CN114409973A - Bio-based blending material and preparation method thereof - Google Patents
Bio-based blending material and preparation method thereof Download PDFInfo
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- CN114409973A CN114409973A CN202210164599.7A CN202210164599A CN114409973A CN 114409973 A CN114409973 A CN 114409973A CN 202210164599 A CN202210164599 A CN 202210164599A CN 114409973 A CN114409973 A CN 114409973A
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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
- C08J3/12—Powdering or granulating
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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
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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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
- 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
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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
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/162—Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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Abstract
The invention belongs to the technical field of biological materials, and discloses a bio-based blending material which is prepared by the following steps: adding sodium alginate into deionized water, soaking, heating to dissolve, adding chitosan, stirring, sterilizing in a high-pressure steam sterilizing pot, and cooling to room temperature to obtain sodium alginate-chitosan mixed solution; slowly adding the sodium alginate chitosan mixed solution into the silver nitrate solution with the same volume, stirring, dropwise adding a calcium chloride aqueous solution to enable sodium alginate droplets to be crosslinked and gelatinized to form calcium alginate microspheres, stirring and solidifying, adding anhydrous ether to dehydrate, filtering, washing with the anhydrous ether for 1, and drying at room temperature to obtain the blend material microspheres with the biological groups. The preparation process is simple and convenient, and the production efficiency is high.
Description
Technical Field
The invention belongs to the technical field of biological materials, and particularly relates to a bio-based blending material and a preparation method thereof.
Background
Chitosan is an N-deacetylation product of chitin, and is a natural polymer and biological macromolecular material of biological polysaccharides with abundant sources in nature. Since its discovery in 1859, chitosan has received much attention from researchers. Because of abundant sources, low price, good degradability, film-forming property and the like, the chitosan is widely applied to the chemical and chemical fields of water treatment, food preservation and the like. The chitosan has good film forming property, biocompatibility, degradability, wide source and unique broad-spectrum antibacterial property. Therefore, the chitosan and other materials are blended to form the complementary advantages among the components of the materials, which is beneficial to improving the mechanical property and overcoming the defects that the bio-based materials are easy to breed and infect bacteria.
The sodium alginate aqueous solution can form hydrogel with higher mechanical strength when meeting divalent cations such as calcium, barium and the like at room temperature. The calcium ion is the first choice for preparing the sodium alginate gel from the aspects of ion binding strength and ion toxicity. The calcium alginate microcapsule beads have strong hydrophilicity, good biocompatibility and biodegradability, and more importantly, the calcium alginate microcapsule beads also have the advantages of no toxicity, sensitive pH value, mild preparation conditions and the like. In the prior art, other materials are immobilized on sodium alginate, and calcium chloride is used for crosslinking and curing to prepare the calcium alginate biopolymer antibacterial microspheres, so that the sodium alginate has many excellent properties, the antibacterial materials have wider application, and the application range of the sodium alginate is expanded.
The microspheres are mostly prepared from biodegradable high-molecular nontoxic natural materials such as gelatin, chitosan, sodium alginate and the like, and the preparation method usually adopts a dripping method, a spraying method, an in-situ polymerization method, an electrostatic method, an emulsification method and the like, but the methods all have certain disadvantages: firstly, chemical organic solvents are required, which not only causes problems of toxic substance residue and the like, but also can cause the loss of activity of the medicine; and secondly, complex production equipment is needed, the production efficiency is low, and the obstacle is caused to the industrial production of the microspheres.
Disclosure of Invention
In order to overcome the technical defects in the prior art, the invention aims to provide a bio-based blending material.
Still another object of the present invention is to provide a method for preparing the above bio-based blend material.
In order to achieve the purpose, the invention is realized by the following technical scheme.
A bio-based blending material, which is prepared according to the following steps:
step 1) adding sodium alginate into deionized water for soaking, heating for dissolving, then adding chitosan, stirring, then placing into a high-pressure steam sterilization pot for sterilization, and cooling to room temperature to obtain a sodium alginate-chitosan mixed solution;
and 2) slowly adding the sodium alginate-chitosan mixed solution into the silver nitrate solution with the same volume, stirring at 50-500rpm for 1-10min, dropwise adding a calcium chloride aqueous solution to enable sodium alginate droplets to be crosslinked and gelatinized to form calcium alginate microspheres, stirring and curing for 5-50min, adding anhydrous ether to dehydrate for 5-30min, filtering, washing with the anhydrous ether for 1-3 times, and drying at room temperature to obtain the bio-based blended material microspheres.
Preferably, the first and second electrodes are formed of a metal,
in the step 1), the ratio of sodium alginate to deionized water is 1 g: 10-40 ml.
Preferably, the first and second electrodes are formed of a metal,
in the step 1), the soaking time is 12-48 h.
Preferably, the first and second electrodes are formed of a metal,
in the step 1), the heating temperature is 60-75 ℃.
Preferably, the first and second electrodes are formed of a metal,
in the step 1), stirring is carried out at 100-300rpm for 2-20 min.
Preferably, the first and second electrodes are formed of a metal,
in the step 1), the addition amount of the chitosan is one tenth to one third of the mass of the sodium alginate.
Preferably, the first and second electrodes are formed of a metal,
in the step 2), the concentration of the silver nitrate solution is 0.05-1M.
Preferably, the first and second electrodes are formed of a metal,
in the step 2), the mass fraction of the calcium chloride aqueous solution is 3-6%.
The invention also claims a preparation method of the bio-based blending material.
The invention also claims the bio-based blending material obtained by the preparation method.
The beneficial effects achieved by the invention mainly comprise but are not limited to the following aspects:
the chitosan has unique broad-spectrum antibacterial performance, and the biological composite material prepared by blending the chitosan can form the advantage complementation among all components of the material, thereby not only being beneficial to improving the mechanical performance of the biological base material, but also having the defect that the material is easy to breed and infect bacteria.
The bio-based blending material microsphere prepared by the method has the advantages of high mechanical strength, regular shape and uniform size, the particle size of the microsphere is between 300 and 400nm, and the encapsulation rate reaches more than 95 percent.
The preparation method is simple and convenient in preparation process and high in production efficiency, and provides important basis for industrial production of the microsphere preparation.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments, which are given by way of example only to illustrate the present invention and not to limit the scope of the present invention. It is intended that all modifications or alterations to the methods, procedures or conditions of the present invention be made without departing from the spirit and substance of the invention.
Example 1
A bio-based blending material is prepared by the following method:
adding 50g of sodium alginate into 1000ml of deionized water, soaking for 24h, heating at 65 ℃ for dissolving, then adding 10g of chitosan, stirring for 5min at 200rpm, then placing into a high-pressure steam sterilization pot for sterilization, and cooling to room temperature to obtain a sodium alginate chitosan mixed solution; slowly adding the sodium alginate chitosan mixed solution into 0.1M silver nitrate solution with the same volume, stirring at 100rpm for 5min, then dropwise adding 5% of calcium chloride aqueous solution to enable sodium alginate droplets to be crosslinked and gelatinized to form calcium alginate microspheres, stirring and curing for 15min, then adding 200ml of anhydrous ether to dehydrate for 10min, filtering, washing for 3 times by using 100ml of anhydrous ether, and drying at room temperature to obtain the bio-based blend material microspheres.
And (3) quality detection: the bio-based blending material microsphere prepared by the method has high mechanical strength, regular shape and uniform size, the particle size of the microsphere is between 300 and 400nm, the average particle size is 345nm, and the encapsulation rate of the nano-silver reaches 97.4 percent.
Example 2
A bio-based blending material is prepared by the following method:
adding 60g of sodium alginate into 1000ml of deionized water, soaking for 24h, heating at 70 ℃ for dissolving, then adding 8g of chitosan, stirring for 3min at 300rpm, then placing into a high-pressure steam sterilization pot for sterilization, and cooling to room temperature to obtain a sodium alginate chitosan mixed solution; slowly adding the sodium alginate-chitosan mixed solution into 0.05M silver nitrate solution with the same volume, stirring at 100rpm for 10min, then dropwise adding 4 mass percent calcium chloride aqueous solution to enable sodium alginate droplets to be crosslinked and gelatinized to form calcium alginate microspheres, stirring and curing for 20min, then adding 200ml of anhydrous ether to dehydrate for 12min, filtering, washing for 2 times by using 150ml of anhydrous ether, and drying at room temperature to obtain the bio-based blend material microspheres.
And (3) quality detection: the bio-based blending material microsphere prepared by the method has high mechanical strength, regular shape and uniform size, the particle size of the microsphere is between 300 and 400nm, the average particle size is 362nm, and the encapsulation rate of the nano-silver reaches 95.1 percent.
Example 3
A bio-based blending material is prepared by the following method:
adding 700g of sodium alginate into 1000ml of deionized water, soaking for 24h, heating at 70 ℃ for dissolving, then adding 12g of chitosan, stirring for 10min at 100rpm, then placing into a high-pressure steam sterilization pot for sterilization, and cooling to room temperature to obtain a sodium alginate chitosan mixed solution;
slowly adding the sodium alginate-chitosan mixed solution into 0.08M silver nitrate solution with the same volume, stirring at 100rpm for 8min, then dropwise adding 4 mass percent calcium chloride aqueous solution to enable sodium alginate droplets to be crosslinked and gelatinized to form calcium alginate microspheres, stirring and curing for 30min, then adding 200ml of anhydrous ether to dehydrate for 20min, filtering, washing for 2 times by using 100ml of anhydrous ether, and drying at room temperature to obtain the bio-based blend material microspheres.
And (3) quality detection: the bio-based blending material microsphere prepared by the method has high mechanical strength, regular shape and uniform size, the particle size of the microsphere is between 300 and 400nm, the average particle size is 354nm, and the encapsulation rate of the nano-silver reaches 96.6 percent.
Example 4
A bio-based blending material is prepared by the following method:
adding 55g of sodium alginate into 1000ml of deionized water, soaking for 30h, heating at 65 ℃ for dissolving, then adding 10g of chitosan, stirring for 4min at 200rpm, then placing into a high-pressure steam sterilization pot for sterilization, and cooling to room temperature to obtain a sodium alginate chitosan mixed solution; slowly adding the sodium alginate chitosan mixed solution into 0.1M silver nitrate solution with the same volume, stirring at 100rpm for 5min, then dropwise adding 5% of calcium chloride aqueous solution to enable sodium alginate droplets to be crosslinked and gelatinized to form calcium alginate microspheres, stirring and curing for 25min, then adding 300ml of anhydrous ether to dehydrate for 15min, filtering, washing for 3 times by using 200ml of anhydrous ether, and drying at room temperature to obtain the bio-based blend material microspheres.
And (3) quality detection: the bio-based blending material microsphere prepared by the method has high mechanical strength, regular shape and uniform size, the particle size of the microsphere is between 300 and 400nm, the average particle size is 337nm, and the encapsulation rate of the nano-silver reaches 95.4 percent.
Example 5
A bio-based blending material is prepared by the following method:
adding 45g of sodium alginate into 1000ml of deionized water, soaking for 28h, heating at 68 ℃ for dissolving, then adding 8g of chitosan, stirring for 6min at 150rpm, then placing into a high-pressure steam sterilization pot for sterilization, and cooling to room temperature to obtain a sodium alginate chitosan mixed solution; slowly adding the sodium alginate chitosan mixed solution into 0.07M silver nitrate solution with the same volume, stirring at 100rpm for 5min, then dropwise adding 6 mass percent calcium chloride aqueous solution to enable sodium alginate droplets to be crosslinked and gelatinized to form calcium alginate microspheres, stirring and curing for 15min, then adding 300ml of anhydrous ether to dehydrate for 15min, filtering, washing for 3 times by using 200ml of anhydrous ether, and drying at room temperature to obtain the bio-based blend material microspheres.
And (3) quality detection: the bio-based blending material microsphere prepared by the method has high mechanical strength, regular shape and uniform size, the particle size of the microsphere is between 300 and 400nm, the average particle size is 369nm, and the encapsulation rate of the nano-silver reaches 94.9 percent.
The above description of the embodiments is only intended to illustrate the method of the invention and its core idea. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made to the present invention, and these improvements and modifications will also fall into the protection scope of the claims of the present invention.
Claims (10)
1. A bio-based blending material, which is prepared according to the following steps:
step 1) adding sodium alginate into deionized water for soaking, heating for dissolving, then adding chitosan, stirring, then placing into a high-pressure steam sterilization pot for sterilization, and cooling to room temperature to obtain a sodium alginate-chitosan mixed solution;
and 2) slowly adding the sodium alginate-chitosan mixed solution into the silver nitrate solution with the same volume, stirring at 50-500rpm for 1-10min, dropwise adding a calcium chloride aqueous solution to enable sodium alginate droplets to be crosslinked and gelatinized to form calcium alginate microspheres, stirring and curing for 5-50min, adding anhydrous ether to dehydrate for 5-30min, filtering, washing with the anhydrous ether for 1-3 times, and drying at room temperature to obtain the bio-based blended material microspheres.
2. The bio-based blend material according to claim 1, wherein in step 1), the ratio of sodium alginate to deionized water is 1 g: 10-40 ml.
3. The biobased blend material of claim 1, wherein in step 1), the soaking time is 12-48 h.
4. The biobased blend material of claim 1, wherein in step 1), the heating temperature is 60-75 ℃.
5. The bio-based blend material according to claim 1, wherein in the step 1), stirring is performed at 100-300rpm for 2-20 min.
6. The bio-based blend material according to claim 1, wherein in step 1), the chitosan is added in an amount of one tenth to one third of the mass of sodium alginate.
7. The biobased blend material of claim 1, wherein in step 2) the concentration of the silver nitrate solution is 0.05-1M.
8. The bio-based blend material according to claim 1, wherein the mass fraction of the calcium chloride aqueous solution in the step 2) is 3-6%.
9. A method of making the bio-based blend material of claims 1-8.
10. A biobased blend material obtained by the method of claim 9.
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