquid is added to the surface of the resin particles; the super absorbent resin is obtained by cooling and sieving; a large number of hydrophilic groups are introduced through the interpenetrating polymers, thereby improving the water absorption and retention properties of the super absorbent resin. The preparation method of the super absorbent resin gives priority to water absorption, but there are still shortcomings, and the comfort and antibacterial properties when applied to the personal care field are ignored. Therefore, the super absorbent resin needs to be further improved. Summary of the invention In view of the technical problems existing in the above-mentioned prior art, the present invention provides an antibacterial super absorbent resin for diapers and a preparation method thereof, so as to meet the water absorption and retention and antibacterial properties of the super absorbent resin while meeting the comfort requirements.
[0004] The objective of the present invention is achieved through the following technical solutions: In a first aspect, the present invention provides a method for preparing an antibacterial superabsorbent resin for diapers, the method comprising the following steps: Step (1): heating and stirring the hydrophobic solvent and Span-80 at 90-105° C. for 20-30 minutes to obtain an oil phase; Step (2): dispersing bone powder in deionized water, then adding acrylamide, tert-butylaminoethyl methacrylate, N,N-methylenebisacrylamide and initiator, reacting in a water bath at 30-40° C. for 1-1.5 h, filtering, washing and drying, and then converting the tert-butylamino group into a quaternary ammonium salt through a quaternization reaction, followed by water washing and drying to obtain modified bone powder, wherein the mass ratio of the bone powder, acrylamide, tert-butylaminoethyl methacrylate, N,N-methylenebisacrylamide and initiator is 1-3:2-6:3-5:0.01-0.05:0.1-0.15; Step (3): adding acrylic acid, acrylamide, modified bone powder and 2-acrylamide-2-methylpropane sulfonic acid into deionized water to obtain an aqueous phase, wherein the mass ratio of the acrylic acid, acrylamide, modified bone powder and 2-acrylamide-2-methylpropane sulfonic acid is 1.5-5:1-3:0.5-2:0.1-0.5; Step (4): Add potassium persulfate KPS and MBA solution to the aqueous phase obtained in step (3), stir in a water bath at 90-105° C. for 4-6 hours, and then drop into the oil phase obtained in step (1). After the reaction is completed, filter, wash and dry to obtain an antibacterial super absorbent resin.
[0005] Preferably, the hydrophobic solvent in step (1) is one of petroleum ether, n-hexane and paraffin.
[0006] Preferably, the mass ratio of the hydrophobic solvent to Span-80 in step (1) is 40-50:1.
[0007] Preferably, the specific steps of step (2) are as follows: The bone powder is dispersed in deionized water, and then acrylamide, tert-butylaminoethyl methacrylate, N,N-methylenebisacrylamide and an initiator are added, and the mixture is reacted in a water bath at 30-40°C for 1-1.5 hours, filtered, washed and dried, and an anhydrous organic solvent is added after drying, and then an alkyl halide is added, and the mixture is stirred at 80-100°C for 4-6 hours, and then washed with water and dried to obtain modified bone powder, wherein the mass ratio of the bone powder, acrylamide, tert-butylaminoethyl methacrylate, N,N-methylenebisacrylamide and the initiator is 1-3:2-6:3-5:0.01-0.05:0.1-0.15.
[0008] Preferably, the alkane halide is one of alkyl bromide, ethyl iodide and alkyl chloride.
[0009] Preferably, the anhydrous organic solvent is one of ethanol, diethyl ether and N,N-dimethylacetamide.
[0010] Preferably, the preparation method of the bone powder is as follows: The chicken bones were chopped and placed in 0.5 mol·L-1 The samples were decalcified by stirring in disodium ethylenediaminetetraacetic acid for 24 h and then washed with deionized water. -1 Soak in NaOH solution for 24 h, wash with deionized water until neutral; then soak in 15% isopropanol solution for 24 h, wash with deionized water and dry.
[0011] Preferably, the initiator in step (2) is one of sodium persulfate, ammonium persulfate and potassium persulfate.
[0012] Preferably, in step (2), the drying temperature is 80-100° C. and the drying time is 2-3 h.
[0013] In a second aspect, the present invention provides an antibacterial superabsorbent resin for diapers, which is obtained according to the above preparation method.
[0014] The present invention has the following beneficial effects: The present invention provides a method for preparing an antibacterial superabsorbent resin for diapers, and adopts modified bone powder to prepare the superabsorbent resin, thereby increasing the water absorption rate of the superabsorbent resin; at the same time, further improving the antibacterial performance of the superabsorbent resin.
[0015] The invention provides a method for preparing an antibacterial super absorbent resin for diapers. Under the action of an initiator, acrylamide, tert-butylaminoethyl methacrylate and N,N-methylenebisacrylamide are polymerized on the surface of bone powder, and then the tert-butylamino group is converted into a quaternary ammonium salt through a quaternization reaction to obtain a modified bone powder with a quaternary ammonium salt network structure on the surface. The network structure formed on the surface of the bone powder improves the water absorption and retention performance of the super absorbent resin. At the same time, the tert-butylamino group is converted into a quaternary ammonium salt through a quaternization reaction, which not only improves the antibacterial performance of the super absorbent resin, but also improves its softness and increases the comfort.
[0016] The invention provides a method for preparing an antibacterial superabsorbent resin for diapers. When a quaternary ammonium salt is constructed on the surface of bone powder, 2-acrylamide-2-methylpropane sulfonic acid is added during secondary network formation to promote network formation, which is beneficial to improving water absorption and retention and softness. DETAILED DESCRIPTION
[0017] The following examples also describe certain specific aspects and embodiments, which are provided for illustrative purposes only and should not be construed as limiting the scope of the invention in any way.
[0018] Example 1 An antibacterial super absorbent resin for diapers, the specific preparation method is as follows: (1) Add 1 g of Span-80 to 40 g of n-hexane, heat and stir in a 90°C water bath for 20 minutes to obtain an oil phase; (2) Chop the chicken bones and place them in 0.5 mol·L -1 The samples were decalcified by stirring in disodium ethylenediaminetetraacetic acid for 24 h and then washed with deionized water. -1 Soak in NaOH solution for 24 hours, wash with deionized water until neutral; then soak in 15% isopropanol solution for 24 hours, wash with deionized water after soaking, and dry to obtain bone powder; Weigh 1 g of bone powder and disperse it in 60 g of deionized water, then add 2 g of acrylamide, 3 g of tert-butylaminoethyl methacrylate, 0.01 g of N,N-methylenebisacrylamide and 0.1 g of sodium persulfate, react in a 30°C water bath for 1 h, filter, wash and dry after the reaction, add 100 g of ethanol after drying, then add 80 g of bromoalkane, stir at 80°C for 4 h, then wash with water and dry at 80°C for 2 h to obtain modified bone powder; (3) adding 1.5 g of acrylic acid, 1 g of acrylamide, 0.5 g of modified bone meal and 0.1 g of 2-acrylamide-2-methylpropanesulfonic acid to 70 g of deionized water to obtain an aqueous phase; (4) Add 0.25 g of 1% potassium persulfate KPS and 0.25 g of 1% MBA solution to the aqueous phase obtained in step (3), stir in a 90°C water bath for 4 h, and then drop into the oil phase obtained in step (1). After the reaction is completed, filter, wash, and dry in a 100°C drying oven for 24 h to obtain an antibacterial superabsorbent resin.
[0019] Example 2 An antibacterial super absorbent resin for diapers, the specific preparation method is as follows: (1) Add 1 g of Span-80 to 50 g of paraffin, heat and stir in a water bath at 100°C for 25 minutes to obtain an oil phase; (2) Chop the chicken bones and place them in 0.5 mol·L -1 The samples were decalcified by stirring in disodium ethylenediaminetetraacetic acid for 24 h and then washed with deionized water. -1 Soak in NaOH solution for 24 hours, wash with deionized water until neutral; then soak in 15% isopropanol solution for 24 hours, wash with deionized water after soaking, and dry to obtain bone powder; Weigh 2 g of bone powder and disperse it in 70 g of deionized water, then add 4 g of acrylamide, 4 g of tert-butylaminoethyl methacrylate, 0.03 g of N,N-methylenebisacrylamide and 0.13 g of ammonium persulfate, react in a 35°C water bath for 1 h, filter, wash and dry after the reaction, add 100 g of ether after drying, and then add 80 g of iodine, stir at 90°C for 5 h, then wash with water and dry at 90°C for 2.5 h to obtain modified bone powder; (3) adding 2 g of acrylic acid, 1 g of acrylamide, 1 g of modified bone powder and 0.3 g of 2-acrylamide-2-methylpropanesulfonic acid to 80 g of deionized water to obtain an aqueous phase; (4) Add 0.5 g of 1% potassium persulfate KPS and 0.5 g of 1% MBA solution to the aqueous phase obtained in step (3), stir in a 100°C water bath for 5 h, and then drop into the oil phase obtained in step (1). After the reaction is completed, filter, wash, and dry in a 100°C drying oven for 24 h to obtain an antibacterial superabsorbent resin.
[0020] Example 3 An antibacterial super absorbent resin for diapers, the specific preparation method is as follows: (1) Add 1 g of Span-80 to 40 g of petroleum ether, heat and stir in a water bath at 100°C for 30 minutes to obtain an oil phase; (2) Chop the chicken bones and place them in 0.5 mol·L -1 The samples were decalcified by stirring in disodium ethylenediaminetetraacetic acid for 24 h and then washed with deionized water. -1 Soak in NaOH solution for 24 hours, wash with deionized water until neutral; then soak in 15% isopropanol solution for 24 hours, wash with deionized water after soaking, and dry to obtain bone powder; Weigh 2.5 g of bone powder and disperse it in 75 g of deionized water, then add 5 g of acrylamide, 4 g of tert-butylaminoethyl methacrylate, 0.04 g of N,N-methylenebisacrylamide and 0.13 g of ammonium persulfate, react in a 35°C water bath for 1 h, filter, wash and dry after the reaction, add 100 g of N,N-dimethylacetamide after drying, and then add 80 g of chloroalkane, stir at 100°C for 6 h, then wash with water and dry at 100°C for 3 h to obtain modified bone powder; (3) adding 2.5 g of acrylic acid, 1 g of acrylamide, 1.5 g of modified bone powder and 0.35 g of 2-acrylamide-2-methylpropanesulfonic acid to 90 g of deionized water to obtain an aqueous phase; (4) Add 0.75 g of 1% potassium persulfate KPS and 0.75 g of 1% MBA solution to the aqueous phase obtained in step (3), stir in a 100°C water bath for 6 h, and then drop into the oil phase obtained in step (1). After the reaction is completed, filter, wash, and dry in a 100°C drying oven for 24 h to obtain an antibacterial superabsorbent resin.
[0021] Example 4 An antibacterial super absorbent resin for diapers, the specific preparation method is as follows: (1) Add 1 g of Span-80 to 60 g of petroleum ether, heat and stir in a water bath at 105°C for 30 minutes to obtain an oil phase; (2) Chop the chicken bones and place them in 0.5 mol·L -1 The samples were decalcified by stirring in disodium ethylenediaminetetraacetic acid for 24 h and then washed with deionized water. -1 Soak in NaOH solution for 24 hours, wash with deionized water until neutral; then soak in 15% isopropanol solution for 24 hours, wash with deionized water after soaking, and dry to obtain bone powder; Weigh 3 g of bone powder and disperse it in 80 g of deionized water, then add 6 g of acrylamide, 5 g of tert-butylaminoethyl methacrylate, 0.05 g of N,N-methylenebisacrylamide and 0.15 g of ammonium persulfate, react in a 40°C water bath for 1 h, filter, wash and dry after the reaction, add 100 g of ether after drying, then add 80 g of chloroalkane, stir at 100°C for 6 h, then wash with water and dry at 100°C for 6 h to obtain modified bone powder; (3) adding 5 g of acrylic acid, 3 g of acrylamide, 2 g of modified bone powder and 0.5 g of 2-acrylamide-2-methylpropanesulfonic acid to 90 g of deionized water to obtain an aqueous phase; (4) Add 0.75 g of 1% potassium persulfate KPS and 0.75 g of 1% MBA solution to the aqueous phase obtained in step (3). After the reaction is completed, filter, wash, and dry in a drying oven at 100° C. for 24 h to obtain an antibacterial superabsorbent resin.
[0022] Comparative Example 1 The difference between Comparative Example 1 and Example 3 is that: bone powder is not added in step (3); The specific steps are as follows: (1) Add 1 g of Span-80 to 40 g of petroleum ether, heat and stir in a water bath at 100°C for 30 minutes to obtain an oil phase; (3) adding 2.5 g of acrylic acid, 1 g of acrylamide and 0.35 g of 2-acrylamide-2-methylpropanesulfonic acid to 90 g of deionized water to obtain an aqueous phase; (4) Add 0.75 g of 1% potassium persulfate KPS and 0.75 g of 1% MBA solution to the aqueous phase obtained in step (3), stir in a 100°C water bath for 6 h, and then drop into the oil phase obtained in step (1). After the reaction is completed, filter, wash, and dry in a 100°C drying oven for 24 h to obtain an antibacterial superabsorbent resin.
[0023] Comparative Example 2 The difference between Comparative Example 2 and Example 3 is that the modified bone powder in step (3) is replaced with bone powder; The specific steps are as follows: (1) Add 1 g of Span-80 to 40 g of petroleum ether, heat and stir in a water bath at 100°C for 30 minutes to obtain an oil phase; (2) Chop the chicken bones and place them in 0.5 mol·L -1 The samples were decalcified by stirring in disodium ethylenediaminetetraacetic acid for 24 h and then washed with deionized water. -1 Soak in NaOH solution for 24 hours, wash with deionized water until neutral; then soak in 15% isopropanol solution for 24 hours, wash with deionized water after soaking, and dry to obtain bone powder; (3) adding 2.5 g of acrylic acid, 1 g of acrylamide, 1.5 g of bone powder and 0.35 g of 2-acrylamide-2-methylpropanesulfonic acid to 90 g of deionized water to obtain an aqueous phase; (4) Add 0.75 g of 1% potassium persulfate KPS and 0.75 g of 1% MBA solution to the aqueous phase obtained in step (3), stir in a 100°C water bath for 6 h, and then drop into the oil phase obtained in step (1). After the reaction is completed, filter, wash, and dry in a 100°C drying oven for 24 h to obtain an antibacterial superabsorbent resin.
[0024] Comparative Example 3 The difference between Comparative Example 3 and Example 3 is that: in step (2), tert-butylaminoethyl methacrylate is replaced by acrylamide; The specific steps are as follows: (1) Add 1 g of Span-80 to 40 g of petroleum ether, heat and stir in a water bath at 100°C for 30 minutes to obtain an oil phase; (2) Chop the chicken bones and place them in 0.5 mol·L -1 The samples were decalcified by stirring in disodium ethylenediaminetetraacetic acid for 24 h and then washed with deionized water. -1Soak in NaOH solution for 24 hours, wash with deionized water until neutral; then soak in 15% isopropanol solution for 24 hours, wash with deionized water after soaking, and dry to obtain bone powder; Weigh 2.5 g of bone powder and disperse it in 75 g of deionized water, then add 9 g of acrylamide, 0.04 g of N,N-methylenebisacrylamide and 0.13 g of ammonium persulfate, react in a 35°C water bath for 1 h, filter and wash after the reaction, and dry at 100°C for 3 h to obtain modified bone powder; (3) adding 2.5 g of acrylic acid, 1 g of acrylamide, 1.5 g of modified bone powder and 0.35 g of 2-acrylamide-2-methylpropanesulfonic acid to 90 g of deionized water to obtain an aqueous phase; (4) Add 0.75 g of 1% potassium persulfate KPS and 0.75 g of 1% MBA solution to the aqueous phase obtained in step (3), stir in a 100°C water bath for 6 h, and then drop into the oil phase obtained in step (1). After the reaction is completed, filter, wash, and dry in a 100°C drying oven for 24 h to obtain an antibacterial superabsorbent resin.
[0025] Comparative Example 4 The difference between Comparative Example 4 and Example 3 is that: in step (2), 5 g of acrylamide, 4 g of tert-butylaminoethyl methacrylate, 0.04 g of N,N-methylenebisacrylamide and 0.13 g of ammonium persulfate are reacted in a water bath at 35° C. for 1 h, filtered, washed and dried after the reaction is completed, 100 g of N,N-dimethylacetamide is added after drying, and then 80 g of chloroalkane is added, and stirred at 100° C. for 6 h to obtain a quaternary ammonium salt, which is then mixed with bone powder to obtain a mixture; The specific steps are as follows: (1) Add 1 g of Span-80 to 40 g of petroleum ether, heat and stir in a water bath at 100°C for 30 minutes to obtain an oil phase; (2) Chop the chicken bones and place them in 0.5 mol·L -1 The samples were decalcified by stirring in disodium ethylenediaminetetraacetic acid for 24 h and then washed with deionized water. -1 Soak in NaOH solution for 24 hours, wash with deionized water until neutral; then soak in 15% isopropanol solution for 24 hours, wash with deionized water after soaking, and dry to obtain bone powder; First, 5 g of acrylamide, 4 g of tert-butylaminoethyl methacrylate, 0.04 g of N,N-methylenebisacrylamide and 0.13 g of ammonium persulfate are reacted in a 35° C. water bath for 1 h. After the reaction is completed, the mixture is filtered, washed and dried. After drying, 100 g of N,N-dimethylacetamide is added, and then 80 g of chloroalkane is added. The mixture is stirred at 100° C. for 6 h to obtain a quaternary ammonium salt. Then, 75 g of deionized water and 2.5 g of bone powder are added to obtain a mixture. (3) adding 2.5 g of acrylic acid, 1 g of acrylamide, 1.5 g of the mixture and 0.35 g of 2-acrylamide-2-methylpropanesulfonic acid to 90 g of deionized water to obtain an aqueous phase; (4) Add 0.75 g of 1% potassium persulfate KPS and 0.75 g of 1% MBA solution to the aqueous phase obtained in step (3), stir in a 100°C water bath for 6 h, and then drop into the oil phase obtained in step (1). After the reaction is completed, filter, wash, and dry in a 100°C drying oven for 24 h to obtain an antibacterial superabsorbent resin.
[0026] Comparative Example 5 The difference between Comparative Example 5 and Example 3 is that: 2-acrylamide-2-methylpropanesulfonic acid is not added in step (3); The specific steps are as follows: (1) Add 1 g of Span-80 to 40 g of petroleum ether, heat and stir in a water bath at 100°C for 30 minutes to obtain an oil phase; (2) Chop the chicken bones and place them in 0.5 mol·L -1 The samples were decalcified by stirring in disodium ethylenediaminetetraacetic acid for 24 h and then washed with deionized water. -1 Soak in NaOH solution for 24 hours, wash with deionized water until neutral; then soak in 15% isopropanol solution for 24 hours, wash with deionized water after soaking, and dry to obtain bone powder; Weigh 2.5 g of bone powder and disperse it in 75 g of deionized water, then add 5 g of acrylamide, 4 g of tert-butylaminoethyl methacrylate, 0.04 g of N,N-methylenebisacrylamide and 0.13 g of ammonium persulfate, react in a 35°C water bath for 1 h, filter, wash and dry after the reaction, add 100 g of N,N-dimethylacetamide after drying, and then add 80 g of chloroalkane, stir at 100°C for 6 h, then wash with water and dry at 100°C for 3 h to obtain modified bone powder; (3) Add 2.5 g of acrylic acid, 1 g of acrylamide, and 1.5 g of modified bone powder to 90 g of deionized water to obtain an aqueous phase; (4) Add 0.75 g of 1% potassium persulfate KPS and 0.75 g of 1% MBA solution to the aqueous phase obtained in step (3), stir in a 100°C water bath for 6 h, and then drop into the oil phase obtained in step (1). After the reaction is completed, filter, wash, and dry in a 100°C drying oven for 24 h to obtain an antibacterial superabsorbent resin.
[0027] Performance Testing: 1. Determination of water absorption rate: Weigh the net bag (mass m1) and a certain amount of dry resin (mass m0) respectively, put them into the net bag and place them in 100 g of deionized saline solution, and let it stand for 48 hours. After standing, wipe the moisture on the surface of the net bag, weigh the total weight of the net bag after saturation, and measure its water absorption rate Q after swelling equilibrium, which can reflect the maximum water absorption capacity of the super absorbent resin. Q = (m-m1-m0) / m0; 2. Determination of water retention performance: Accurately weigh a certain amount of resin and put it into physiological saline. After saturation with water, put the absorbent gel into a centrifuge and centrifuge it at a fixed speed for a certain period of time. Weigh the wet weight after centrifugation to reflect the water retention capacity of the highly absorbent resin after absorbing water, which directly affects its comfort and use effect in diapers. The calculation formula is as follows: R n =m n / m1×100%, Among them, R n is the water retention rate of super absorbent resin at a fixed speed for a certain period of time, %; m n is the mass of the super absorbent resin gel after centrifugation at a fixed speed for a certain period of time, g; m1 is the initial weight of the super absorbent resin gel, g; 3. Determination of water absorption rate: Weigh a certain amount of dry resin (mass m0), and measure the mass m of the highly absorbent resin gel within a specified time (1 minute, 5 minutes). v , the higher the water absorption rate, the more water-absorbent resin can quickly absorb a large amount of wild liquid in a short time, prevent leakage, and improve comfort and protection. The calculation formula is as follows: R v =(m v -m0) / m0×100%, 4. Determination of antibacterial properties: The antibacterial ring method is used to test the antibacterial properties of the resin. The highly absorbent resin is placed on an agar plate and the size of the inhibition zone formed around it is measured to evaluate the antibacterial properties. 5. Softness test: Use a softness tester to measure the bending resistance of the sample itself and the maximum vector sum of the friction between the sample and the gap, expressed in millinewton (mN). The smaller the resin, the softer the sample.
[0028] Table 1 Performance test results
[0029] Data Analysis: From the data of Examples 1-4 in Table 1, it can be seen that the water absorption rate, water retention rate and water absorption rate of the super absorbent resin prepared by the present invention are relatively excellent, the water absorption rate reaches more than 650 g / g, and the water retention rate can reach more than 80%, indicating that the diapers prepared by the super absorbent resin prepared by the present invention have better comfort and use effect, and can effectively prevent leakage; the diameter of the antibacterial ring reaches about 25 mm, indicating that the super absorbent resin prepared by the present invention has a good antibacterial effect, and the softness reaches 8.5 mN, indicating that the personal care products prepared by the super absorbent resin prepared by the present invention have better comfort.
[0030] It can be seen from the data of Example 2 and Comparative Example 1 that the modified bone meal helps to improve the water absorption, water retention and water absorption rate of the resin, which is mainly due to the porous structure of the bone meal and the hydrophilic cross-linked network on the surface. Most importantly, the addition of modified bone meal can significantly improve the antibacterial properties of the resin, which is mainly due to the synergistic antibacterial effect of the bone meal and the quaternary ammonium salt on the surface of the modified bone meal. In addition, the cross-linked network structure formed between the modified bone meal and the matrix resin gives the resin higher softness.
[0031] It can be seen from the data of Example 2 and Comparative Example 2 that the surface modification of bone meal can further improve the water absorption and water retention of the resin, and most importantly, improve the antibacterial properties and softness, which is mainly due to the quaternary ammonium salt in the bone meal surface network and the cross-linking effect between the bone meal surface network and the matrix network.
[0032] It can be seen from the data of Example 3 and Comparative Examples 3 and 4 that, under the action of an initiator, acrylamide, tert-butylaminoethyl methacrylate and N,N-methylenebisacrylamide are polymerized on the surface of bone powder, and the tert-butylamino group is converted into a quaternary ammonium salt through a quaternization reaction to construct a modified bone powder containing a quaternary ammonium salt network structure on the surface, which can improve water absorption and retention, mainly because the network structure is formed by polymerization on the surface of the bone powder, and at the same time improve the antibacterial effect and softness, mainly because the tert-butylamino group is converted into a quaternary ammonium salt through a quaternization reaction.
[0033] From the data of Example 3 and Comparative Example 5, it can be seen that adding 2-acrylamide-2-methylpropane sulfonic acid and constructing a modified bone powder with a quaternary ammonium salt network structure on the surface can improve water absorption and softness, which is mainly because the combination of sulfonic group and ammonium group promotes the formation of a network structure.
[0034] The above description is only a preferred embodiment of the present invention, but is not intended to limit the present invention. Those skilled in the art may make possible changes and modifications to the present invention using the technical contents disclosed above without departing from the scope of the technical solution of the present invention, or modify it into an equivalent embodiment of equivalent changes. Any simple modification, equivalent change and modification made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention shall fall within the protection scope of the technical solution of the present invention.
Claims
1. A method for preparing an antibacterial superabsorbent resin for diapers, characterized in that: The method comprises the following steps: Step (1): heating and stirring the hydrophobic solvent and Span-80 at 90-105° C. for 20-30 minutes to obtain an oil phase; Step (2): dispersing bone powder in deionized water, then adding acrylamide, tert-butylaminoethyl methacrylate, N,N-methylenebisacrylamide and initiator, reacting in a water bath at 30-40° C. for 1-1.5 h, filtering, washing and drying, and then converting the tert-butylamino group into a quaternary ammonium salt through a quaternization reaction, followed by water washing and drying to obtain modified bone powder, wherein the mass ratio of the bone powder, acrylamide, tert-butylaminoethyl methacrylate, N,N-methylenebisacrylamide and initiator is 1-3:2-6:3-5:0.01-0.05:0.1-0.15; Step (3): adding acrylic acid, acrylamide, modified bone powder and 2-acrylamide-2-methylpropane sulfonic acid into deionized water to obtain an aqueous phase, wherein the mass ratio of the acrylic acid, acrylamide, modified bone powder and 2-acrylamide-2-methylpropane sulfonic acid is 1.5-5:1-3:0.5-2:0.1-0.5; Step (4): Add potassium persulfate KPS and MBA solution to the aqueous phase obtained in step (3), stir in a water bath at 90-105° C. for 4-6 hours, and then drop into the oil phase obtained in step (1). After the reaction is completed, filter, wash and dry to obtain an antibacterial super absorbent resin.
2. The method for preparing the antibacterial super absorbent resin for diapers according to claim 1, characterized in that: The hydrophobic solvent in step (1) is one of petroleum ether, n-hexane and paraffin.
3. The method for preparing the antibacterial super absorbent resin for diapers according to claim 1, characterized in that: The mass ratio of the hydrophobic solvent to Span-80 in step (1) is 40-50:
1.
4. The method for preparing the antibacterial superabsorbent resin for diapers according to claim 1, characterized in that: Step (2) The specific steps are as follows: The bone powder is dispersed in deionized water, and then acrylamide, tert-butylaminoethyl methacrylate, N,N-methylenebisacrylamide and an initiator are added, and the mixture is reacted in a water bath at 30-40°C for 1-1.5 hours, filtered, washed and dried, and an anhydrous organic solvent is added after drying, and then an alkyl halide is added, and the mixture is stirred at 80-100°C for 4-6 hours, and then washed with water and dried to obtain modified bone powder, wherein the mass ratio of the bone powder, acrylamide, tert-butylaminoethyl methacrylate, N,N-methylenebisacrylamide and the initiator is 1-3:2-6:3-5:0.01-0.05:0.1-0.
15.
5. The method for preparing the antibacterial super absorbent resin for diapers according to claim 4, characterized in that: The alkane halide is one of alkyl bromide, ethyl iodide and alkyl chloride.
6. The method for preparing the antibacterial super absorbent resin for diapers according to claim 4, characterized in that: The anhydrous organic solvent is one of ethanol, ether and N,N-dimethylacetamide.
7. The method for preparing the antibacterial super absorbent resin for diapers according to claim 1, characterized in that: The preparation method of the bone meal is as follows: The chicken bones were chopped and placed in 0.5 mol·L -1 The samples were decalcified by stirring in disodium ethylenediaminetetraacetic acid for 24 h and then washed with deionized water. -1 Soak in NaOH solution for 24 h, wash with deionized water until neutral; then soak in 15% isopropanol solution for 24 h, wash with deionized water and dry.
8. The method for preparing the antibacterial super absorbent resin for diapers according to claim 1, characterized in that: The initiator in step (2) is one of sodium persulfate, ammonium persulfate and potassium persulfate.
9. The method for preparing the antibacterial super absorbent resin for diapers according to claim 1, characterized in that: In step (2), the drying temperature is 80-100°C and the drying time is 2-3h.
10. An antibacterial superabsorbent resin for diapers, characterized in that: Obtained according to the preparation method according to any one of claims 1 to 8.
Citation Information
Patent Citations
Super absorbent resin and preparation method
CN112552468A