CN101463145A - Carboxymethyl chitosan / oxidized sodium alginate self-crosslinking antibacterial hydrogel material - Google Patents
Carboxymethyl chitosan / oxidized sodium alginate self-crosslinking antibacterial hydrogel material Download PDFInfo
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Abstract
The invention discloses a self-crosslinking antibacterial hydrogel material containing carboxymethyl chitosan/oxidized sodium alginate. The material is made from the following components by mass percent: 1-35% of carboxymethyl chitosan, 1-25% of oxidized sodium alginate, 0.01-0.5% of nano-silver and distilled water. The material is prepared by the following steps: preparing the carboxymethyl chitosan by a carboxymethylation reaction of chitosan at the temperature of 10-80 DEG C; preparing the oxidized sodium alginate by an oxidation reaction of sodium alginate at the temperature of 10-45 DEG C; respectively preparing aqueous solution of the carboxymethyl chitosan and aqueous solution of the oxidized sodium alginate; adding the nano-silver solution and blending at certain ratio; and allowing self-crosslinking of the components at the temperature of 10-50 DEG C to produce the antibacterial hydrogel material. The antibacterial hydrogel material has the advantages of low cost, environmental protection, simple process and the like; as the carboxymethyl chitosan has good biocompatibility, the oxidized sodium alginate is nontoxic to human body, and the nano-silver has excellent antibacterial property, the obtained material can be applied to wound dressing, hemostatic materials and the like.
Description
Technical field
The present invention relates to the polymer material science field, particularly a kind of carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material and preparation method thereof.
Background technology
Cm-chitosan is the soluble derivative of chitosan behind carboxymethylation reaction, and the introducing of carboxyl has improved the water-soluble of chitosan on the one hand greatly, it is become a kind ofly not only contained amino but also contain the Amphiphatic high polymer ionogen of carboxyl.Compare with chitosan, the good water solubility of cm-chitosan has excellent biological compatibility and bioadhesive, can degrade fully in vivo.The oxidized sodium alginate that sodium alginate makes through sodium periodate oxidation has the dialdehyde based structures, the formaldehyde that can replace using always, glutaraldehyde etc. are poisoned bigger linking agent to human body, and both are through blended cross linking and introduce the good nanometer silver of anti-microbial property and can obtain a kind of, biocompatibility good, bacteriostasis property good novel self-crosslinking antibacterial hydrogel material with medical potentiality nontoxic to human body.
The report of at present relevant carboxymethyl chitosan hydrogel is all less both at home and abroad, mainly concentrates on the research for preparing hydrogel as linking agent with formaldehyde, glutaraldehyde etc.And still do not have report for the carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material.
Summary of the invention
Technical problem to be solved by this invention is: a kind of water content height, good biocompatibility, the good carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material of bacteriostasis property are provided, and this preparation methods.
The present invention solves its technical problem and adopts following technical scheme:
Carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material provided by the invention is made by following raw material, the shared weight percent of each raw material is: cm-chitosan 1～35%, oxidized sodium alginate 1～25%, nanometer silver 0.01～0.5%, distilled water surplus.
Above-mentioned carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material provided by the invention, its preparation method is: comprise the preparation of batching, carboxymethyl chitosan sugar aqueous solution, the preparation of the oxidized sodium alginate aqueous solution.Wherein:
(1) batching:
Take by weighing raw material, the shared weight percent of each raw material is: cm-chitosan 1～35%, oxidized sodium alginate 1～25%, nanometer silver 0.01～0.5%, distilled water surplus;
(2) the cm-chitosan adding distil water is made into the aqueous solution of cm-chitosan, the weight percent that cm-chitosan accounts for the described aqueous solution is 0.5～18%;
(3) the oxidized sodium alginate adding distil water is made into the aqueous solution of oxidized sodium alginate, the weight percent that oxidized sodium alginate accounts for the described aqueous solution is 1～30%;
(4) be after mix 1:0.5～1 with the weight ratio with the carboxymethyl chitosan sugar aqueous solution and the oxidized sodium alginate aqueous solution, weight percent by mixed solution is 0.01～0.5% adding Nano silver solution again, treat that it in 10～50 ℃ of following self-crosslinking reactions, obtains the carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material.
Described cm-chitosan can be made by following method:
(1) batching: take by weighing chitosan 10g, Virahol 100～500mL and Mono Chloro Acetic Acid 5～25g;
(2) be that reaction medium disperses with chitosan with 100～500mL Virahol, in 5～30min, add Mono Chloro Acetic Acid 5～25g in batches; 10～80 ℃ are reacted 6-8h down, and purifying gets cm-chitosan.
Described oxidized sodium alginate can be made by following method:
(1) batching: take by weighing sodium alginate 10g, sodium periodate 3～30g, ethylene glycol 1～10mL and NaCl 1～15g;
(2) the 10g sodium alginate is dissolved in 50～200mL distilled water, adds 3～30g sodium periodate, in 10～50 ℃ of lucifuge reaction 2～8h;
(3) add 1～10mL ethylene glycol and 1～15gNaCl and stir 5～30min termination reaction, purifying gets oxidized sodium alginate.
Described nanometer silver can be made by following method:
(1) batching: take by weighing Silver Nitrate 0.01～0.5g;
(2) 0.01～1g Silver Nitrate is dissolved in 50～200mL distilled water, adding 1～15mL weight percent is 0.5～6% trisodium citrate aqueous solution, and reaction 2～8h promptly gets nanometer silver under 10～50 ℃.
Above-mentioned carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material provided by the invention, its application in preparation wound dressings, styptic sponge.
The present invention compared with prior art mainly contains following significant effect:
The medical function that is had in view of cm-chitosan and oxidized sodium alginate, the present invention is with their aqueous solution blend, and behind the adding Nano silver solution, the present invention is with their aqueous solution blend, and the adding Nano silver solution is prepared carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material (hereinafter to be referred as hydrogel material).Nanometer silver can be made hydrogel etc. with cm-chitosan and oxidized sodium alginate by simple mechanical blending, reaches the synergy of two kinds of material physiological functions, behind the adding Nano silver solution, makes this hydrogel material possess good bacteriostasis again.Because cm-chitosan and oxidized sodium alginate all possess good biocompatibility, and be nontoxic to human body, so this hydrogel material can be applicable to novel wound dressings and styptic sponge etc.
Hydrogel material provided by the invention, its stable preparation process is easy to realize suitability for industrialized production, and cost is low, environmental protection, technology are simple.And prepared hydrogel material water content height, with good biocompatibility, bacteriostasis property is good.And possess some special medical function, and having the potentiality of applying, market outlook are wide.
Embodiment
The present invention is by the simple and effective method of this raising macromolecular material performance of blending and modifying, with carboxymethyl chitosan sugar aqueous solution and the blend of the oxidized sodium alginate aqueous solution, in the hope of obtaining comparatively ideal carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material of over-all properties.
The invention will be further described below in conjunction with embodiment, but do not limit the present invention.
Embodiment 1: the preparation of carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material
By weight, cm-chitosan 5%, oxidized sodium alginate 4% and distilled water 90.9% are mixed with blend behind both aqueous solution, add nanometer silver 0.1%, treat that under 10～50 ℃ its self-crosslinking obtains the carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material.
Embodiment 2: the preparation of carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material
By weight, cm-chitosan 8%, oxidized sodium alginate 6% and distilled water 85.95% are mixed with blend behind both aqueous solution, add nanometer silver 0.05%, treat that under 10～50 ℃ its self-crosslinking obtains the carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material.
Embodiment 3: the preparation of carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material
By weight, cm-chitosan 14%, oxidized sodium alginate 11% and distilled water 86.9% are mixed with blend behind both aqueous solution, add nanometer silver 0.5%, treat that under 10～50 ℃ its self-crosslinking obtains the carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material.
Embodiment 4: the preparation of carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material
By weight, cm-chitosan 3%, oxidized sodium alginate 4% and distilled water 92.93% are mixed with blend behind both aqueous solution, add nanometer silver 0.07%, treat that under 10～50 ℃ its self-crosslinking obtains the carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material.
Embodiment 5: the preparation of carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material
By weight, cm-chitosan 17%, oxidized sodium alginate 13% and distilled water 69.8% are mixed with blend behind both aqueous solution, add nanometer silver 0.2%, treat that under 10～50 ℃ its self-crosslinking obtains the carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material.
Embodiment 6: the preparation of carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material
By weight, cm-chitosan 20%, oxidized sodium alginate 19% and distilled water 60.6% are mixed with blend behind both aqueous solution, add nanometer silver 0.4%, treat that under 10～50 ℃ its self-crosslinking obtains the carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material.
Embodiment 7: the preparation of carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material
By weight, cm-chitosan 31%, oxidized sodium alginate 23% and distilled water 45.94% are mixed with blend behind both aqueous solution, add nanometer silver 0.06%, treat that under 10～50 ℃ its self-crosslinking obtains the carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material.
Embodiment 8: the preparation of carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material
By weight, cm-chitosan 35%, oxidized sodium alginate 25% and distilled water 39.8% are mixed with blend behind both aqueous solution, add nanometer silver 0.2%, treat that under 10～50 ℃ its self-crosslinking obtains the carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material.
Embodiment 9: the preparation of carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material
By weight, cm-chitosan 26%, oxidized sodium alginate 22% and distilled water 51.7% are mixed with blend behind both aqueous solution, add nanometer silver 0.3%, treat that under 10～50 ℃ its self-crosslinking obtains the carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material.
Claims (6)
1. carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material, it is characterized in that being made by following raw material, the shared weight percent of each raw material is: cm-chitosan 1～35%, oxidized sodium alginate 1～25%, nanometer silver 0.01～0.5%, distilled water surplus.
2. the purposes of carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material according to claim 1 is characterized in that the application in preparation wound dressings or hemostasis gel.
3. a carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel preparation methods comprises the aqueous solution preparation of batching, cm-chitosan and the aqueous solution preparation of oxidized sodium alginate, it is characterized in that:
(1) batching:
Take by weighing raw material, the shared weight percent of each raw material is: cm-chitosan 1～35%, oxidized sodium alginate 1～25%, nanometer silver 0.01～0.5%, distilled water surplus;
(2) the cm-chitosan adding distil water is made into the aqueous solution of cm-chitosan, the weight percent that cm-chitosan accounts for the described aqueous solution is 0.5～18%;
(3) the oxidized sodium alginate adding distil water is made into the aqueous solution of oxidized sodium alginate, the weight percent that oxidized sodium alginate accounts for the described aqueous solution is 1～30%;
(4) be after mix 1:0.5～1 with the weight ratio with the carboxymethyl chitosan sugar aqueous solution and the oxidized sodium alginate aqueous solution, weight percent by mixed solution is 0.01～0.5% adding Nano silver solution again, treat that it in 10～50 ℃ of following self-crosslinking reactions, obtains the carboxymethyl chitosan/oxidized sodium alginate self-crosslinking antibacterial hydrogel material.
2. preparation method according to claim 1 is characterized in that cm-chitosan made by following method:
(1) batching: take by weighing chitosan 10g, Virahol 100～500mL and Mono Chloro Acetic Acid 5～25g;
(2) be that reaction medium disperses with chitosan with 100～500mL Virahol, in 5～30min, add Mono Chloro Acetic Acid 5～25g in batches; 10～80 ℃ are reacted 6-8h down, and purifying gets cm-chitosan.
3. preparation method according to claim 1 is characterized in that oxidized sodium alginate made by following method:
(1) batching: take by weighing sodium alginate 10g, sodium periodate 3～30g, ethylene glycol 1～10mL and NaCl 1～15g;
(2) the 10g sodium alginate is dissolved in 50～200mL distilled water, adds 3～30g sodium periodate, in 10～50 ℃ of lucifuge reaction 2～8h;
(3) add 1～10mL ethylene glycol and 1～15gNaCl and stir 5～30min termination reaction, purifying gets oxidized sodium alginate.
4. preparation method according to claim 1 is characterized in that nanometer silver made by following method:
(1) batching: take by weighing Silver Nitrate 0.01～0.5g;
(2) 0.01～1g Silver Nitrate is dissolved in 50～200mL distilled water, adding 1～15mL weight percent is 0.5～6% trisodium citrate aqueous solution, and reaction 2～8h promptly gets nanometer silver under 10～50 ℃.
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