CN111744059A - Preparation method of stable magnetic material capable of being injected under mucosa - Google Patents
Preparation method of stable magnetic material capable of being injected under mucosa Download PDFInfo
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- 210000004877 mucosa Anatomy 0.000 title claims abstract description 22
- 239000000696 magnetic material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 15
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 14
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 9
- 238000011065 in-situ storage Methods 0.000 claims description 9
- 239000002135 nanosheet Substances 0.000 claims description 9
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 238000002604 ultrasonography Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 abstract description 15
- 239000002114 nanocomposite Substances 0.000 abstract description 7
- 230000007774 longterm Effects 0.000 abstract description 3
- 239000012567 medical material Substances 0.000 abstract description 2
- 230000008961 swelling Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 25
- 230000000694 effects Effects 0.000 description 6
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 238000001356 surgical procedure Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- 206010030111 Oedema mucosal Diseases 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000003745 diagnosis Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000017 hydrogel Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 description 1
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 230000001079 digestive effect Effects 0.000 description 1
- 238000002224 dissection Methods 0.000 description 1
- 238000001839 endoscopy Methods 0.000 description 1
- 229920002674 hyaluronan Polymers 0.000 description 1
- 229960003160 hyaluronic acid Drugs 0.000 description 1
- 230000003902 lesion Effects 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 238000002324 minimally invasive surgery Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003387 muscular Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
Images
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/12—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L31/121—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix
- A61L31/122—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix of carbon
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/06—Flowable or injectable implant compositions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Abstract
The invention belongs to the technical field of medical material preparation, and particularly relates to a preparation method of a stable magnetic material capable of being injected under mucosa, which comprises the following steps: s1: obtaining graphene by taking graphite powder as a raw material and adopting a Hummers method; s2: placing the graphite in a DEG solution and then carrying out ultrasonic treatment to obtain a graphene solution; according to the preparation method of the stable magnetic material capable of being injected under the mucosa, the graphene-ferroferric oxide nano composite material with strong magnetic property and high stability is extracted, the graphene-ferroferric oxide nano composite material has high stability, is not easily biodegraded, has biological safety, can play a key role in clinical application scenes needing long mucosa swelling maintaining time, such as complex ESD/EMR operation, preoperative endoscopic marking positioning and even long-term positioning marking, focus tracking and the like when used for preparing the material for injecting under the mucosa, and the graphene-ferroferric oxide nano composite material with high stability is widely applied in multiple fields.
Description
Technical Field
The invention relates to the technical field of medical material preparation, in particular to a preparation method of a stable magnetic material capable of being injected under a mucosa.
Background
The minimally invasive surgery is a technology which only causes tiny wound to a patient in the surgery treatment process and only leaves tiny wound after the surgery, has the characteristics of small incision, small wound, quick recovery and less pain compared with the traditional surgery, and is one of the directions of the surgery development.
In a new medical age advocating minimally invasive diagnosis and treatment, diagnosis and treatment technologies under the digestive endoscopy, including ESD, EMR, and emerging intraoperative endoscope positioning marks, are more and more widely and mature in clinical application. One key to the success of ESD, EMR, and other techniques is the use of submucosal injection materials that can also improve the safety of endoscopic procedures by separating the mucosal layer from the intrinsic muscular layer to help complete dissection of the lesion. The commonly used submucosal injection materials include normal saline, hyaluronic acid, sodium alginate, etc., and the magnetic materials capable of being injected under the mucosa are gradually developed and applied.
The stability and viscosity of the submucosally injected material under endoscope are very critical for separating the focus, and the emphasis of the current research and development of the submucosally injectable magnetic material is also to improve the stability in the tissues.
However, neither the magnetofluid nor the magnetic hydrogel has a satisfactory mucosal lifting maintenance effect, is poor in stability, is easy to degrade, is difficult to locate for a long time due to the marking effect, is not sufficient for the periodicity of long mucosal lifting maintenance time required for tracking a focus, and is not beneficial to improving the application effect of the material and application and development in multiple fields.
Disclosure of Invention
The invention aims to provide a preparation method of a stable magnetic material capable of being injected under mucosa, which aims to solve the problems that the existing magnetic fluid or magnetic hydrogel does not obtain a satisfactory enough mucosa lifting maintaining effect, is poor in stability, easy to degrade, difficult to locate a marking effect for a long time, insufficient in periodicity of long mucosa lifting maintaining time required for tracking a focus, and not beneficial to improving the application effect of the material and application and development in multiple fields.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a stable magnetic material capable of being injected under mucosa comprises the following steps:
s1: obtaining graphene by taking graphite powder as a raw material and adopting a Hummers method;
s2: placing the graphite in a DEG solution and then carrying out ultrasonic treatment to obtain a graphene solution;
s3: the nano ferroferric oxide particles generated in situ on the graphene nano-sheet are prepared from FeCl3 solution and FeSO 4.7H 2O, wherein the molar ratio of Fe3+ to Fe2+ is 1.5: 1;
s4: treating the three solutions under ultrasound, adding NaOH, and performing ultrasound treatment for 15-20 min to generate black precipitates;
s5: the black precipitate is bathed for 15min to 30min at the temperature of 40 ℃ to 65 ℃ to obtain a mixture containing the graphene-ferroferric oxide nano complex;
s6: and repeatedly washing the mixture for 3-5 times by using deionized water and ethanol to obtain the purified graphene-ferroferric oxide nano complex.
Preferably, the content of the particles with the particle size of less than 15-30 μm of the graphite powder is more than 80-95 percent, and the carbon content is 97-99.85 percent.
Preferably, a reaction bottle is required to be assembled in the water bath, the capacity of the reaction bottle is 150 ml-250 ml, concentrated sulfuric acid is added into the reaction bottle, the reaction temperature is controlled not to exceed 15-20 ℃, and the temperature is increased to 30-40 ℃ after stirring for 5-8 min.
Preferably, the mixing ratio of the deionized water to the ethanol is 3: 0.5-3: 1.5.
compared with the prior art, the invention has the beneficial effects that: according to the preparation method of the stable magnetic material capable of being injected under the mucosa, the ferroferric oxide nano particles are generated in situ by carrying out chemical reaction on the prepared graphene nano sheets, so that the graphene-ferroferric oxide nano composite material with strong magnetic property and high stability is extracted, the graphene-ferroferric oxide nano composite material has high stability, is not easy to biodegrade and has biological safety, and the graphene-ferroferric oxide nano composite material used for preparing the injection material under the mucosa can play a key role in clinical application scenes such as complex ESD/EMR operation, preoperative endoscopic marking positioning and even long-term positioning marking, focus tracking and the like which need long mucosal swelling maintaining time, and the graphene-ferroferric oxide composite material with high stability can be widely applied in various fields such as industry and the like.
Drawings
FIG. 1 is a schematic view of the preparation process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: a preparation method of a stable magnetic material capable of being injected under mucosa comprises the following steps:
s1: obtaining graphene by taking graphite powder as a raw material and adopting a Hummers method;
s2: placing the graphite in a DEG solution and then carrying out ultrasonic treatment to obtain a graphene solution;
s3: the nano ferroferric oxide particles generated in situ on the graphene nano-sheet are prepared from FeCl3 solution and FeSO 4.7H 2O, wherein the molar ratio of Fe3+ to Fe2+ is 1.5: 1;
s4: treating the three solutions under ultrasound, adding NaOH, and performing ultrasound treatment for 15-20 min to generate black precipitates;
s5: the black precipitate is bathed for 15min to 30min at the temperature of 40 ℃ to 65 ℃ to obtain a mixture containing the graphene-ferroferric oxide nano complex;
s6: and repeatedly washing the mixture for 3-5 times by using deionized water and ethanol to obtain the purified graphene-ferroferric oxide nano complex.
Wherein, the content of the particles with the granularity of less than 15 to 30 mu m of the graphite powder is more than 80 to 95 percent, and the carbon content is 97 to 99.85 percent; assembling a reaction bottle in the water bath, wherein the capacity of the reaction bottle is 150-250 ml, adding concentrated sulfuric acid into the reaction bottle, controlling the reaction temperature to be not more than 15-20 ℃, stirring for 5-8 min, and then heating to 30-40 ℃; the mixing ratio of the deionized water to the ethanol is 3: 0.5-3: 1.5.
example 1
A preparation method of a stable magnetic material capable of being injected under mucosa comprises the following steps:
s1: obtaining graphene by taking graphite powder as a raw material and adopting a Hummers method;
s2: placing the graphite in a DEG solution and then carrying out ultrasonic treatment to obtain a graphene solution;
s3: the nano ferroferric oxide particles generated in situ on the graphene nano-sheet are prepared from FeCl3 solution and FeSO 4.7H 2O, wherein the molar ratio of Fe3+ to Fe2+ is 1.5: 1;
s4: treating the three solutions under ultrasound, adding NaOH, and performing ultrasound treatment for 15min to generate black precipitate;
s5: placing the black precipitate in water bath at 40 ℃ for 15min to obtain a mixture containing the graphene-ferroferric oxide nano complex;
s6: and repeatedly washing the mixture for 3 times by using deionized water and ethanol to obtain a purified graphene-ferroferric oxide nano complex.
Wherein, the content of the particles with the granularity of less than 15 μm of the graphite powder is more than 80 percent, and the carbon content is 97 percent; assembling a reaction bottle in the water bath, wherein the capacity of the reaction bottle is 150ml, adding concentrated sulfuric acid into the reaction bottle, controlling the reaction temperature not to exceed 15 ℃, stirring for 5min, and then heating to 30 ℃; the mixing ratio of the deionized water to the ethanol is 3: 0.5.
Example 2
S1: obtaining graphene by taking graphite powder as a raw material and adopting a Hummers method;
s2: placing the graphite in a DEG solution and then carrying out ultrasonic treatment to obtain a graphene solution;
s3: the nano ferroferric oxide particles generated in situ on the graphene nano-sheet are prepared from FeCl3 solution and FeSO 4.7H 2O, wherein the molar ratio of Fe3+ to Fe2+ is 1.5: 1;
s4: treating the three solutions under ultrasound, adding NaOH, and performing ultrasound treatment for 20min to generate black precipitate;
s5: placing the black precipitate in water bath at 65 ℃ for 30min to obtain a mixture containing the graphene-ferroferric oxide nano complex;
s6: and repeatedly washing the mixture for 5 times by using deionized water and ethanol to obtain a purified graphene-ferroferric oxide nano complex.
Wherein, the content of the particles with the granularity of less than 30 μm of the graphite powder is more than 95 percent, and the carbon content is 99.85 percent; assembling a reaction bottle in the water bath, wherein the capacity of the reaction bottle is 250ml, adding concentrated sulfuric acid into the reaction bottle, controlling the reaction temperature not to exceed 20 ℃, stirring for 8min, and heating to 40 ℃; the mixing ratio of the deionized water to the ethanol is 3: 1.5.
example 3
S1: obtaining graphene by taking graphite powder as a raw material and adopting a Hummers method;
s2: placing the graphite in a DEG solution and then carrying out ultrasonic treatment to obtain a graphene solution;
s3: the nano ferroferric oxide particles generated in situ on the graphene nano-sheet are prepared from FeCl3 solution and FeSO 4.7H 2O, wherein the molar ratio of Fe3+ to Fe2+ is 1.5: 1;
s4: treating the three solutions under ultrasound, adding NaOH, and performing ultrasound treatment for 18min to generate black precipitate;
s5: placing the black precipitate in water bath at 50 ℃ for 20min to obtain a mixture containing the graphene-ferroferric oxide nano complex;
s6: and repeatedly washing the mixture for 4 times by using deionized water and ethanol to obtain a purified graphene-ferroferric oxide nano complex.
Wherein, the content of the particles with the granularity of less than 20 μm of the graphite powder is more than 90 percent, and the carbon content is 99 percent; assembling a reaction bottle in the water bath, wherein the capacity of the reaction bottle is 200ml, adding concentrated sulfuric acid into the reaction bottle, controlling the reaction temperature not to exceed 18 ℃, stirring for 6min, and heating to 35 ℃; the mixing ratio of the deionized water to the ethanol is 3: 0.8.
Example 4
S1: obtaining graphene by taking graphite powder as a raw material and adopting a Hummers method;
s2: placing the graphite in a DEG solution and then carrying out ultrasonic treatment to obtain a graphene solution;
s3: the nano ferroferric oxide particles generated in situ on the graphene nano-sheet are prepared from FeCl3 solution and FeSO 4.7H 2O, wherein the molar ratio of Fe3+ to Fe2+ is 1.5: 1;
s4: treating the three solutions under ultrasound, adding NaOH, and performing ultrasound treatment for 17min to generate black precipitate;
s5: placing the black precipitate in water bath at 55 ℃ for 25min to obtain a mixture containing the graphene-ferroferric oxide nano complex;
s6: and repeatedly washing the mixture for 4 times by using deionized water and ethanol to obtain a purified graphene-ferroferric oxide nano complex.
Wherein, the content of the graphite powder particles with the granularity less than 26 μm is more than 93 percent, and the carbon content is 98 percent; assembling a reaction bottle in the water bath, wherein the capacity of the reaction bottle is 180ml, adding concentrated sulfuric acid into the reaction bottle, controlling the reaction temperature not to exceed 15 ℃, stirring for 6min, and then heating to 35 ℃; the mixing ratio of the deionized water to the ethanol is 3: 1.
In summary, according to the preparation method of the stable magnetic material capable of being injected under the mucosa, the ferroferric oxide nanoparticles are generated in situ by carrying out chemical reaction on the prepared graphene nanosheets, so that the graphene-ferroferric oxide nano composite material with strong magnetic property and high stability is extracted, has high stability, is not easily biodegraded and biosafety, can play a key role in preparing the material for injection under the mucosa in clinical application scenes such as complicated ESD/EMR operation, preoperative endoscopic marking positioning and even long-term positioning marking, focus tracking and the like which need long mucosal swelling maintaining time, and the graphene-ferroferric oxide composite material with high stability can be widely applied in various fields such as industry and the like.
While the invention has been described above with reference to an embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the various features of the embodiments disclosed herein may be used in any combination, provided that there is no structural conflict, and the combinations are not exhaustively described in this specification merely for the sake of brevity and conservation of resources. Therefore, it is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (4)
1. A preparation method of a stable magnetic material capable of being injected under a mucosa is characterized by comprising the following steps: the method comprises the following steps:
s1: obtaining graphene by taking graphite powder as a raw material and adopting a Hummers method;
s2: placing the graphite in a DEG solution and then carrying out ultrasonic treatment to obtain a graphene solution;
s3: the nano ferroferric oxide particles generated in situ on the graphene nano-sheet are prepared from FeCl3 solution and FeSO 4.7H 2O, wherein the molar ratio of Fe3+ to Fe2+ is 1.5: 1;
s4: treating the three solutions under ultrasound, adding NaOH, and performing ultrasound treatment for 15-20 min to generate black precipitates;
s5: the black precipitate is bathed for 15min to 30min at the temperature of 40 ℃ to 65 ℃ to obtain a mixture containing the graphene-ferroferric oxide nano complex;
s6: and repeatedly washing the mixture for 3-5 times by using deionized water and ethanol to obtain the purified graphene-ferroferric oxide nano complex.
2. The method for preparing a stable magnetic material capable of being injected under mucosa according to claim 1, wherein the method comprises the following steps: the particle size of the graphite powder is less than 15-30 μm, the content is more than 80-95%, and the carbon content is 97-99.85%.
3. The method for preparing a stable magnetic material capable of being injected under mucosa according to claim 1, wherein the method comprises the following steps: and assembling a reaction bottle in the water bath, wherein the capacity of the reaction bottle is 150-250 ml, adding concentrated sulfuric acid into the reaction bottle, controlling the reaction temperature to be not more than 15-20 ℃, stirring for 5-8 min, and then heating to 30-40 ℃.
4. The method for preparing a stable magnetic material capable of being injected under mucosa according to claim 1, wherein the method comprises the following steps: the mixing ratio of the deionized water to the ethanol is 3: 0.5-3: 1.5.
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Citations (9)
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|---|---|---|---|---|
| CN101941842A (en) * | 2010-10-11 | 2011-01-12 | 东华大学 | Method for preparing graphene loaded ferroferric oxide magnetic nanometer particle composite material |
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