CN113230987A - Simple preparation method of magnetic chitosan aerogel - Google Patents
Simple preparation method of magnetic chitosan aerogel Download PDFInfo
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- CN113230987A CN113230987A CN202110563319.5A CN202110563319A CN113230987A CN 113230987 A CN113230987 A CN 113230987A CN 202110563319 A CN202110563319 A CN 202110563319A CN 113230987 A CN113230987 A CN 113230987A
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 77
- 239000004964 aerogel Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 18
- 230000032683 aging Effects 0.000 claims abstract description 10
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000004729 solvothermal method Methods 0.000 claims abstract description 8
- 238000004108 freeze drying Methods 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 22
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 17
- 239000011324 bead Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 8
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 8
- 239000001632 sodium acetate Substances 0.000 claims description 8
- 235000017281 sodium acetate Nutrition 0.000 claims description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000003929 acidic solution Substances 0.000 claims description 6
- 238000004132 cross linking Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 claims description 3
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 3
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000008569 process Effects 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000001879 gelation Methods 0.000 abstract description 2
- 239000007783 nanoporous material Substances 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 4
- 230000002431 foraging effect Effects 0.000 description 4
- 238000007710 freezing Methods 0.000 description 4
- 230000008014 freezing Effects 0.000 description 4
- 230000005415 magnetization Effects 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 230000004224 protection Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000009509 drug development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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Abstract
The invention belongs to the field of preparation processes of functional nano porous materials, and relates to a simple preparation method of a magnetic chitosan aerogel. The material prepared by the invention has a typical three-dimensional porous network structure, and belongs to an obvious aerogel structure. The invention takes chitosan and ferric chloride as main materials, and the preparation method comprises the steps of solvothermal reaction, pH inversion gelation, gel aging and finally freeze drying. The preparation method is simple in process and easy to operate, can realize magnetic recovery and magnetic orientation in the application process, and has a multi-field application prospect.
Description
Technical Field
The invention belongs to the field of preparation processes of nano porous materials, and particularly relates to a simple preparation method of a magnetic chitosan aerogel.
Background
Chitosan is a chitin N-deacetylation product, with free amino groups, making it the only basic polysaccharide in natural polysaccharides. The chitosan has multiple physiological functions of biodegradability, biocompatibility, nontoxicity, bacteriostasis, cancer resistance, lipid reduction, immunity enhancement and the like, and is widely applied to various fields of food additives, textile, agriculture, environmental protection, beauty and health care, cosmetics, antibacterial agents, medical fibers, medical dressings, artificial tissue materials, drug slow release materials, biomedical fields, medical absorbable materials, tissue engineering carrier materials, medical treatment, drug development and the like and other daily chemical industries.
The aerogel material is a new material with multiple pores, and has the excellent characteristics of large porosity, large comparative area and the like. Aerogel materials have been widely used in the field of military thermal insulation. But the outstanding porosity can be well applied to the fields of environment-friendly adsorption, nano drug loading and the like under the support of a pore size regulation means. Wherein, the chitosan aerogel material prepared by the aperture regulation and control technology can be well applied to various fields. And the chitosan with wide raw materials is used as the raw material for preparing the aerogel, so that the popularization bottleneck of the industrialization of the aerogel material can be controlled from the source.
In a comprehensive view, the material is expected to meet the requirements of environmental protection treatment, nano drug loading and the like at present. And the simple preparation method of the magnetic chitosan aerogel is expected to well promote the development of the aerogel industrialization. The problem of high price in the prior aerogel preparation is solved, and the aerogel has a wider application prospect in the fields of heavy metal ion adsorption, crude oil chain oil stain treatment, biomedical dressing, nano-drug carriers and the like.
Disclosure of Invention
The invention aims to provide a simple preparation method of a magnetic aerogel material, and expand the development and application transformation of the aerogel material industry.
The technical scheme of the invention is as follows: a simple preparation method of a magnetic chitosan aerogel material comprises the following specific steps:
(1) magnetic nano Fe3O4Preparation of granules
Uniformly dispersing ferric chloride and sodium acetate in ethylene glycol, sealing the ethylene glycol in a solvothermal reaction kettle, and carrying out solvothermal reaction; after the reaction is finished, taking out the product, washing the product with ethanol, and drying the product for later use to prepare the hydrophilic magnetic nano Fe3O4Particles;
(2) preparation of magnetic chitosan sol
Dissolving chitosan in an acid solution to prepare chitosan sol; hydrophilic magnetic nano Fe3O4The particles are uniformly dispersed in the chitosan sol to form stable magnetic chitosan sol;
(3) preparation of magnetic chitosan aerogel
Extracting the magnetic chitosan sol by using an injector and dripping the magnetic chitosan sol into an alkaline solution to form magnetic chitosan condensation beads, and performing freeze drying after aging crosslinking and solvent replacement; and preparing the magnetic chitosan aerogel.
Preferably, the molar ratio of ferric chloride, sodium acetate and ethylene glycol in step (1) is 1: (5-20): (100- > 200); the temperature of the solvothermal reaction is 150-220 ℃, and the reaction time is 6-12 h.
Preferably, the acidic solution in the step (2) is an acetic acid, hydrochloric acid, nitric acid or sulfuric acid solution, and the mass concentration of the acidic solution is 1-5%.
Preferably, the ratio of the mass of chitosan to the volume of the acidic solution in step (2) is (0.01-0.05) g/ml.
Preferably, the ratio of the mass of the hydrophilic magnetic nano Fe3O4 particles to the volume of the chitosan sol in the step (2) is (0.1-0.9) mg/ml.
Preferably, the alkali solution in the step (3) is LiOH or NaOH solution; the concentration of the alkali solution is 0.1-1M.
Preferably, the aging liquid in the step (3) is glutaraldehyde, epichlorohydrin, formaldehyde or ethylene glycol diglycidyl ether; the aging liquid has a mass concentration of 1-25% and an aging time of 12-48 h.
Preferably, the solvent in the step (3) is replaced by water every 6 to 8 hours for 3 to 6 times.
The invention takes chitosan and nano ferric oxide as main materials, and the preparation method comprises the steps of solvothermal reaction, pH inversion gelation, gel aging and finally freeze drying. The preparation method is simple in process and easy to operate, can realize magnetic recovery and magnetic orientation in the application process, and has a multi-field application prospect. The prepared magnetic chitosan aerogel material has a thickness of more than 200cm3Specific surface area per gram, and also has certain magnetic response.
Has the advantages that:
(1) compared with the traditional preparation of magnetic aerogel, the preparation method has the advantages of low requirement on preparation conditions, convenience in operation and extremely high success rate.
(2) Compared with the traditional preparation process of the aerogel composite material, the preparation method can be directly prepared in a short time through flow process, the parameters of the produced sample can be simply adjusted according to the performance requirements, the product stability is good, and industrialization is expected to be realized.
(3) The magnetic chitosan aerogel material prepared by the invention can realize the extensive application of multiple ways and multiple fields such as magnetic recovery, magnetic guidance and the like by applying external magnetic field mediation.
Drawings
Fig. 1 is a macroscopic digital picture of the magnetic chitosan aerogel prepared in example 1;
fig. 2 is an SEM image of the magnetic chitosan aerogel prepared in example 1;
FIG. 3 is a BET and pore size distribution plot of the magnetic chitosan aerogel prepared in example 1;
fig. 4 is a magnetic hysteresis loop diagram of the magnetic chitosan aerogel prepared in example 1.
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of protection.
Example 1
0.01mol of ferric chloride, 0.2mol of sodium acetate and 2mol of ethylene glycol are uniformly mixed and sealed in a reaction kettle, the reaction temperature is 220 ℃, and the reaction time is 12 hours. Cleaning the product with ethanol, and drying in an oven to obtain the magnetic nanometer Fe3O4And (3) granules.
A chitosan sol was prepared by dissolving 3g of chitosan in 100ml of a 3 wt% acetic acid solution. 30mg of the magnetic nano Fe prepared in the above way3O4The particles are uniformly dispersed in the chitosan sol to form stable magnetic chitosan sol.
The magnetic chitosan sol was extracted with a syringe and added dropwise to a 0.1M NaOH solution to form magnetic chitosan beads. And (3) placing the condensed beads in a 5 w% glutaraldehyde solution for aging and crosslinking for 48 h. And soaking the aged beads in water, replacing the water every 6 hours, and directly freezing and drying after replacing for 4 times to obtain the magnetic chitosan aerogel.
The macroscopic digital picture of the prepared magnetic chitosan aerogel is shown in figure 1; the SEM image of the prepared magnetic chitosan aerogel is shown in figure 2, and a better pore structure in the whole aerogel structure can be seen;
the BET and pore size distribution diagram of the prepared magnetic chitosan aerogel is shown in FIG. 3, and the specific surface area of the sample can be observed to be 424m2(ii)/g; the average pore diameter is 16 nm;
the hysteresis loop of the prepared magnetic chitosan aerogel is shown in figure 4, and the saturation magnetization is 2.2 emu/g.
Example 2
0.01mol of ferric chloride, 0.1mol of sodium acetate and 1mol of ethylene glycol are uniformly mixed and sealed in a reaction kettle, the reaction temperature is 150 ℃, and the reaction time is 10 hours. Cleaning the product with ethanol, and drying in an oven to obtain the magnetic nanometer Fe3O4And (3) granules.
The chitosan sol was prepared by dissolving 5g of chitosan in 100ml of a 5 wt% hydrochloric acid solution. 90mg of the magnetic nano Fe prepared in the above way3O4The particles are uniformly dispersed in the chitosan sol to form stable magnetic chitosan sol.
The magnetic chitosan sol was extracted using a syringe and added dropwise to a 1M LiOH solution to form magnetic chitosan beads. The beads are placed in 25w percent formaldehyde solution for aging and crosslinking for 12 hours. And soaking the aged beads in water, replacing the water every 8 hours, and directly freezing and drying after 6 times of replacement to obtain the magnetic chitosan aerogel.
The specific surface area of the magnetic chitosan aerogel sample prepared in example 2 was 362m 2/g; the average pore diameter was 18nm and the saturation magnetization was 2.6 emu/g.
Example 3
0.1mol of ferric chloride, 0.5mol of sodium acetate and 20mol of ethylene glycol are uniformly mixed and sealed in a reaction kettle, the reaction temperature is 200 ℃, and the reaction time is 6h. Cleaning the product with ethanol, and drying in an oven to obtain the magnetic nanometer Fe3O4And (3) granules.
The chitosan sol was prepared by dissolving 1g of chitosan in 100ml of a 1 wt% nitric acid solution. 60mg of the magnetic nano Fe prepared in the above way3O4The particles are uniformly dispersed in the chitosan sol to form stable magnetic chitosan sol.
The magnetic chitosan sol was extracted with a syringe and added dropwise to a 0.5M NaOH solution to form magnetic chitosan beads. And (3) placing the coagulated beads in a 10 w% epichlorohydrin solution for aging and crosslinking for 24 hours. And soaking the aged beads in water, replacing the water every 7h for 3 times, and directly freezing and drying to obtain the magnetic chitosan aerogel.
The specific surface area of the magnetic chitosan aerogel sample prepared in example 3 was 273m 2/g; the average pore diameter was 31nm and the saturation magnetization was 3.2 emu/g.
Example 4
0.05mol of ferric chloride, 1mol of sodium acetate and 5mol of ethylene glycol are uniformly mixed and sealed in a reaction kettle, the reaction temperature is 160 ℃, and the reaction time is 8 hours. And cleaning the product by using ethanol, and drying in an oven to obtain the magnetic nano Fe3O4 particles.
The chitosan sol was prepared by dissolving 3g of chitosan in 100ml of a 2 wt% sulfuric acid solution. And (3) uniformly dispersing 10mg of the prepared magnetic nano Fe3O4 particles in the chitosan sol to form stable magnetic chitosan sol.
The magnetic chitosan sol was extracted using a syringe and added dropwise to a 0.2M LiOH solution to form magnetic chitosan beads. And (3) placing the coagulated beads in a 1 w% ethylene glycol diglycidyl ether solution for aging and crosslinking for 36 h. And soaking the aged beads in water, replacing the water every 7h for 5 times, and directly freezing and drying to obtain the magnetic chitosan aerogel.
The specific surface area of the magnetic chitosan aerogel sample prepared in example 4 was 421m 2/g; the average pore diameter was 28nm and the saturation magnetization was 8.1 emu/g.
Claims (8)
1. A simple preparation method of a magnetic chitosan aerogel material comprises the following specific steps:
(1) magnetic nano Fe3O4Preparation of granules
Uniformly dispersing ferric chloride and sodium acetate in ethylene glycol, sealing the ethylene glycol in a solvothermal reaction kettle, and carrying out solvothermal reaction; after the reaction is finished, taking out the product, washing the product with ethanol, and drying the product for later use to prepare the hydrophilic magnetic nano Fe3O4Particles;
(2) preparation of magnetic chitosan sol
Dissolving chitosan in an acid solution to prepare chitosan sol; hydrophilic magnetic nano Fe3O4The particles are uniformly dispersed in the chitosan sol to form stable magnetic chitosan sol;
(3) preparation of magnetic chitosan aerogel
Dropwise adding the magnetic chitosan sol into an alkali solution to form magnetic chitosan beads, and performing freeze drying after aging crosslinking and solvent replacement; and preparing the magnetic chitosan aerogel.
2. The production method according to claim 1, wherein the molar ratio of ferric chloride, sodium acetate and ethylene glycol in the step (1) is 1: (5-20): (100- > 200); the temperature of the solvothermal reaction is 150-220 ℃, and the reaction time is 6-12 h.
3. The production method according to claim 1, characterized in that the acidic solution in the step (2) is an acetic acid, hydrochloric acid, nitric acid or sulfuric acid solution, and the mass concentration of the acidic solution is 1 to 5%.
4. The method according to claim 1, wherein the ratio of the mass of chitosan to the volume of the acidic solution in the step (2) is (0.01-0.05) g/ml.
5. The preparation method according to claim 1, characterized in that the ratio of the mass of the hydrophilic magnetic nano Fe3O4 particles to the volume of the chitosan sol in step (2) is (0.1-0.9) mg/ml.
6. The method according to claim 1, wherein the alkali solution in the step (3) is LiOH or NaOH solution; the concentration of the alkali solution is 0.1-1M.
7. The production method according to claim 1, characterized in that the aging liquid in the step (3) is glutaraldehyde, epichlorohydrin, formaldehyde or ethylene glycol diglycidyl ether; the aging liquid has a mass concentration of 1-25% and an aging time of 12-48 h.
8. The method according to claim 1, wherein the solvent in step (3) is replaced with water every 6 to 8 hours for 3 to 6 times.
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Application publication date: 20210810 |