CN117186576A - Hydrogel with controllable response lubricating property and preparation method and application thereof - Google Patents
Hydrogel with controllable response lubricating property and preparation method and application thereof Download PDFInfo
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- 230000001050 lubricating effect Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 230000004044 response Effects 0.000 title abstract description 25
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 140
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 140
- 239000007864 aqueous solution Substances 0.000 claims abstract description 92
- 239000007788 liquid Substances 0.000 claims abstract description 58
- 239000002243 precursor Substances 0.000 claims abstract description 53
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 31
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 30
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000661 sodium alginate Substances 0.000 claims abstract description 30
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 30
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- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims abstract description 30
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims abstract description 22
- 238000000465 moulding Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 46
- 238000010257 thawing Methods 0.000 claims description 34
- 238000002156 mixing Methods 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 22
- 238000006136 alcoholysis reaction Methods 0.000 claims description 17
- 230000008014 freezing Effects 0.000 claims description 17
- 238000007710 freezing Methods 0.000 claims description 17
- 239000006228 supernatant Substances 0.000 claims description 15
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 13
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 12
- 239000003431 cross linking reagent Substances 0.000 claims description 12
- 239000003999 initiator Substances 0.000 claims description 12
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000499 gel Substances 0.000 claims description 8
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical group C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000008367 deionised water Substances 0.000 description 32
- 229910021641 deionized water Inorganic materials 0.000 description 32
- 238000003760 magnetic stirring Methods 0.000 description 27
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 20
- 239000001263 FEMA 3042 Substances 0.000 description 20
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 20
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 20
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Abstract
The invention provides a hydrogel with controllable response lubricating performance, which is mucin-polyvinyl alcohol hydrogel, mucin-polyvinyl alcohol/sodium alginate hydrogel, mucin-polyvinyl alcohol/sodium carboxymethyl cellulose hydrogel, mucin-acrylamide hydrogel or mucin-hydroxyethyl methacrylate hydrogel, and is obtained through preparation of mucin aqueous solution, hydrogel precursor liquid and molding treatment. The hydrogel with controllable response lubricating property provided by the invention has a low friction coefficient, and can be applied to the preparation of soft robots.
Description
Technical Field
The invention belongs to the technical field of hydrogels, and particularly relates to a hydrogel with controllable response lubricating performance, and a preparation method and application thereof.
Background
When an object moves or tends to move relative to another object in a tangential direction of the contact surfaces, there is a force between the contact surfaces of the two objects that resists their relative movement, which force is called friction, and this phenomenon or characteristic between the contact surfaces is called "friction". The energy lost by friction in the world accounts for about 23% of the global energy consumption every year, so the reduction of the harm caused by friction has great practical significance. Lubrication is required for reducing friction, and is an effective technical measure for improving the friction state of friction pairs to reduce friction resistance and reduce wear.
Hydrogel (Hydrogel) is a gel using water as a dispersion medium, is a polymer network system, has soft properties, can maintain a certain shape, and is widely used in various fields, such as: drought resistance in arid areas, facial masks, antipyretic patches, analgesic patches and the like in cosmetics, however, practical application of hydrogels in various scenes is limited due to poor friction and abrasion performance. It is currently desirable how to prepare hydrogels with lubricating properties.
Disclosure of Invention
The invention aims to solve the problems that: hydrogel with controllable response lubricating performance, and preparation method and application thereof, so as to solve the problems of poor lubricating performance and narrow application range of the hydrogel.
The technical scheme adopted for solving the technical problems is to provide the hydrogel with controllable response lubricating performance, wherein the hydrogel is mucin-polyvinyl alcohol hydrogel, mucin-polyvinyl alcohol/sodium alginate hydrogel, mucin-polyvinyl alcohol/sodium carboxymethyl cellulose hydrogel, mucin-acrylamide hydrogel or mucin-hydroxyethyl methacrylate hydrogel.
The invention also provides a preparation method of the hydrogel with controllable response lubricating property, which comprises the following steps:
(1) Dissolving mucin in water, centrifuging, and collecting supernatant to obtain mucin water solution;
(2) Preparing a base solution; the base solution is a polyvinyl alcohol aqueous solution, a mixed solution of polyvinyl alcohol and sodium alginate, a mixed solution of polyvinyl alcohol and sodium carboxymethyl cellulose, an acrylamide-mucin aqueous solution or a hydroxyethyl methacrylate-mucin aqueous solution;
(3) Preparing hydrogel precursor liquid; the hydrogel precursor liquid is obtained by mixing a base liquid containing polyvinyl alcohol with a mucin aqueous solution, or is obtained by adding an initiator and a cross-linking agent into a base liquid without the polyvinyl alcohol;
(4) And (3) performing molding treatment on the hydrogel precursor liquid to obtain the hydrogel.
Preferably, the concentration of mucin aqueous solution is 30-90 mg/mL, the centrifugal speed is 12000r/min, and the centrifugal time is 20min.
Preferably, the hydrogel is a mucin-polyvinyl alcohol hydrogel, which is prepared by the steps of:
(1) Mixing polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99% with water, and stirring for 3h at 98 ℃ to obtain a polyvinyl alcohol aqueous solution; the concentration of the polyvinyl alcohol aqueous solution is 10-20wt%;
(2) Mixing a polyvinyl alcohol aqueous solution and a mucin aqueous solution according to a volume ratio of 1:1 to obtain hydrogel precursor liquid;
(3) Freezing the hydrogel precursor liquid at-40 ℃ for 8 hours, thawing at 25-30 ℃ for 8 hours, and performing freeze thawing cycle for 1-3 times to obtain the gel.
Preferably, the hydrogel is mucin-polyvinyl alcohol/sodium alginate hydrogel, which is prepared by the following steps:
(1) Mixing polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99% with water, stirring at 98 ℃ for 2h, adding sodium alginate, and mixing uniformly to obtain a mixed solution of polyvinyl alcohol and sodium alginate; the concentration of the mixed solution of polyvinyl alcohol and sodium alginate is 10-25 wt%; the mass ratio of the polyvinyl alcohol to the sodium alginate is 25:4;
(2) Mixing the mixed solution of polyvinyl alcohol and sodium alginate with mucin water solution according to the volume ratio of 1:1 to obtain hydrogel precursor liquid;
(3) Freezing the hydrogel precursor liquid at-40 ℃ for 8 hours, thawing at 25-30 ℃ for 8 hours, and performing freeze thawing cycle for 1-3 times to obtain the gel.
Preferably, the hydrogel is a mucin-polyvinyl alcohol/sodium carboxymethyl cellulose hydrogel, which is prepared by the following steps:
(1) Mixing polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99% with water, stirring for 3h at 98 ℃, adding sodium carboxymethylcellulose, and mixing uniformly to obtain a mixed solution of polyvinyl alcohol and sodium carboxymethylcellulose; the concentration of the mixed solution of polyvinyl alcohol and sodium carboxymethyl cellulose is 10-25 wt%; the mass ratio of the polyvinyl alcohol to the sodium carboxymethyl cellulose is 25:4;
(2) Mixing a mixed solution of polyvinyl alcohol and sodium carboxymethyl cellulose with a mucin aqueous solution according to a volume ratio of 1:1 to obtain hydrogel precursor liquid;
(3) Freezing the hydrogel precursor liquid at-40 ℃ for 8 hours, thawing at 25-30 ℃ for 8 hours, and performing freeze thawing cycle for 1-3 times to obtain the gel.
Preferably, the hydrogel is a mucin-acrylamide hydrogel, which is prepared by the steps of:
(1) Dissolving acrylamide in a mucin aqueous solution to obtain an acrylamide-mucin aqueous solution; the concentration of the acrylamide-mucin aqueous solution is 15-20wt%; the mass ratio of the acrylamide to the mucin is 25:3-9;
(2) Sequentially adding a cross-linking agent and an initiator into the acrylamide-mucin aqueous solution, stirring and dissolving to obtain hydrogel precursor liquid; the addition amount of the initiator and the cross-linking agent is 1% of the mass of the acrylamide;
(3) Placing the hydrogel precursor liquid at 50 ℃ for 6 hours to obtain the hydrogel.
Preferably, the hydrogel is a mucin-hydroxyethyl methacrylate hydrogel, which is prepared by the steps of:
(1) Dissolving hydroxyethyl methacrylate in a mucin aqueous solution to obtain a hydroxyethyl methacrylate-mucin aqueous solution; the concentration of the hydroxyethyl methacrylate-mucin aqueous solution is 30-45 wt%; the mass ratio of the hydroxyethyl methacrylate to the mucin is 667:30-90;
(2) Sequentially adding a cross-linking agent and an initiator into the hydroxyethyl methacrylate-mucin aqueous solution, and stirring and dissolving to obtain hydrogel precursor liquid; the addition amount of the initiator and the cross-linking agent is 1% of the mass of the hydroxyethyl methacrylate;
(3) The hydrogel precursor liquid is reacted for 6 hours at the temperature of 25-30 ℃ to obtain the hydrogel.
Preferably, the cross-linking agent is N, N-methylene bisacrylamide, and the initiator is ammonium persulfate.
The invention also provides application of the hydrogel with controllable response lubricating property in preparation of soft robots.
The invention has the following beneficial effects:
(1) The hydrogel with controllable response lubricating property can effectively reduce friction coefficient, has excellent lubricating property, and can realize friction regulation and control under the action of tannic acid;
(2) The hydrogel prepared by the invention is nontoxic and harmless, has good biocompatibility, and is suitable for multifunctional and multi-scene application;
(3) The hydrogel has the advantages of cheap and easily available raw materials, simple synthesis steps and suitability for industrial production.
Drawings
FIG. 1 is a graph showing the comparison of the friction Coefficients (COFs) of mucin-polyvinyl alcohol/sodium alginate hydrogels, mucin-polyvinyl alcohol/sodium carboxymethyl cellulose hydrogels, polyvinyl alcohol/sodium alginate hydrogels, and polyvinyl alcohol/sodium carboxymethyl cellulose hydrogels;
FIG. 2 is a graph of the comparative coefficient of friction (COF) of mucin-acrylamide hydrogels, mucin-hydroxyethyl methacrylate hydrogels, acrylamide hydrogels, and hydroxyethyl methacrylate hydrogels;
FIG. 3 is a graph showing the comparison of the coefficient of friction (COF) of mucin-polyvinyl alcohol hydrogels after treatment with different concentrations of tannic acid in water.
Detailed Description
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
A hydrogel with controllable response lubricating property is mucin-polyvinyl alcohol hydrogel.
The mucin-polyvinyl alcohol hydrogel in this example was prepared by the following steps:
(1) Weighing 0.3g of mucin (mucin) and adding into 10mL of deionized water, using magnetic stirring to completely dissolve the mucin (mucin), then pouring the solution into a centrifuge tube, putting into the centrifuge, centrifuging at 12000r/min for 20min, and taking supernatant to obtain mucin aqueous solution with the concentration of 30 mg/mL;
(2) 2.5g of polyvinyl alcohol (PVA) with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99 percent and 10mL of deionized water are mixed and heated to 98 ℃ for magnetic stirring for 3 hours, so as to obtain a polyvinyl alcohol aqueous solution with concentration of 20 weight percent;
(3) Placing 5mL of polyvinyl alcohol aqueous solution into a beaker, stirring, adding 5mL of mucin aqueous solution, and uniformly mixing to obtain hydrogel precursor liquid;
(4) Placing hydrogel precursor liquid into a template with the thickness of D=35 mm and H=2.4 mm, then placing the template into a refrigerator with the temperature of minus 40 ℃ for freezing for 8 hours, then taking out the template, thawing the template at the temperature of 28 ℃ for 8 hours, and performing freeze thawing cycle for 3 times to obtain the mucin-polyvinyl alcohol hydrogel.
Example 2
A hydrogel with controllable response lubricating property is mucin-polyvinyl alcohol hydrogel.
The mucin-polyvinyl alcohol hydrogel in this example was prepared by the following steps:
(1) Weighing 0.6g of mucin, adding into 10mL of deionized water, using magnetic stirring to completely dissolve the mucin, then pouring the solution into a centrifuge tube, putting into the centrifuge, centrifuging at 12000r/min for 20min, and taking supernatant to obtain mucin aqueous solution with the concentration of 60 mg/mL;
(2) 2.5g of polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99 percent and 10mL of deionized water are mixed and heated to 98 ℃ for magnetic stirring for 3 hours, so as to obtain a polyvinyl alcohol aqueous solution with concentration of 20 weight percent;
(3) Placing 5mL of polyvinyl alcohol aqueous solution into a beaker, stirring, adding 5mL of mucin aqueous solution, and uniformly mixing to obtain hydrogel precursor liquid;
(4) Placing hydrogel precursor liquid into a template with the thickness of D=35 mm and H=2.4 mm, then placing the template into a refrigerator with the temperature of minus 40 ℃ for freezing for 8 hours, then taking out the template, thawing the template at the temperature of 25 ℃ for 8 hours, and performing freeze thawing cycle for 3 times to obtain the mucin-polyvinyl alcohol hydrogel.
Example 3
A hydrogel with controllable response lubricating property is mucin-polyvinyl alcohol hydrogel.
The mucin-polyvinyl alcohol hydrogel in this example was prepared by the following steps:
(1) Weighing 0.9g of mucin, adding into 10mL of deionized water, using magnetic stirring to completely dissolve the mucin, then pouring the solution into a centrifuge tube, putting into the centrifuge, centrifuging at 12000r/min for 20min, and taking the supernatant to obtain a mucin aqueous solution with the concentration of 90 mg/mL;
(2) 2.5g of polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99 percent and 10mL of deionized water are mixed and heated to 98 ℃ for magnetic stirring for 3 hours, so as to obtain a polyvinyl alcohol aqueous solution with concentration of 20 weight percent;
(3) Placing 5mL of polyvinyl alcohol aqueous solution into a beaker, stirring, adding 5mL of mucin aqueous solution, and uniformly mixing to obtain hydrogel precursor liquid;
(4) Placing hydrogel precursor liquid into a template with the thickness of D=35 mm and H=2.4 mm, then placing the template into a refrigerator with the temperature of minus 40 ℃ for freezing for 8 hours, then taking out the template, thawing the template at the temperature of 30 ℃ for 8 hours, and performing freeze thawing cycle for 3 times to obtain the mucin-polyvinyl alcohol hydrogel.
Example 4
A hydrogel with controllable response lubricating property is mucin-polyvinyl alcohol hydrogel.
The mucin-polyvinyl alcohol hydrogel in this example was prepared by the following steps:
(1) Weighing 0.3g of mucin, adding into 10mL of deionized water, using magnetic stirring to completely dissolve the mucin, then pouring the solution into a centrifuge tube, putting into the centrifuge, centrifuging at a speed of 12000r/min for 20min, and taking the supernatant to obtain a mucin aqueous solution with a concentration of 30 mg/mL;
(2) 2.5g of polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99 percent and 10mL of deionized water are mixed and heated to 98 ℃ for magnetic stirring for 3 hours, so as to obtain a polyvinyl alcohol aqueous solution with concentration of 20 weight percent;
(3) Placing 5mL of polyvinyl alcohol aqueous solution into a beaker, stirring, adding 5mL of mucin aqueous solution, and uniformly mixing to obtain hydrogel precursor liquid;
(4) Placing hydrogel precursor liquid into a template with the thickness of D=35 mm and H=2.4 mm, then placing the template into a refrigerator with the temperature of minus 40 ℃ for freezing for 8 hours, then taking out the template, thawing the template at the temperature of 30 ℃ for 8 hours, and performing freeze thawing cycle for 1 time to obtain the mucin-polyvinyl alcohol hydrogel.
Example 5
A hydrogel with controllable response lubricating property is mucin-polyvinyl alcohol hydrogel.
The mucin-polyvinyl alcohol hydrogel in this example was prepared by the following steps:
(1) Weighing 0.3g of mucin, adding into 10mL of deionized water, using magnetic stirring to completely dissolve the mucin, then pouring the solution into a centrifuge tube, putting into the centrifuge, centrifuging at a speed of 12000r/min for 20min, and taking the supernatant to obtain a mucin aqueous solution with a concentration of 30 mg/mL;
(2) 2.5g of polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99 percent and 10mL of deionized water are mixed and heated to 98 ℃ for magnetic stirring for 3 hours, so as to obtain a polyvinyl alcohol aqueous solution with concentration of 20 weight percent;
(3) Placing 5mL of polyvinyl alcohol aqueous solution into a beaker, stirring, adding 5mL of mucin aqueous solution, and uniformly mixing to obtain hydrogel precursor liquid;
(4) Placing hydrogel precursor liquid into a template with the thickness of D=35 mm and H=2.4 mm, then placing the template into a refrigerator with the temperature of minus 40 ℃ for freezing for 8 hours, then taking out the template, thawing the template at the temperature of 30 ℃ for 8 hours, and performing freeze thawing cycle for 2 times to obtain the mucin-polyvinyl alcohol hydrogel.
Example 6
A hydrogel with controllable response lubricating property is mucin-polyvinyl alcohol hydrogel.
The mucin-polyvinyl alcohol hydrogel in this example was prepared by the following steps:
(1) Weighing 0.6g of mucin, dissolving in 10mL of deionized water, completely dissolving by using magnetic stirring, pouring the solution into a centrifuge tube, centrifuging at 12000r/min for 20min in the centrifuge, and collecting supernatant to obtain mucin aqueous solution with the concentration of 60 mg/mL;
(2) 2.5g of polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99 percent and 10mL of deionized water are mixed and heated to 98 ℃ for magnetic stirring for 3 hours, so as to obtain a polyvinyl alcohol aqueous solution with concentration of 20 weight percent;
(3) Placing 5mL of polyvinyl alcohol aqueous solution into a beaker, stirring, adding 5mL of mucin aqueous solution, and uniformly mixing to obtain hydrogel precursor liquid;
(4) Placing hydrogel precursor liquid into a template with the thickness of D=35 mm and H=2.4 mm, then placing the template into a refrigerator with the temperature of minus 40 ℃ for freezing for 8 hours, then taking out the template, thawing the template at the temperature of 30 ℃ for 8 hours, and performing freeze thawing cycle for 1 time to obtain the mucin-polyvinyl alcohol hydrogel.
Example 7
A hydrogel with controllable response lubricating property is mucin-polyvinyl alcohol hydrogel.
The mucin-polyvinyl alcohol hydrogel in this example was prepared by the following steps:
(1) Weighing 0.6g of mucin, adding into 10mL of deionized water, using magnetic stirring to completely dissolve the mucin, then pouring the solution into a centrifuge tube, putting into the centrifuge, centrifuging at 12000r/min for 20min, and taking supernatant to obtain mucin aqueous solution with the concentration of 60 mg/mL;
(2) 2.5g of polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99 percent and 10mL of deionized water are mixed and heated to 98 ℃ for magnetic stirring for 3 hours, so as to obtain a polyvinyl alcohol aqueous solution with concentration of 20 weight percent;
(3) Placing 5mL of polyvinyl alcohol aqueous solution into a beaker, stirring, adding 5mL of mucin aqueous solution, and uniformly mixing to obtain hydrogel precursor liquid;
(4) Placing hydrogel precursor liquid into a template with the thickness of D=35 mm and H=2.4 mm, then placing the template into a refrigerator with the temperature of minus 40 ℃ for freezing for 8 hours, then taking out the template, thawing the template at the temperature of 30 ℃ for 8 hours, and performing freeze thawing cycle for 2 times to obtain the mucin-polyvinyl alcohol hydrogel.
Example 8
A hydrogel with controllable response lubricating property is mucin-polyvinyl alcohol hydrogel.
The mucin-polyvinyl alcohol hydrogel in this example was prepared by the following steps:
(1) Weighing 0.6g of mucin, adding into 10mL of deionized water, using magnetic stirring to completely dissolve the mucin, then pouring the solution into a centrifuge tube, putting into the centrifuge, centrifuging at 12000r/min for 20min, and taking supernatant to obtain mucin aqueous solution with the concentration of 60 mg/mL;
(2) 2.5g of polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99 percent and 10mL of deionized water are mixed and heated to 98 ℃ for magnetic stirring for 3 hours, so as to obtain a polyvinyl alcohol aqueous solution with concentration of 20 weight percent;
(3) Placing 5mL of polyvinyl alcohol aqueous solution into a beaker, stirring, adding 5mL of mucin aqueous solution, and uniformly mixing to obtain hydrogel precursor liquid;
(4) Placing hydrogel precursor liquid into a template with the thickness of D=35 mm and H=2.4 mm, then placing the template into a refrigerator with the temperature of minus 40 ℃ for freezing for 8 hours, then taking out the template, thawing the template at the temperature of 30 ℃ for 8 hours, and performing freeze thawing cycle for 1 time to obtain the mucin-polyvinyl alcohol hydrogel.
Example 9
A hydrogel with controllable response lubricating property is mucin-polyvinyl alcohol hydrogel.
The mucin-polyvinyl alcohol hydrogel in this example was prepared by the following steps:
(1) Weighing 0.9g of mucin, adding into 10mL of deionized water, using magnetic stirring to completely dissolve the mucin, then pouring the solution into a centrifuge tube, putting into the centrifuge, centrifuging at 12000r/min for 20min, and taking the supernatant to obtain a mucin aqueous solution with the concentration of 90 mg/mL;
(2) 2.5g of polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99 percent and 10mL of deionized water are mixed and heated to 98 ℃ for magnetic stirring for 3 hours, so as to obtain a polyvinyl alcohol aqueous solution with concentration of 20 weight percent;
(3) Placing 5mL of polyvinyl alcohol aqueous solution into a beaker, stirring, adding 5mL of mucin aqueous solution, and uniformly mixing to obtain hydrogel precursor liquid;
(4) Placing hydrogel precursor liquid into a template with the thickness of D=35 mm and H=2.4 mm, then placing the template into a refrigerator with the temperature of minus 40 ℃ for freezing for 8 hours, then taking out the template, thawing the template at the temperature of 30 ℃ for 8 hours, and performing freeze thawing cycle for 2 times to obtain the mucin-polyvinyl alcohol hydrogel.
Example 10
A hydrogel with controllable response lubricating property is mucin-polyvinyl alcohol/sodium alginate hydrogel.
The mucin-polyvinyl alcohol/sodium alginate hydrogel in this example was prepared by the following steps:
(1) Weighing 0.9g of mucin, adding into 10mL of deionized water, using magnetic stirring to completely dissolve the mucin, then pouring the solution into a centrifuge tube, putting into the centrifuge, centrifuging at 12000r/min for 20min, and taking the supernatant to obtain a mucin aqueous solution with the concentration of 90 mg/mL;
(2) Mixing 2.5g of polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99% with 10mL of deionized water, heating to 98 ℃ and magnetically stirring for 2 hours, adding 0.4g of Sodium Alginate (SA), and stirring to uniformly mix to obtain a mixed solution of polyvinyl alcohol and sodium alginate with concentration of 22.48 wt%;
(3) Placing 5mL of a mixed solution of polyvinyl alcohol and sodium alginate in a beaker, stirring and adding 5mL of mucin aqueous solution, and uniformly mixing the mixed solution of polyvinyl alcohol and sodium alginate with the mucin aqueous solution to obtain hydrogel precursor liquid;
(4) Placing hydrogel precursor liquid into a D=35 mm template and a H=2.4 mm template, then placing into a refrigerator at the temperature of minus 40 ℃ for freezing for 8 hours, and thawing for 8 hours at the temperature of 30 ℃, and performing freeze thawing cycle for 3 times to obtain mucin-polyvinyl alcohol/sodium alginate hydrogel.
Example 11
A hydrogel with controllable response lubricating property is mucin-polyvinyl alcohol/sodium carboxymethyl cellulose hydrogel.
The mucin-polyvinyl alcohol/sodium carboxymethyl cellulose hydrogel in this example was prepared by the following steps:
(1) Weighing 0.9g of mucin, adding into 10mL of deionized water, using magnetic stirring to completely dissolve the mucin, then pouring the solution into a centrifuge tube, putting into the centrifuge, centrifuging at 12000r/min for 20min, and taking the supernatant to obtain a mucin aqueous solution with the concentration of 90 mg/mL;
(2) Mixing 2.5g of polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99 percent with 10mL of deionized water, heating to 98 ℃ and magnetically stirring for 3 hours, adding 0.4g of sodium carboxymethyl cellulose (CMC), and stirring to uniformly mix to obtain a mixed solution of polyvinyl alcohol with concentration of 22.48 weight percent and sodium carboxymethyl cellulose;
(3) Placing 5mL of a mixed solution of polyvinyl alcohol and sodium carboxymethyl cellulose in a beaker, stirring and adding 5mL of a mucin aqueous solution, and uniformly mixing the mixed solution of polyvinyl alcohol and sodium carboxymethyl cellulose with the mucin aqueous solution to obtain hydrogel precursor liquid;
(4) Placing hydrogel precursor liquid into a D=35 mm template and a H=2.4 mm template, then placing into a refrigerator at the temperature of minus 40 ℃ for freezing for 8 hours, and thawing for 8 hours at the temperature of 30 ℃, and performing freeze thawing cycle for 3 times to obtain mucin-polyvinyl alcohol/sodium carboxymethyl cellulose hydrogel.
Example 12
A hydrogel with controllable response lubricating property is disclosed, which is mucin-acrylamide hydrogel.
The mucin-acrylamide hydrogel in this example was prepared by the following steps:
(1) Weighing 0.9g of mucin, adding into 10mL of deionized water, using magnetic stirring to completely dissolve the mucin, then pouring the solution into a centrifuge tube, putting into the centrifuge, centrifuging at 12000r/min for 20min, and taking the supernatant to obtain a mucin aqueous solution with the concentration of 90 mg/mL;
(2) 2.5g of Acrylamide (AM) was dissolved in 10mL of an aqueous mucin solution and completely dissolved by magnetic stirring to obtain an aqueous acrylamide-mucin solution having a concentration of 20wt%;
(3) Placing 5mL of acrylamide-mucin aqueous solution into a beaker, adding 0.025g of N, N-methylene bisacrylamide, adding 0.025g of ammonium persulfate, and magnetically stirring to completely dissolve the acrylamide aqueous solution to obtain hydrogel precursor liquid;
(4) Placing hydrogel precursor liquid into a D=35 mm template and a H=2.4 mm template, and then placing the template liquid into a 50 ℃ oven for 6 hours to obtain the mucin-acrylamide hydrogel.
Example 13
A hydrogel with controllable response lubricating property is mucin-hydroxyethyl methacrylate hydrogel.
The mucin-hydroxyethyl methacrylate hydrogel in this example was prepared by the following steps:
(1) Weighing 0.9g of mucin, adding into 10mL of deionized water, using magnetic stirring to completely dissolve the mucin, then pouring the solution into a centrifuge tube, putting into the centrifuge, centrifuging at 12000r/min for 20min, and taking the supernatant to obtain a mucin aqueous solution with the concentration of 90 mg/mL;
(2) 6.67g of hydroxyethyl methacrylate (HEMA) was dissolved in 10mL of an aqueous mucin solution and completely dissolved by using magnetic stirring to obtain a 40wt% concentration of hydroxyethyl methacrylate-mucin solution;
(3) Placing 5mL of hydroxyethyl methacrylate-mucin aqueous solution into a beaker, adding 0.025g of N, N-methylene bisacrylamide, adding 0.025g of ammonium persulfate, and magnetically stirring to completely dissolve the mixture to obtain hydrogel precursor liquid;
(4) Placing the gel precursor liquid into a template with the thickness of D=35 mm and H=2.4 mm, and then reacting for 6 hours at the temperature of 30 ℃ to obtain the mucin-hydroxyethyl methacrylate hydrogel.
Comparative example 1
A hydrogel is polyvinyl alcohol hydrogel.
The procedure for the preparation of the polyvinyl alcohol hydrogel in this example is different from that in example 3 in that: step (2) was omitted, the mucin aqueous solution in step (4) was replaced with an equal amount of deionized water, and the rest was the same as in example 3.
Comparative example 2
A hydrogel is polyvinyl alcohol/sodium alginate hydrogel.
The procedure for the preparation of the polyvinyl alcohol/sodium alginate hydrogel in this example is different from that in example 10 in that: step (2) was omitted, the mucin aqueous solution in step (4) was replaced with an equal amount of deionized water, and the rest was the same as in example 10.
Comparative example 3
A hydrogel is polyvinyl alcohol/sodium carboxymethylcellulose hydrogel.
The procedure for the preparation of the polyvinyl alcohol/sodium carboxymethyl cellulose hydrogel in this example differs from that in example 11 in that: step (2) was omitted, the mucin aqueous solution in step (4) was replaced with an equal amount of deionized water, and the rest was the same as in example 11.
Comparative example 4
A hydrogel is acrylamide hydrogel.
The acrylamide hydrogel in this example was prepared by a procedure different from that of example 12 in that: step (2) was omitted, the mucin aqueous solution in step (3) was replaced with an equal amount of deionized water, and the rest was the same as in example 12.
Comparative example 5
A hydrogel is hydroxyethyl methacrylate hydrogel.
The preparation process of hydroxyethyl methacrylate hydrogel in this example is different from that of example 13 in that: step (2) was omitted, the mucin aqueous solution in step (3) was replaced with an equal amount of deionized water, and the rest was the same as in example 13.
Experimental example
1. Friction coefficient test of hydrogels
The friction test was performed on a conventional ball-and-disc reciprocating friction meter (tribometer UMT-2, CETR, bruker, USA). Under a load of 1N, a stainless steel contact ball (diameter 6 mm) performs a reciprocating linear motion on the hydrogel surface at a shear rate of 0.5 mm/s. One reciprocating linear motion is marked as one shear cycle, with a sliding distance of 5mm. The friction coefficients of the hydrogels prepared in examples 1 to 13 and comparative examples 1 to 5 are shown in Table 1, FIG. 1 and FIG. 2.
TABLE 1
| Project | Coefficient of friction | Project | Coefficient of friction | Project | Coefficient of friction |
| Example 1 | 0.022 | Example 7 | 0.018 | Example 13 | 0.026 |
| Example 2 | 0.01 | Example 8 | 0.02 | Comparative example 1 | 0.18 |
| Example 3 | 0.008 | Example 9 | 0.012 | Comparative example 2 | 0.09 |
| Example 4 | 0.053 | Example 10 | 0.021 | Comparative example 3 | 0.082 |
| Example 5 | 0.036 | Example 11 | 0.018 | Comparative example 4 | 0.32 |
| Example 6 | 0.034 | Example 12 | 0.031 | Comparative example 5 | 0.56 |
As shown in fig. 1 and table 1, the COF values of the hydrogels prepared in comparative examples 10 and 11 and comparative examples 2 and 3, which had the response lubrication performance, were lower than those of the polyvinyl alcohol/sodium alginate hydrogels, and similarly, the COF values of the mucin-polyvinyl alcohol/sodium carboxymethyl cellulose hydrogels were lower than those of the polyvinyl alcohol/sodium carboxymethyl cellulose hydrogels, and the results showed that mucin had a good lubrication effect and a wide application range.
As shown in fig. 2 and table 1, the COF values of hydrogels prepared in comparative examples 12 and 13 and comparative examples 4 and 5, which had response lubricating properties, were lower than those of acrylamide hydrogels, and similarly, the COF values of mucin-hydroxyethyl methacrylate hydrogels were lower than those of hydroxyethyl methacrylate hydrogels, indicating that mucin had excellent lubricating effects and a wide range of applications.
2. Friction coefficient test of mucin-polyvinyl alcohol hydrogel treated with tannic acid solution
1g of Tannic Acid (TA) was weighed and dissolved in 9mL of deionized water, and the tannic acid was completely dissolved by using magnetic stirring to obtain an aqueous tannic acid solution having a concentration of 10 wt%; 1.5g of Tannic Acid (TA) is weighed and dissolved in 8.5mL of deionized water, and magnetic stirring is used for completely dissolving the Tannic Acid (TA) to obtain a tannic acid aqueous solution with the concentration of 15 wt%; 2g of Tannic Acid (TA) was then weighed and dissolved in 8mL of deionized water, and the solution was completely dissolved by magnetic stirring to obtain an aqueous tannic acid solution having a concentration of 20 wt%.
After the mucin-polyvinyl alcohol hydrogel was treated with tannic acid aqueous solutions having concentrations of 10wt%, 15wt% and 20wt%, respectively, for 1min, the friction coefficients of the mucin-polyvinyl alcohol hydrogel treated with the tannic acid aqueous solutions having the above three different concentrations and the untreated mucin-polyvinyl alcohol hydrogel were examined, and the results are shown in fig. 3.
As can be seen from fig. 3, the friction coefficient of the hydrogel after the tannic acid treatment tends to increase, and the higher the tannic acid concentration, the higher the friction coefficient increases, because of the interaction between mucin and polyphenol groups of tannic acid, mucin aggregation and precipitation can be caused, thereby realizing friction control.
While the invention has been described in terms of the foregoing embodiments, it will be understood that the embodiments are not intended to limit the invention in any way, but are intended to cover modifications of the invention using equivalent alternatives or modifications.
Claims (10)
1. A hydrogel having controlled responsive lubricating properties, characterized by: the hydrogel is mucin-polyvinyl alcohol hydrogel, mucin-polyvinyl alcohol/sodium alginate hydrogel, mucin-polyvinyl alcohol/sodium carboxymethyl cellulose hydrogel, mucin-acrylamide hydrogel or mucin-hydroxyethyl methacrylate hydrogel.
2. A method of preparing a hydrogel having controlled responsive lubricating properties as claimed in claim 1, comprising the steps of:
(1) Dissolving mucin in water, centrifuging, and collecting supernatant to obtain mucin water solution;
(2) Preparing a base solution; the base solution is a polyvinyl alcohol aqueous solution, a mixed solution of polyvinyl alcohol and sodium alginate, a mixed solution of polyvinyl alcohol and sodium carboxymethyl cellulose, an acrylamide-mucin aqueous solution or a hydroxyethyl methacrylate-mucin aqueous solution;
(3) Preparing hydrogel precursor liquid; the hydrogel precursor liquid is obtained by mixing a base liquid containing polyvinyl alcohol with a mucin aqueous solution, or is obtained by adding an initiator and a cross-linking agent into a base liquid without the polyvinyl alcohol;
(4) And (3) performing molding treatment on the hydrogel precursor liquid to obtain the hydrogel.
3. The method of manufacturing as claimed in claim 2, wherein: the concentration of the mucin aqueous solution is 30-90 mg/mL, the centrifugal speed is 12000r/min, and the centrifugal time is 20min.
4. The method of claim 3, wherein the hydrogel is a mucin-polyvinyl alcohol hydrogel, prepared by the steps of:
(1) Mixing polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99% with water, and stirring for 3h at 98 ℃ to obtain a polyvinyl alcohol aqueous solution; the concentration of the polyvinyl alcohol aqueous solution is 10-20wt%;
(2) Mixing a polyvinyl alcohol aqueous solution and a mucin aqueous solution according to a volume ratio of 1:1 to obtain hydrogel precursor liquid;
(3) Freezing the hydrogel precursor liquid at-40 ℃ for 8 hours, thawing at 25-30 ℃ for 8 hours, and performing freeze thawing cycle for 1-3 times to obtain the gel.
5. The method of claim 3, wherein the hydrogel is a mucin-polyvinyl alcohol/sodium alginate hydrogel, and is prepared by the steps of:
(1) Mixing polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99% with water, stirring at 98 ℃ for 2h, adding sodium alginate, and mixing uniformly to obtain a mixed solution of polyvinyl alcohol and sodium alginate; the concentration of the mixed solution of polyvinyl alcohol and sodium alginate is 10-25wt%; the mass ratio of the polyvinyl alcohol to the sodium alginate is 25:4;
(2) Mixing the mixed solution of polyvinyl alcohol and sodium alginate with mucin water solution according to the volume ratio of 1:1 to obtain hydrogel precursor liquid;
(3) Freezing the hydrogel precursor liquid at-40 ℃ for 8 hours, thawing at 25-30 ℃ for 8 hours, and performing freeze thawing cycle for 1-3 times to obtain the gel.
6. The method of claim 3, wherein the hydrogel is a mucin-polyvinyl alcohol/sodium carboxymethyl cellulose hydrogel, and is prepared by the steps of:
(1) Mixing polyvinyl alcohol with molecular weight of 100000 ～ 150000 and alcoholysis degree of 99% with water, stirring for 3h at 98 ℃, adding sodium carboxymethylcellulose, and mixing uniformly to obtain a mixed solution of polyvinyl alcohol and sodium carboxymethylcellulose; the concentration of the mixed solution of polyvinyl alcohol and sodium carboxymethyl cellulose is 10-25 wt%; the mass ratio of the polyvinyl alcohol to the sodium carboxymethyl cellulose is 25:4;
(2) Mixing a mixed solution of polyvinyl alcohol and sodium carboxymethyl cellulose with a mucin aqueous solution according to a volume ratio of 1:1 to obtain hydrogel precursor liquid;
(3) Freezing the hydrogel precursor liquid at-40 ℃ for 8 hours, thawing at 25-30 ℃ for 8 hours, and performing freeze thawing cycle for 1-3 times to obtain the gel.
7. A method of preparation according to claim 3, wherein the hydrogel is a mucin-acrylamide hydrogel prepared by the steps of:
(1) Dissolving acrylamide in a mucin aqueous solution to obtain an acrylamide-mucin aqueous solution; the concentration of the acrylamide-mucin aqueous solution is 15-20wt%; the mass ratio of the acrylamide to the mucin is 25:3-9;
(2) Sequentially adding a cross-linking agent and an initiator into the acrylamide-mucin aqueous solution, stirring and dissolving to obtain hydrogel precursor liquid; the addition amount of the initiator and the cross-linking agent is 1% of the mass of the acrylamide;
(3) Placing the hydrogel precursor liquid at 50 ℃ for 6 hours to obtain the hydrogel.
8. A method of preparation according to claim 3, wherein the hydrogel is a mucin-hydroxyethyl methacrylate hydrogel, prepared by the steps of:
(1) Dissolving hydroxyethyl methacrylate in a mucin aqueous solution to obtain a hydroxyethyl methacrylate-mucin aqueous solution; the concentration of the hydroxyethyl methacrylate-mucin aqueous solution is 30-45 wt%; the mass ratio of the hydroxyethyl methacrylate to the mucin is 667:30-90;
(2) Sequentially adding a cross-linking agent and an initiator into the hydroxyethyl methacrylate-mucin aqueous solution, and stirring and dissolving to obtain hydrogel precursor liquid; the addition amount of the initiator and the cross-linking agent is 1% of the mass of the hydroxyethyl methacrylate;
(3) The hydrogel precursor liquid is reacted for 6 hours at the temperature of 25-30 ℃ to obtain the hydrogel.
9. The production method according to any one of claims 7 to 8, wherein: the cross-linking agent is N, N-methylene bisacrylamide, and the initiator is ammonium persulfate.
10. Use of the hydrogel of claim 1 in the preparation of a soft robot.
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