CN110157012A - A kind of preparation method of high-intensity and high-tenacity gelatin based aquagel - Google Patents
A kind of preparation method of high-intensity and high-tenacity gelatin based aquagel Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
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- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F120/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C08J2333/00—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C08J2433/00—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of preparation methods of high-intensity and high-tenacity gelatin based aquagel, specifically, obtaining aqueous gelatin solution firstly, gelatin, functional material are uniformly mixed with water；Acrylic monomer and initiator is added into aqueous gelatin solution again, polymerization reaction is carried out under conditions of ultraviolet light-initiated, it is dry, obtain dry hydrogel；It is swollen finally, immersing in deionized water, high-intensity and high-tenacity gelatin based aquagel can be obtained.The gelatin based aquagel that the present invention is prepared is hydrogen bond crosslinks hydrogel, and without chemical crosslinking, the gelatin hydrogel being prepared has the advantages that high-intensity and high-tenacity, and fracture strength is up to 5MPa, and modulus can reach 10MPa or more, and energy of rupture is up to 8000J/m2；In addition, preparation method is simple, and it is low in cost, large-scale promotion production can be carried out.
Description
Technical field
The invention belongs to hydrogel material preparation technical fields, and in particular to a kind of high-intensity and high-tenacity gelatin based aquagel
Preparation method.
Background technique
Hydrogel is that one kind can be swollen in water and retain a large amount of water, but not soluble in water has three-dimensional net structure
Polymer material, drug delivery, tissue engineering bracket, artificial articular cartilage, in terms of have and widely answer
With prospect, so preparation is high-intensitive and the hydrogel of high tenacity becomes research hotspot in recent years.Gelatin is that a kind of biology is big
Molecule is the catabolite of collagen, nontoxic, has good biocompatibility and biodegradability and environment friendly.Greatly
Hydrogel material of the part based on protein is that low tenacity and high brittleness are low intensive, and gelatin is as a kind of protein substrate
Material, it may have disadvantage mentioned above, which has limited gelatin in terms of bio-medical material, especially as in tissue engineering bracket material
Material, soft tissue replacement material (such as artificial cartilage), etc. biomaterial application.
In order to overcome this disadvantage, there are a large amount of methods reports for improving gelatin hydrogel intensity, including utilizing gelatin
Or gelatin modified object and synthesis macromolecule network it is compound to improve its engineering properties (M.A.Daniele, Biomaterials 35
(2014) 1845-1856), gelatin and boiomacromolecule, such as cellulose, chitosan, sodium alginate are compound again by physics phase
Interaction or chemical bond crosslinking are to obtain hydrogel material (A.J.Ragauskas, the Carbohydrate with some strength
Polymers 91(2013)638–645；R.D.K.Misra,Acta Biomaterialia 36(2016)143–151；
X.Cao, Carbohydrate Polymers 168 (2017) 147-152), macromolecule is compound adds nanometer again for gelatin and synthesis
Particle enhances (S.Faghihi, J.Appl.Phys.115,083513 (2014)) etc..Gelatin water-setting can be improved in the above method
The intensity of glue, and the application potential with corresponding bio-medical material, however, these methods are there are process complexity, intensity is not
The big problem of sufficient (modulus is difficult to reach MPa) or brittleness.This limits it in bio-medical material, especially to a certain extent
Application potential in terms of soft tissue replacement material.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of high-intensity and high-tenacity gelatin based aquagel, solve existing
The problem that gelatin-based hydrogel intensity is low, toughness is low.
The technical scheme adopted by the invention is that a kind of preparation method of high-intensity and high-tenacity gelatin based aquagel, specifically
It follows the steps below to implement:
Step 1, gelatin, functional material are uniformly mixed with water, obtain aqueous gelatin solution；
Step 2, acrylic monomer and initiator are added into the aqueous gelatin solution obtained after step 1, in ultraviolet light
Polymerization reaction is carried out under conditions of initiation, is dried later, and dry hydrogel is obtained；
Step 3, the hydrogel of the drying obtained after step 2 is immersed in deionized water and is swollen, height can be obtained
Strength high toughness gelatin based aquagel.
The features of the present invention also characterized in that
In step 1, functional material is chitosan, hyaluronic acid or antibacterial nano-silver particle；Gelatin, functional material
Expect, the mass ratio of water is 1~2.5:0~0.3:7.5~9.
In step 2, reaction temperature is 1 DEG C~15 DEG C, and the reaction time is 1h~for 24 hours；Drying temperature is 1 DEG C~27 DEG C, is done
The dry time is 2h~for 24 hours.
In step 2, aqueous gelatin solution, acrylic monomer, initiator mass ratio be 0.15~2:0.0003~0.01:
1。
In step 2, acrylic monomer be acrylic acid, methacrylic acid, any one in dimethacrylate, two kinds and
Two or more mixtures.
In step 2, initiator is α-ketoglutaric acid, 2,2- azo two (2- methyl-propyl miaow) dihydrochloride, 2- hydroxyl-
Any one in 4 '-(2- hydroxy ethoxy) -2- methyl phenyl ketones.
In step 3,1 DEG C~27 DEG C of swelling temperature, swelling time is 1h~200h.
The beneficial effects of the present invention are:
The gelatin based aquagel that the present invention is prepared is that hydrogen bond crosslinks hydrogel is prepared without chemical crosslinking
Gelatin hydrogel has the advantages that high-intensity and high-tenacity, and for fracture strength up to 5MPa, modulus can reach 10MPa or more, destroys
It can be up to 8000J/m2；In addition, preparation method is simple, and it is low in cost, large-scale promotion production can be carried out.
Detailed description of the invention
Fig. 1 is the stress-strain test figure of the gelatin-based high intensity hydrogel of the method for the present invention preparation；
Fig. 2 is the structure chart of the gelatin-based high intensity hydrogel of the method for the present invention preparation.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of high-intensity and high-tenacity gelatin based aquagel of the present invention, is specifically implemented according to the following steps:
Step 1, gelatin, functional material are uniformly mixed with water, obtain aqueous gelatin solution；
Functional material is water-soluble biological macromolecular, and functional material is that chitosan, hyaluronic acid or antibiotic property are received
Rice Argent grain；
Gelatin, functional material, water mass ratio be 1~2.5:0~0.3:7.5~9；
Step 2, acrylic monomer and initiator are added into the aqueous gelatin solution obtained after step 1, in ultraviolet light
Carry out polymerization reaction under conditions of initiation, reaction temperature is 1 DEG C~15 DEG C, and the reaction time is 1h~for 24 hours；It is dried later,
Obtain dry hydrogel, drying temperature is 1 DEG C~27 DEG C, and drying time is 2h~for 24 hours；
Acrylic monomer can form more stable hydrogen bond action with gelatin；
Aqueous gelatin solution, acrylic monomer, initiator mass ratio be 0.15~2:0.0003~0.01:1；
Acrylic monomer is acrylic acid, methacrylic acid, any one in dimethacrylate, two kinds and two or more
Mixture；
Initiator is water-soluble light trigger, and initiator is α-ketoglutaric acid, 2,2- azo two (2- methyl-propyl miaow) two
Any one in hydrochloride, 2- hydroxyl -4 '-(2- hydroxy ethoxy) -2- methyl phenyl ketone；
Step 3, the hydrogel of the drying obtained after step 2 is immersed in deionized water and is swollen, 1 DEG C of swelling temperature
~27 DEG C, swelling time is 1h~200h, and high-intensity and high-tenacity gelatin based aquagel can be obtained；
The mass ratio of dry hydrogel and deionized water is greater than 1:1.
Embodiment 1
A kind of preparation method of high-intensity and high-tenacity gelatin based aquagel of the present invention, is specifically implemented according to the following steps:
Step 1, gelatin is uniformly mixed with water, obtains aqueous gelatin solution；
Gelatin, water mass ratio be 1:7.5；
Step 2, acrylic monomer and initiator are added into the aqueous gelatin solution obtained after step 1, in ultraviolet light
Polymerization reaction is carried out under conditions of initiation, reaction temperature is 10 DEG C, reaction time 5h；It is dried later, obtains drying
Hydrogel, drying temperature are 10 DEG C, drying time 2h；
Aqueous gelatin solution, acrylic monomer, initiator mass ratio be 0.15:0.0003:1；
Acrylic monomer is methacrylic acid；
Initiator is α-ketoglutaric acid；
Step 3, the hydrogel of the drying obtained after step 2 is immersed in deionized water and is swollen, swelling temperature 10
DEG C, high-intensity and high-tenacity gelatin based aquagel can be obtained in swelling time 10h；
The mass ratio of dry hydrogel and deionized water is greater than 1:1.
The modulus of obtained hydrogel is 5.7MPa, energy of rupture 4118J/m2。
Embodiment 2
A kind of preparation method of high-intensity and high-tenacity gelatin based aquagel of the present invention, is specifically implemented according to the following steps:
Step 1, gelatin, functional material are uniformly mixed with water, obtain aqueous gelatin solution；
Functional material is chitosan；
Gelatin, functional material, water mass ratio be 1~2.5:0.1:7.5~9；
Step 2, acrylic monomer and initiator are added into the aqueous gelatin solution obtained after step 1, in ultraviolet light
Polymerization reaction is carried out under conditions of initiation, reaction temperature is 5 DEG C, reaction time 8h；It is dried later, obtains dry water
Gel, drying temperature are 15 DEG C, drying time 10h；
Aqueous gelatin solution, acrylic monomer, initiator mass ratio be 0.15~2:0.0003~0.01:1；
Acrylic monomer is acrylic acid；
Initiator is 2,2- azo two (2- methyl-propyl miaow) dihydrochloride；
Step 3, the hydrogel of the drying obtained after step 2 is immersed in deionized water and is swollen, swelling temperature 12
DEG C, high-intensity and high-tenacity gelatin based aquagel can be obtained in swelling time 20h；
The mass ratio of dry hydrogel and deionized water is greater than 1:1.
The modulus of obtained hydrogel is 4.7MPa, and tensile break stress is that 0.8MPa energy of rupture is 117J/m2。
Embodiment 3
A kind of preparation method of high-intensity and high-tenacity gelatin based aquagel of the present invention, is specifically implemented according to the following steps:
Step 1, gelatin, functional material are uniformly mixed with water, obtain aqueous gelatin solution；
Functional material is hyaluronic acid；
Gelatin, functional material, water mass ratio be 1.5:0.2:8；
Step 2, acrylic monomer and initiator are added into the aqueous gelatin solution obtained after step 1, in ultraviolet light
Polymerization reaction is carried out under conditions of initiation, reaction temperature is 10 DEG C, reaction time 2h；It is dried later, obtains drying
Hydrogel, drying temperature are 20 DEG C, drying time 20h；
Aqueous gelatin solution, acrylic monomer, initiator mass ratio be 2:0.0008:1；
Acrylic monomer is dimethacrylate；
Initiator is 2- hydroxyl -4 '-(2- hydroxy ethoxy) -2- methyl phenyl ketone；
Step 3, the hydrogel of the drying obtained after step 2 is immersed in deionized water and is swollen, swelling temperature 15
DEG C, high-intensity and high-tenacity gelatin based aquagel can be obtained in swelling time 5h；
The mass ratio of dry hydrogel and deionized water is greater than 1:1.
Embodiment 4
A kind of preparation method of high-intensity and high-tenacity gelatin based aquagel of the present invention, is specifically implemented according to the following steps:
Step 1, gelatin, functional material are uniformly mixed with water, obtain aqueous gelatin solution；
Functional material is antibacterial nano-silver particle；
Gelatin, functional material, water mass ratio be 2:0.3:9；
Step 2, acrylic monomer and initiator are added into the aqueous gelatin solution obtained after step 1, in ultraviolet light
Polymerization reaction is carried out under conditions of initiation, reaction temperature is 12 DEG C, reaction time 18h；It is dried later, obtains drying
Hydrogel, drying temperature are 5 DEG C, drying time 10h；
Aqueous gelatin solution, acrylic monomer, initiator mass ratio be 0.15:0.01:1；
Acrylic monomer is methacrylic acid；
Initiator is α-ketoglutaric acid；
Step 3, the hydrogel of the drying obtained after step 2 is immersed in deionized water and is swollen, swelling temperature 18
DEG C, high-intensity and high-tenacity gelatin based aquagel can be obtained in swelling time 18h；
The mass ratio of dry hydrogel and deionized water is greater than 1:1.
Embodiment 5
A kind of preparation method of high-intensity and high-tenacity gelatin based aquagel of the present invention, is specifically implemented according to the following steps:
Step 1, gelatin, functional material are uniformly mixed with water, obtain aqueous gelatin solution；
Functional material is chitosan；
Gelatin, functional material, water mass ratio be 2.5:0.3:9；
Step 2, acrylic monomer and initiator are added into the aqueous gelatin solution obtained after step 1, in ultraviolet light
Polymerization reaction is carried out under conditions of initiation, reaction temperature is 15 DEG C, and the reaction time is for 24 hours；It is dried later, obtains drying
Hydrogel, drying temperature are 27 DEG C, and drying time is for 24 hours；
Aqueous gelatin solution, acrylic monomer, initiator mass ratio be 2:0.01:1；
Acrylic monomer is dimethacrylate；
Initiator is 2,2- azo two (2- methyl-propyl miaow) dihydrochloride；
Step 3, the hydrogel of the drying obtained after step 2 is immersed in deionized water and is swollen, swelling temperature 27
DEG C, high-intensity and high-tenacity gelatin based aquagel can be obtained in swelling time 18h；The matter of dry hydrogel and deionized water
Amount is than being greater than 1:1.
Gelatin hydrogel and existing gelatin after gelatin hydrogel prepared by the method for the present invention is polymerize with one-step method
Hydrogel carries out in stress-strain test, as shown in Figure 1, as shown in Figure 1, the gelatin hydrogel of the method for the present invention preparation is answered
Power and strain are all larger than the gelatin gel of other two methods preparation, this illustrates the gelatin based aquagel of the method for the present invention preparation
Stress-strain value is higher.
The gelatin hydrogel of the method for the present invention preparation, structure is as shown in Fig. 2, the structure of the gelatin hydrogel is to form half
It mutually passes or mutually passes network aqueous gel, for gelatin as the first layer network, the second layer network is linear or gathering containing a small amount of crosslinking agent
Acrylic compounds network, the second layer network are interacted by hydrogen bond and the first layer network.
High intensity gelatin based aquagel of the invention the preparation method comprises the following steps: using gelatin solution low temperature gel property, be added
Easily with gelatine molecular weight polar functional group such as-COOH ,-NH2,-CO-NH- etc. form the bifunctionality monomer of hydrogen bond, at low temperature
Direct polymerization, then the combination of the method promotion hydrogen bond by drying-swelling, ultimately form the gelatin hydrogel of high-intensity and high-tenacity
Material.
In addition, the gelatin double-network hydrogel, bright that gelatin hydrogel prepared by the method for the present invention is prepared with existing method
Glue-guar gum aqueous ionomer gel, modified gelatin-acrylamide composite hydrogel and chitin/gelatin-compounded hydrogel carry out
Mechanics Performance Testing, as shown in table 1, as shown in Table 1, the modulus of gelatin hydrogel of the method for the present invention preparation, fracture strength with
And breaking strain is all larger than the gelatin gel of other two methods preparation, this illustrates the gelatin based aquagel of the method for the present invention preparation
Mechanical property is preferable.
The mechanical property comparison of the different gelatin based aquagels of table 1
Claims (7)
1. a kind of preparation method of high-intensity and high-tenacity gelatin based aquagel, which is characterized in that be specifically implemented according to the following steps:
Step 1, gelatin, functional material are uniformly mixed with water, obtain aqueous gelatin solution；
Step 2, acrylic monomer and initiator are added into the aqueous gelatin solution obtained after step 1, ultraviolet light-initiated
Under conditions of carry out polymerization reaction, be dried later, obtain dry hydrogel；
Step 3, the hydrogel of the drying obtained after step 2 is immersed in deionized water and is swollen, high intensity can be obtained
High tenacity gelatin based aquagel.
2. a kind of preparation method of high-intensity and high-tenacity gelatin based aquagel according to claim 1, which is characterized in that institute
It states in step 1, functional material is chitosan, hyaluronic acid or antibacterial nano-silver particle；Gelatin, functional material, water
Mass ratio be 1~2.5:0~0.3:7.5~9.
3. a kind of preparation method of high-intensity and high-tenacity gelatin based aquagel according to claim 1, which is characterized in that institute
It states in step 2, reaction temperature is 1 DEG C~15 DEG C, and the reaction time is 1h~for 24 hours；Drying temperature is 1 DEG C~27 DEG C, drying time
For 2h~for 24 hours.
4. a kind of preparation method of high-intensity and high-tenacity gelatin based aquagel according to claim 1, which is characterized in that institute
State in step 2, aqueous gelatin solution, acrylic monomer, initiator mass ratio be 0.15~2:0.0003~0.01:1.
5. a kind of preparation method of high-intensity and high-tenacity gelatin based aquagel according to claim 1, which is characterized in that institute
State in step 2, acrylic monomer be acrylic acid, methacrylic acid, any one in dimethacrylate, two kinds and two kinds with
On mixture.
6. a kind of preparation method of high-intensity and high-tenacity gelatin based aquagel according to claim 1, which is characterized in that institute
It states in step 2, initiator is α-ketoglutaric acid, 2,2- azo two (2- methyl-propyl miaow) dihydrochloride, 2- hydroxyl -4 '-(2- hydroxyl
Ethyoxyl) any one in -2- methyl phenyl ketone.
7. a kind of preparation method of high-intensity and high-tenacity gelatin based aquagel according to claim 1, which is characterized in that institute
It states in step 3,1 DEG C~27 DEG C of swelling temperature, swelling time is 1h~200h.
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| CN113667037A (en) * | 2021-08-19 | 2021-11-19 | 中国石油大学(华东) | Photosensitive modified chitosan and preparation method and application thereof |
| CN113667037B (en) * | 2021-08-19 | 2023-06-27 | 中国石油大学(华东) | Photosensitive modified chitosan and preparation method and application thereof |
| CN115624651A (en) * | 2022-09-30 | 2023-01-20 | 中国人民解放军军事科学院军事医学研究院 | Adhesive ionic conductive hydrogel patch and preparation method thereof |
| CN115286820A (en) * | 2022-10-10 | 2022-11-04 | 佛山科学技术学院 | Photo-crosslinking collagen-based hydrogel and preparation method and application thereof |
| CN115286820B (en) * | 2022-10-10 | 2022-12-16 | 佛山科学技术学院 | Photo-crosslinking collagen-based hydrogel and preparation method and application thereof |
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