CN113577271A - Preparation method of graphene-ferroferric oxide composite magnetic carrier - Google Patents
Preparation method of graphene-ferroferric oxide composite magnetic carrier Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000010894 electron beam technology Methods 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- -1 hydroxide compound Chemical class 0.000 claims abstract description 6
- 239000013077 target material Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 5
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 5
- 150000003624 transition metals Chemical class 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- 238000001556 precipitation Methods 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 239000002905 metal composite material Substances 0.000 claims abstract description 3
- 239000012716 precipitator Substances 0.000 claims abstract description 3
- 239000000725 suspension Substances 0.000 claims abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 8
- 230000008685 targeting Effects 0.000 abstract description 8
- 239000003937 drug carrier Substances 0.000 abstract description 5
- 230000005389 magnetism Effects 0.000 abstract description 2
- 239000003814 drug Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 16
- 229940079593 drug Drugs 0.000 description 10
- 206010006187 Breast cancer Diseases 0.000 description 6
- 208000026310 Breast neoplasm Diseases 0.000 description 6
- 238000011068 loading method Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 206010028980 Neoplasm Diseases 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000002626 targeted therapy Methods 0.000 description 3
- MWWSFMDVAYGXBV-FGBSZODSSA-N (7s,9s)-7-[(2r,4s,5r,6s)-4-amino-5-hydroxy-6-methyloxan-2-yl]oxy-6,9,11-trihydroxy-9-(2-hydroxyacetyl)-4-methoxy-8,10-dihydro-7h-tetracene-5,12-dione;hydron;chloride Chemical compound Cl.O([C@H]1C[C@@](O)(CC=2C(O)=C3C(=O)C=4C=CC=C(C=4C(=O)C3=C(O)C=21)OC)C(=O)CO)[C@H]1C[C@H](N)[C@@H](O)[C@H](C)O1 MWWSFMDVAYGXBV-FGBSZODSSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 201000011510 cancer Diseases 0.000 description 2
- 229960003265 epirubicin hydrochloride Drugs 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000006249 magnetic particle Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 208000017667 Chronic Disease Diseases 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000002651 drug therapy Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000010253 intravenous injection Methods 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- 210000005075 mammary gland Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000036285 pathological change Effects 0.000 description 1
- 231100000915 pathological change Toxicity 0.000 description 1
- 238000001959 radiotherapy Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7028—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages
- A61K31/7034—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a carbocyclic compound, e.g. phloridzin
- A61K31/704—Compounds having saccharide radicals attached to non-saccharide compounds by glycosidic linkages attached to a carbocyclic compound, e.g. phloridzin attached to a condensed carbocyclic ring system, e.g. sennosides, thiocolchicosides, escin, daunorubicin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/02—Inorganic compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P15/00—Drugs for genital or sexual disorders; Contraceptives
- A61P15/14—Drugs for genital or sexual disorders; Contraceptives for lactation disorders, e.g. galactorrhoea
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P35/00—Antineoplastic agents
-
- 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
- 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
- C01B32/198—Graphene oxide
-
- 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
- C01G49/06—Ferric oxide [Fe2O3]
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- Medicinal Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Epidemiology (AREA)
- Engineering & Computer Science (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Pregnancy & Childbirth (AREA)
- Gynecology & Obstetrics (AREA)
- Molecular Biology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Endocrinology (AREA)
- Reproductive Health (AREA)
- Carbon And Carbon Compounds (AREA)
- Compounds Of Iron (AREA)
- Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
Abstract
A preparation method of a graphene-ferroferric oxide composite magnetic carrier comprises the following steps: dissolving soluble ferric salt in deionized water; dripping a precipitator into the uniform solution; weighing graphite and potassium permanganate, mixing, adding concentrated sulfuric acid and phosphoric acidAdding hydroxide compound into a three-neck flask mixed with acid liquor for precipitation, and slowly adding H2O2Obtaining a suspension of transition metal hydroxide/graphene oxide; washing and centrifuging the product, and drying and roasting to obtain the metal composite oxide/graphene; and (3) placing the composite magnetic target material in a high-current pulse electron beam instrument, and bombarding the composite material by using a high-frequency high-pulse electron beam to obtain the composite magnetic target material. The iron oxide/graphene composite material prepared by the method is used as a medical magnetic targeting drug carrier, the mechanical stability of the carrier is enhanced, and the graphene load magnetism per unit mass is enhanced.
Description
Technical Field
The invention belongs to the technical field of medical materials, and relates to a preparation method of a graphene-ferroferric oxide composite magnetic carrier.
Background
Among the current diseases, breast cancer is a serious chronic disease seriously threatening the health of women, the incidence rate of breast cancer in China is higher and higher, and the death rate is high. At present, the methods for treating cancers such as breast cancer mainly comprise methods such as drug therapy, radiotherapy, surgical excision and the like. Among the many approaches, targeted drug-targeted therapy is currently the dominant approach. The magnetic targeting drug loading method is adopted to treat the cancer, so that the side effect can be well weakened, the pain of a patient can be greatly relieved, the life quality of the patient is improved, and the life happiness and comfort of the patient are brought. Magnetic drug targeted therapy is one type of targeted therapy that treats a tumor site with a magnetic targeted drug delivery system (MTDS). The magnetic targeting preparation consists of magnetic substances, medicines and framework materials. Under the action of an external magnetic field, the carrier carries the medicine to directionally move in vivo, has the advantages of simple and convenient use, capability of increasing the medicine concentration of a pathological change part, reduction of the toxic and side effects of the medicine, improvement of the medicine effect and the like, and has important application in the field of biomedicine. At present, the research on compound magnetic targeting drug carriers is a hot topic at home and abroad, and particularly, the research on ferroferric oxide as a carrier is more endlessly developed. However, most of the current researches face the following problems: the drug loading capacity of the composite carrier, the structural property of the carrier and the final biocompatibility of the magnetic carrier and a human body are not well solved.
Disclosure of Invention
The invention provides a preparation method of a graphene-ferroferric oxide composite magnetic carrier, which comprises the steps of taking graphene oxide as a carrier, taking a novel carbon skeleton structure coated magnetic iron oxide nano particle as a magnetic particle, compounding the magnetic particle with ferroferric oxide by utilizing excellent performance of the graphene, and finally preparing a metal oxide/graphene magnetic targeting drug carrier composite material with high drug loading, high performance and high biocompatibility through the treatment of a high-current pulsed electron beam.
The technical scheme of the invention is as follows:
a preparation method of a graphene-ferroferric oxide composite magnetic carrier comprises the following steps:
(1) dissolving soluble ferric salt in deionized water according to a ratio, and uniformly mixing to form a uniform solution;
(2) dropwise adding a precipitant into the uniform solution, continuously stirring in the dropwise adding process until the pH value of the solution reaches above 10, stopping dropwise adding, continuously stirring for 1-3 h, standing at room temperature, aging for 4h, performing hydrothermal reaction, filtering and washing to be neutral, and drying to obtain a transition metal hydroxide compound precipitate;
(3) weighing the components in a mass ratio of 1: 5-15 parts of graphite and potassium permanganate are uniformly mixed, added into a three-neck flask filled with 98% concentrated sulfuric acid and phosphoric acid mixed acid solution, continuously stirred and reacted for 12 hours to obtain a gray green solution, then ice-water bath is carried out for 2 hours, an appropriate amount of hydroxide compound obtained in the step (2) is added for precipitation, and then 5-15 mL of H is slowly added2O2At the moment, the solution is quickly changed from grey green to bright yellow, and ultrasonic dispersion is carried out for 1-2 hours after the solution is continuously stirred for 30-40 minutes to obtain a suspension of transition metal hydroxide/graphene oxide;
(4) washing and centrifuging the product obtained in the step (3), drying and roasting to obtain a metal composite oxide/graphene;
(5) and (4) placing the composite magnetic target material obtained in the step (4) in a high-current pulse electron beam instrument, bombarding the composite material by using a high-frequency high-pulse electron beam, and changing the structure and the performance of the composite material to obtain the composite magnetic target material.
In the step (1), the soluble ferric salt is one of ferric nitrate, ferric sulfate or ferric chloride, and the soluble ferric salt is used as a matrix.
The mass ratio of the deionized water to the soluble ferric salt in the step (1) is 10-30: 1.
The hydrothermal reaction temperature in the step (2) is 110-;
in the step (2), the precipitator is one of sodium hydroxide, ammonia water or urea, and the dropping speed is 1-400 drops/min.
The hydrothermal reaction in the step (2) is carried out in a hydrothermal reaction kettle.
The mass ratio of the graphite to the hydroxide composite precipitate in the step (3) is 0.01-20: 100.
The roasting temperature in the step (4) is 300-500 ℃, and the roasting time is 3-6 h.
The roasting atmosphere in the step (4) is an oxygen-free atmosphere, a nitrogen atmosphere or an inert gas atmosphere.
The drying in the step (4) is carried out in a vacuum drying oven, and the drying temperature is 60 ℃.
The iron oxide/graphene composite material prepared by the method is used as a medical magnetic targeting drug carrier, the mechanical stability of the carrier is enhanced, and the graphene load magnetism per unit mass is enhanced. Through detection, the magnetic targeting material of the product is loaded with the third-generation drug epirubicin hydrochloride (EPI), the performance is greatly improved, and the drug loading is improved by 50-70% compared with the previous data. The composite particles loaded with the medicine enter blood in an intravenous injection mode, a magnetic field is applied to the outside, the specific focus part of the mammary gland is attracted directionally through the external magnetic field, and the medicine-loaded particles are gathered at the focus and release the medicine, so that the medicine is combined with breast cancer cells, and the purpose of treating breast cancer is achieved. The carrier has good biocompatibility and wide development prospect. After the breast cancer is successfully treated, the method can be popularized to the treatment of other cancer cells.
According to the method, the hydroxide compound of the metallic iron is directly added in the process of synthesizing the graphene oxide by adopting an in-situ synthesis method, so that the process is simple and easy to operate, and the production cost is low. The product has a core-shell structure, the specific surface area reaches 100-200m2/g, and the graphene is uniformly dispersed among gaps of product particles, so that the structure can effectively improve the contact area of the combination of the drug and the carrier, and greatly improve the drug loading capacity of the drug. The composite material is treated under the action of a high-current pulse electron beam for the first time, and the structure and the performance of the material are greatly improved under the action of a high electron beam.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
(1) dissolving a certain amount of ferric nitrate in deionized water, and uniformly mixing and stirring to obtain a uniform solution; (2) adding ammonia water into the solution at a rate of 100 drops/min until the pH value reaches 10, continuously stirring for 2 hours to completely precipitate, standing and aging at room temperature for 4 hours, placing the solution into a hydrothermal reaction kettle, carrying out hydrothermal reaction at 160 ℃ for 6 hours, filtering and washing the solution to be neutral, and drying the solution to obtain iron hydroxide compound precipitate; (3) graphite oxide was prepared using a modified Hummers method: weighing a certain amount of graphite and potassium permanganate, uniformly mixing, adding the graphite and potassium permanganate into a three-neck flask filled with 98% mixed acid solution of concentrated sulfuric acid and phosphoric acid, continuously stirring for reaction for 12 hours to obtain a gray green solution, carrying out ice-water bath for 2 hours, adding the hydroxide compound of iron extracted in the step (2) for precipitation, and slowly adding 10mL of H2O2At the moment, the solution quickly changes from gray green to bright yellow, and ultrasonic dispersion is carried out for 1h after the solution is continuously stirred for 30 min; (4) washing and centrifuging the product obtained in the step (3), putting the filter cake into a vacuum drying oven at 60 ℃ for fully drying, and roasting at 400 ℃ for 4 hours in a nitrogen atmosphere to obtain an iron oxide/graphene composite material; (5) bombarding the composite material obtained in the step (4) for 1 hour under the action of a high-current pulse electron beam to finally obtain the magnetic targeting drug carrier material.
Claims (10)
1. A preparation method of a graphene-ferroferric oxide composite magnetic carrier is characterized by comprising the following steps:
(1) dissolving soluble ferric salt in deionized water according to a ratio, and uniformly mixing to form a uniform solution;
(2) dropwise adding a precipitant into the uniform solution, continuously stirring in the dropwise adding process until the pH value of the solution reaches above 10, stopping dropwise adding, continuously stirring for 1-3 h, standing at room temperature, aging for 4h, performing hydrothermal reaction, filtering and washing to be neutral, and drying to obtain a transition metal hydroxide compound precipitate;
(3) weighing the components in a mass ratio of 1: 5-15 parts of graphite and potassium permanganate are uniformly mixed, added into a three-neck flask filled with 98% concentrated sulfuric acid and phosphoric acid mixed acid solution, continuously stirred and reacted for 12 hours to obtain a gray green solution, then, after ice-water bath is carried out for 2 hours, the hydroxide compound obtained in the step (2) is added for precipitation, and then, 5-15 mL of H is slowly added2O2At the moment, the solution is quickly changed from grey green to bright yellow, and ultrasonic dispersion is carried out for 1-2 hours after the solution is continuously stirred for 30-40 minutes to obtain a suspension of transition metal hydroxide/graphene oxide;
(4) washing and centrifuging the product obtained in the step (3), drying and roasting to obtain a metal composite oxide/graphene;
(5) and (4) placing the composite magnetic target material obtained in the step (4) in a high-current pulse electron beam instrument, bombarding the composite material by using a high-frequency high-pulse electron beam, and changing the structure and the performance of the composite material to obtain the composite magnetic target material.
2. The preparation method of the graphene-ferroferric oxide composite magnetic carrier according to claim 1, which is characterized by comprising the following steps: in the step (1), the soluble ferric salt is one of ferric nitrate, ferric sulfate or ferric chloride, and the soluble ferric salt is used as a matrix.
3. The preparation method of the graphene-ferroferric oxide composite magnetic carrier according to claim 1 or 2, which is characterized by comprising the following steps: the mass ratio of the deionized water to the soluble ferric salt in the step (1) is 10-30: 1.
4. The preparation method of the graphene-ferroferric oxide composite magnetic carrier according to claim 1 or 2, which is characterized by comprising the following steps: the hydrothermal reaction temperature in the step (2) is 110-170 ℃, and the time is 3-10 h.
5. The preparation method of the graphene-ferroferric oxide composite magnetic carrier according to claim 1 or 2, which is characterized by comprising the following steps: in the step (2), the precipitator is one of sodium hydroxide, ammonia water or urea, and the dropping speed is 1-400 drops/min.
6. The preparation method of the graphene-ferroferric oxide composite magnetic carrier according to claim 1 or 2, which is characterized by comprising the following steps: the hydrothermal reaction in the step (2) is carried out in a hydrothermal reaction kettle.
7. The preparation method of the graphene-ferroferric oxide composite magnetic carrier according to claim 1 or 2, which is characterized by comprising the following steps: the mass ratio of the graphite to the hydroxide precipitate in the step (3) is 0.01-20: 100.
8. The preparation method of the graphene-ferroferric oxide composite magnetic carrier according to claim 1 or 2, which is characterized by comprising the following steps: the roasting temperature in the step (4) is 300-500 ℃, and the roasting time is 3-6 h.
9. The preparation method of the graphene-ferroferric oxide composite magnetic carrier according to claim 1 or 2, which is characterized by comprising the following steps: and (4) the roasting atmosphere in the step (4) is an oxygen-free atmosphere, a nitrogen atmosphere or an inert gas atmosphere.
10. The preparation method of the graphene-ferroferric oxide composite magnetic carrier according to claim 1 or 2, which is characterized by comprising the following steps: the drying in the step (4) is carried out in a vacuum drying oven, and the drying temperature is 60 ℃.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104562098A (en) * | 2014-12-30 | 2015-04-29 | 沈阳理工大学 | Method for synthesizing titanium-nickel alloy layer through electron beam |
| CN109671937A (en) * | 2018-12-21 | 2019-04-23 | 东北大学 | A kind of in-situ synthetic method of transiens metal oxide/graphene composite material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104562098A (en) * | 2014-12-30 | 2015-04-29 | 沈阳理工大学 | Method for synthesizing titanium-nickel alloy layer through electron beam |
| CN109671937A (en) * | 2018-12-21 | 2019-04-23 | 东北大学 | A kind of in-situ synthetic method of transiens metal oxide/graphene composite material |
Non-Patent Citations (1)
| Title |
|---|
| 赵晖等: "电子束表面改性的研究进展", 《沈阳理工大学学报》 * |
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Application publication date: 20211102 |