CN109988343B - Alkali-soluble chitosan-sodium alginate hydrogel material with shape memory function and preparation method thereof - Google Patents
Alkali-soluble chitosan-sodium alginate hydrogel material with shape memory function and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an alkali-soluble chitosan-sodium alginate hydrogel material with a shape memory function and a preparation method thereof. Fully swelling chitosan powder and sodium alginate powder in a mixed aqueous solution of lithium hydroxide monohydrate and urea, performing freezing-unfreezing processes for multiple times, then preparing a sample, gelatinizing the solution, and dialyzing in deionized water completely to obtain an alkali-soluble chitosan-sodium alginate gel strip; after imparting a second shape to the gel strip, transfer to Ca2+Soaking in solution for fixing in a second shape, taking out, and removing surface residual Ca with deionized water2+Put in a container containing CO3 2‑The gel strip can be fixed in the solution to recover the initial shape of the gel strip, namely, the shape memory process is realized, and the gel strip can realize more than 3 times of shape memory circulation in the two solutions. At the same time, when the gel strip is at Ca2+After the semi-interpenetrating polymer network structure is soaked in the solution, the semi-interpenetrating polymer network structure is obtained, and the mechanical property is improved. The shape memory hydrogel material is expected to be applied to the fields of biological medicine and the like.
Description
Technical Field
The invention belongs to the field of shape memory hydrogel preparation, and particularly relates to an alkali-soluble chitosan-sodium alginate hydrogel material with a shape memory function and a preparation method thereof.
Background
Shape memory polymers, also known as shape memory polymers, refer to polymeric materials that can recover their original shape after an article having the original shape is fixed after its original condition is changed under certain conditions, and stimulated by external conditions (such as heat, electricity, light, chemical induction, etc.). Due to the shape memory property, the material can be widely applied to the fields of aviation and aerospace deployment components and structures, intelligent materials and fabrics, heat shrinkable films of electronic packages or tubes, intelligent medical devices and the like.
Sodium alginate is a byproduct after iodine and mannitol are extracted from brown algae such as kelp or gulfweed, the molecule of sodium alginate is formed by connecting beta-D-mannuronic acid (beta-D-mannuronic, M) and alpha-L-guluronic acid (alpha-L-guluronic acid, G) according to a (1 → 4) bond, and the sodium alginate is a natural polysaccharide. It has stability, solubility, viscosity and safety required for pharmaceutical preparation excipients, and thus is widely used in the fields of food industry, medicine, and the like.
Chitosan is the deacetylated product of chitin, is the second largest natural polymer material with the next best storage amount to cellulose in nature, is the only biologically renewable alkaline polysaccharide biopolymer, has the characteristics of good biocompatibility, biodegradability, no toxicity and the like, and can be widely applied to the fields of biomedical industry and the like. The hydrogel is prepared by using sodium alginate and chitosan as raw materials, so that the material has excellent mechanical property and shape memory property, and the two raw materials have outstanding biocompatibility, and the material is expected to be applied to the fields of biomedicine and the like.
Disclosure of Invention
The invention aims to provide an alkali-soluble chitosan-sodium alginate hydrogel material with a shape memory function and a preparation method thereof.
The invention is realized by adopting the following technical scheme:
firstly, preparing an alkali-soluble chitosan-sodium alginate solution, casting the solution into a mould for sample preparation after centrifugal defoaming, and obtaining an alkali-soluble chitosan-sodium alginate gel strip after the solution is completely gelatinized; transferring to a concentration of Ca after a second shape is imparted to the gel strip2+Soaking in the solution for a certain time for shape fixation, taking out, and removing surface residual Ca with deionized water2+Then put in a reactor containing CO3 2-Can be released from the solution to restore the original shape of the gel strip, namely realizing the shape memory process.
The preparation method and the shape memory process of the alkali-soluble chitosan-sodium alginate hydrogel material are specifically realized by the following steps:
1) weighing the following components in percentage by mass: 1-10% of chitosan, 1-10% of sodium alginate, 4-15% of lithium hydroxide monohydrate, 3-10% of urea and the balance of water; the molecular weight of the chitosan is 200000-; the viscosity (10g/L, 20 ℃) of the sodium alginate is 0.02-0.1 Pa.s; mixing the above components, swelling, and freezing and thawing for multiple times to obtain alkali-soluble chitosan-sodium alginate solution;
2) centrifuging and defoaming the alkali-soluble chitosan-sodium alginate solution prepared in the step 1), casting the alkali-soluble chitosan-sodium alginate solution into a mold, transferring the mold into a 60 ℃ oven, heating for two hours to realize gelation, and dialyzing the solution by deionized water to be neutral to obtain alkali-soluble chitosan-sodium alginate gel;
3) adding the alkali-soluble chitosan-sodium alginate gel strip into a second shape, and transferring to 0.2-2M Ca2+Soaking in the solution for 5-30min to fix the shape of gel strip;
4) taking out the gel strip, and removing the residual Ca on the surface by using deionized water2+；
5) The gel strip was transferred to 0.2-2M CO3 2-Soaking in the solution for 1-10h to recover the shape of the gel strip.
Wherein, Ca is described in step 3)2+The solution is calcium chloride, calcium nitrate and the like; CO in step 5)3 2-The solution is sodium carbonate, potassium carbonate, etc.
Compared with the prior art, the invention has the following advantages:
1) the alkali-soluble chitosan-sodium alginate gel can contain Ca2+And CO3 2-The shape memory process is realized in the solution, more than 3 times of circulation process can be realized, and the recovery degree can reach more than 50 percent;
2) the hydrogel with the shape memory function has simple preparation process, and the shape memory process can be realized in simple salt solution;
3) due to sodium alginate and Ca2+A temporary cross-linking point is formed through coordination, so that a semi-interpenetrating polymer network structure can be formed by the chitosan and the sodium alginate, and the mechanical property of the gel is improved;
4) the chitosan and the sodium alginate are used as raw materials, the biocompatibility of the material is excellent, and the shape memory characteristic of the material can be applied to the relevant fields of biomedicine and the like.
The specific implementation mode is as follows:
the present invention is further illustrated by the following specific examples.
Example 1:
1) weighing the following components in percentage by mass: 2% of chitosan, 2% of sodium alginate, 8% of lithium hydroxide monohydrate, 6% of urea and the balance of water; the molecular weight of the chitosan is 2000000; the viscosity (10g/L, 20 ℃) of the sodium alginate is 0.04 Pa.s; mixing the above components, swelling, and freezing and thawing for several times;
2) centrifuging and defoaming the alkali-soluble chitosan-sodium alginate solution prepared in the step 1), casting the alkali-soluble chitosan-sodium alginate solution into a mold, transferring the mold into a 60 ℃ oven, heating for two hours to realize gelation, and dialyzing the solution by deionized water until the pH value is approximately equal to 7 to obtain the alkali-soluble chitosan-sodium alginate gel;
3) endowing the prepared alkali-soluble chitosan-sodium alginate gel strip with a second shape, transferring the gel strip into 0.2M calcium chloride solution, and soaking for 20min to realize the fixation of the gel strip shape;
4) taking out the gel strip, and using deionized waterRemoving Ca remained on the surface2+；
5) Transferring the gel strip into 0.5M sodium carbonate solution, and soaking for 4h to realize the recovery of the gel strip shape, wherein the recovery degree reaches 81%;
6) by the third time, the degree of recovery reached 57% after 7h of soaking in 0.5M sodium carbonate solution.
Example 2:
1) weighing the following components in percentage by mass: 1% of chitosan, 3% of sodium alginate, 10% of lithium hydroxide monohydrate, 3% of urea and the balance of water; the molecular weight of the chitosan is 800000; the viscosity (10g/L, 20 ℃) of the sodium alginate is 0.05 Pa.s; mixing the above components, swelling, and freezing and thawing for several times;
2) centrifuging and defoaming the alkali-soluble chitosan-sodium alginate solution prepared in the step 1), casting the alkali-soluble chitosan-sodium alginate solution into a mold, transferring the mold into a 60 ℃ oven, heating for two hours to realize gelation, and dialyzing the solution by deionized water until the pH value is approximately equal to 7 to obtain the alkali-soluble chitosan-sodium alginate gel;
3) endowing the prepared alkali-soluble chitosan-sodium alginate gel strip with a second shape, and transferring the gel strip into 0.5M calcium nitrate solution for soaking for 10min to realize the fixation of the gel strip shape;
4) taking out the gel strip, and removing the residual Ca on the surface by using deionized water2+；
5) Transferring the gel strip into 0.1M sodium carbonate solution, and soaking for 1h to realize the recovery of the gel strip shape, wherein the recovery degree can reach 87%;
6) by the third time, the degree of recovery reached 64% after 5h of immersion in 0.1M sodium carbonate solution.
Example 3:
1) weighing the following components in percentage by mass: 8% of chitosan, 1% of sodium alginate, 12% of lithium hydroxide monohydrate, 4% of urea and the balance of water; the molecular weight of the chitosan is 300000; the viscosity (10g/L, 20 ℃) of the sodium alginate is 0.02 Pa.s; mixing the above components, swelling, and freezing and thawing for several times;
2) centrifuging and defoaming the alkali-soluble chitosan-sodium alginate solution prepared in the step 1), casting the alkali-soluble chitosan-sodium alginate solution into a mold, transferring the mold into a 60 ℃ oven, heating for two hours to realize gelation, and dialyzing the solution by deionized water until the pH value is approximately equal to 7 to obtain the alkali-soluble chitosan-sodium alginate gel;
3) endowing the prepared alkali-soluble chitosan-sodium alginate gel strip with a second shape, transferring the gel strip into 0.6M calcium chloride solution, and soaking for 20min to realize the fixation of the gel strip shape;
4) taking out the gel strip, and removing the residual Ca on the surface by using deionized water2+；
5) And transferring the gel strip into 0.9M potassium carbonate solution, and soaking for 8h to realize the recovery of the gel strip shape, wherein the recovery degree can reach 74%.
6) By the third time, the degree of recovery reached 51% after 10h of soaking in 0.9M potassium carbonate solution.
Example 4:
1) weighing the following components in percentage by mass: 2% of chitosan, 3% of sodium alginate, 8% of lithium hydroxide monohydrate, 5% of urea and the balance of water; the molecular weight of the chitosan is 400000; the viscosity (10g/L, 20 ℃) of the sodium alginate is 0.06 Pa.s; mixing the above components, swelling, and freezing and thawing for several times;
2) centrifuging and defoaming the alkali-soluble chitosan-sodium alginate solution prepared in the step 1), casting the alkali-soluble chitosan-sodium alginate solution into a mold, transferring the mold into a 60 ℃ oven, heating for two hours to realize gelation, and dialyzing the solution by deionized water until the pH value is approximately equal to 7 to obtain the alkali-soluble chitosan-sodium alginate gel;
3) endowing the prepared alkali-soluble chitosan-sodium alginate gel strip with a second shape, transferring the gel strip into a 1M calcium nitrate solution, and soaking for 20min to realize the fixation of the gel strip shape;
4) taking out the gel strip, and removing the residual Ca on the surface by using deionized water2+；
5) And transferring the gel strip into 0.8M potassium carbonate solution, and soaking for 4h to realize the recovery of the gel strip shape, wherein the recovery degree can reach 78%.
6) By the third time, the degree of recovery reached 53% after 6h soaking in 0.8M potassium carbonate solution.
Example 5:
1) weighing the following components in percentage by mass: 1% of chitosan, 8% of sodium alginate, 4% of lithium hydroxide monohydrate, 3% of urea and the balance of water; the molecular weight of the chitosan is 2200000; the viscosity (10g/L, 20 ℃) of the sodium alginate is 0.08 Pa.s; mixing the above components, swelling, and freezing and thawing for several times;
2) centrifuging and defoaming the alkali-soluble chitosan-sodium alginate solution prepared in the step 1), casting the alkali-soluble chitosan-sodium alginate solution into a mold, transferring the mold into a 60 ℃ oven, heating for two hours to realize gelation, and dialyzing the solution by deionized water until the pH value is approximately equal to 7 to obtain the alkali-soluble chitosan-sodium alginate gel;
3) endowing the prepared alkali-soluble chitosan-sodium alginate gel strip with a second shape, transferring the gel strip into a 1M calcium chloride solution, and soaking for 8min to realize the fixation of the gel strip shape;
4) taking out the gel strip, and removing the residual Ca on the surface by using deionized water2+；
5) And transferring the gel strip into a 1.2M sodium carbonate solution, and soaking for 8h to realize the recovery of the gel strip shape, wherein the recovery degree can reach 89%.
6) By the third time, the degree of recovery reached 68% after 10h of immersion in 1.2M sodium carbonate solution.
Claims (3)
1. An alkali-soluble chitosan-sodium alginate hydrogel material with a shape memory function is characterized in that: the hydrogel is prepared from alkali-soluble chitosan and sodium alginate, and can contain Ca2+To neutralize the CO-containing solution3 2-The process of shape fixation and recovery is realized in the solution;
the hydrogel is prepared by the following specific steps:
1) weighing the following components in percentage by mass: 1-10% of chitosan, 1-10% of sodium alginate, 4-15% of lithium hydroxide monohydrate, 3-10% of urea and the balance of water; the molecular weight of the chitosan is 200000-; the viscosity of the sodium alginate at the concentration of 10g/L and the temperature of 20 ℃ is 0.02-0.1 Pa.s; mixing the above components, swelling, and freezing and thawing for multiple times to obtain alkali-soluble chitosan-sodium alginate solution;
2) centrifuging and defoaming the alkali-soluble chitosan-sodium alginate solution prepared in the step 1), casting the alkali-soluble chitosan-sodium alginate solution into a mold, transferring the mold into a 60 ℃ oven, heating for two hours to realize gelation, and dialyzing the solution by deionized water until the solution is neutral to obtain the alkali-soluble chitosan-sodium alginate gel with the shape memory function;
the specific shape memory function is realized as follows:
1) endowing the alkali-soluble chitosan-sodium alginate gel strip with a second shape, and transferring the alkali-soluble chitosan-sodium alginate gel strip to 0.2-2M Ca2+Soaking in the solution for 5-30min to fix the gel strip in the second shape;
2) taking out the gel strip, and removing the residual Ca on the surface by using deionized water2+；
3) The gel strip was transferred to 0.2-2M CO3 2-Soaking in the solution for 1-10h to realize the recovery of the shape of the gel strip; the shape memory process of the gel material can realize more than 3 times of circulation, and the recovery degree can reach more than 50%.
2. The alkali-soluble chitosan-sodium alginate hydrogel material with the shape memory function as claimed in claim 1, which is characterized in that: the Ca content in the process of realizing the shape memory function2+The solution of (A) is calcium chloride and calcium nitrate solution.
3. The alkali-soluble chitosan-sodium alginate hydrogel material with the shape memory function as claimed in claim 1, which is characterized in that: said CO-containing in the process of shape memory function realization3 2-The solution of (A) is sodium carbonate and potassium carbonate solution.
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Inventor after: Jin Xiaoqiang Inventor after: Jiang Huihong Inventor after: Bao Xiaojiong Inventor after: Fu Beijia Inventor after: Qiao Fenghui Inventor after: Jiang Zhiqi Inventor after: Hu Qiaoling Inventor after: Wang Zhengke Inventor before: Wang Zhengke Inventor before: Jin Xiaoqiang Inventor before: Jiang Huihong Inventor before: Bao Xiaojiong Inventor before: Fu Beijia Inventor before: Qiao Fenghui Inventor before: Jiang Zhiqi Inventor before: Hu Qiaoling |