CN111423542A - Multiple chemical crosslinking high-strength polyvinyl alcohol hydrogel and preparation method thereof - Google Patents
Multiple chemical crosslinking high-strength polyvinyl alcohol hydrogel and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of polyvinyl alcohol hydrogel, and discloses a multiple chemical crosslinking high-strength polyvinyl alcohol hydrogel, which comprises the following formula raw materials and components: alkenyl polyvinyl alcohol, acrylamide, alkenyl sodium alginate, ammonium persulfate, sodium bisulfite, N' -methylene bisacrylamide and boric acid. According to the high-strength polyvinyl alcohol hydrogel with multiple chemical crosslinks, ammonium persulfate and sodium bisulfite are used as a redox initiation system, alkenyl polyvinyl alcohol, alkenyl sodium alginate and acrylamide are copolymerized to form a polyvinyl alcohol-sodium alginate-acryloyl copolymer which is used as a first double chemical crosslink, N, N' -methylene bisacrylamide is crosslinked to form a three-dimensional network structure which is used as a second double chemical crosslink, boric acid and hydroxyl are crosslinked to form an interpenetrating network which is used as a third double chemical crosslink, and the compression modulus, the compression strength and the toughness of the polyvinyl alcohol composite hydrogel are remarkably improved.
Description
Technical Field
The invention relates to the technical field of polyvinyl alcohol hydrogel, in particular to high-strength polyvinyl alcohol hydrogel with multiple chemical crosslinks and a preparation method thereof.
Background
The hydrogel is a three-dimensional structure gel material with strong hydrophilicity, can rapidly swell in water and can keep a large volume of water without dissolving, such as polysaccharide hydrogel such as chitosan and sodium alginate, polypeptide hydrogel such as poly L-lysine and poly L-glutamic acid, and gel materials such as acrylamide and acrylic acid.
Polyvinyl alcohol has good hydrophilicity, chemical stability and biocompatibility, hydrogel can be formed in a physical crosslinking mode, the polyvinyl alcohol hydrogel has important application in the fields of industry, agriculture, medical treatment and the like, but the traditional polyvinyl alcohol hydrogel is physical gel, the gel can be converted from solid to liquid at high temperature, and the traditional polyvinyl alcohol hydrogel has poor mechanical properties such as toughness, compressive strength and the like, and cannot meet the requirements of practical use.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a multiple chemical crosslinking high-strength polyvinyl alcohol hydrogel and a preparation method thereof, and solves the problem that the traditional polyvinyl alcohol physical hydrogel is poor in toughness and compressive strength.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a multiple chemical crosslinking high-strength polyvinyl alcohol hydrogel comprises the following raw materials and components: alkenyl polyvinyl alcohol, acrylamide, alkenyl sodium alginate, ammonium persulfate, sodium bisulfite, N' -methylene bisacrylamide and boric acid in a mass ratio of 100:4-8:15-40:0.008-0.015:0.04-0.08:0.01-0.025: 0.2-1.
Preferably, the preparation method of the multiple chemically crosslinked high-strength polyvinyl alcohol hydrogel comprises the following steps:
(1) adding distilled water solvent and sodium alginate into a reaction bottle, stirring and dissolving at 40-60 ℃, adding a mixed dimethyl sulfoxide solution of 4-dimethylaminopyridine and glycidyl methacrylate slowly dropwise into the reaction bottle at room temperature in a nitrogen atmosphere by using a reagent sampling device, stirring at a constant speed for reaction for 36-72h, adding an ethanol solvent until a large amount of precipitate is separated out, filtering to remove the solvent, washing a solid product by using ethanol, and drying to prepare the alkenyl sodium alginate.
(2) Adding a dimethyl sulfoxide solvent and polyvinyl alcohol into a reaction bottle, stirring and dissolving at 80-100 ℃, reducing the temperature to 50-60 ℃, slowly dropwise adding the dimethyl sulfoxide solution of maleic anhydride by using a reagent sampling device, stirring at a constant speed and reacting for 2-6h, placing the solution in an ice water bath for cooling, adding an acetone solvent until a large amount of precipitate is formed, filtering, washing and drying to prepare the alkenyl polyvinyl alcohol.
(3) Adding a distilled water solvent, alkenyl polyvinyl alcohol, acrylamide, alkenyl sodium alginate and N, N' -methylene bisacrylamide into a reaction bottle, swelling for 2-4h at 40-50 ℃, stirring uniformly, slowly dropwise adding a mixed aqueous solution of ammonium persulfate and sodium bisulfite, stirring at a constant speed for reacting for 3-6h, adding a boric acid aqueous solution, stirring uniformly, standing for crosslinking for 20-30h, filtering the solution to remove the solvent, placing a solid gel product into a dialysis bag, and dialyzing by using distilled water and ethanol to prepare the multi-chemical crosslinking high-strength polyvinyl alcohol hydrogel.
Preferably, reagent sampling device in step (1) includes the base, and the base top is provided with the reaction flask, the fixed fixedly connected with threaded rod in base both sides, threaded rod swing joint has the gear, gear swing joint has connecting rod, connecting rod fixedly connected with spring, spring swing joint has the cardboard, cardboard swing joint has the sample injector, sample injector swing joint has the homogeneous mixing chamber of appearance of advance.
Preferably, the mass ratio of the sodium alginate to the 4-dimethylaminopyridine to the glycidyl methacrylate in the step (1) is 100:15-35: 10-20.
Preferably, the mass ratio of the polyvinyl alcohol to the maleic anhydride in the step (2) is 100: 10-30.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the multiple chemical crosslinking high-strength polyvinyl alcohol hydrogel is prepared by respectively using maleic anhydride to graft and modify polyvinyl alcohol, using glycidyl methacrylate to graft and modify sodium alginate to obtain alkenyl polyvinyl alcohol and alkenyl sodium alginate, using ammonium persulfate and sodium bisulfite as redox initiation systems to copolymerize alkenyl polyvinyl alcohol, alkenyl sodium alginate and acrylamide to form a polyvinyl alcohol-sodium alginate-acryloyl copolymer as a first heavy chemical crosslinking system, crosslinking N, N' -methylene bisacrylamide and alkenyl functional groups of acrylamide, alkenyl polyvinyl alcohol and alkenyl sodium alginate to form a three-dimensional network structure as a second heavy chemical crosslinking system, crosslinking borate hydrolyzed by boric acid and hydroxyl functional groups of alkenyl polyvinyl alcohol and alkenyl sodium alginate to form an interpenetrating network as a third heavy chemical crosslinking system, the compression modulus of the polyvinyl alcohol composite hydrogel is obviously improved, and the polyvinyl alcohol composite hydrogel has excellent compression strength and toughness.
Drawings
FIG. 1 is a schematic front view of a sample injector;
FIG. 2 is an enlarged schematic view of the injector;
FIG. 3 is an enlarged view of the card.
1-a base; 2-reaction flask; 3-a threaded rod; 4-a gear; 5-a connecting rod; 6-a spring; 7-clamping plate; 8-sample injector; 9-homogenizing chamber.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: a multiple chemical crosslinking high-strength polyvinyl alcohol hydrogel comprises the following raw materials and components: alkenyl polyvinyl alcohol, acrylamide, alkenyl sodium alginate, ammonium persulfate, sodium bisulfite, N' -methylene bisacrylamide and boric acid in a mass ratio of 100:4-8:15-40:0.008-0.015:0.04-0.08:0.01-0.025: 0.2-1.
The preparation method of the multiple chemically crosslinked high-strength polyvinyl alcohol hydrogel comprises the following steps:
(1) adding distilled water solvent and sodium alginate into a reaction bottle, stirring and dissolving at 40-60 ℃, adding a mixed dimethyl sulfoxide solution of 4-dimethylaminopyridine and glycidyl methacrylate slowly dropwise by using a reagent sample injection device in a nitrogen atmosphere at room temperature, wherein the mass ratio of the sodium alginate to the 4-dimethylaminopyridine to the glycidyl methacrylate is 100:15-35:10-20, the reagent sample injection device comprises a base, a reaction bottle is arranged above the base, threaded rods are fixedly connected to two sides of the base, gears are movably connected to the threaded rods, connecting rods are movably connected to the gears, springs are fixedly connected to the connecting rods, clamping plates are movably connected to the springs, sample injectors are movably connected to the clamping plates, the uniform stirring reaction is carried out for 36-72h, an ethanol solvent is added until a large amount of precipitate is precipitated, filtering to remove the solvent, washing the solid product with ethanol and drying to prepare the alkenyl sodium alginate.
(2) Adding a dimethyl sulfoxide solvent and polyvinyl alcohol into a reaction bottle, stirring and dissolving at 80-100 ℃, reducing the temperature to 50-60 ℃, slowly dropwise adding a dimethyl sulfoxide solution of maleic anhydride by using a reagent sampling device, wherein the mass ratio of the polyvinyl alcohol to the maleic anhydride is 100:10-30, stirring at a constant speed for reacting for 2-6h, cooling the solution in an ice-water bath, adding an acetone solvent until a large amount of precipitate is formed, filtering, washing and drying to prepare the alkenyl polyvinyl alcohol.
(3) Adding a distilled water solvent, alkenyl polyvinyl alcohol, acrylamide, alkenyl sodium alginate and N, N' -methylene bisacrylamide into a reaction bottle, swelling for 2-4h at 40-50 ℃, stirring uniformly, slowly dropwise adding a mixed aqueous solution of ammonium persulfate and sodium bisulfite, stirring at a constant speed for reacting for 3-6h, adding a boric acid aqueous solution, stirring uniformly, standing for crosslinking for 20-30h, filtering the solution to remove the solvent, placing a solid gel product into a dialysis bag, and dialyzing by using distilled water and ethanol to prepare the multi-chemical crosslinking high-strength polyvinyl alcohol hydrogel.
Example 1
(1) Adding distilled water solvent and sodium alginate into a reaction bottle, stirring and dissolving at 40 ℃, adding a mixed dimethyl sulfoxide solution of 4-dimethylaminopyridine and glycidyl methacrylate slowly dropwise by using a reagent sampling device in a nitrogen atmosphere at room temperature, wherein the mass ratio of the sodium alginate to the 4-dimethylaminopyridine to the glycidyl methacrylate is 100:15:10, the reagent sampling device comprises a base, a reaction bottle is arranged above the base, threaded rods are fixedly connected to two sides of the base, the threaded rods are movably connected with gears, the gears are movably connected with connecting rods, the connecting rods are fixedly connected with springs, the springs are movably connected with clamping plates, the clamping plates are movably connected with sample injectors, the sample injectors are movably connected with sample injection homogenizing chambers, stirring and reacting at constant speed for 36 hours, adding ethanol solvent until a large amount of precipitate is separated out, filtering and removing the solvent, washing the solid product with ethanol and drying to prepare the alkenyl sodium alginate.
(2) Adding a dimethyl sulfoxide solvent and polyvinyl alcohol into a reaction bottle, stirring and dissolving at 80 ℃, reducing the temperature to 50 ℃, slowly dropwise adding a dimethyl sulfoxide solution of maleic anhydride by using a reagent sampling device, wherein the mass ratio of the polyvinyl alcohol to the maleic anhydride is 100:10, stirring at a constant speed for reaction for 2 hours, placing the solution in an ice water bath for cooling, adding an acetone solvent until a large amount of precipitate is formed, filtering, washing and drying to prepare the alkenyl polyvinyl alcohol.
(3) Adding a distilled water solvent and alkenyl polyvinyl alcohol, acrylamide, alkenyl sodium alginate and N, N '-methylene bisacrylamide into a reaction bottle, swelling for 2h at 40 ℃, stirring uniformly, slowly dropwise adding a mixed aqueous solution of ammonium persulfate and sodium bisulfite, stirring at a constant speed for reaction for 3h, adding a boric acid aqueous solution, wherein the mass ratio of the alkenyl polyvinyl alcohol, the acrylamide, the alkenyl sodium alginate, the ammonium persulfate, the sodium bisulfite, the N, N' -methylene bisacrylamide and the boric acid is 100:4:15:0.008:0.04:0.01:0.2, stirring uniformly, standing for crosslinking for 20h, filtering the solution to remove the solvent, and dialyzing a solid gel product in a dialysis bag by using distilled water and ethanol to prepare the multiple chemically crosslinked high-strength polyvinyl alcohol hydrogel material 1.
Example 2
(1) Adding distilled water solvent and sodium alginate into a reaction bottle, stirring and dissolving at 60 ℃, adding a mixed dimethyl sulfoxide solution of 4-dimethylaminopyridine and glycidyl methacrylate slowly dropwise by using a reagent sampling device in a nitrogen atmosphere at room temperature, wherein the mass ratio of the sodium alginate to the 4-dimethylaminopyridine to the glycidyl methacrylate is 100:20:14, the reagent sampling device comprises a base, a reaction bottle is arranged above the base, threaded rods are fixedly connected to two sides of the base, the threaded rods are movably connected with gears, the gears are movably connected with connecting rods, the connecting rods are fixedly connected with springs, the springs are movably connected with clamping plates, the clamping plates are movably connected with sample injectors, the sample injectors are movably connected with sample injection homogenizing chambers, stirring and reacting at constant speed for 72 hours, adding ethanol solvent until a large amount of precipitate is separated out, filtering and removing the solvent, washing the solid product with ethanol and drying to prepare the alkenyl sodium alginate.
(2) Adding a dimethyl sulfoxide solvent and polyvinyl alcohol into a reaction bottle, stirring and dissolving at 80 ℃, reducing the temperature to 60 ℃, slowly dropwise adding a dimethyl sulfoxide solution of maleic anhydride by using a reagent sampling device, wherein the mass ratio of the polyvinyl alcohol to the maleic anhydride is 100:15, stirring at a constant speed for reaction for 4 hours, placing the solution in an ice water bath for cooling, adding an acetone solvent until a large amount of precipitate is formed, filtering, washing and drying to prepare the alkenyl polyvinyl alcohol.
(3) Adding a distilled water solvent and alkenyl polyvinyl alcohol, acrylamide, alkenyl sodium alginate and N, N '-methylene bisacrylamide into a reaction bottle, swelling for 4 hours at 50 ℃, stirring uniformly, slowly dropwise adding a mixed aqueous solution of ammonium persulfate and sodium bisulfite, stirring at a constant speed for reaction for 3 hours, adding a boric acid aqueous solution, wherein the mass ratio of the alkenyl polyvinyl alcohol, the acrylamide, the alkenyl sodium alginate, the ammonium persulfate, the sodium bisulfite, the N, N' -methylene bisacrylamide and the boric acid is 100:5:22:0.01:0.06:0.015:0.5, stirring uniformly, standing for crosslinking for 30 hours, filtering the solution to remove the solvent, and dialyzing a solid gel product in a dialysis bag by using distilled water and ethanol to prepare the multi-chemical crosslinked high-strength polyvinyl alcohol hydrogel material 2.
Example 3
(1) Adding distilled water solvent and sodium alginate into a reaction bottle, stirring and dissolving at 50 ℃, adding a mixed dimethyl sulfoxide solution of 4-dimethylaminopyridine and glycidyl methacrylate slowly dropwise by using a reagent sampling device in a nitrogen atmosphere at room temperature, wherein the mass ratio of the sodium alginate to the 4-dimethylaminopyridine to the glycidyl methacrylate is 100:28:16, the reagent sampling device comprises a base, a reaction bottle is arranged above the base, threaded rods are fixedly connected to two sides of the base, the threaded rods are movably connected with gears, the gears are movably connected with connecting rods, the connecting rods are fixedly connected with springs, the springs are movably connected with clamping plates, the clamping plates are movably connected with sample injectors, the sample injectors are movably connected with sample injection homogenizing chambers, stirring and reacting at a constant speed for 48 hours, adding ethanol solvent until a large amount of precipitate is separated out, filtering and removing the solvent, washing the solid product with ethanol and drying to prepare the alkenyl sodium alginate.
(2) Adding a dimethyl sulfoxide solvent and polyvinyl alcohol into a reaction bottle, stirring and dissolving at 90 ℃, reducing the temperature to 55 ℃, slowly dropwise adding a dimethyl sulfoxide solution of maleic anhydride by using a reagent sampling device, wherein the mass ratio of the polyvinyl alcohol to the maleic anhydride is 100:22, stirring at a constant speed for reaction for 4 hours, placing the solution in an ice water bath for cooling, adding an acetone solvent until a large amount of precipitate is formed, filtering, washing and drying to prepare the alkenyl polyvinyl alcohol.
(3) Adding a distilled water solvent and alkenyl polyvinyl alcohol, acrylamide, alkenyl sodium alginate and N, N '-methylene bisacrylamide into a reaction bottle, swelling for 3h at 45 ℃, stirring uniformly, slowly dropwise adding a mixed aqueous solution of ammonium persulfate and sodium bisulfite, stirring at a constant speed for 5h, adding a boric acid aqueous solution, stirring uniformly, standing for crosslinking for 25h, filtering the solution to remove the solvent, putting a solid gel product into a dialysis bag, and dialyzing by using distilled water and ethanol to prepare the multi-chemical crosslinked high-strength polyvinyl alcohol hydrogel material 3, wherein the mass ratio of the alkenyl polyvinyl alcohol, the acrylamide, the alkenyl sodium alginate, the ammonium persulfate, the sodium bisulfite, the N, N' -methylene bisacrylamide and the boric acid is 100:6.5:30:0.012:0.06:0.02: 0.8.
Example 4
(1) Adding distilled water solvent and sodium alginate into a reaction bottle, stirring and dissolving at 60 ℃, adding a mixed dimethyl sulfoxide solution of 4-dimethylaminopyridine and glycidyl methacrylate slowly dropwise by using a reagent sampling device in a nitrogen atmosphere at room temperature, wherein the mass ratio of the sodium alginate to the 4-dimethylaminopyridine to the glycidyl methacrylate is 100:35:20, the reagent sampling device comprises a base, a reaction bottle is arranged above the base, threaded rods are fixedly connected to two sides of the base, the threaded rods are movably connected with gears, the gears are movably connected with connecting rods, the connecting rods are fixedly connected with springs, the springs are movably connected with clamping plates, the clamping plates are movably connected with sample injectors, the sample injectors are movably connected with sample injection homogenizing chambers, stirring and reacting at constant speed for 72 hours, adding ethanol solvent until a large amount of precipitate is separated out, filtering and removing the solvent, washing the solid product with ethanol and drying to prepare the alkenyl sodium alginate.
(2) Adding a dimethyl sulfoxide solvent and polyvinyl alcohol into a reaction bottle, stirring and dissolving at 100 ℃, reducing the temperature to 60 ℃, slowly dropwise adding a dimethyl sulfoxide solution of maleic anhydride by using a reagent sampling device, wherein the mass ratio of the polyvinyl alcohol to the maleic anhydride is 100:30, stirring at a constant speed for reacting for 6 hours, placing the solution in an ice water bath for cooling, adding an acetone solvent until a large amount of precipitate is formed, filtering, washing and drying to prepare the alkenyl polyvinyl alcohol.
(3) Adding a distilled water solvent and alkenyl polyvinyl alcohol, acrylamide, alkenyl sodium alginate and N, N '-methylene bisacrylamide into a reaction bottle, swelling for 4 hours at 50 ℃, stirring uniformly, slowly dropwise adding a mixed aqueous solution of ammonium persulfate and sodium bisulfite, stirring at a constant speed for reaction for 6 hours, adding a boric acid aqueous solution, wherein the mass ratio of the alkenyl polyvinyl alcohol, the acrylamide, the alkenyl sodium alginate, the ammonium persulfate, the sodium bisulfite, the N, N' -methylene bisacrylamide and the boric acid is 100:8:40:0.015:0.08:0.025:1, stirring uniformly, standing for crosslinking for 30 hours, filtering the solution to remove the solvent, and dialyzing a solid gel product in a dialysis bag by using distilled water and ethanol to prepare the multi-chemical crosslinking high-strength polyvinyl alcohol hydrogel material 4.
Comparative example 1
(1) Adding distilled water solvent and sodium alginate into a reaction bottle, stirring and dissolving at 60 ℃, adding a mixed dimethyl sulfoxide solution of 4-dimethylaminopyridine and glycidyl methacrylate slowly dropwise by using a reagent sampling device in a nitrogen atmosphere at room temperature, wherein the mass ratio of the sodium alginate to the 4-dimethylaminopyridine to the glycidyl methacrylate is 100:12:7, the reagent sampling device comprises a base, a reaction bottle is arranged above the base, threaded rods are fixedly connected to two sides of the base, the threaded rods are movably connected with gears, the gears are movably connected with connecting rods, the connecting rods are fixedly connected with springs, the springs are movably connected with clamping plates, the clamping plates are movably connected with sample injectors, the sample injectors are movably connected with sample injection homogenizing chambers, stirring and reacting at a constant speed for 60 hours, adding ethanol solvent until a large amount of precipitate is separated out, filtering and removing the solvent, washing the solid product with ethanol and drying to prepare the alkenyl sodium alginate.
(2) Adding a dimethyl sulfoxide solvent and polyvinyl alcohol into a reaction bottle, stirring and dissolving at 100 ℃, reducing the temperature to 60 ℃, slowly dropwise adding a dimethyl sulfoxide solution of maleic anhydride by using a reagent sampling device, wherein the mass ratio of the polyvinyl alcohol to the maleic anhydride is 100:35, stirring at a constant speed for reaction for 1h, placing the solution in an ice water bath for cooling, adding an acetone solvent until a large amount of precipitate is formed, filtering, washing and drying to prepare the alkenyl polyvinyl alcohol.
(3) Adding a distilled water solvent and alkenyl polyvinyl alcohol, acrylamide, alkenyl sodium alginate and N, N '-methylene bisacrylamide into a reaction bottle, swelling for 4 hours at 50 ℃, stirring uniformly, slowly dropwise adding a mixed aqueous solution of ammonium persulfate and sodium bisulfite, stirring at a constant speed for reaction for 3 hours, adding a boric acid aqueous solution, wherein the alkenyl polyvinyl alcohol, the acrylamide, the alkenyl sodium alginate, the ammonium persulfate, the sodium bisulfite, the N, N' -methylene bisacrylamide and boric acid are mixed according to a mass ratio of 100:3:45:0.005:0.03:0.03:1.5, stirring uniformly, standing for crosslinking for 30 hours, filtering the solution to remove the solvent, and dialyzing a solid gel product in a dialysis bag by using distilled water and ethanol to prepare the multiple chemically crosslinked high-strength polyvinyl alcohol hydrogel comparison material 1.
The compressive strength and compressive modulus of the multiple chemically crosslinked high strength polyvinyl alcohol hydraulics of the examples and comparative examples were tested using a B L D-609A compressive strength tester, test standard GB/T26691-.
The multiple chemical crosslinking high-strength polyvinyl alcohol hydrogel is prepared by respectively using maleic anhydride to graft and modify polyvinyl alcohol, using glycidyl methacrylate to graft and modify sodium alginate to obtain alkenyl polyvinyl alcohol and alkenyl sodium alginate, using ammonium persulfate and sodium bisulfite as redox initiation systems to copolymerize alkenyl polyvinyl alcohol, alkenyl sodium alginate and acrylamide to form a polyvinyl alcohol-sodium alginate-acryloyl copolymer as a first heavy chemical crosslinking system, crosslinking N, N' -methylene bisacrylamide and alkenyl functional groups of acrylamide, alkenyl polyvinyl alcohol and alkenyl sodium alginate to form a three-dimensional network structure as a second heavy chemical crosslinking system, crosslinking borate hydrolyzed by boric acid and hydroxyl functional groups of alkenyl polyvinyl alcohol and alkenyl sodium alginate to form an interpenetrating network as a third heavy chemical crosslinking system, the compression modulus of the polyvinyl alcohol composite hydrogel is obviously improved, and the polyvinyl alcohol composite hydrogel has excellent compression strength and toughness.
Claims (5)
1. A multiple chemical crosslinking high-strength polyvinyl alcohol hydrogel comprises the following raw materials and components, and is characterized in that: alkenyl polyvinyl alcohol, acrylamide, alkenyl sodium alginate, ammonium persulfate, sodium bisulfite, N' -methylene bisacrylamide and boric acid in a mass ratio of 100:4-8:15-40:0.008-0.015:0.04-0.08:0.01-0.025: 0.2-1.
2. The multiple chemically crosslinked, high strength polyvinyl alcohol hydrogel of claim 1 wherein: the preparation method of the multiple chemically crosslinked high-strength polyvinyl alcohol hydrogel comprises the following steps:
(1) adding sodium alginate into a distilled water solvent, stirring and dissolving at 40-60 ℃, adding a reagent sample introduction device in a nitrogen atmosphere at room temperature, slowly dropwise adding a mixed dimethyl sulfoxide solution of 4-dimethylaminopyridine and glycidyl methacrylate, reacting for 36-72h, precipitating, filtering, washing and drying to prepare the alkenyl sodium alginate;
(2) adding polyvinyl alcohol into a dimethyl sulfoxide solvent, stirring and dissolving at 80-100 ℃, reducing the temperature to 50-60 ℃, slowly dropwise adding a dimethyl sulfoxide solution of maleic anhydride by using a reagent sampling device, reacting for 2-6h, cooling, precipitating, filtering, washing and drying to prepare alkenyl polyvinyl alcohol;
(3) adding alkenyl polyvinyl alcohol, acrylamide, alkenyl sodium alginate and N, N' -methylene bisacrylamide into a distilled water solvent, swelling for 2-4h at 40-50 ℃, stirring uniformly, slowly dropwise adding a mixed aqueous solution of ammonium persulfate and sodium bisulfite, reacting for 3-6h, adding a boric acid aqueous solution, stirring uniformly, standing for crosslinking for 20-30h, filtering and dialyzing to prepare the multiple chemical crosslinking high-strength polyvinyl alcohol hydrogel.
3. The multiple chemically crosslinked, high strength polyvinyl alcohol hydrogel of claim 2 wherein: the reagent sampling device in step (1) comprises a base, wherein a reaction bottle is arranged above the base, threaded rods are fixedly connected to two sides of the base, gears are movably connected to the threaded rods, connecting rods and springs are movably connected to the gears, clamping plates are movably connected to the springs, sample injectors are movably connected to the clamping plates, and sample injection mixing chambers are movably connected to the clamping plates.
4. The multiple chemically crosslinked, high strength polyvinyl alcohol hydrogel of claim 2 wherein: the mass ratio of the sodium alginate, the 4-dimethylaminopyridine and the glycidyl methacrylate in the step (1) is 100:15-35: 10-20.
5. The multiple chemically crosslinked, high strength polyvinyl alcohol hydrogel of claim 2 wherein: the mass ratio of the polyvinyl alcohol to the maleic anhydride in the step (2) is 100: 10-30.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113235298A (en) * | 2021-06-15 | 2021-08-10 | 吴江市南麻恒兴丝织厂 | Preparation method of skin-friendly polyester cotton linen fabric |
| CN115232581A (en) * | 2022-08-30 | 2022-10-25 | 陕西科技大学 | Acrylic resin binder with interpenetrating network structure and preparation method thereof |
-
2020
- 2020-04-30 CN CN202010363171.6A patent/CN111423542A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113235298A (en) * | 2021-06-15 | 2021-08-10 | 吴江市南麻恒兴丝织厂 | Preparation method of skin-friendly polyester cotton linen fabric |
| CN115232581A (en) * | 2022-08-30 | 2022-10-25 | 陕西科技大学 | Acrylic resin binder with interpenetrating network structure and preparation method thereof |
| CN115232581B (en) * | 2022-08-30 | 2023-10-20 | 陕西科技大学 | Acrylic resin binder with interpenetrating network structure and preparation method thereof |
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Application publication date: 20200717 |