CN116139325A - Super absorbent filler for adult paper diapers and preparation method thereof - Google Patents
Super absorbent filler for adult paper diapers and preparation method thereof Download PDFInfo
- Publication number
- CN116139325A CN116139325A CN202310157907.8A CN202310157907A CN116139325A CN 116139325 A CN116139325 A CN 116139325A CN 202310157907 A CN202310157907 A CN 202310157907A CN 116139325 A CN116139325 A CN 116139325A
- Authority
- CN
- China
- Prior art keywords
- stirring
- super absorbent
- dmf
- filler
- steps
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/60—Liquid-swellable gel-forming materials, e.g. super-absorbents
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/20—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing organic materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/24—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/40—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing ingredients of undetermined constitution or reaction products thereof, e.g. plant or animal extracts
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/425—Porous materials, e.g. foams or sponges
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/08—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin
- D06M14/10—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Public Health (AREA)
- Materials Engineering (AREA)
- Epidemiology (AREA)
- Hematology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Veterinary Medicine (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Botany (AREA)
- Zoology (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Textile Engineering (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a super absorbent filler for adult paper diapers and a preparation method thereof, wherein polyvinyl alcohol fibers and glycidyl methacrylate are subjected to free radical polymerization under the action of ceric ammonium nitrate to prepare reinforcing fibers, rice hulls are cleaned, acrylic acid, N-methylene bisacrylamide and a modified additive are subjected to graft polymerization on cellulose under the action of potassium persulfate to prepare a pretreatment material, the reinforcing filler and the reinforcing fibers are mixed and react with diethylenetriamine to prepare the super absorbent filler, and the modified additive is added to form a spiral polyacrylic acid molecular coating on the surfaces of the rice hulls.
Description
Technical Field
The invention relates to the field of preparation of water-absorbing materials, in particular to a super-absorbent filler for adult paper diapers and a preparation method thereof.
Background
Paper diapers are a common sanitary article. Generally, diapers consist of three main parts: surface covering layer, absorbent core layer and base fabric. The surface coating may also be referred to as a coating. The absorbent core layer may also be referred to as an absorbent core, or an absorbent body. The coating layer is closely attached to the body of the infant, can promote the urine to quickly permeate and effectively prevent rewet, and ensures that the surface layer of the diaper is kept dry. The coating layer of the paper diaper on the domestic market is basically a non-woven fabric surface layer, the breathable non-woven fabric can improve the breathable degree inside the diaper, water vapor can circulate outside the diaper, moisture and hot air can be timely discharged, and the diaper is soft and comfortable and does not irritate skin. The absorbent core layer may also be referred to as an absorbent core. The main function of the absorbent core layer is to capture and rapidly absorb urine, disperse urine or diffuse urine into the whole core layer by capillary action and finally absorb and store urine, and the absorbent core layer is a water-absorbing filler, but the existing water-absorbing filler cannot meet the absorption of adult urine.
Disclosure of Invention
The invention aims to provide a super absorbent filler for an adult diaper and a preparation method thereof, which solve the problems that the speed of absorbing urine by the adult diaper is common and the pungent smell in the urine can not be removed at present.
The aim of the invention can be achieved by the following technical scheme:
the preparation method of the super absorbent filler for the adult paper diaper specifically comprises the following steps:
step S1: uniformly mixing polyvinyl alcohol fibers, glycidyl methacrylate and deionized water, stirring and adding ceric ammonium nitrate under the condition that the rotating speed is 200-300r/min and the pH value is 3-5, and stirring for 4-6 hours to obtain reinforcing fibers;
step S2: washing rice hulls with deionized water, adding the rice hulls into a sodium hydroxide solution, stirring for 7-9 hours at the rotation speed of 150-200r/min and the temperature of 65-70 ℃, introducing nitrogen for protection, adding potassium persulfate, stirring for 10-15 minutes, adding acrylic acid, N-methylenebisacrylamide and a modification additive, reacting for 2-3 hours, and washing with deionized water to obtain a pretreatment material;
step S3: dispersing the pretreatment material, the reinforcing filler and the reinforcing cellulose in deionized water, adding diethylenetriamine, reacting for 8-10 hours under the conditions of the rotating speed of 60-120r/min and the pH value of 10-11, filtering to remove filtrate, and drying a substrate to obtain the super absorbent filler.
Further, the dosage ratio of the polyvinyl alcohol fiber, the glycidyl methacrylate, the deionized water and the ceric ammonium nitrate in the step S1 is 5g to 3g to 150mL to 60mmol.
Further, the rice hulls, the sodium hydroxide solution, the potassium persulfate, the acrylic acid, the N, N-methylene bisacrylamide and the modifying additive in the step S2 are used in a mass ratio of 1g to 15mL to 50mg to 30mg to 5mg to 30g, and the mass fraction of the sodium hydroxide solution is 20%.
Further, the dosage ratio of the pretreatment material to the reinforcing filler to the reinforcing cellulose in the step S3 is 3:2:1, and the dosage of the diethylenetriamine is 10-15% of the mass of the pretreatment material to the reinforcing filler to the mass of the reinforcing cellulose.
Further, the modified additive is prepared by the following steps:
step A1: uniformly mixing vanillin, pentaerythritol, paratoluenesulfonic acid, DMF and petroleum ether, stirring and refluxing for 10-15 hours at the rotation speed of 200-300r/min and the temperature of 90-100 ℃, adding sodium bicarbonate aqueous solution, standing for precipitation, filtering and removing filtrate to obtain an intermediate 1, uniformly mixing cyanuric chloride, the intermediate 1, triethylamine and DMF, stirring and treating for 6-8 hours at the rotation speed of 150-200r/min and the temperature of 40-50 ℃ to obtain an intermediate 2;
step A2: mixing epoxy chloropropane and tetrabutylammonium bisulfate, adding the intermediate 2 and DMF at the rotating speed of 150-200r/min and the temperature of 0-3 ℃, stirring for 30-40min, adding sodium hydroxide solution, heating to 15-20 ℃, reacting for 3-4h to obtain the intermediate 3, dissolving the intermediate 3 in DMF, adding triethylamine, stirring and adding diethanolamine at the rotating speed of 200-300r/min and the temperature of 80-90 ℃, stirring for 1-1.5h, adding acryloyl chloride, continuously reacting for 3-5h, distilling to remove DMF, and obtaining the modified additive.
Further, the dosage ratio of vanillin, pentaerythritol, DMF, petroleum ether and sodium bicarbonate aqueous solution in the step A1 is 40g:18g:150mL:75mL:500mL, the dosage of p-toluenesulfonic acid is 2% of the sum of the masses of vanillin and pentaerythritol, the mass fraction of sodium bicarbonate aqueous solution is 3-5%, and the molar ratio of cyanuric chloride, intermediate 1 and triethylamine is 1:2:2.1.
Further, the dosage ratio of the epichlorohydrin to the tetrabutylammonium bisulfate to the intermediate 2 to the DMF to the sodium hydroxide solution in the step A2 is 100mmol:8.5mmol:50mmol:200:160mL, the mass fraction of the sodium hydroxide solution is 35%, and the molar ratio of the intermediate 3 to the triethylamine to the diethanolamine to the acryloyl chloride is 1:3.1:1:2.
Further, the reinforcing filler is prepared by the following steps:
mixing natural zeolite, zirconium chloride, terephthalic acid, trimellitic acid, hydrochloric acid and DMF, stirring at a rotation speed of 200-300r/min and a temperature of 20-25 ℃ for 10-15min, heating to a temperature of 120-130 ℃, reacting for 20-25h, filtering to remove filtrate, dispersing a substrate in toluene, adding 2-hydroxy-1, 3-propanediamine and p-toluenesulfonic acid, stirring at a rotation speed of 150-200r/min and a temperature of 115-120 ℃ for reflux for 6-8h, and filtering to remove filtrate to obtain the reinforcing filler.
Further, the dosage ratio of the natural zeolite to the zirconium chloride to the terephthalic acid to the trimellitic acid to the hydrochloric acid to the DMF is 1.5g to 20mmol to 40mmol to 10mmol to 40mmol to 150mL, the molar ratio of carboxyl on the surface of the substrate to 2-hydroxy-1, 3-propanediamine is 1:1, and the dosage of the p-toluenesulfonic acid is 3-5% of the mass of the 2-hydroxy-1, 3-propanediamine.
The invention has the beneficial effects that: the invention provides a super absorbent filler for adult paper diapers, which is prepared by free radical polymerization of polyvinyl alcohol fiber and glycidyl methacrylate under the action of ceric ammonium nitrate, further introducing epoxy groups into the side chains of the fiber to prepare reinforcing fiber, cleaning rice hulls, adding sodium hydroxide solution to dissolve lignin in the rice hulls and swell cellulose, graft polymerizing acrylic acid, N-methylene bisacrylamide and a modifying additive on the cellulose under the action of potassium persulfate to prepare a pretreatment material, mixing the pretreatment material, the reinforcing filler and the reinforcing fiber to react with diethylenetriamine, reacting the epoxy groups on the pretreatment material and the reinforcing fiber with amino groups on the surfaces of the reinforcing filler and amino groups on the diethylenetriamine, and further crosslinking to prepare the super absorbent filler, wherein the modifying additive takes vanillin and pentaerythritol as raw materials, under the action of p-toluenesulfonic acid, the aldehyde group of vanillin and two alcohol hydroxyl groups of pentaerythritol are subjected to diacetal reaction to prepare an intermediate 1, cyanuric chloride and the intermediate 1 are subjected to temperature and dosage control, so that two chlorine atom sites on cyanuric chloride react with phenolic hydroxyl groups on the intermediate 1 to prepare an intermediate 2, epoxy chloropropane reacts with the phenolic hydroxyl groups on the intermediate 2, then the epoxy groups are closed under the action of sodium hydroxide to form end capping, so as to prepare an intermediate 3, the intermediate 3 reacts with diethanol amine to react with chlorine atom sites with secondary amine on diethanol amine, then acryloyl chloride is added to react with the alcohol hydroxyl groups to prepare a modified additive, and the addition of the modified additive forms spiral polyacrylic acid molecular coating on the surface of rice hull fibers, so that the structure can accelerate the water absorption rate of the material, meanwhile, a good water locking effect can be achieved, the dryness of the paper diaper is further guaranteed, the crosslinking density of the pretreatment material, the reinforcing filler, the reinforcing fiber and the diethylenetriamine after crosslinking is improved, the multi-material composite crosslinking structure enables the water absorption capacity of the water absorbing material to be further improved, and the inside of the water absorbing material contains zirconium-based zeolite and a porous spiral structure, so that ammonia odor emitted by urine can be absorbed.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the super absorbent filler for the adult paper diaper specifically comprises the following steps:
step S1: uniformly mixing polyvinyl alcohol fibers, glycidyl methacrylate and deionized water, stirring and adding ceric ammonium nitrate under the conditions of 200r/min rotational speed and 3 pH value, and stirring for 4 hours to obtain reinforced fibers;
step S2: washing rice hulls with deionized water, adding the rice hulls into a sodium hydroxide solution, stirring for 7 hours at the rotating speed of 150r/min and the temperature of 65 ℃, introducing nitrogen for protection, adding potassium persulfate, stirring for 10 minutes, adding acrylic acid, N-methylene bisacrylamide and a modified additive, reacting for 2 hours, and washing with deionized water to obtain a pretreatment material;
step S3: dispersing the pretreatment material, the reinforcing filler and the reinforcing cellulose in deionized water, adding diethylenetriamine, reacting for 8 hours under the condition of the rotating speed of 60r/min and the pH value of 10, filtering to remove filtrate, and drying the substrate to obtain the super absorbent filler.
The dosage ratio of the polyvinyl alcohol fiber, the glycidyl methacrylate, the deionized water and the ceric ammonium nitrate in the step S1 is 5g to 3g to 150mL to 60mmol.
The dosage ratio of the rice hulls to the sodium hydroxide solution to the potassium persulfate to the acrylic acid to the N, N-methylenebisacrylamide to the modifying additive in the step S2 is 1g to 15mL to 50mg to 30mg to 5mg to 30g, and the mass fraction of the sodium hydroxide solution is 20%.
The dosage ratio of the pretreatment material to the reinforcing filler to the reinforcing cellulose in the step S3 is 3:2:1, and the dosage of the diethylenetriamine is 10% of the mass of the pretreatment material to the reinforcing filler to the mass of the reinforcing cellulose.
The modified additive is prepared by the following steps:
step A1: uniformly mixing vanillin, pentaerythritol, paratoluenesulfonic acid, DMF and petroleum ether, stirring and refluxing for 10 hours at the rotation speed of 200r/min and the temperature of 90 ℃, adding sodium bicarbonate aqueous solution, standing for precipitation, filtering to remove filtrate to obtain an intermediate 1, uniformly mixing cyanuric chloride, the intermediate 1, triethylamine and DMF, and stirring and treating for 6 hours at the rotation speed of 150r/min and the temperature of 40 ℃ to obtain an intermediate 2;
step A2: mixing epoxy chloropropane and tetrabutylammonium bisulfate, adding the intermediate 2 and DMF at the rotating speed of 150r/min and the temperature of 0 ℃, stirring for 30min, adding a sodium hydroxide solution, heating to 15 ℃, reacting for 3h to obtain an intermediate 3, dissolving the intermediate 3 in DMF, adding triethylamine, stirring and adding diethanolamine at the rotating speed of 200r/min and the temperature of 80 ℃, stirring for 1h, adding acryloyl chloride, continuously reacting for 3h, and distilling to remove DMF to obtain the modified additive.
The dosage ratio of vanillin, pentaerythritol, DMF, petroleum ether and sodium bicarbonate aqueous solution in the step A1 is 40g:18g:150mL:75mL:500mL, the dosage of p-toluenesulfonic acid is 2% of the sum of the masses of vanillin and pentaerythritol, the mass fraction of sodium bicarbonate aqueous solution is 3-5%, and the molar ratio of cyanuric chloride, intermediate 1 and triethylamine is 1:2:2.1.
The dosage ratio of the epichlorohydrin to the tetrabutylammonium bisulfate to the intermediate 2 to the DMF to the sodium hydroxide solution in the step A2 is 100mmol:8.5mmol:50mmol:200:160mL, the mass fraction of the sodium hydroxide solution is 35%, and the molar ratio of the intermediate 3 to the triethylamine to the diethanolamine to the acryloyl chloride is 1:3.1:1:2.
The reinforcing filler is prepared by the following steps:
mixing natural zeolite, zirconium chloride, terephthalic acid, trimellitic acid, hydrochloric acid and DMF, stirring at a rotation speed of 200r/min and a temperature of 20 ℃ for 10min, heating to a temperature of 120 ℃, reacting for 20h, filtering to remove filtrate, dispersing a substrate in toluene, adding 2-hydroxy-1, 3-propanediamine and p-toluenesulfonic acid, stirring at a rotation speed of 150r/min and a temperature of 115 ℃ and refluxing for 6h, and filtering to remove filtrate to obtain the reinforcing filler.
The dosage ratio of the natural zeolite to the zirconium chloride to the terephthalic acid to the trimellitic acid to the hydrochloric acid to the DMF is 1.5g to 20mmol to 40mmol to 10mmol to 40mmol to 150mL, the molar ratio of carboxyl on the surface of the substrate to 2-hydroxy-1, 3-propanediamine is 1:1, and the dosage of the p-toluenesulfonic acid is 3% of the mass of the 2-hydroxy-1, 3-propanediamine.
Example 2
The preparation method of the super absorbent filler for the adult paper diaper specifically comprises the following steps:
step S1: uniformly mixing polyvinyl alcohol fibers, glycidyl methacrylate and deionized water, stirring and adding ceric ammonium nitrate under the conditions of 200r/min rotational speed and 4 pH value, and stirring for 5 hours to obtain reinforced fibers;
step S2: washing rice hulls with deionized water, adding the rice hulls into a sodium hydroxide solution, stirring for 8 hours at the rotation speed of 200r/min and the temperature of 65 ℃, introducing nitrogen for protection, adding potassium persulfate, stirring for 10 minutes, adding acrylic acid, N-methylene bisacrylamide and a modified additive, reacting for 3 hours, and washing with deionized water to obtain a pretreatment material;
step S3: dispersing the pretreatment material, the reinforcing filler and the reinforcing cellulose in deionized water, adding diethylenetriamine, reacting for 9 hours under the condition of the rotating speed of 60r/min and the pH value of 11, filtering to remove filtrate, and drying the substrate to obtain the super absorbent filler.
The dosage ratio of the polyvinyl alcohol fiber, the glycidyl methacrylate, the deionized water and the ceric ammonium nitrate in the step S1 is 5g to 3g to 150mL to 60mmol.
The dosage ratio of the rice hulls to the sodium hydroxide solution to the potassium persulfate to the acrylic acid to the N, N-methylenebisacrylamide to the modifying additive in the step S2 is 1g to 15mL to 50mg to 30mg to 5mg to 30g, and the mass fraction of the sodium hydroxide solution is 20%.
The dosage ratio of the pretreatment material to the reinforcing filler to the reinforcing cellulose in the step S3 is 3:2:1, and the dosage of the diethylenetriamine is 13% of the mass of the pretreatment material to the reinforcing filler to the mass of the reinforcing cellulose.
The modified additive is prepared by the following steps:
step A1: uniformly mixing vanillin, pentaerythritol, paratoluenesulfonic acid, DMF and petroleum ether, stirring and refluxing for 13 hours at the rotation speed of 200r/min and the temperature of 95 ℃, adding sodium bicarbonate aqueous solution, standing for precipitation, filtering to remove filtrate to obtain an intermediate 1, uniformly mixing cyanuric chloride, the intermediate 1, triethylamine and DMF, and stirring for 7 hours at the rotation speed of 150r/min and the temperature of 45 ℃ to obtain an intermediate 2;
step A2: mixing epoxy chloropropane and tetrabutylammonium bisulfate, adding the intermediate 2 and DMF at the rotating speed of 200r/min and the temperature of 3 ℃, stirring for 35min, adding a sodium hydroxide solution, heating to 20 ℃, reacting for 3h to obtain the intermediate 3, dissolving the intermediate 3 in DMF, adding triethylamine, stirring and adding diethanolamine at the rotating speed of 200r/min and the temperature of 85 ℃, stirring for 1h, adding acryloyl chloride, continuously reacting for 4h, and distilling to remove DMF to obtain the modified additive.
The dosage ratio of vanillin, pentaerythritol, DMF, petroleum ether and sodium bicarbonate aqueous solution in the step A1 is 40g:18g:150mL:75mL:500mL, the dosage of p-toluenesulfonic acid is 2% of the sum of the masses of vanillin and pentaerythritol, the mass fraction of sodium bicarbonate aqueous solution is 4%, and the molar ratio of cyanuric chloride to intermediate 1 to triethylamine is 1:2:2.1.
The dosage ratio of the epichlorohydrin to the tetrabutylammonium bisulfate to the intermediate 2 to the DMF to the sodium hydroxide solution in the step A2 is 100mmol:8.5mmol:50mmol:200:160mL, the mass fraction of the sodium hydroxide solution is 35%, and the molar ratio of the intermediate 3 to the triethylamine to the diethanolamine to the acryloyl chloride is 1:3.1:1:2.
The reinforcing filler is prepared by the following steps:
mixing natural zeolite, zirconium chloride, terephthalic acid, trimellitic acid, hydrochloric acid and DMF, stirring at a rotation speed of 200r/min and a temperature of 25 ℃ for 10min, heating to a temperature of 125 ℃, reacting for 25h, filtering to remove filtrate, dispersing a substrate in toluene, adding 2-hydroxy-1, 3-propanediamine and p-toluenesulfonic acid, stirring at a rotation speed of 150r/min and a temperature of 120 ℃ and refluxing for 7h, and filtering to remove filtrate to obtain the reinforcing filler.
The dosage ratio of the natural zeolite to the zirconium chloride to the terephthalic acid to the trimellitic acid to the hydrochloric acid to the DMF is 1.5g to 20mmol to 40mmol to 10mmol to 40mmol to 150mL, the molar ratio of carboxyl on the surface of the substrate to 2-hydroxy-1, 3-propanediamine is 1:1, and the dosage of the p-toluenesulfonic acid is 4% of the mass of the 2-hydroxy-1, 3-propanediamine.
Example 3
The preparation method of the super absorbent filler for the adult paper diaper specifically comprises the following steps:
step S1: uniformly mixing polyvinyl alcohol fibers, glycidyl methacrylate and deionized water, stirring and adding ceric ammonium nitrate under the conditions of the rotating speed of 300r/min and the pH value of 5, and stirring for 6 hours to obtain reinforced fibers;
step S2: washing rice hulls with deionized water, adding the rice hulls into a sodium hydroxide solution, stirring for 9 hours at the rotation speed of 200r/min and the temperature of 70 ℃, introducing nitrogen for protection, adding potassium persulfate, stirring for 15 minutes, adding acrylic acid, N-methylene bisacrylamide and a modified additive, reacting for 3 hours, and washing with deionized water to obtain a pretreatment material;
step S3: dispersing the pretreatment material, the reinforcing filler and the reinforcing cellulose in deionized water, adding diethylenetriamine, reacting for 10 hours under the conditions of the rotating speed of 120r/min and the pH value of 11, filtering to remove filtrate, and drying the substrate to obtain the super absorbent filler.
The dosage ratio of the polyvinyl alcohol fiber, the glycidyl methacrylate, the deionized water and the ceric ammonium nitrate in the step S1 is 5g to 3g to 150mL to 60mmol.
The dosage ratio of the rice hulls to the sodium hydroxide solution to the potassium persulfate to the acrylic acid to the N, N-methylenebisacrylamide to the modifying additive in the step S2 is 1g to 15mL to 50mg to 30mg to 5mg to 30g, and the mass fraction of the sodium hydroxide solution is 20%.
The dosage ratio of the pretreatment material to the reinforcing filler to the reinforcing cellulose in the step S3 is 3:2:1, and the dosage of the diethylenetriamine is 15% of the mass of the pretreatment material to the reinforcing filler to the mass of the reinforcing cellulose.
The modified additive is prepared by the following steps:
step A1: uniformly mixing vanillin, pentaerythritol, paratoluenesulfonic acid, DMF and petroleum ether, stirring and refluxing for 15 hours at the speed of 300r/min and the temperature of 100 ℃, adding sodium bicarbonate aqueous solution, standing for precipitation, filtering to remove filtrate to obtain an intermediate 1, uniformly mixing cyanuric chloride, the intermediate 1, triethylamine and DMF, and stirring and treating for 8 hours at the speed of 200r/min and the temperature of 50 ℃ to obtain an intermediate 2;
step A2: mixing epoxy chloropropane and tetrabutylammonium bisulfate, adding the intermediate 2 and DMF at the rotation speed of 200r/min and the temperature of 3 ℃, stirring for 40min, adding a sodium hydroxide solution, heating to 20 ℃, reacting for 4h to obtain the intermediate 3, dissolving the intermediate 3 in DMF, adding triethylamine, stirring and adding diethanolamine at the rotation speed of 300r/min and the temperature of 90 ℃, stirring for 1.5h, adding acryloyl chloride, continuously reacting for 5h, and distilling to remove DMF to obtain the modified additive.
The dosage ratio of vanillin, pentaerythritol, DMF, petroleum ether and sodium bicarbonate aqueous solution in the step A1 is 40g:18g:150mL:75mL:500mL, the dosage of p-toluenesulfonic acid is 2% of the sum of the masses of vanillin and pentaerythritol, the mass fraction of sodium bicarbonate aqueous solution is 5%, and the molar ratio of cyanuric chloride to intermediate 1 to triethylamine is 1:2:2.1.
The dosage ratio of the epichlorohydrin to the tetrabutylammonium bisulfate to the intermediate 2 to the DMF to the sodium hydroxide solution in the step A2 is 100mmol:8.5mmol:50mmol:200:160mL, the mass fraction of the sodium hydroxide solution is 35%, and the molar ratio of the intermediate 3 to the triethylamine to the diethanolamine to the acryloyl chloride is 1:3.1:1:2.
The reinforcing filler is prepared by the following steps:
mixing natural zeolite, zirconium chloride, terephthalic acid, trimellitic acid, hydrochloric acid and DMF, stirring at a rotation speed of 300r/min and a temperature of 25 ℃, heating to 130 ℃ after stirring for 15min, reacting for 25h, filtering to remove filtrate, dispersing a substrate in toluene, adding 2-hydroxy-1, 3-propanediamine and p-toluenesulfonic acid, stirring at a rotation speed of 200r/min and a temperature of 120 ℃ and refluxing for 8h, and filtering to remove filtrate to obtain the reinforcing filler.
The dosage ratio of the natural zeolite to the zirconium chloride to the terephthalic acid to the trimellitic acid to the hydrochloric acid to the DMF is 1.5g to 20mmol to 40mmol to 10mmol to 40mmol to 150mL, the molar ratio of carboxyl on the surface of the substrate to 2-hydroxy-1, 3-propanediamine is 1:1, and the dosage of the p-toluenesulfonic acid is 5% of the mass of the 2-hydroxy-1, 3-propanediamine.
Comparative example 1
This comparative example was compared to example 1 without reinforcing fibers added, and the rest of the procedure was the same.
Comparative example 2
This comparative example was compared to example 1 without the addition of reinforcing filler, the remainder of the procedure being identical.
The super absorbent fillers prepared in examples 1 to 3 and comparative examples 1 to 2 were tested for the brine absorption multiple, absorption rate and water retention according to the GB/T22905-2008 standard, the ammonia removal was tested according to the following method, the super absorbent fillers prepared in examples 1 to 3 and comparative examples 1 to 2 were added to a vessel having an inlet and an outlet, ammonia gas having a mass concentration of 30% was added at a temperature of 25℃so that the gas remained in the vessel for 90 minutes and then was discharged, the ammonia gas concentration of the discharged gas was measured, and the ammonia gas removal rate was calculated, and the test results were shown in the following table;
as can be seen from the above table, the high water absorption filler prepared in examples 1-3 has a multiple of 66.3-67.1g/g of physiological saline, an absorption rate of 41.8-42.6s, a water retention capacity of 45.8-46.3g/g and an ammonia removal rate of 89.3-90.1%, which indicates that the high water absorption filler has good water absorption effect and deodorizing effect.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (10)
1. A preparation method of a super absorbent filler for an adult diaper is characterized by comprising the following steps: the method specifically comprises the following steps:
step S1: mixing and stirring polyvinyl alcohol fibers, glycidyl methacrylate and deionized water, adding ammonium ceric nitrate, and stirring to obtain reinforced fibers;
step S2: washing rice hulls with deionized water, adding the rice hulls into a sodium hydroxide solution, stirring, introducing nitrogen for protection, adding potassium persulfate, stirring, adding acrylic acid, N-methylene bisacrylamide and a modification additive, reacting, and washing with deionized water to obtain a pretreatment material;
step S3: dispersing the pretreatment material, the reinforcing filler and the reinforcing cellulose in deionized water, adding diethylenetriamine for reaction, filtering to remove filtrate, and drying the substrate to obtain the super absorbent filler.
2. The method for preparing the super absorbent filler for the adult diaper according to claim 1, wherein the method comprises the following steps: the dosage ratio of the polyvinyl alcohol fiber, the glycidyl methacrylate, the deionized water and the ceric ammonium nitrate in the step S1 is 5g:3g:150mL:60mmo l.
3. The method for preparing the super absorbent filler for the adult diaper according to claim 1, wherein the method comprises the following steps: the dosage ratio of the rice hulls to the sodium hydroxide solution to the potassium persulfate to the acrylic acid to the N, N-methylenebisacrylamide to the modifying additive in the step S2 is 1g to 15mL to 50mg to 30mg to 5mg to 30g, and the mass fraction of the sodium hydroxide solution is 20%.
4. The method for preparing the super absorbent filler for the adult diaper according to claim 1, wherein the method comprises the following steps: the dosage ratio of the pretreatment material to the reinforcing filler to the reinforcing cellulose in the step S3 is 3:2:1, and the dosage of the diethylenetriamine is 10-15% of the mass of the pretreatment material to the reinforcing filler to the mass of the reinforcing cellulose.
5. The method for preparing the super absorbent filler for the adult diaper according to claim 1, wherein the method comprises the following steps: the modified additive is prepared by the following steps:
step A1: mixing vanillin, pentaerythritol, paratoluenesulfonic acid, DMF and petroleum ether, refluxing, adding sodium bicarbonate aqueous solution, standing for precipitation, filtering to remove filtrate to obtain an intermediate 1, mixing cyanuric chloride, the intermediate 1, triethylamine and DMF, and stirring to obtain an intermediate 2;
step A2: mixing epichlorohydrin and tetrabutylammonium bisulfate, adding an intermediate 2 and DMF, stirring, adding a sodium hydroxide solution, heating to react to obtain an intermediate 3, dissolving the intermediate 3 in DMF, adding triethylamine, stirring, adding diethanolamine, stirring, adding acryloyl chloride to continue to react, and distilling to remove DMF to obtain the modified additive.
6. The method for preparing the super absorbent filler for the adult diaper according to claim 5, wherein the method comprises the following steps: the dosage ratio of vanillin, pentaerythritol, DMF, petroleum ether and sodium bicarbonate aqueous solution in the step A1 is 40g:18g:150mL:75mL:500mL, the dosage of p-toluenesulfonic acid is 2% of the sum of the masses of vanillin and pentaerythritol, the mass fraction of sodium bicarbonate aqueous solution is 3-5%, and the molar ratio of cyanuric chloride, intermediate 1 and triethylamine is 1:2:2.1.
7. The method for preparing the super absorbent filler for the adult diaper according to claim 5, wherein the method comprises the following steps: the dosage ratio of the epoxy chloropropane to the tetrabutylammonium bisulfate to the intermediate 2 to the DMF to the sodium hydroxide solution in the step A2 is 100mmo l:8.5mmo l:50mmo l:200:160mL, the mass fraction of the sodium hydroxide solution is 35%, and the molar ratio of the intermediate 3 to the triethylamine to the diethanolamine to the acryloyl chloride is 1:3.1:1:2.
8. The method for preparing the super absorbent filler for the adult diaper according to claim 1, wherein the method comprises the following steps: the reinforcing filler is prepared by the following steps:
mixing natural zeolite, zirconium chloride, terephthalic acid, trimellitic acid, hydrochloric acid and DMF, stirring, heating for reaction, filtering to remove filtrate, dispersing substrate in toluene, adding 2-hydroxy-1, 3-propanediamine and p-toluenesulfonic acid, stirring for reflux, filtering to remove filtrate, and obtaining the reinforcing filler.
9. The method for preparing the super absorbent filler for the adult diaper according to claim 8, wherein the method comprises the following steps: the dosage ratio of the natural zeolite to the zirconium chloride to the terephthalic acid to the trimellitic acid to the hydrochloric acid to the DMF is 1.5g to 20mmol to 40mmol to 10mmol to 40mmol to 150mL, the molar ratio of carboxyl on the surface of the substrate to 2-hydroxy-1, 3-propanediamine is 1:1, and the dosage of the p-toluenesulfonic acid is 3-5% of the mass of the 2-hydroxy-1, 3-propanediamine.
10. A super absorbent filler for an adult diaper, which is characterized in that: the preparation method according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310157907.8A CN116139325B (en) | 2023-02-23 | 2023-02-23 | Super absorbent filler for adult paper diapers and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310157907.8A CN116139325B (en) | 2023-02-23 | 2023-02-23 | Super absorbent filler for adult paper diapers and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116139325A true CN116139325A (en) | 2023-05-23 |
| CN116139325B CN116139325B (en) | 2023-08-01 |
Family
ID=86354087
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310157907.8A Active CN116139325B (en) | 2023-02-23 | 2023-02-23 | Super absorbent filler for adult paper diapers and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116139325B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102784621A (en) * | 2012-08-29 | 2012-11-21 | 西南科技大学 | Method for preparing biomass adsorption material based on modified rice husks |
| CN107513880A (en) * | 2017-07-12 | 2017-12-26 | 马鞍山科信网络科技有限公司 | A kind of fibre-reinforced composite mortar of paper grade (stock) modified coal ash and preparation method thereof |
| CN113605094A (en) * | 2021-08-28 | 2021-11-05 | 李胜 | Antibacterial degradable composite fiber and preparation method thereof |
| CN115369514A (en) * | 2022-08-26 | 2022-11-22 | 山西道空尽电子科技有限公司 | High-strength stab-resistant polyethylene fiber and preparation method thereof |
-
2023
- 2023-02-23 CN CN202310157907.8A patent/CN116139325B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102784621A (en) * | 2012-08-29 | 2012-11-21 | 西南科技大学 | Method for preparing biomass adsorption material based on modified rice husks |
| CN107513880A (en) * | 2017-07-12 | 2017-12-26 | 马鞍山科信网络科技有限公司 | A kind of fibre-reinforced composite mortar of paper grade (stock) modified coal ash and preparation method thereof |
| CN113605094A (en) * | 2021-08-28 | 2021-11-05 | 李胜 | Antibacterial degradable composite fiber and preparation method thereof |
| CN115369514A (en) * | 2022-08-26 | 2022-11-22 | 山西道空尽电子科技有限公司 | High-strength stab-resistant polyethylene fiber and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116139325B (en) | 2023-08-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7455902B2 (en) | Mixed polymer superabsorbent fibers | |
| US6500947B1 (en) | Superabsorbent polymer | |
| US4880868A (en) | Extended shelf life water-absorbing composition which facilitates fiber formation | |
| US4731067A (en) | Extended shelf life water-absorbing composition which facilitates fiber formation | |
| CA2488887C (en) | Chemically cross-linked cellulosic fiber and method of making same | |
| US20080079188A1 (en) | Methods for the preparation of mixed polymer superabsorbent fibers | |
| CA2602985A1 (en) | Mixed polymer superabsorbent fibers and method for their preparation | |
| JP2707089B2 (en) | Water absorbing composition | |
| CN101385868A (en) | Mixed polymer superabsorbent fibers containing cellulose | |
| US7749317B2 (en) | Fibrous blend and method of making | |
| CN101220556A (en) | Methods for the preparation of crosslinked carboxyalkyl cellulose fibers having permanent and non-permanent crosslinks | |
| CN108659434A (en) | Water-absorbent resin and method for producing same | |
| CN106987075A (en) | A kind of synthetic method with new structure water-absorbing resin | |
| CN109942753A (en) | A kind of macromolecule water uptake resin, composite absorption core and preparation method thereof | |
| CN116139325B (en) | Super absorbent filler for adult paper diapers and preparation method thereof | |
| CN109925127A (en) | A kind of absorbent article and its core | |
| EP0436514A2 (en) | Polymer compositions and absorbent fibers produced therefrom | |
| CN108914679B (en) | Paper special for paper diaper and production process thereof | |
| CN114288091B (en) | Preparation method of plant-based foam core | |
| CN106589243A (en) | Preparation method of bio-base superabsorbent resin composite absorbent core material | |
| US7300965B2 (en) | Mixed polymer network | |
| US5079306A (en) | Polymer compositions and absorbent fibers produced therefrom | |
| JP2003183528A (en) | Absorbent, absorber and absorptive product using the same | |
| CN114575141A (en) | Nano sea-island fibre/terylene composite material and its preparing method | |
| CN113756092A (en) | Washable antibacterial fabric and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |