CN110551298B - Hydrogel with high shape recovery rate and preparation method thereof - Google Patents
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Abstract
The invention discloses a hydrogel with high shape recovery rate, which is composed of the following components: acrylic acid, chitosan, caCl 2 0 to 5 percent of acacia, ammonium persulfate and the balance of water; the preparation method comprises the following steps: mixing acrylic acid and chitosan, adding water with the weight being 8 to 10 times that of the chitosan, and stirring for 0.5 to 1.5h; adding CaCl 2 Stirring for 25 to 35min; adding Arabic gum and ammonium persulfate, adding water for dilution, and uniformly stirring; removing air bubbles, and heating for 6 to 8 hours at the temperature of 55 to 65 ℃; taking out, cleaning, and drying at 55 to 65 ℃ for 45 to 50h to obtain the hydrogel with high shape recovery rate; during the polymerization process of the hydrogel, hydrogen bonds are formed, and the coordination of amino groups on the chitosan and calcium ions are cooperated with each other to form a gel network; the hydrogel with high recovery rate prepared by the invention belongs to pure physical crosslinking, and has the properties of high strength, fatigue resistance and electric conduction.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a hydrogel with high shape recovery rate and a preparation method thereof.
Background
Chitosan (chitosan), also known as chitosan, is obtained by deacetylation of chitin (chitin) widely existing in nature and is chemically known as polyglucosamine (1-4) -2-amino-B-D glucose. Such natural polymers have been widely used in various industries for their excellent properties such as biological functionality, compatibility, blood compatibility, safety, and biodegradability, and have made great progress in the research of applications in various fields such as medicine, food, chemical engineering, cosmetics, water treatment, metal extraction and recovery, biochemistry, and biomedical engineering. While gum arabic is the oldest, most well-known natural gum in the world. Arabic gum contains high molecular polysaccharides and its calcium, magnesium and potassium salts. Mainly comprises arabinose, galactose, glucuronic acid and the like. However, natural polysaccharide molecules often have the defects of strong crystallinity, difficult processing and forming, poor mechanical properties, poor material recovery and the like.
Hydrogel is a hydrophilic three-dimensional network high molecular polymer, can absorb a large amount of water, is soft, is similar to a living tissue material, has good biocompatibility, and is widely applied. Can be used in the fields of biomedicine, tissue engineering and the like, such as tissue fillers, drug sustained release agents, enzyme embedding, protein electrophoresis, contact lenses, artificial blood plasma, artificial skin, tissue engineering scaffold materials and the like. In addition, based on the molecular unit structure of the polysaccharide, a large number of hydrogen bonds exist in the molecule and among the molecules, and specific functional groups possessed by different kinds of polysaccharides enable the gel to have different structural properties. However, the properties of single polysaccharide molecules are single, and most of the existing polysaccharide hydrogel products have the problems of complex preparation process and poor mechanical properties, thereby greatly limiting the wide application of the polysaccharide hydrogel products. Therefore, the development of the polysaccharide-based hydrogel which is simple to prepare and excellent in material performance has far-reaching significance.
Both hydrogels and elastomers have similar properties as polymeric materials, such as softness and stretchability, and are widely used in many similar fields, such as machinery, biology, medical treatment, etc. However, the different structures of the two make both hydrogels and elastomers unique applications in specific areas. The elastomer has unique characteristics such as stability under various environments, high mechanical strength, excellent recovery, etc., and the hydrogel has unique characteristics including high water content, good biocompatibility, etc. Similarly, the disadvantages of both are quite obvious, and the biocompatibility and the ion permeability of the elastomer are not strong, so that the application in the medical field is limited. Whereas hydrogels have poor mechanical strength compared to elastomers and recovery speed are far apart compared to elastomers. Therefore, combining the advantages of both elastomers and hydrogels to compensate for their deficiencies is a popular direction in the current field of hydrogel research.
To achieve the above object, there are two methods today, one is to improve the strength and recovery of the gel by adhering the hydrogel to the elastomer by means of a combination of the hydrogel and the elastomer. However, the gel prepared by the method is greatly dependent on the strength of adhesion between the gel and the elastomer, and the application range is limited, so that the gel is generally used for wound dressings and is difficult to apply to in vivo environments. Another approach is to increase the strength and recovery of the gel. The crosslinking mode in the gel is classified into chemical crosslinking and physical crosslinking. However, today's gels still need to overcome the problems of low recovery rate and long recovery time.
Disclosure of Invention
The invention aims to solve the problems of low recovery rate and long recovery time of the existing hydrogel, and provides the hydrogel with high shape recovery rate and the preparation method thereof.
A hydrogel with high shape recovery rate comprises the following components in percentage by weight: 18 to 22 percent of acrylic acid, 1 to 4 percent of chitosan and 0.5 to 1.5 percent of CaCl with the concentration of 1M 2 0 to 5 percent of Arabic gum, 0.1 to 0.3 percent of ammonium persulfate with the concentration of 0.7mmol, and the balance of water;
20% of acrylic acid, 4% of chitosan and 3% of Arabic gum.
A method for preparing a hydrogel with high shape recovery rate, which comprises the following steps:
1) Weighing the acrylic acid, the chitosan and the CaCl 2 Gum arabic and ammonium persulfate; mixing acrylic acid and chitosan, adding water with the weight being 8 to 10 times that of the chitosan, and stirring for 0.5 to 1.5h; adding CaCl 2 Stirring for 25 to 35min; adding Arabic gum and ammonium persulfate, adding water for dilution, and uniformly stirring; removing air bubbles, and heating for 6 to 8 hours at the temperature of 55 to 65 ℃;
2) Taking out, washing, and drying at 55 to 65 ℃ for 45 to 50h to obtain the hydrogel with high shape recovery rate;
putting the hydrogel with the high shape recovery rate obtained in the step 2) into an aqueous solution containing an active substance for 40 to 50h;
heating at 60 ℃ for 7h as described in step 1);
drying at 60 ℃ for 48h as described in step 2).
The invention provides a hydrogel with high shape recovery rate, which comprises the following components in percentage by weight: 18 to 22 percent of acrylic acid, 1 to 4 percent of chitosan and 0.5 to 1.5 percent of CaCl with the concentration of 1M 2 0 to 5 percent of Arabic gum, 0.1 to 0.3 percent of ammonium persulfate with the concentration of 0.7mmol, and the balance of water; the preparation method comprises the following steps: mixing acrylic acid and chitosan, adding water with the weight being 8-10 times that of the chitosan, and stirring for 0.5-1.5 h; adding CaCl 2 Stirring for 25 to 35min; adding Arabic gum and ammonium persulfate, adding water for dilution, and uniformly stirring; removing air bubbles, and heating for 6 to 8 hours at the temperature of 55 to 65 ℃; taking out, washing, and drying at 55 to 65 ℃ for 45 to 50h to obtain the hydrogel with high shape recovery rate; the hydrogel is synthesized by Acrylic Acid (AA), chitosan (Chitosan) and Arabic Gum (AG), in the polymerization process, AA is used as a monomer for copolymerization to generate a PAA long chain, meanwhile, electrostatic interaction is formed between amino on the Chitosan and carboxyl on the PAA and carboxyl on the Arabic gum, hydrogen bonds are formed between hydroxyl on the Chitosan and carboxyl on the PAA and hydroxyl on the Arabic gum, and the coordination of the amino on the Chitosan and calcium ions are cooperated with each other to form a gel network; the hydrogel with high recovery rate prepared by the invention belongs to pure physical crosslinking, and has the properties of high strength, fatigue resistance and electric conduction.
Drawings
FIG. 1 is a schematic diagram of the hydrogel preparation steps;
FIG. 2 shows the results of the mechanical strength test of the hydrogel;
FIG. 3 results of cyclic stretching experiments; a is a first, fifth and tenth cyclic stretch diagram; b is the maximum mechanical strength of the ten-cycle stretching; c, ten-cycle stretching deformation conditions of the gel; d is visual comparison of shape change after cyclic stretching;
FIG. 4 effect of chitosan addition on gels;
FIG. 5 Effect of gum arabic addition on gels.
Detailed Description
EXAMPLE 1 preparation of a high shape recovery hydrogel
1. Preparation method
1) Preparing an acrylic acid/chitosan aqueous solution: adding 7.6ml of acrylic acid into a beaker, adding 1.6g of chitosan and 15ml of water, and stirring for 1 hour;
2) Preparing a hydrogel: adding CaCl with a concentration of 1M 2 4ml, stirring for 30min; adding 1.2g of Arabic gum and 0.08g (0.7 mmol) of Ammonium Persulfate (APS) and simultaneously adding water to dilute until the total mass is 40g, and continuously stirring for 30min to obtain a uniform mixed solution; injecting into a mold, removing bubbles by ultrasonic waves, putting the mold into a 60 ℃ oven after bubbles are removed, heating for 7h, and gelling to obtain hydrogel;
3) Preparation of high shape recovery hydrogels: taking the gel out of the mold, washing the unreacted residue on the surface of the gel with deionized water, and putting the gel into an oven at 60 ℃ for 48h to completely dry the gel to obtain the hydrogel with high shape recovery rate (the preparation steps are shown in figure 1).
2. Application method
When in use, the hydrogel with high shape recovery rate is put into an aqueous solution containing active substances for 48 hours, and the hydrogel is taken out for standby after the colloid is swelled and balanced; the prior hydrogel can not restore to the original state due to the change of a reticular structure after being dried; after the hydrogel is dried and rehydrated, the shape of the hydrogel is basically recovered to the shape before drying, and the swelling property (rehydration property) is better.
Example 2 mechanical Property testing
Mechanical property test was performed using the hydrogel prepared in example 1;
1. tensile recovery test
The method comprises the following steps: cutting the prepared high-strength hydrogel with ultrahigh shape recovery rate into a dumbbell-shaped structure with the width of 4cm, the thickness of 3cm and the length of 6cm, taking 3 sample bars under the conditions of the embodiment, performing a mechanical tensile experiment on an Instron6022 universal material testing machine, measuring the gauge length of 10mm and the tensile speed of 50mm/min, and measuring the mechanical property of the hydrogel;
1) The tensile strength is calculated as follows:
σt=P/S
in the formula: p is the maximum load in N, S is the cross-sectional area of the sample in mm;
2) The elongation at break was calculated by the following formula
ε=L/L0×100%
In the formula: l is the stretching length of the stretcher, and the unit is cm; l0 is the original length of the sample in cm;
the result shows that the material has larger mechanical strength; as shown in FIG. 2a, the maximum tensile strength of the hydrogel is as high as 2.2MPa, and a reaction kettle with a weight of 3KG can be easily lifted. Meanwhile, the hydrogel also has excellent shape recovery capability; the hydrogel can be stretched to 100% deformation and then quickly return to its original shape, as shown in figure 2b, while the broken two parts of the gel can also quickly return to their original shape after being snapped off. This indicates that the hydrogel has a large tensile strength and a strong shape recovery (recovery rate 100%).
2. Cyclic stretching experiment
The method comprises the following steps: cutting the prepared high-strength hydrogel with ultrahigh shape recovery rate into a dumbbell-shaped structure with the width of 4cm, the thickness of 2cm and the length of 6cm, taking 3 sample bars under the conditions of the embodiment, performing 10 times of cyclic mechanical tensile experiments on an Instron6022 universal material testing machine, wherein the gauge length is 10mm, the tensile speed is 50mm/min, the cyclic tensile deformation is 400%, and measuring the length after cyclic tensile; and (3) performing ten times of cyclic stretching on the same gel, wherein the gel is unloaded from the clamp and soaked in distilled water for five minutes every time of cyclic stretching, so that the water lost in the stretching process of the gel is recovered.
1) The cyclic tensile strength is calculated as follows:
σt=P/S
in the formula: p is the maximum load in N, S is the cross-sectional area of the sample in mm;
2) The shape recovery rate was calculated as follows
Δ= L0/ L×100%
In the formula: l is the length after cyclic stretching, and the unit is cm; l0 is the original length of the sample in cm;
FIG. 3a shows a first, fifth, and tenth cyclic stretch; FIG. 3b shows the maximum mechanical strength of the tensile at ten cycles; the ten-cycle stretching of the gel fig. 3c is the change of the maximum stretching mechanics of the ten-cycle stretching and the deformation after stretching, and fig. 3d is the visual comparison of the shape change after the three-cycle stretching. As can be seen, the maximum mechanical strength of the gel after ten cycles of stretching is small and there is almost no change in shape. The hydrogel has a larger crosslinking density due to the multiple acting force synergistic effect of the hydrogel, and the molecular chains in the hydrogel can not generate relative slippage of chain segments and can only expand and contract, so that the hydrogel has no residual deformation in the cyclic stretching process, which indicates that the hydrogel has extremely strong shape recovery capability.
Example 3 Effect of reactant addition on gel Performance
1. Influence of the amount of chitosan added on the gel
1. Effect of different amounts of Chitosan on gels
Under the conditions that the Arabic gum is 3wt%, the acrylic acid is 20wt% and the calcium ion concentration is 0.1M, the influence of different chitosan contents (0 to 4 wt%) on the mechanical strength of the hydrogel is researched; as shown in fig. 4a-c, in the case of 3wt% gum arabic, 20wt% acrylic acid, and 0.1M calcium ion concentration, the system did not gel at a chitosan content of 0%; in the process that the content of the chitosan is gradually increased from 1 to 4 percent, the tensile strength of the hydrogel is increased from 62.9kPa to 2198kPa. The deformation amount increases from 147% to 618%. At the same time, the breaking energy is from 0.048kJ/m 2 Increase to 5.333kJ/m 2 The modulus increased from 38.95kPa to 506.62kPa. This is because as the content of chitosan increases, hydroxyl groups on chitosan will form a large number of hydrogen bonds with each other and amino groups coordinated with calcium ions increase, and at the same time, the electrostatic interaction between amino groups and carboxyl groups on acrylic acid and gum arabic increases, and these forces cooperate with each other to make hydrogel have a large number of hydrogen bondsThe mechanical strength is obviously improved.
2. Comparison of Performance before and after drying
Meanwhile, the performance of the hydrogel before drying (undried hydrogel) is tested and compared with the hydrogel with high shape recovery rate (hydrogel rehydrated after drying); the results are shown in Table 1; the results show that the influence trend of the addition amount of chitosan on the gel is the same before and after drying; the mechanical strength of the undried hydrogel is low; the elastic material can not be recovered after being stretched and has poor elasticity; the dried gel had high strength and could recover shape instantly (less than 0.5 second) after stretching, which is a characteristic not possessed by the gel before drying, indicating that drying improves gel elasticity.
2. Effect of the amount of Arabic gum added on the gel
1. Effect of different amounts of acacia gum on gels
When the chitosan is 4wt%, the acrylic acid is 20wt% and the calcium ion concentration is 0.1M, the influence of different Arabic gum contents (0 to 5 wt%) on the mechanical strength of the hydrogel is researched; as shown in fig. 5a-c, the mechanical strength of the hydrogel increased from 981.70kPa to 2198.15kPa as the gum arabic content increased from 0% to 3%. The deformation amount is reduced from 979% to 619%. The modulus is increased from 148.42kPa to 506.62kPa, and the breaking energy is increased from 4.33 kJ/m 2 Increased to 5.33 kJ/m 2 . The reason is that the increase of the Arabic gum content can introduce a large amount of hydroxyl in polysaccharide in the Arabic gum to form a large amount of hydrogen bonds with hydroxyl on chitosan and carboxyl on acrylic acid, and simultaneously, the electrostatic interaction between carboxyl on glucuronic acid in the Arabic gum and amino on chitosan as well as the electrostatic interaction between amino on a small amount of amino acid in the Arabic gum and carboxyl on acrylic acid is gradually enhanced, so that the crosslinking density of the hydrogel is increased, the deformation amount of the hydrogel is gradually reduced, and the mechanical strength is increased. When the content of the Arabic gum is increased from 3% to 5%, the tensile strength of the gel is reduced from 2198.15kPa to 1691.45kPa, and the deformation amount is reduced from 617% to 3And 63 percent. Energy at break of from 5.33 kJ/m 2 Reduced to 2.26kJ/m 2 While the modulus increased from 506.62kPa to 830.33kPa. This is because, as the gum arabic is added continuously, the synergy becomes stronger and the crosslinking density becomes higher, so that the modulus of the hydrogel increases, and this also makes the extent of molecular chain extension in the hydrogel smaller, so that the deformation amount of the gel becomes smaller and the breaking energy becomes smaller.
2. Comparison of Performance before and after drying
Meanwhile, the performance of the hydrogel before drying (undried hydrogel) is tested and compared with the hydrogel with high shape recovery rate (hydrogel rehydrated after drying); the results are shown in Table 2; the results show that the influence trend of the addition amount of the Arabic gum on the gel is the same before and after drying; the mechanical strength of the undried hydrogel is low; the elastic material can not be recovered after being stretched and has poor elasticity; the dried gel has high strength and can recover shape instantly (time is less than 0.5 second) after stretching, which is a characteristic that the gel before drying does not have, and the drying improves the elasticity of the gel.
Claims (5)
1. A preparation method of hydrogel with high shape recovery rate is characterized by comprising the following steps: it includes:
1) Weighing acrylic acid, chitosan and CaCl 2 Gum arabic and ammonium persulfate; mixing acrylic acid and chitosan, adding water with the weight being 8 to 10 times that of the chitosan, and stirring for 0.5 to 1.5h; adding CaCl 2 Stirring for 25 to 35min; adding Arabic gum and ammonium persulfate, adding water for dilution, and uniformly stirring; removing air bubbles, and heating for 6 to 8 hours at the temperature of 55 to 65 ℃;
2) Taking out, washing, and drying at 55 to 65 ℃ for 45 to 50h to completely dry the colloid to obtain the hydrogel with high shape recovery rate; the weight ratio of the raw materials is as follows: 18 to 22 percent of acrylic acid, 1 to 4 percent of chitosan and 0.5 to 1.5 percent of CaCl with the concentration of 1M 2 0 to 5 percent of Arabic gum, 0.1 to 0.3 percent of ammonium persulfate with the concentration of 0.7mmol, and the balanceIs water.
2. The method for preparing a hydrogel with high shape recovery rate according to claim 1, wherein the method comprises the following steps: rehydrating the hydrogel with high shape recovery rate obtained in the step 2).
3. The method for preparing a hydrogel with high shape recovery rate according to claim 2, wherein the method comprises the following steps: the heating in the step 1) is carried out for 7 hours at the temperature of 60 ℃.
4. The method for preparing a hydrogel with high shape recovery rate according to claim 3, wherein the method comprises the following steps: the drying in the step 2) is carried out for 48 hours at the temperature of 60 ℃.
5. The method for preparing a hydrogel with high shape recovery rate according to claim 1, 2, 3 or 4, wherein the method comprises the following steps: the raw materials comprise 20% of acrylic acid, 4% of chitosan and 3% of Arabic gum.
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| Optimization Of Swelling, Drug Loading And Release From Natural Polymer Hydrogels;M. K Younis，et al;《INTERNATIONAL CONFERENCE ON MATERIALS ENGINEERING AND SCIENCE》;20180809;第454卷;摘要，第2.2节 * |
| Strong and tough fully physically crosslinked double network hydrogels with tunable mechanics and high self-healing performance;Wang XH，et al;《CHEMICAL ENGINEERING JOURNAL》;20180514;第349卷;第4.2节,第589页左栏第二段，第590页左栏最后一段至右栏第一段 * |
| 聚乙烯醇-壳聚糖复合水凝胶的溶胀性能;吴国杰等;《精细化工》;20060630;第23卷(第6期);第532-535页 * |
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