CN117069993A - Preparation method of polyvinyl alcohol spongy gel - Google Patents
Preparation method of polyvinyl alcohol spongy gel Download PDFInfo
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- CN117069993A CN117069993A CN202311268791.1A CN202311268791A CN117069993A CN 117069993 A CN117069993 A CN 117069993A CN 202311268791 A CN202311268791 A CN 202311268791A CN 117069993 A CN117069993 A CN 117069993A
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- polyvinyl alcohol
- gel
- inorganic salt
- sponge
- effect
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- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 106
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000000694 effects Effects 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 239000000839 emulsion Substances 0.000 claims abstract description 20
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000005185 salting out Methods 0.000 claims abstract description 11
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 11
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 10
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 6
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 229940093476 ethylene glycol Drugs 0.000 claims description 4
- 229960005150 glycerol Drugs 0.000 claims description 4
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 4
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- 239000011592 zinc chloride Substances 0.000 claims description 4
- 235000005074 zinc chloride Nutrition 0.000 claims description 4
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- 229960002920 sorbitol Drugs 0.000 claims description 3
- 229920005862 polyol Polymers 0.000 claims description 2
- 150000003077 polyols Chemical class 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 229920000642 polymer Polymers 0.000 abstract description 2
- 239000000499 gel Substances 0.000 description 31
- 239000000243 solution Substances 0.000 description 19
- 229920002472 Starch Polymers 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 235000019698 starch Nutrition 0.000 description 4
- 239000008107 starch Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000004760 aramid Substances 0.000 description 3
- 229920003235 aromatic polyamide Polymers 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000005187 foaming Methods 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 206010052428 Wound Diseases 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000004964 aerogel Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 208000002847 Surgical Wound Diseases 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229920006231 aramid fiber Polymers 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010097 foam moulding Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0023—Use of organic additives containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/05—Open cells, i.e. more than 50% of the pores are open
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2207/00—Foams characterised by their intended use
- C08J2207/12—Sanitary use, e.g. diapers, napkins or bandages
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Emergency Medicine (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention discloses a preparation method of polyvinyl alcohol spongy gel, and belongs to the technical field of polymer gel preparation. The polyvinyl alcohol composite emulsion is prepared by heating and dissolving a polyvinyl alcohol solution, sequentially adding micromolecular polyalcohol, inorganic salt with salt dissolving effect and inorganic salt with salting-out effect into the polyvinyl alcohol solution, stirring and uniformly mixing, and curing the emulsion at normal temperature to obtain spongy gel with an open-cell structure, wherein the gel has extremely fast liquid absorption capacity and obvious negative pressure drainage effect, and can be used in the fields of biomedical and the like. Meanwhile, the polyvinyl alcohol spongy gel can still maintain its shape after repeated water loss and rehydration.
Description
Technical Field
The invention belongs to the technical field of polymer gel preparation, and particularly relates to a preparation method of polyvinyl alcohol spongy gel.
Background
Polyvinyl alcohol is a water-soluble polymer with the characteristic of being biodegradable and is commonly used as a biomedical material. The polyvinyl alcohol sponge can be used as a dressing for surgical wound negative pressure drainage. The preparation method of the polyvinyl alcohol sponge disclosed at present comprises the following steps: pore-forming agent filling pore-forming method, chemical foaming method, mechanical stirring method, and combination of the three. The pore-forming agent filling pore-forming method is to adopt starch as a pore-forming agent, then add a cross-linking agent, remove the pore-forming agent starch from the sponge after cross-linking and solidification, and obtain the porous polyvinyl alcohol sponge. However, the method has the disadvantages of high environmental protection pressure, large water consumption and high manufacturing cost, and a large amount of water is needed to wash out starch. The chemical foaming method is to add substances capable of generating gases such as carbon dioxide or nitrogen through chemical reaction in the production process, and then to obtain the polyvinyl alcohol sponge through solidification under the actions of homogenizing and stabilizing bubbles of the surfactant. The mechanical stirring foaming method is to add a surfactant into a polyvinyl alcohol solution, generate bubbles under high-speed stirring, and then add a cross-linking agent for curing to obtain the polyvinyl alcohol sponge. In all these methods, an aldehyde crosslinking agent is used, and an acid is added to effect catalytic crosslinking. Therefore, both the conditions for the acetal reaction and the process conditions for foam molding are required. Has high process requirements. And the addition of acids and aldehydes also damages the biocompatibility of the polyvinyl alcohol.
In order to solve the above problems, chinese patent CN 103554801a discloses a modified polyvinyl alcohol sponge and a preparation method thereof, the preparation method of the sponge comprises: adding 80-150 parts by weight of polyvinyl alcohol into 600-1800 parts by weight of water, stirring, heating to 60-98 ℃ to form a stable solution, and adding 20-200 parts by weight of starch and 10-100 parts by weight of hexamethylenetetramine into the stable solution to form a mixed solution. Adding 10-400 parts by weight of sulfuric acid or hydrochloric acid into the mixed solution, uniformly stirring, heating to 50-85 ℃ for solidification for 8-20 hours, cooling, demolding and cleaning to obtain the polyvinyl alcohol sponge. The problems of odor, inconvenience in operation of workers, low production efficiency and the like caused by formaldehyde in each link in the production process of the polyvinyl alcohol sponge product are solved, the wetting rate of the product is improved, and the softness of the dry state of the product is improved. The polyvinyl alcohol solution can also be frozen and thawed or chemically crosslinked to obtain polyvinyl alcohol gel, and then the polyvinyl alcohol gel is frozen and dried, supercritical dried and other methods to obtain the polyvinyl alcohol sponge. However, due to limitations of freeze drying, supercritical drying and other methods, the method is difficult to industrially produce polyvinyl alcohol sponge. For example, chinese patent CN 104045852a discloses a preparation method of polyvinyl alcohol sponge dressing, which fully uses ultraviolet light curing and freeze thawing technology to form a polyvinyl alcohol sponge dressing with a three-dimensional network structure combining chemical crosslinking and physical crosslinking. The polyvinyl alcohol sponge dressing prepared by the method has good biocompatibility and wet strength, soft texture, good compliance with wound surface and good application property, and can be widely used for drainage of the wound surface. Chinese patent CN 115368625a discloses a method for preparing an aramid-assisted polyvinyl alcohol aerogel. The preparation method comprises the following steps: providing a composite dispersion liquid containing polyvinyl alcohol, aramid nanofibers and an organic solvent, and taking the composite dispersion liquid as a precursor to contact with water to realize sol-gel conversion so as to obtain aramid-assisted polyvinyl alcohol hydrogel; and then carrying out solvent replacement or not, and then drying to obtain the aramid fiber-assisted polyvinyl alcohol aerogel. However, an organic solvent such as dimethyl sulfoxide is used in the preparation process.
Aiming at the defects of the prior art, the invention designs a preparation method of polyvinyl alcohol spongy gel, which utilizes the synergistic effect of the protection effect of organic micromolecular polyalcohol and the salting-out effect of inorganic salt to prepare the polyvinyl alcohol spongy gel which can be molded at normal temperature and normal pressure.
Disclosure of Invention
The invention aims to provide a preparation method of polyvinyl alcohol spongy gel. The polyvinyl alcohol sponge is prepared by curing under normal temperature through the synergistic effect of the organic micromolecular polyalcohol and the inorganic salt salting-out effect, has an obvious open pore structure, and can realize a rapid water absorption and dehydration process.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a polyvinyl alcohol spongy gel is prepared by the following steps:
(1) Under the heating condition, dissolving polyvinyl alcohol with deionized water to prepare a polyvinyl alcohol solution;
(2) Sequentially adding small molecular polyalcohol, inorganic salt with salt dissolution effect and inorganic salt with salting-out effect into the polyvinyl alcohol solution, and uniformly stirring and mixing to obtain polyvinyl alcohol composite emulsion;
(3) And (3) introducing the polyvinyl alcohol composite emulsion into a mold, and sealing and curing the polyvinyl alcohol composite emulsion in an environment of 0-50 ℃ for 1-10 hours to obtain the polyvinyl alcohol spongy gel.
Further, the heating temperature in the step 1) is 80-100 ℃.
Further, the polyvinyl alcohol used in the step 1) may be one or more of 1788, 1799, 2088, 2099, 2688, 2699.
Further, the concentration of the polyvinyl alcohol solution obtained in the step 1) is 1-20wt%.
Further, the amount of the micromolecular polyol in the step 2) is 50 wt% -300 wt% of the amount of the polyvinyl alcohol; the small molecular polyalcohol is one or more selected from ethylene glycol, glycerol, sorbitol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600 and the like.
Further, the using amount of the inorganic salt with the salt dissolving effect is 10 wt% -100 wt% of the using amount of the polyvinyl alcohol; the inorganic salt with salt dissolving effect is one or more selected from lithium chloride, calcium chloride, magnesium chloride, zinc chloride, calcium nitrate, zinc nitrate and magnesium nitrate.
Further, the using amount of the inorganic salt with the salting-out effect is 50 wt% -200 wt% of the using amount of the polyvinyl alcohol; the inorganic salt with salting-out effect is one or more of sodium chloride, sodium carbonate, sodium sulfate and sodium citrate.
The polyvinyl alcohol spongy gel has obvious open pore structure, high biocompatibility, strong liquid absorption capacity and obvious negative pressure drainage effect, can still keep the shape after repeated dehydration and rehydration, and can be applied to medical sponges or other liquid absorption places.
The invention has the remarkable advantages that:
(1) The preparation method of the polyvinyl alcohol spongy gel is simple; the prepared polyvinyl alcohol sponge has an obvious open pore structure, can realize rapid water absorption and dehydration, and can be repeated;
(2) The polyvinyl alcohol sponge prepared by the invention can be used as a water-absorbing sponge for domestic kitchens and toilets or used in the biomedical field, such as a blood-absorbing washing liquid sponge for operation and the like.
Drawings
FIG. 1 is a sample of the polyvinyl alcohol sponge-like gel prepared in example 1.
FIG. 2 is a microstructure of the polyvinyl alcohol sponge-like gel prepared in example 1. As can be seen from the figure, the obtained polyvinyl alcohol sponge-like gel has a remarkable open cell structure.
FIG. 3 is a graph showing the comparative state of the polyvinyl alcohol sponge-like gel (left) prepared in example 1 and the gel after drying at 60℃for 10. 10 h (right). The gel after drying is soaked in water for 1 minute, so that the gel can be recovered into a spongy state.
FIG. 4 shows the density and porosity values of the polyvinyl alcohol sponge-like gel prepared in example 1 (left) and after drying the gel at 60℃for 10 h (right).
FIG. 5 shows the adsorption effect of the polyvinyl alcohol sponge-like gel prepared in example 1 on various liquids. As can be seen from the figure, the obtained polyvinyl alcohol sponge gel has good adsorption performance on water.
Detailed Description
A polyvinyl alcohol spongy gel is prepared by the following steps:
(1) Dissolving polyvinyl alcohol with deionized water at 80-100 ℃ to prepare a polyvinyl alcohol solution with the weight percent of 1-20%;
(2) Sequentially adding 50-300-wt% of small molecular polyalcohol, 10-wt-100-wt% of inorganic salt with salt dissolution effect and 50-wt-200-wt% of inorganic salt with salting-out effect into a polyvinyl alcohol solution, and uniformly stirring and mixing to obtain a polyvinyl alcohol composite emulsion;
(3) And (3) introducing the polyvinyl alcohol composite emulsion into a mold, and sealing and curing the polyvinyl alcohol composite emulsion in an environment of 0-50 ℃ for 1-10 hours to obtain the polyvinyl alcohol spongy gel.
Wherein, the polyvinyl alcohol can be one or more of 1788, 1799, 2088, 2099, 2688 and 2699. The small molecular polyalcohol is one or more selected from ethylene glycol, glycerol, sorbitol, polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 600. The inorganic salt with salt dissolving effect is one or more selected from lithium chloride, calcium chloride, magnesium chloride, zinc chloride, calcium nitrate, zinc nitrate and magnesium nitrate. The inorganic salt with salting-out effect is one or more of sodium chloride, sodium carbonate, sodium sulfate and sodium citrate.
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
Example 1
Adding 1 g polyvinyl alcohol 1799 into 6 mL deionized water, heating and dissolving in water bath at 95 ℃ to obtain polyvinyl alcohol solution, adding 2 g ethylene glycol, 0.2 g magnesium chloride and 3 g sodium sulfate into the polyvinyl alcohol solution to obtain uniform composite emulsion, introducing the composite emulsion into a mold for sealing, and standing and curing at 20 ℃ for 1 h to obtain polyvinyl alcohol spongy gel.
Example 2
Adding 1 g polyvinyl alcohol 1799 into 6 mL deionized water, heating and dissolving in water bath at 95deg.C to obtain polyvinyl alcohol solution, adding 2 g glycerin, 0.2 g calcium chloride and 3 g sodium citrate into the polyvinyl alcohol solution to obtain uniform composite emulsion, introducing the composite emulsion into a mold, sealing, and aging at 30deg.C for 2 h to obtain polyvinyl alcohol sponge gel.
Example 3
Adding 1 g polyvinyl alcohol 2099 into 6 mL deionized water, heating and dissolving in water bath at 95 ℃ to obtain polyvinyl alcohol solution, adding 2 g polyethylene glycol 200, 0.2 g lithium chloride and 3 g sodium chloride into the polyvinyl alcohol solution to obtain uniform composite emulsion, introducing the composite emulsion into a mold for sealing, and standing and curing at 30 ℃ for 2 h to obtain polyvinyl alcohol spongy gel.
Example 4
Adding 1 g polyvinyl alcohol 2699 into 7 mL deionized water, heating and dissolving in water bath at 95 ℃ to obtain polyvinyl alcohol solution, adding 2 g polyethylene glycol 200, 0.2 g lithium chloride and 3 g sodium chloride into the polyvinyl alcohol solution to obtain uniform composite emulsion, introducing the composite emulsion into a mold for sealing, and standing and curing at 30 ℃ for 2 h to obtain polyvinyl alcohol spongy gel.
Example 5
Adding 1 g polyvinyl alcohol 2688 into 7 mL deionized water, heating and dissolving in water bath at 95 ℃ to obtain polyvinyl alcohol solution, adding 2 g polyethylene glycol 400, 0.2 g zinc chloride and 3 g sodium chloride into the polyvinyl alcohol solution to obtain uniform composite emulsion, introducing the composite emulsion into a mold for sealing, and standing and curing at 30 ℃ for 2 h to obtain polyvinyl alcohol spongy gel.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (7)
1. The preparation method of the polyvinyl alcohol spongy gel is characterized by comprising the following steps of:
(1) Under the heating condition, dissolving polyvinyl alcohol with deionized water to prepare a polyvinyl alcohol solution;
(2) Sequentially adding small molecular polyalcohol, inorganic salt with salt dissolution effect and inorganic salt with salting-out effect into the polyvinyl alcohol solution, and uniformly stirring and mixing to obtain polyvinyl alcohol composite emulsion;
(3) And (3) introducing the polyvinyl alcohol composite emulsion into a mold, and sealing and curing for 1-10 hours in an environment of 0-50 ℃ to obtain the polyvinyl alcohol spongy gel.
2. The method for preparing a polyvinyl alcohol sponge-like gel according to claim 1, wherein: the heating temperature in the step 1) is 80-100 ℃.
3. The method for preparing a polyvinyl alcohol sponge-like gel according to claim 1, wherein: the concentration of the polyvinyl alcohol solution obtained in the step 1) is 1-20wt%.
4. The method for preparing a polyvinyl alcohol sponge-like gel according to claim 1, wherein: the consumption of the micromolecular polyol in the step 2) is 50 wt% -300 wt% of the consumption of the polyvinyl alcohol; the small molecular polyalcohol is one or more selected from ethylene glycol, glycerol, sorbitol, polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 600.
5. The method for preparing a polyvinyl alcohol sponge-like gel according to claim 1, wherein: the consumption of the inorganic salt with the salt dissolution effect is 10 wt% -100 wt% of the consumption of the polyvinyl alcohol; the inorganic salt with salt dissolving effect is one or more selected from lithium chloride, calcium chloride, magnesium chloride, zinc chloride, calcium nitrate, zinc nitrate and magnesium nitrate.
6. The method for preparing a polyvinyl alcohol sponge-like gel according to claim 1, wherein: the use amount of the inorganic salt with the salting-out effect is 50-wt% -200-wt% of the use amount of the polyvinyl alcohol; the inorganic salt with salting-out effect is one or more of sodium chloride, sodium carbonate, sodium sulfate and sodium citrate.
7. A polyvinyl alcohol sponge-like gel prepared by the method of claims 1-6.
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