CN112266486A - Tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel and preparation method thereof - Google Patents
Tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of functional materials, and particularly relates to a tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel and a preparation method thereof. The preparation method comprises the following steps: regulating the pH value of the nano-cellulose suspension to 7.5-8.5 by using a Tris buffer solution, and then adding a certain amount of tannic acid to obtain a tannic acid coated nano-cellulose suspension; adding acrylic acid monomer into deionized water, adding natural polymer, mixing uniformly, and adding cross-linking agent and initiator; adding a certain amount of the obtained tannic acid coated nanocellulose suspension into the obtained solution, and uniformly stirring; and injecting the mixed solution into a mold, and carrying out water bath for 3-5 h at 40-60 ℃ to obtain the tannin-coated nanocellulose/polyacrylic acid hydrogel with high toughness, antibacterial property and self-adhesiveness, wherein the adopted raw materials have the advantages of good biocompatibility, low cost and safety, and have good application prospects in the field of tissue engineering.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel and a preparation method thereof.
Background
The hydrogel is a three-dimensional network material formed by hydrophilic macromolecules or polymers through the crosslinking of covalent bonds, hydrogen bonds, van der waals force and the like. In recent years, with the continuous and intensive research on multifunctional hydrogel, the adhesive performance of hydrogel is also concerned, the research on hydrogel is gradually increased, and the requirements of different fields are gradually expanded, so that the rational design of the bio-inspired multipurpose adhesive hydrogel opens up a new way for exploring a new generation of tissue adhesive soft material in the applications of wound dressings, medical electrodes, tissue adhesion, portable devices and the like.
The marine mussels can be firmly adhered to the surfaces of various bases such as organic or inorganic bases, hydrophilic bases or hydrophobic bases, smooth bases or rough bases, and can also keep strong adhesion capacity in a seabed humid environment. Inspired by mussel adhesion mechanism, the method for constructing the adhesive hydrogel by introducing the catechol group with adhesiveness into the polymer by a chemical synthesis or grafting method is concerned, but the chemical synthesis or grafting process is complicated, is not easy to operate and may have the phenomenon of low grafting rate; or directly adding dopamine to a gel system to provide catechol groups to prepare a hydrogel with adhesiveness, may raise concerns about its practical application due to the high cost and neurological effects of dopamine.
Most of the conventional adhesive hydrogels have poor mechanical properties, and to solve this problem, one usually adds some nanoparticles to the gel system, such as: graphene oxide, nanoclay, and the like, but the nanoparticles have poor dispersibility in an aqueous solution and are easily agglomerated in a hydrogel network, which affects the mechanical properties of the hydrogel and cannot fundamentally solve the problem of poor mechanical properties of the adhesive hydrogel. Therefore, the preparation of adhesive hydrogels with good mechanical properties is a problem to be solved urgently.
Disclosure of Invention
Aiming at the technical problems, the invention provides the tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel and the preparation method thereof, the method is low in cost, high in effectiveness and simple to operate, and the obtained hydrogel has good adhesion, mechanical properties and antibacterial activity.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a preparation method of tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel comprises the following steps:
(1) regulating the pH value of a nano-cellulose suspension (commercially available, a liquid is water, and the concentration is 1.2 wt%) to 7.5-8.5 by using a Tris buffer solution (the concentration of Tris is 0.8-1.2 mol/L, and the pH value is 8.5-9.5), adding a certain amount of tannic acid, and stirring and dispersing (at room temperature) for 5-10 hours to obtain a tannic acid coated nano-cellulose suspension; preferably, the concentration of the tannin-coated nanocellulose suspension is 3.5-7.5 wt% (based on the weight sum of nanocellulose and tannin);
(2) adding acrylic acid monomer into deionized water, adding natural polymer, mixing, adding cross-linking agent and initiator, and magnetically stirring for 10-20 min;
(3) adding a certain amount of the tannic acid coated nanocellulose suspension obtained in the step (1) into the solution obtained in the step (2), and uniformly stirring; and injecting the mixed solution into a mold, and carrying out water bath for 3-5 h at the temperature of 40-60 ℃ to obtain the product.
Preferably, the tannin-coated nanocellulose suspension in the step (1) is prepared and then stored at a temperature of 4 ℃ for later use.
Preferably, the natural polymer is at least one of starch, protein, lignin, pectin, xanthan gum, collagen and carboxymethyl cellulose.
Preferably, the crosslinking agent is at least one of N, N-methylene bisacrylamide, polyethylene glycol diacrylate, ethylene glycol dimethacrylate, and diaminodiphenylmethane.
Preferably, the initiator is at least one of ammonium persulfate, potassium persulfate, azobisisobutyronitrile and di-t-butyl peroxide.
Preferably, the weight ratio of the acrylic monomer, the natural polymer, the initiator and the cross-linking agent is 100: (7-10): (4-6): (0.1-1).
Preferably, the weight-to-volume ratio of the acrylic acid monomer used in step (3) to the tannic acid-coated nanocellulose suspension used is 1 g: 1-2 mL.
Preferably, the step (3) is performed with ultrasonic treatment for 10min before coating the nano-cellulose suspension with tannic acid, so that the nano-cellulose suspension is dispersed uniformly and air bubbles are discharged.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention does not utilize a chemical synthesis or grafting method to introduce catechol groups with adhesiveness into the polymer, but introduces catechol or catechol functional groups by adding tannic acid into the polymer, thereby effectively solving the defects of time consumption and low grafting rate of grafting.
2. The added nano-cellulose has ideal performances of good biocompatibility, excellent mechanical property, good dispersibility, high crystallinity and the like, and the mechanical property of the hydrogel is improved by introducing the nano-cellulose serving as a filler into the polymer hydrogel by a physical method and effectively dissipating energy through the breakage of reversible sacrificial bonds.
3. According to the invention, acrylic acid with certain antibacterial activity is used as a raw material, the catechol group of tannic acid added into the gel system also has good antibacterial activity, and the combination of the two materials enables the prepared adhesive hydrogel to have excellent antibacterial property.
4. The invention provides a preparation method of tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel, which has the advantages of easily available raw materials, low price, simple process, short experimental period, room-temperature operation, no toxic substance generation, environmental friendliness and higher practical application value.
Drawings
FIG. 1 is a molecular structural diagram of tannic acid used in the present invention.
FIG. 2 is a molecular structural diagram of a nanocellulose crystal used in the present invention.
FIG. 3 is a transmission electron micrograph of the nanocellulose used in the present invention.
FIG. 4 is a transmission electron microscope image of the tannin-coated nanocellulose obtained in example 1 of the present invention.
It can be seen that compared with pure nanocellulose, the size of the tannic acid coated nanocellulose is significantly increased, and further the success of the tannic acid coating on the nanocellulose is verified.
FIG. 5 is a photograph of polyacrylic acid hydrogel (PAA) obtained in comparative example 1, pectin/polyacrylic acid hydrogel (P-PAA) obtained in comparative example 2, and tannin-coated nanocellulose/polyacrylic acid hydrogel obtained in examples 2, 3, 1, 5. It was found that the color of the hydrogel became darker with the increase of the concentration of the tannic acid-coated nanocellulose.
Fig. 6 is a picture of the adhesion effect of the tannin coated nanocellulose/polyacrylic acid hydrogel obtained in example 1 of the present invention on the surface of different materials. It was found that the hydrogel prepared according to the invention could be adhered to different materials such as glass, teflon, polypropylene, crucible and iron.
FIG. 7 is a graph showing the antibacterial effect of the tannic acid-coated nanocellulose/polyacrylic acid adhesive hydrogel obtained in example 5 of the present invention (E.coli). Wherein the left figure is the antibacterial figure of the polyacrylic acid hydrogel obtained in the comparative example 1, and the right figure is the antibacterial figure of the 7.5wt% tannin coated nano-cellulose/polyacrylic acid hydrogel. Compared with polyacrylic acid hydrogel, the hydrogel added with the tannin coated nanocellulose has a better antibacterial effect.
Detailed Description
The invention will now be further described with reference to the following examples, but the embodiments of the invention are not limited thereto, and the materials referred to in the following examples are commercially available.
Example 1
A preparation method of tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel comprises the following steps:
(1) tris buffer (1 mol/L, pH 8.5) was added dropwise to 100g of nanocellulose suspension (concentration 1.2 wt%, containing about 1.2g of nanocellulose) with magnetic stirring until the pH was adjusted to 8.0. Subsequently, 5.4429 g of tannic acid was added and the resulting suspension was magnetically stirred at room temperature for 6 h to obtain a tannic acid-coated nanocellulose suspension with a concentration of 6.0 wt%, which was stored at 4 ℃ until use.
(2) Adding 2.7 g of acrylic acid into 6 mL of deionized water, then adding 10% of pectin based on the mass of the acrylic acid, uniformly mixing, then adding 5% of initiator ammonium persulfate based on the mass of the acrylic acid and 1% of cross-linking agent polyethylene glycol diacrylate 600, and magnetically stirring for 10min to uniformly mix the solution.
(3) And (3) carrying out ultrasonic treatment on the tannin-coated nanocellulose suspension for 10min to uniformly disperse the tannin-coated nanocellulose suspension, adding 4mL of the tannin-coated nanocellulose suspension into the pectin/acrylic acid mixed solution, carrying out magnetic stirring for 10min to uniformly mix the solution, injecting the hydrogel into a corresponding mould, and carrying out water bath at 50 ℃ for 4h to obtain the tannin-coated nanocellulose/polyacrylic acid hydrogel.
Example 2
A preparation method of tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel comprises the following steps:
(1) tris buffer (1 mol/L, pH 8.5) was added dropwise to 100g of nanocellulose suspension (concentration 1.2 wt%, containing about 1.2g of nanocellulose) with magnetic stirring until the pH was adjusted to 8.0. Subsequently, 2.1717 g of tannic acid was added and the resulting suspension was magnetically stirred at room temperature for 6 h to obtain a tannic acid-coated nanocellulose suspension with a concentration of 3.0wt%, which was stored at 4 ℃ until use.
(2) Adding 2.7 g of acrylic acid into 6 mL of deionized water, then adding pectin accounting for 10% of the mass of the acrylic acid, uniformly mixing, then adding initiator ammonium persulfate accounting for 5% of the mass of the acrylic acid and 1% of cross-linking agent polyethylene glycol diacrylate 600, and magnetically stirring for 10min to uniformly mix the solution.
(3) And (3) carrying out ultrasonic treatment on the tannin-coated nanocellulose suspension for 10min to uniformly disperse the tannin-coated nanocellulose suspension, adding 4mL of the tannin-coated nanocellulose suspension into the pectin/acrylic acid mixed solution, carrying out magnetic stirring for 10min to uniformly mix the solution, injecting the hydrogel into a corresponding mold, and carrying out water bath at 50 ℃ for 4h to obtain the tannin-coated nanocellulose/polyacrylic acid hydrogel.
Example 3
A preparation method of tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel comprises the following steps:
(1) tris buffer (1 mol/L, pH 8.5) was added dropwise to 100g of nanocellulose suspension (concentration 1.2 wt%, containing about 1.2g of nanocellulose) with magnetic stirring until the pH was adjusted to 8.0. Subsequently, 3.7800 g of tannic acid was added and the resulting suspension was magnetically stirred at room temperature for 6 h to obtain a 4.5wt% concentration of tannic acid coated nanocellulose suspension, which was stored at 4 ℃ until use.
(2) Adding 2.7 g of acrylic acid into 6 mL of deionized water, adding xanthan gum accounting for 10% of the mass of the acrylic acid, uniformly mixing, adding initiator ammonium persulfate accounting for 5% of the mass of the acrylic acid and cross-linking agent polyethylene glycol diacrylate 600 accounting for 1%, and magnetically stirring for 10min to uniformly mix the solution.
(3) And (3) carrying out ultrasonic treatment on the tannin-coated nanocellulose suspension for 10min to uniformly disperse the tannin-coated nanocellulose suspension, adding 4mL of the tannin-coated nanocellulose suspension into the pectin/acrylic acid mixed solution, carrying out magnetic stirring for 10min to uniformly mix the solution, injecting the hydrogel into a corresponding mold, and carrying out water bath at 50 ℃ for 4h to obtain the tannin-coated nanocellulose/polyacrylic acid hydrogel.
Example 4
A preparation method of tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel comprises the following steps:
(1) tris buffer (1 mol/L, pH 8.5) was added dropwise to 100g of nanocellulose suspension (concentration 1.2 wt%, containing about 1.2g of nanocellulose) with magnetic stirring until the pH was adjusted to 8.0. Subsequently, 1.6461 g of tannic acid was added and the resulting suspension was magnetically stirred at room temperature for 6 h to obtain a tannic acid-coated nanocellulose suspension with a concentration of 2.0 wt%, which was stored at 4 ℃ until use.
(2) Adding 2.5 g of acrylic acid into 6 mL of deionized water, then adding collagen with the mass of 7% of the acrylic acid, uniformly mixing, then adding initiator ammonium persulfate with the mass of 5% of the acrylic acid and 0.1% of cross-linking agent ethylene glycol dimethacrylate, and magnetically stirring for 10min to uniformly mix the solution.
(3) And (3) carrying out ultrasonic treatment on the tannin-coated nanocellulose suspension for 10min to uniformly disperse the tannin-coated nanocellulose suspension, adding 4mL of the tannin-coated nanocellulose suspension into the pectin/acrylic acid mixed solution, carrying out magnetic stirring for 10min to uniformly mix the solution, injecting the hydrogel into a corresponding mold, and carrying out water bath at 50 ℃ for 4h to obtain the tannin-coated nanocellulose/polyacrylic acid hydrogel.
Example 5
A preparation method of tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel comprises the following steps:
(1) tris buffer (1 mol/L, pH 8.5) was added dropwise to 100g of nanocellulose suspension (concentration 1.2 wt%, containing about 1.2g of nanocellulose) with magnetic stirring until the pH was adjusted to 8.0. Subsequently, 7.1584 g of tannic acid were introduced and the resulting suspension was magnetically stirred at room temperature for 6 h to obtain a tannic acid-coated nanocellulose suspension with a concentration of 7.5% by weight, which was kept at 4 ℃ until use.
(2) Adding 2.7 g of acrylic acid into 6 mL of deionized water, then adding pectin accounting for 10% of the mass of the acrylic acid, uniformly mixing, then adding initiator ammonium persulfate accounting for 5% of the mass of the acrylic acid and 0.1% of cross-linking agent polyethylene glycol diacrylate 600, and magnetically stirring for 10min to uniformly mix the solution.
(3) And (3) carrying out ultrasonic treatment on the tannin-coated nanocellulose suspension for 10min to uniformly disperse the tannin-coated nanocellulose suspension, adding 4mL of the tannin-coated nanocellulose suspension into the pectin/acrylic acid mixed solution, carrying out magnetic stirring for 10min to uniformly mix the solution, injecting the hydrogel into a corresponding mold, and carrying out water bath at 50 ℃ for 4h to obtain the tannin-coated nanocellulose/polyacrylic acid hydrogel.
Example 6
A preparation method of tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel comprises the following steps:
(1) tris buffer (1 mol/L, pH 8.5) was added dropwise to 100g of nanocellulose suspension (concentration 1.2 wt%, containing about 1.2g of nanocellulose) with magnetic stirring until the pH was adjusted to 8.0. Subsequently, 1.6461 g of tannic acid were introduced and the resulting suspension was magnetically stirred at room temperature for 6 h to obtain a tannic acid-coated nanocellulose suspension with a concentration of 2.5% by weight, which was kept at 4 ℃ until use.
(2) Adding 2.0 g of acrylic acid into deionized water, then adding 10% of carboxymethyl cellulose by mass of the acrylic acid, uniformly mixing, then adding 5% of initiator potassium persulfate by mass of the acrylic acid and 0.2% of cross-linking agent N, N-methylene bisacrylamide, and magnetically stirring for 10min to uniformly mix the solution.
(3) And (3) carrying out ultrasonic treatment on the tannin-coated nanocellulose suspension for 10min to uniformly disperse the tannin-coated nanocellulose suspension, adding 4mL of the tannin-coated nanocellulose suspension into the lignin/acrylic acid mixed solution, carrying out magnetic stirring for 10min to uniformly mix the solution, injecting the hydrogel into a corresponding mold, and carrying out water bath at 50 ℃ for 4h to obtain the tannin-coated nanocellulose/polyacrylic acid hydrogel.
Comparative example 1
Preparation of polyacrylic acid hydrogel: adding 2.5 g of acrylic acid into 10 mL of deionized water, then adding initiator ammonium persulfate accounting for 5% of the mass of the acrylic acid and 1% of cross-linking agent polyethylene glycol diacrylate 600, and magnetically stirring for 10min to uniformly mix the solution. Thereafter, the hydrogel was injected into the corresponding mold and a water bath at 50 ℃ gave a polyacrylic acid hydrogel.
Comparative example 2
Preparation of pectin/polyacrylic acid hydrogel: adding 2.5 g of acrylic acid into 10 mL of deionized water, then adding pectin accounting for 10% of the mass of the acrylic acid, uniformly mixing, then adding initiator ammonium persulfate accounting for 5% of the mass of the acrylic acid and 1% of cross-linking agent polyethylene glycol diacrylate 600, and magnetically stirring for 10min to uniformly mix the solution. Thereafter, the hydrogel was injected into the corresponding mold and water bath at 50 ℃ to obtain pectin/polyacrylic acid hydrogel.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be regarded as equivalent replacements, modifications, and improvements may be made without departing from the spirit and scope of the present invention, and these improvements and improvements should fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of tannin-coated nanocellulose/polyacrylic acid adhesive hydrogel is characterized by comprising the following steps:
(1) regulating the pH value of the nano-cellulose suspension to 7.5-8.5 by using a Tris buffer solution, adding a certain amount of tannic acid, and stirring and dispersing to obtain a tannic acid coated nano-cellulose suspension;
(2) adding an acrylic monomer into deionized water, adding a natural polymer, uniformly mixing, adding a cross-linking agent and an initiator, and performing magnetic stirring;
(3) adding a certain amount of the tannic acid coated nanocellulose suspension obtained in the step (1) into the solution obtained in the step (2), and uniformly stirring; and injecting the mixed solution into a mold, and carrying out water bath for 3-5 h at the temperature of 40-60 ℃ to obtain the product.
2. The method of claim 1, wherein: the concentration of the Tris buffer solution used in the step (1) is 0.8-1.2 mol/L, and the pH value is 8.5-9.5; the concentration of the nanocellulose suspension used was 1.2 wt%.
3. The method of claim 1, wherein: stirring for 5-10 h at room temperature under the stirring dispersion condition of the step (1); and (2) storing the tannin-coated nano cellulose suspension at 4 ℃ for later use after the tannin-coated nano cellulose suspension is prepared.
4. The method of claim 1, wherein: the amount of tannic acid used in step (1) is such that the resulting tannic acid-coated nanocellulose suspension has a concentration of 3.5 to 7.5% by weight, based on the sum of the weight of nanocellulose and tannic acid.
5. The method of claim 1, wherein: the natural polymer is at least one of starch, protein, lignin, pectin, xanthan gum, collagen and carboxymethyl cellulose.
6. The method of claim 1, wherein: the cross-linking agent is at least one of N, N-methylene bisacrylamide, polyethylene glycol diacrylate, ethylene glycol dimethacrylate and diaminodiphenylmethane; the initiator is at least one of ammonium persulfate, potassium persulfate, azobisisobutyronitrile and di-tert-butyl peroxide.
7. The method of claim 1, wherein: the weight ratio of the acrylic monomer to the natural polymer to the initiator to the cross-linking agent is 100: (7-10): (4-6): (0.1-1).
8. The method of claim 1, wherein: the weight-volume ratio of the high molecular monomer used in the step (3) to the tannin-coated nanocellulose suspension is 1 g: 1-2 mL.
9. The method of claim 1, wherein: and (3) performing ultrasonic treatment for 10min before coating the nano-cellulose suspension with the tannic acid to uniformly disperse the nano-cellulose suspension and discharge air bubbles.
10. The tannin coated nanocellulose/polyacrylic acid adhesive hydrogel prepared by the preparation method as set forth in any one of claims 1 to 9.
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| CN112979997B (en) * | 2021-02-22 | 2022-01-21 | 厦门大学 | Preparation method of anisotropic cellulose-based hydrogel |
| CN113248730A (en) * | 2021-04-22 | 2021-08-13 | 上海健康医学院 | Polyacrylamide-nanocellulose crystal-silver nanoparticle composite conductive anti-freezing organic hydrogel and preparation method and application thereof |
| CN113287614A (en) * | 2021-06-02 | 2021-08-24 | 天津大学 | Red tide algae algaecide based on natural polyphenol modified nano-cellulose and application thereof |
| CN115067339A (en) * | 2022-06-22 | 2022-09-20 | 扬州工业职业技术学院 | Polydopamine-nanocellulose composite antibacterial material |
| CN115067339B (en) * | 2022-06-22 | 2023-07-04 | 扬州工业职业技术学院 | Polydopamine-nanocellulose composite antibacterial material |
| US20230331938A1 (en) * | 2022-06-29 | 2023-10-19 | Shaanxi University Of Science & Technology | Dual-network collagen-based supramolecular hydrogel and its preparation method |
| CN115137694A (en) * | 2022-07-15 | 2022-10-04 | 上海市第一人民医院 | Hydrogel material for spinal cord injury and preparation method and application thereof |
| WO2024031904A1 (en) * | 2022-08-12 | 2024-02-15 | 齐鲁工业大学 | Nanocellulose-based multifunctional electrically-conductive composite hydrogel and preparation method therefor |
| CN115581229A (en) * | 2022-09-29 | 2023-01-10 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Preparation method and antibacterial application of tannin interface modified prochloraz ethyl cellulose nanoparticles |
| CN115893496A (en) * | 2022-11-10 | 2023-04-04 | 北京科技大学 | Composite anode material MnF2@ C of lithium ion battery and preparation method |
| CN115893496B (en) * | 2022-11-10 | 2024-02-20 | 北京科技大学 | Composite anode material MnF2@C of lithium ion battery and preparation method thereof |
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Application publication date: 20210126 |