Preparation method of dual-network hygroscopic hydrogel
By constructing a network of metal phenolic compounds using auxiliary ultrasound at room temperature and crosslinking with ε-polylysine and lactonic acid, the problem of difficulty in the prior art to easily prepare dual-network crosslinked hygroscopic hydrogels at room temperature is solved, and a low-cost and easy-to-scale production of hygroscopic hydrogels are achieved.
Patent Information
- Application Number
- CN202510277946.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-10
- Publication Date
- 2025-05-30
AI Technical Summary
The prior art is difficult to easily prepare dual network cross-linked hygroscopic hydrogels at room temperature, and the existing methods are costly and are not easy to produce on a large scale.
The metal phenolic compound network was constructed at room temperature by auxiliary ultrasound, and the metal phenolic compound network was formed by using proanthocyanins and Mn2+, and a network crosslink was formed with ε-polylysine and lactonic acid to prepare a dual-network hygroscopic hydrogel.
It realizes the easy preparation of dual-network cross-linked hygroscopic hydrogels at room temperature, reduces raw material costs, is easy to produce on a large scale, and has good application prospects in the field of biomedical materials.
Smart Images
Figure CN120059228A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the field of biomedical materials, and particularly relates to a preparation method of a double-network hygroscopic hydrogel. Background Art
[0002] Proanthocyanidins (PAC) are a kind of functional factors, which are derived from various plant tissues, such as grape seeds. Due to its polyphenolic hydroxyl structure, it has been proven to have various biological activities. The metal phenolic compound network is formed by the coordination between polyphenolic compounds and metal ions, and has the dual excellent properties of polyphenolic compounds and metal ions, as well as good biocompatibility.
[0003] ε-Polylysine is a polymer of L-lysine with preservative function purified by ion exchange resin from the controlled fermentation broth of Streptomyces chromogenes producing amylase. It is a highly efficient and broad-spectrum bacteriostatic agent, and ε-polylysine has good inhibitory effects on Gram-positive bacteria, Gram-negative bacteria, molds, yeasts, and viruses.
[0004] Lactic acid lactose is a novel polyhydroxy organic acid formed by connecting one molecule of galactose and one molecule of gluconic acid through an ether bond. It is also known as the third-generation fruit acid and has biological properties such as good water retention, hygroscopicity, film-forming property, antioxidant property, and promoting wound healing. Summary of the Invention
[0005] The purpose of the present invention is to provide a preparation method of a hygroscopic hydrogel with simple operation and capable of double-network crosslinking at room temperature.
[0006] In order to achieve the above purpose, the present invention adopts the following technical solutions:
[0007] A hygroscopic hydrogel based on double-network construction, wherein the gel system uses proanthocyanidins as functional factors and Mn 2+ to form a metal phenolic compound network, which is crosslinked with the network formed by ε-polylysine and lactic acid lactose. The preparation method includes the following steps:
[0008] Step 1: Dissolve proanthocyanidins and MnSO 4 in water, and drop proanthocyanidins into the aqueous solution containing metal ions according to a certain molar ratio, and fully oscillate and mix to obtain a mixed solution A.
[0009] Step 2: Add a NaOH solution to the mixed solution A, then quickly perform ultrasonic treatment, and after the ultrasonic treatment ends, stir magnetically for 2 h to obtain a mixed solution B.
[0010] Step 3: Add the precipitate obtained by centrifuging the mixed solution B into a solution containing a certain proportion of ε-polylysine and lactic acid lactose, mix evenly, and then perform freeze-drying treatment to obtain a double-network hygroscopic hydrogel.
[0011] Further, in step one, the molar ratio of the proanthocyanidins and MnSO 4 is 1:1 to 5.
[0012] Further, in step two, the concentration of the NaOH is 2 to 10 mg / mL.
[0013] Further, in step two, the ultrasonic power is 10 W to 80 W, and the time is 0.5 to 3 min.
[0014] Further, in step two, the stirring speed during dispersion is 100 to 500 rmp.
[0015] Further, in step three, the solvent for dissolving ε-polylysine and lactobionic acid is an aqueous solution.
[0016] Further, in step three, the molar ratio of the ε-polylysine and lactobionic acid is 1:1 to 5.
[0017] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0018] The present invention adopts an assisted ultrasonic method to provide a preparation method for constructing a metal phenolic compound network at room temperature. The present invention uses proanthocyanidins as functional factors and Mn 2+ to form a metal phenolic compound network.
[0019] The method of the present invention is based on a hygroscopic hydrogel constructed by a double network, and the preparation method is simple and mild. The raw materials used in the present invention have low costs, are carried out at room temperature, are easy to scale up production, and have good research and application prospects in the field of biomedical materials. Description of the Drawings
[0020] Figure 1 SEM image of the nanoparticles constructed from the proanthocyanidins and Mn 2+ obtained in the example;
[0021] Figure 2 Hygroscopic hydrogel diagram of double network crosslinking obtained in the example. Detailed Embodiments
[0022] The technical solutions in the present invention will be clearly and completely described below with reference to the drawings and embodiments. Obviously, the described embodiments are only a part of the embodiments of the invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.
[0023] The present invention adopts a preparation method for a hygroscopic hydrogel with simple operation and capable of double network crosslinking at room temperature, using proanthocyanidins as functional factors and Mn2+ A metal phenolic compound network is formed and crosslinked with the network formed by ε-polylysine and lactobionic acid, thereby constructing a gel system.
[0024] Example 1
[0025] A method for preparing a double-network hygroscopic hydrogel, comprising the following steps:
[0026] First step: Dissolve proanthocyanidins and MnSO 4 in water, and drop proanthocyanidins into an aqueous solution containing metal ions according to a certain molar ratio, and fully oscillate and mix to obtain a mixed solution A. Among them, the molar ratio of proanthocyanidins to MnSO 4 is 1:1.
[0027] Second step: Add 2 mg / mL NaOH solution to the mixed solution A, then quickly perform ultrasonic treatment, with an ultrasonic power of 10 W and a time of 0.5 min. After the ultrasonic treatment, stir magnetically at 100 rmp for 2 h to obtain a mixed solution B.
[0028] Step three: Add the precipitate after centrifugation of the mixed solution B to an aqueous solution with a molar ratio of ε-polylysine to lactobionic acid of 1:1, mix evenly and then perform freeze-drying treatment to obtain a double-network hygroscopic hydrogel.
[0029] Example 2
[0030] A method for preparing a double-network hygroscopic hydrogel, comprising the following steps:
[0031] First step: Dissolve proanthocyanidins and MnSO 4 in water, and drop proanthocyanidins into an aqueous solution containing metal ions according to a certain molar ratio, and fully oscillate and mix to obtain a mixed solution A. Among them, the molar ratio of proanthocyanidins to MnSO 4 is 1:3.
[0032] Second step: Add 5 mg / mL NaOH solution to the mixed solution A, then quickly perform ultrasonic treatment, with an ultrasonic power of 60 W and a time of 2 min. After the ultrasonic treatment, stir magnetically at 300 rmp for 2 h to obtain a mixed solution B.
[0033] Step three: Add the precipitate after centrifugation of the mixed solution B to an aqueous solution with a molar ratio of ε-polylysine to lactobionic acid of 1:3, mix evenly and then perform freeze-drying treatment to obtain a double-network hygroscopic hydrogel.
[0034] Example 3
[0035] A method for preparing a double-network hygroscopic hydrogel, comprising the following steps:
[0036] First step: Dissolve proanthocyanidins and MnSO 4Dissolve it in water, and add procyanidins dropwise to an aqueous solution containing metal ions according to a certain molar ratio, and fully oscillate and mix to obtain a mixed solution A. Among them, the molar ratio of procyanidins to MnSO 4 is 1:5.
[0037] Step 2: Add 5 mg / mL NaOH solution to the mixed solution A, then quickly perform ultrasonic treatment. The ultrasonic power is 80 W and the time is 3 min. After the ultrasonic treatment, stir magnetically at 500 rmp for 2 h to obtain a mixed solution B.
[0038] Step 3: Add the precipitate after centrifugation of the mixed solution B to an aqueous solution with a molar ratio of ε-polylysine to lactobionic acid of 1:5, mix evenly and then perform freeze-drying treatment to obtain a double-network hygroscopic hydrogel.
[0039] Figure 1 For the SEM image of the nanoparticles constructed by the procyanidins and Mn 2+ obtained in the example, it can be seen that the system presents a regular spherical structure, and the particle size range is less than 50 nm.
[0040] Figure 2 It is the image of the double-network crosslinked hygroscopic hydrogel obtained in the example.
[0041] In addition, it should be understood that although this specification is described according to the embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. A hygroscopic hydrogel based on double network construction, characterized in that: With proanthocyanidins as functional factors and Mn 2+ A metal phenol compound network is formed, which is cross-linked with a network formed by ε-polylysine and lactobionic acid. The preparation method comprises the following steps: Step 1: dissolving proanthocyanidins and MnSO4 in water, adding proanthocyanidins dropwise into the aqueous solution containing metal ions according to a certain molar ratio, and oscillating and mixing thoroughly to obtain a mixed solution A; Step 2: Add NaOH solution to the mixed solution A, then quickly perform ultrasonication, and magnetically stir for 2 hours after the ultrasonication to obtain a mixed solution B; Step 3: The precipitate after centrifugation of the mixed solution B is added to a solution containing a certain proportion of ε-polylysine and lactobionic acid, mixed evenly and freeze-dried to obtain a double network hygroscopic hydrogel.
2. The preparation method according to claim 1, characterized in that: In step 1, the molar ratio of proanthocyanidins to MnSO4 is 1:1-5.
3. The preparation method according to claim 1, characterized in that: In step 2, the concentration of NaOH is 2-10 mg / mL.
4. The preparation method according to claim 1, characterized in that: In step 2, the ultrasonic power is 10W to 80W, and the time is 0.5 to 3 minutes.
5. The preparation method according to claim 1, characterized in that: In step 2, the stirring speed during the dispersion is 100 to 500 rpm.
6. The preparation method according to claim 1, characterized in that: In step 3, the solvent for dissolving ε-polylysine and lactobionic acid is an aqueous solution.
7. The preparation method according to claim 1, characterized in that: In step 3, the molar ratio of ε-polylysine to lactobionic acid is 1:1-5.
8. A method for preparing a double network hygroscopic hydrogel, characterized in that: Prepared according to the method according to any one of claims 1 to 7.