CN109988343A - A kind of alkali soluble chitin-sodium alginate hydrogel material and preparation method thereof with shape memory function - Google Patents

A kind of alkali soluble chitin-sodium alginate hydrogel material and preparation method thereof with shape memory function Download PDF

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CN109988343A
CN109988343A CN201910202695.4A CN201910202695A CN109988343A CN 109988343 A CN109988343 A CN 109988343A CN 201910202695 A CN201910202695 A CN 201910202695A CN 109988343 A CN109988343 A CN 109988343A
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sodium alginate
solution
alkali soluble
shape
shape memory
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CN109988343B (en
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王征科
金晓强
姜慧虹
鲍晓炯
傅倍佳
乔丰慧
姜质琦
胡巧玲
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Zhejiang University ZJU
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075—Macromolecular gels
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
    • C08J2305/04—Alginic acid; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
    • C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/04—Alginic acid; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Materials For Medical Uses (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The invention discloses a kind of alkali soluble chitin-sodium alginate hydrogel material and preparation method thereof with shape memory function.Be by Chitosan powder and sodium alginate powder a hydronium(ion) lithia, urea mixed aqueous solution in be sufficiently swollen, through multiple freeze-thaw process, sample preparation waits for solution gels again, obtains alkali soluble chitin-sodium alginate gel strips after dialysing completely in deionized water；After assigning one the second shape of gel strips, it is transferred to Ca2+The second shape can be carried out by, which impregnating in solution, fixes, and removes remained on surface Ca using deionized water after taking-up2+, it is put into containing CO3 2‑Solution in can solve fixation, restore gel strips original shape, i.e. realization shape recovery process, and the gel strips can realize 3 times or more memory cycles in above two solution.Meanwhile when gel strips are in Ca2+After being impregnated in solution, semi-interpenetrating polymer network structure is obtained, mechanical property gets a promotion.The shape memory gel material is expected to be applied to the fields such as bio-medical.

Description

A kind of alkali soluble chitin-sodium alginate hydrogel material with shape memory function And preparation method thereof
Technical field
The invention belongs to shape memory gel preparation fields, and in particular to a kind of alkali soluble shell with shape memory function Glycan-Sodium Alginate Hydrogel Films material and preparation method thereof.
Background technique
Shape-memory polymer, also known as shape memory high molecule refer to the product with original shape in certain item After changing its primary condition under part and fixing, it can be restored again by the stimulation of external condition (such as heat, electricity, light, chemical co-ordination) The high molecular material of its original shape.Due to its shape memory characteristic, which can be widely applied to the deployment of Aeronautics and Astronautics The fields such as component and the heat shrink films of structure, intellectual material and fabric, electronic packaging or pipe, intelligent medical devices.
Sodium alginate is the by-product after extracting iodine and mannitol in the kelp or sargassum of brown algae, molecule by Beta-D-mannuronic acid (β-D-mannuronic, M) and α-L- guluronic acid (α-L-guluronic, G) press (1 → 4) key company It connects, is a kind of natural polysaccharide.Since it is with stability needed for pharmaceutical preparation auxiliary material, dissolubility, viscosity and safety, It is therefore widely used in food industry and medicine and other fields.
Chitosan is the product after de-acetyl chitin, is that reserves are only second to the second largest natural of cellulose in nature High molecular material, be unique one kind can bio-regeneration alkaline polysaccharide class boiomacromolecule, have good biocompatibility, can biology The features such as degrading, is nontoxic, can be widely used in the fields such as biologic medical industry.Made simultaneously using sodium alginate and chitosan Hydrogel is prepared for raw material, material can be assigned with excellent mechanical property and shape-memory properties, and two kinds of raw materials are equal With biocompatibility outstanding, it is expected to the material being applied to the fields such as bio-medical.
Summary of the invention
The alkali soluble chitin-sodium alginate water-setting glue material with shape memory function that it is an object of the present invention to provide a kind of Material and preparation method thereof.
The present invention is implemented with the following technical solutions:
Alkali soluble chitin-sodium alginate solution is prepared first, is cast to sample preparation in mold after evacuation and centrifugal degassing, it is complete to solution Alkali soluble chitin-sodium alginate gel strips are obtained after gelation；After revesting one the second shape of gel strips, it is transferred to certain dense The Ca of degree2+Certain time progress shape is impregnated in solution to fix, and removes remained on surface Ca using deionized water after taking-up2+, then It is put into containing CO3 2-Solution in can solve fixation, reply gel strips original shape, i.e. realization shape recovery process.
The preparation method and shape recovery process of above-mentioned alkali soluble chitin-sodium alginate hydrogel material, it is specific real Existing process is as follows:
1) each component is weighed according to mass percent: chitosan 1%-10%, sodium alginate 1%-10%, a hydrated hydroxide Change lithium 4-15%, urea 3-10%, remaining is water；The molecular weight of chitosan is 200000-2500000；The seaweed Sour sodium viscosity (10g/L, 20 DEG C) is 0.02-0.1Pas；After said components are mixed swelling, through multiple freeze-thaw process Alkali soluble chitin-sodium alginate solution is made；
2) by above-mentioned steps 1) in prepare alkali soluble chitin-sodium alginate solution evacuation and centrifugal degassing, pour and cast from mold, and It is transferred in 60 DEG C of baking ovens and heats two hours to realize gelation, gather after deionized water dialysis to neutrality to get alkali soluble shell Sugar-sodium alginate gel；
3) it after revesting one the second shape of alkali soluble chitin-sodium alginate gel strips obtained above, is transferred into The Ca of 0.2-2M2+In solution impregnate 5-30min, it can be achieved that gel strip fixation；
4) gel strips are taken out, remove Ca remained on surface using deionized water2+；
5) gel strips are then transferred to the CO of 0.2-2M3 2-In solution, gel strip can be realized after impregnating 1-10h It replys.
Wherein, Ca described in step 3)2+Solution is the solution such as calcium chloride, calcium nitrate；CO described in step 5)3 2-Solution For solution such as sodium carbonate, potassium carbonate.
Compared with the existing technology, the invention has the following advantages that
1) the alkali soluble chitin-sodium alginate gel can contain Ca2+And CO3 2-Solution in realize shape recovery process, and And can realize 3 times or more cyclic processes, degree is replied up to 50% or more；
2) hydrogel with shape memory function, preparation process is simple, and shape recovery process is in simple salting liquid In can be realized；
3) due to sodium alginate and Ca2+Interim crosslinking points are formed by coordination, so chitosan and sodium alginate meeting Semi-interpenetrating polymer network structure is formed, gel mechanical property is made to get a promotion；
4) use chitosan and sodium alginate as raw material, Biocompatibility is excellent, can be by its shape memory characteristic Applied to related fieldss such as bio-medicals.
Specific embodiment:
The present invention is further illustrated below with reference to specific example.
Example 1:
1) each component is weighed according to mass percent: chitosan 2%, sodium alginate 2%, a hydronium(ion) lithia 8%, urine Element 6%, remaining is water；The molecular weight of chitosan is 2000000；The sodium alginate viscosity (10g/L, 20 DEG C) is 0.04Pa·s；After said components are mixed swelling, it is made through multiple freeze-thaw process；
2) by above-mentioned steps 1) in prepare alkali soluble chitin-sodium alginate solution evacuation and centrifugal degassing, pour and cast from mold, and It is transferred in 60 DEG C of baking ovens and heats two hours to realize gelation, gather after deionized water dialysis to pH ≈ 7 to get alkali soluble shell Sugar-sodium alginate gel；
3) it after revesting one the second shape of alkali soluble chitin-sodium alginate gel strips obtained above, is transferred into 20min is impregnated in the calcium chloride solution of 0.2M, to realize the fixation of gel strip；
4) gel strips are taken out, remove Ca remained on surface using deionized water2+；
5) gel strips are then transferred in the sodium carbonate liquor of 0.5M, returning for gel strip can be realized after impregnating 4h Multiple, reply degree reaches 81%；
6) when repeating to third time, 7h reply degree is impregnated in 0.5M sodium carbonate liquor and reaches 57%.
Example 2:
1) weigh each component according to mass percent: chitosan 1%, sodium alginate 3%, a hydronium(ion) lithia 10%, Urea 3%, remaining is water；The molecular weight of chitosan is 800000；The sodium alginate viscosity (10g/L, 20 DEG C) is 0.05Pa·s；After said components are mixed swelling, it is made through multiple freeze-thaw process；
2) by above-mentioned steps 1) in prepare alkali soluble chitin-sodium alginate solution evacuation and centrifugal degassing, pour and cast from mold, and It is transferred in 60 DEG C of baking ovens and heats two hours to realize gelation, gather after deionized water dialysis to pH ≈ 7 to get alkali soluble shell Sugar-sodium alginate gel；
3) it after revesting one the second shape of alkali soluble chitin-sodium alginate gel strips obtained above, is transferred into 10min is impregnated in the calcium nitrate solution of 0.5M, to realize the fixation of gel strip；
4) gel strips are taken out, remove Ca remained on surface using deionized water2+；
5) gel strips are then transferred in the sodium carbonate liquor of 0.1M, returning for gel strip can be realized after impregnating 1h It is multiple, degree is replied up to 87%；
6) when repeating to third time, 5h reply degree is impregnated in 0.1M sodium carbonate liquor and reaches 64%.
Example 3:
1) weigh each component according to mass percent: chitosan 8%, sodium alginate 1%, a hydronium(ion) lithia 12%, Urea 4%, remaining is water；The molecular weight of chitosan is 300000；The sodium alginate viscosity (10g/L, 20 DEG C) is 0.02Pa·s；After said components are mixed swelling, it is made through multiple freeze-thaw process；
2) by above-mentioned steps 1) in prepare alkali soluble chitin-sodium alginate solution evacuation and centrifugal degassing, pour and cast from mold, and It is transferred in 60 DEG C of baking ovens and heats two hours to realize gelation, gather after deionized water dialysis to pH ≈ 7 to get alkali soluble shell Sugar-sodium alginate gel；
3) it after revesting one the second shape of alkali soluble chitin-sodium alginate gel strips obtained above, is transferred into 20min is impregnated in the calcium chloride solution of 0.6M, to realize the fixation of gel strip；
4) gel strips are taken out, remove Ca remained on surface using deionized water2+；
5) gel strips are then transferred in the solution of potassium carbonate of 0.9M, returning for gel strip can be realized after impregnating 8h It is multiple, degree is replied up to 74%.
6) when repeating to third time, 10h reply degree is impregnated in 0.9M solution of potassium carbonate and reaches 51%.
Example 4:
1) each component is weighed according to mass percent: chitosan 2%, sodium alginate 3%, a hydronium(ion) lithia 8%, urine Element 5%, remaining is water；The molecular weight of chitosan is 400000；The sodium alginate viscosity (10g/L, 20 DEG C) is 0.06Pa·s；After said components are mixed swelling, it is made through multiple freeze-thaw process；
2) by above-mentioned steps 1) in prepare alkali soluble chitin-sodium alginate solution evacuation and centrifugal degassing, pour and cast from mold, and It is transferred in 60 DEG C of baking ovens and heats two hours to realize gelation, gather after deionized water dialysis to pH ≈ 7 to get alkali soluble shell Sugar-sodium alginate gel；
3) it after revesting one the second shape of alkali soluble chitin-sodium alginate gel strips obtained above, is transferred into 20min is impregnated in the calcium nitrate solution of 1M, to realize the fixation of gel strip；
4) gel strips are taken out, remove Ca remained on surface using deionized water2+；
5) gel strips are then transferred in the solution of potassium carbonate of 0.8M, returning for gel strip can be realized after impregnating 4h It is multiple, degree is replied up to 78%.
6) when repeating to third time, 6h reply degree is impregnated in 0.8M solution of potassium carbonate and reaches 53%.
Example 5:
1) each component is weighed according to mass percent: chitosan 1%, sodium alginate 8%, a hydronium(ion) lithia 4%, urine Element 3%, remaining is water；The molecular weight of chitosan is 2200000；The sodium alginate viscosity (10g/L, 20 DEG C) is 0.08Pa·s；After said components are mixed swelling, it is made through multiple freeze-thaw process；
2) by above-mentioned steps 1) in prepare alkali soluble chitin-sodium alginate solution evacuation and centrifugal degassing, pour and cast from mold, and It is transferred in 60 DEG C of baking ovens and heats two hours to realize gelation, gather after deionized water dialysis to pH ≈ 7 to get alkali soluble shell Sugar-sodium alginate gel；
3) it after revesting one the second shape of alkali soluble chitin-sodium alginate gel strips obtained above, is transferred into 8min is impregnated in the calcium chloride solution of 1M, to realize the fixation of gel strip；
4) gel strips are taken out, remove Ca remained on surface using deionized water2+；
5) gel strips are then transferred in the sodium carbonate liquor of 1.2M, returning for gel strip can be realized after impregnating 8h It is multiple, degree is replied up to 89%.
6) when repeating to third time, 10h reply degree is impregnated in 1.2M sodium carbonate liquor and reaches 68%.

Claims (6)

1. a kind of alkali soluble chitin-sodium alginate hydrogel material with shape memory function, it is characterised in that: hydrogel is Using alkali soluble chitosan and sodium alginate as raw material, and Ca can contained2+Solution neutralize contain CO3 2-Solution in realize shape note The process recalled and replied.
2. the alkali soluble chitin-sodium alginate hydrogel material according to claim 1 with shape memory function, special Sign is: the shape recovery process of the gel rubber material can realize 3 times or more and recycle, and reply degree can reach 50% with On.
3. a kind of alkali soluble chitin-sodium alginate hydrogel material described in claim 1 with shape memory function, special Sign is that specific preparation process is as follows:
1) each component is weighed according to mass percent: chitosan 1%-10%, sodium alginate 1%-10%, a hydronium(ion) lithia 4-15%, urea 3-10%, remaining is water；The molecular weight of chitosan is 200000-2500000；The sodium alginate Viscosity (10g/L, 20 DEG C) is 0.02-0.1Pas；After said components are mixed swelling, it is made through multiple freeze-thaw process Alkali soluble chitin-sodium alginate solution；
2) by above-mentioned steps 1) in prepare alkali soluble chitin-sodium alginate solution evacuation and centrifugal degassing, pour and cast from mold, and shift Two hours are heated in 60 DEG C of baking ovens to realize gelation, to get with shape memory after deionized water dialysis to neutrality The alkali soluble chitin-sodium alginate gel of function.
4. a kind of alkali soluble chitin-sodium alginate hydrogel material described in claim 1 with shape memory function, special Sign is that concrete shape memory function realizes that process is as follows:
1) after assigning one the second shape of alkali soluble chitin-sodium alginate gel strips obtained above, then it is transferred into 0.2- The Ca of 2M2+In solution, 5-30min is impregnated to realize the fixation of the second shape of gel strips；
2) gel strips are taken out, remove Ca remained on surface using deionized water2+；
3) gel strips are then transferred to the CO of 0.2-2M3 2-In solution, the reply of gel strip can be realized after immersion 1-10h.
5. the shape memory function implementation method according to claim 4, it is characterised in that: described to contain Ca2+Solution be chlorine Change the solution such as calcium, calcium nitrate.
6. the shape memory function implementation method according to claim 4, it is characterised in that: described to contain CO3 2-Solution be carbon The solution such as sour sodium, potassium carbonate.
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CN115025277A (en) * 2022-06-17 2022-09-09 浙江大学 Injectable chitosan-graphene oxide hydrogel wound dressing with shear thinning and self-healing performances and preparation method thereof

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CN115025277B (en) * 2022-06-17 2023-12-01 浙江大学 Injectable chitosan-graphene oxide hydrogel wound dressing with shear thinning and self-healing properties and preparation method thereof

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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