CN114735714B - Mg 1-x R x B 2 Preparation method and application of material - Google Patents
Mg 1-x R x B 2 Preparation method and application of material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/04—Metal borides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/22—Boron compounds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
- A61P17/02—Drugs for dermatological disorders for treating wounds, ulcers, burns, scars, keloids, or the like
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P7/00—Drugs for disorders of the blood or the extracellular fluid
- A61P7/04—Antihaemorrhagics; Procoagulants; Haemostatic agents; Antifibrinolytic agents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses a Mg 1‑x R x B 2 The preparation method of the material and the application thereof, wherein the preparation method comprises the following steps: weighing magnesium powder, R powder and boron powder according to a molar ratio of 1-1.5:0-0.25:2, wherein R is at least one of aluminum, zinc, calcium, iron and potassium; mixing the magnesium powder, the R powder and the boron powder for 1 to 3 hours in an inert gas atmosphere; placing the mixed mixture into an inert gas atmosphere at 800-1000 ℃ for heat preservation for 4-6 hours; and reducing the temperature to normal temperature, and then crushing and grinding to obtain Mg 1‑x R x B 2 A material. The simple components of the material can realize the functions of resisting bacteria, resisting oxidation, easing pain, stopping bleeding, promoting the efficient repair of chronic wound surfaces and the like. The invention has wide application prospect.
Description
Technical Field
The present invention relates to the field of materials,in particular to a Mg 1-x R x B 2 A preparation method and application of the material.
Background
Magnesium boride is an ionic compound and the crystal structure belongs to a hexagonal crystal system. It is an intercalation compound, and magnesium layers and boron layers are alternately arranged. Researchers have found in 2001 that this seemingly no-eye compound magnesium boride turns into a superconductor at temperatures slightly near 40K absolute (corresponding to-233 c). Its transition temperature is almost twice as high as that of other superconductors of the same type, and its actual operating temperature is 20-30K. The temperature reduction can be accomplished by liquid neon, liquid hydrogen or a closed-loop refrigerator. These methods are both simple and cost effective compared to the current industry where liquid helium is used to cool the niobium alloy (4K). Once doped with carbon or other impurities, magnesium boride is not inferior to niobium alloys in its ability to maintain superconductivity in the presence of a magnetic field or current flow. Potential applications include superconducting magnets, power transmission lines, and sensitive magnetic field detectors.
However, the preparation method of magnesium boride is complex, such as the reactive liquid infiltration method used in the prior art, and has complex process and high cost. The invention aims to provide a novel method for preparing magnesium boride materials, which has simple and easily controlled process and low cost, and creatively provides a novel application of the magnesium boride materials in the novel field.
Disclosure of Invention
A first object of the present invention is to provide a method for producing Mg 1-x R x B 2 The preparation method of the material has simple and easily controlled process and low cost.
A second object of the present invention is to provide Mg 1-x R x B 2 The material is applied to the new technical field.
To achieve the above object, the present invention provides a method for preparing Mg 1-x R x B 2 A method of making a material, the method comprising the steps of: weighing magnesium powder, R powder and boron powder according to a molar ratio of 1-1.5:0-0.25:2, wherein R is at least one of aluminum, zinc, calcium, iron and potassium; in an inert gas atmosphereMixing the magnesium powder, the R powder and the boron powder for 1-3 hours; placing the mixed mixture into an inert gas atmosphere at 800-1000 ℃ for heat preservation for 4-6 hours; and reducing the temperature to normal temperature, and then crushing and grinding to obtain Mg 1-x R x B 2 A material. The method is a high-temperature self-propagating combustion method; wherein the boron powder is amorphous boron powder. Wherein, the value of x is not less than 0 and not more than x<1, preferably 0<x<0.25, x can take on the value 0, mg at this time 1-x R x B 2 Is MgB 2 For example, x may also take on values of 0.1, 0.2, 0.25, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8 or 0.9.
Mg 1-x R x B 2 The material exhibits microscopically extremely rich bonding modes, such as covalent B-B bonds and ionic B-Metal bonds. At Mg 1-x R x B 2 In the hydrolysis process, ionic B-Metal bond is preferentially broken, mg/R ions are released, and the respective physiological functions (such as pain relieving and hemostasis) are exerted; the relatively stable covalent B-B bond can react with the ROS in the wound microenvironment to play a role in scavenging ROS; then a large amount of boron dihydroxyl is generated, and the boron dihydroxyl has better complexation effect on saccharides with ortho-dihydroxyl under the assistance of alkaline microenvironment generated by hydrolysis of the boron dihydroxyl, and can react with bacterial lipopolysaccharide, blood sugar and starch polysaccharide, so that the boron dihydroxyl has a series of functions of easing pain, stopping bleeding, diminishing inflammation, resisting bacteria, promoting chronic wound repair and the like.
Further, the preparation method further comprises the steps of: the Mg is added with 1-x R x B 2 Blending the material and polyvinylpyrrolidone (PVP) according to a molar ratio of 1:1.5-2, performing ultrasonic treatment in an ethanol phase for 4-6 hours, and then placing the mixture into a 30-50-DEG C oven for drying for 3-6 hours, preferably 40℃, thereby obtaining PVP modified Mg 1-x R x B 2 A material. Preferably, the steps are performed before being put into the oven: excess PVP was washed off by centrifugation. PVP modified Mg 1-x R x B 2 The material has better water dispersibility and biological safety.
Further, the purities of the magnesium powder, the R powder and the boron powder are more than 99 percent, and the purities of the magnesium powder, the R powder and the boron powder are more than 95 percent below a 200-mesh sieve.
Further, the inert gas atmosphere is argon and oxygenWherein the volume ratio of oxygen is 0-5%. The preferred volume ratio of oxygen is V%: 0<V is less than or equal to 5 percent, a small amount of oxygen can react with excessive Mg in an exothermic way, and the synthesis of the material at a lower temperature is assisted, which is favorable for Mg 1-x R x B 2 Nanocrystallization of the material; in addition, the generated magnesia shell inhibits the overquick growth of crystals through the crystal boundary pinning effect, thereby further promoting Mg 1-x R x B 2 Nanocrystallization of the material.
The invention also provides Mg 1-x R x B 2 A material of the Mg 1-x R x B 2 The material is prepared by the preparation method.
The invention also discloses the Mg 1-x R x B 2 The material is applied to the preparation of antibacterial drugs.
The invention also discloses the Mg 1-x R x B 2 The material is applied to the preparation of anti-inflammatory drugs.
The invention also discloses the Mg 1-x R x B 2 The material is applied to the preparation of anti-infective drugs.
The invention also discloses the Mg 1-x R x B 2 The material is applied to the preparation of analgesic drugs.
The invention also discloses the Mg 1-x R x B 2 The material is applied to the preparation of hemostatic drugs.
The invention also discloses the Mg 1-x R x B 2 The material is applied to the preparation of medicines for promoting wound healing. Wound types include: skin is not infected and the wound surface is an internal wound surface such as gastric ulcer.
The invention discloses Mg 1-x R x B 2 Preparation method and application of material, and improved self-propagating combustion method is adopted to prepare Mg 1-x R x B 2 The material has a structure composed of hexagonal close-packed Mg/R layers and B layers of graphite honeycomb structure alternately, and the special intercalation structure endows Mg with 1-x R x B 2 The material has excellent multifunctional characteristics, and can utilize wound tissue fluid to slowly actHydrolysis produces boron hydroxyl, magnesium and R ions, while the local microenvironment can be regulated to be alkaline and low Reactive Oxygen Species (ROS) characteristics. The microenvironment can promote boron hydroxyl and magnesium ions to inhibit bacterial growth; the variable price of boron element in the hydrolysis process obviously improves the antioxidation capability of the wound surface and is beneficial to wound surface repair; r ions continuously generated in the hydrolysis process can activate thrombin to promote coagulation, and magnesium ions can realize a long-time pain relieving effect; it is worth mentioning that the material is also suitable for repairing the damage of internal organs such as stomach. In conclusion, the simple components of the material can realize the functions of resisting bacteria, resisting oxidation, easing pain, stopping bleeding, promoting the efficient repair of chronic wound surfaces and the like. The invention has wide application prospect.
Drawings
FIG. 1 shows a schematic of a magnesium calcium boride material and SEM/TEM photographs.
Figure 2 shows that magnesium calcium boride has hemostatic function.
Fig. 3 shows that magnesium diboride has an antibacterial function.
Fig. 4 shows that magnesium diboride has the function of promoting normal wound healing.
Figure 5 shows that magnesium diboride has the function of promoting healing of infected wounds.
Detailed Description
"Range" is disclosed herein in the form of lower and upper limits. There may be one or more lower limits and one or more upper limits, respectively. The given range is defined by selecting a lower limit and an upper limit. The selected lower and upper limits define the boundaries of the particular ranges. All ranges that can be defined in this way are inclusive and combinable, i.e., any lower limit can be combined with any upper limit to form a range. For example, ranges of 60-120 and 80-110 are listed for specific parameters, with the understanding that ranges of 60-110 and 80-120 are also contemplated. Furthermore, if the minimum range values 1 and 2 are listed, and if the maximum range values 3,4 and 5 are listed, the following ranges are all contemplated: 1-3, 1-4, 1-5, 2-3, 2-4 and 2-5. In the present invention, all the embodiments mentioned herein and the preferred embodiments may be combined with each other to form new technical solutions, if not specifically described.
In the present invention, all technical features mentioned herein and preferred features may be combined with each other to form new technical solutions, if not specifically stated.
In the present invention, all the steps mentioned herein may be performed sequentially or randomly, but are preferably performed sequentially, unless otherwise specified.
Example 1: magnesium calcium boride Mg 1-x Ca x B 2 Is prepared from
1) Weighing magnesium powder, calcium powder and amorphous boron powder according to a molar ratio of 1-1.5:0-0.25:2, mixing for 1-3 hours under inert gas, then placing raw materials into an inert gas atmosphere at 800-1000 ℃, preserving heat for 4-6 hours, cooling to normal temperature, crushing and grinding to obtain Mg 1-x Ca x B 2 A powder;
2) The Mg obtained in step 1) is reacted with 1-x Ca x B 2 Mixing the powder and polyvinylpyrrolidone (PVP) according to a molar ratio of 1:1.5-2, performing ultrasonic treatment in an ethanol phase for 4-6 hours, centrifuging to wash out superfluous PVP, and putting the product into a 40-DEG C oven for drying for 3-6 hours to obtain PVP modified Mg 1-x Ca x B 2 And (3) powder.
The experimental results are shown in fig. 1: the magnesium calcium boride material was successfully synthesized and the material structure was characterized (fig. 1 a). Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) images showed that magnesium calcium boride had good dispersibility with particle size dimensions of about 200nm (fig. 1b & c). HRTEM showed clear lattice fringes (fig. 1 d); indicating successful synthesis of the magnesium calcium boride material.
Example 2: the magnesium calcium boride has hemostatic effect
(1) Mouse in-vivo hemostatic model
1) SPF grade 7-8w week Balb/c male mice were ordered, weighed and grouped;
2) Exposing liver layer by layer, and cutting off 3mm x 6mm liver lobes at the lower edge of the left lobe of the liver at the same part of each animal;
3) After the wound surface is full of blood, the wound of the blank control group is not coated with a sample, the experimental group is coated with magnesium calcium boride, and filter paper is used for filling the space below the wound surface, so that the hemostatic effect is observed;
the experimental results are shown in figure 2, and the magnesium calcium boride has remarkable hemostatic function.
It is worth noting that this example describes Mg by magnesium calcium boride 1-x R x B 2 The preparation and use of the material, in fact, can be successfully prepared by the same preparation method when R is not used or is selected as aluminum, zinc, iron or potassium, and can achieve the application effect which is not inferior to that of magnesium calcium boride, for example, when R is not contained, the material is magnesium diboride which also has the function similar to that of magnesium calcium boride. Examples are as follows:
example 3: the magnesium diboride has good antibacterial effect
(1) In vitro anti-pseudomonas aeruginosa activity of magnesium diboride
1) Inoculating single bacterial colony of pseudomonas aeruginosa into LB culture medium, and shaking culturing at 37 ℃ and 220rpm for overnight;
2) The following day, the overnight-cultured pseudomonas aeruginosa was inoculated into fresh LB medium at 1%, cultured with shaking at 37 ℃,220rpm, and the OD600 of the bacteria was measured every 0.5 hour;
3) When od600=0.5, the bacterial load is about 2×10 8 ～1*10 9 CFU/mL；
4) Taking 100 mu L of bacterial liquid in a 1.5mL sterilizing centrifuge tube, and centrifuging at 6000rpm for 5min;
5) Discarding the supernatant, and adding 1mL of phosphate buffer solution for resuspension for later use;
6) Magnesium diboride solutions of different concentrations prepared the day before and control PBS were added to sterile 96-well plates, 90 μl per well, and each concentration was repeated 3 times;
7) Then adding 10 mu L of resuspended Pseudomonas aeruginosa into 90 mu L of magnesium diboride solution with different concentrations respectively, and incubating for 6 hours in a 37 ℃ incubator;
8) The cells were subjected to gradient dilution with PBS, spot plate counts, and the survival amount of Pseudomonas aeruginosa was counted.
(2) In vitro anti-staphylococcus aureus activity of magnesium diboride
1) Selecting staphylococcus aureus single colony to inoculate in TSB culture medium, shaking culture at 37 deg.C and 220rpm for overnight;
2) The following day, overnight-cultured staphylococcus aureus was inoculated into fresh TSB medium at 4%, cultured with shaking at 37 ℃,220rpm, and the OD600 of the bacteria was measured every 0.5 hour;
3) When the OD600 value reaches 0.6-0.8, the bacterial amount is about 1-2 x 10 8 CFU/mL；
4) Taking 100 mu L of bacterial liquid in a 1.5mL sterilizing centrifuge tube, and centrifuging at 6000rpm for 5min;
5) Discarding the supernatant, and adding 1mL of phosphate buffer solution for resuspension for later use;
6) Magnesium diboride solutions of different concentrations prepared the day before and control PBS were added to sterile 96-well plates, 90 μl per well, and each concentration was repeated 3 times;
7) Then adding 10 mu L of resuspended staphylococcus aureus into 90 mu L of magnesium diboride solution with different concentrations respectively, and incubating for 6 hours in a 37 ℃ incubator;
8) The viability of staphylococcus aureus was counted by performing gradient dilutions in PBS, spot plate counts.
The experimental result is shown in figure 3, and the graph a compares the antibacterial effect of magnesium diboride with different concentrations, and the result shows that the magnesium diboride has remarkable effect of resisting pseudomonas aeruginosa, and when the concentration reaches 12.5 mug/mL, bacteria can be killed completely, and the survival amount of bacteria under the magnesium diboride with different concentrations in the graph a is quantified; panel b shows that magnesium diboride also has a pronounced antibacterial effect against Staphylococcus aureus and quantifies the survival of bacteria under different concentrations of magnesium diboride in panel b. In summary, magnesium diboride not only inhibits the activity of gram negative bacteria (e.g., pseudomonas aeruginosa) but also inhibits the activity of gram positive bacteria (e.g., staphylococcus aureus).
Constructing a diabetes mouse model;
1) Preparation of STZ buffer: 2.1g of citric acid is weighed and dissolved in pure water to prepare solution A, 2.94g of trisodium citrate is weighed and dissolved in pure water to prepare solution B, the solution A and the solution B are mixed according to the volume ratio of 1:1, the pH value is regulated to be about 4.2-4.5, the mixed solution is filtered and sterilized by a 0.22 mu m filter membrane, and the solution is prepared for use;
2) Preparation of STZ solution: the amount of STZ injected into each mouse is 60mg/kg, the required amount of STZ is calculated according to the weight and the number of the mice, the STZ is weighed out in a dark place and dissolved in the buffer solution prepared (for preparation at present);
3) Selecting a Balb/c mouse with the week number of 7-8, injecting an STZ solution into the abdominal cavity, keeping out of the sun as much as possible during injection, and stopping drug administration after continuous abdominal cavity drug administration for 5 days;
4) The middle interval is 10 days, the blood is taken from the tail tip of the mouse on the 16 th day, the blood sugar is measured, and the induction is successful when the empty abdomen blood sugar is more than 11.1 mmol/L.
Diabetes mouse wound model experiment
1) Weighing the weight of the mice, and randomly dividing the weight into 2 groups, namely a control group and an experimental group;
2) Injecting the alfudine into the abdominal cavity, anaesthetizing the mice, shaving the back hair of the mice by a shaver, and applying depilatory cream to clean the residual microvilli;
3) The next day, mice were anesthetized and wounds with a diameter of 8mm were cut on their backs.
Example 4: magnesium diboride for promoting wound healing of diabetic mice
1) Taking the established diabetic mouse wound surface model as a research object, firstly applying OPSITE Flexifix adhesive plaster with moderate size on a wound;
2) The wound of the mice in the experimental group is injected with 100 mu L of magnesium diboride solution with the concentration of 100 mu g/mL, and the control group is injected with PBS with the same volume;
3) Photographing the wound part of the mouse every 3 days, counting the area of the wound, and analyzing the healing speed of the wound;
4) Quantitative statistical analysis was performed on wound healing rate with Image J software.
The experimental result is shown in figure 4, and the magnesium diboride has the function of promoting the wound healing of the diabetic mice.
Example 5: function of magnesium diboride for promoting healing of diabetic mice infected wound
1) Taking the established diabetic mouse wound surface model as a research object, firstly applying OPSITE Flexifix adhesive plaster with moderate size on a wound;
2) After infection with pseudomonas aeruginosa (bacterial load: 1*10 6 ) AddingAdding a magnesium diboride solution;
3) Then, photographing every 3 days until the wound heals;
4) Quantitative statistical analysis is carried out on the wound healing rate by Image J software;
the experimental results are shown in figure 5, and the magnesium diboride has the efficacy of promoting the wound healing of the diabetic mice.
The foregoing description of the preferred embodiments of the present invention is not intended to limit the scope of the claims, which follow, as defined in the claims.
Claims (6)
1. Preparation of Mg 1-x R x B 2 A method of making a material, the method comprising the steps of:
weighing magnesium powder, R powder and boron powder according to a molar ratio of 1-1.5:0-0.25:2, wherein R is at least one of aluminum, zinc, calcium, iron and potassium;
mixing the magnesium powder, the R powder and the boron powder for 1 to 3 hours in an inert gas atmosphere;
placing the mixed mixture into an inert gas atmosphere at 800-1000 ℃ for heat preservation for 4-6 hours; and
cooling to normal temperature, crushing and grinding to obtain Mg 1-x R x B 2 The material is characterized in that the inert gas atmosphere is a mixed gas of argon and oxygen, wherein the volume ratio of the oxygen is more than 0 and less than or equal to 5 percent.
2. The process according to claim 1 for preparing Mg 1-x R x B 2 A method of making a material, the method further comprising the steps of:
the Mg is added with 1-x R x B 2 Blending the material and polyvinylpyrrolidone (PVP) according to a molar ratio of 1:1.5-2, performing ultrasonic treatment in an ethanol phase for 4-6 hours, and then placing the mixture into a 30-50 ℃ oven for drying for 3-6 hours to obtain PVP modified Mg 1-x R x B 2 A material.
3. Such asThe method for producing Mg according to claim 1 1-x R x B 2 The material is characterized in that the purities of the magnesium powder, the R powder and the boron powder are more than 99 percent, and the purities of the magnesium powder, the R powder and the boron powder are more than 95 percent below a 200-mesh sieve.
4. Mg (magnesium) 1-x R x B 2 The material is characterized in that the Mg 1-x R x B 2 The material prepared by the preparation method as claimed in any one of claims 1 to 3, wherein x has a value of 0.1 < x < 1.
5. The Mg produced by the production process according to any one of claims 1 to 3 1-x R x B 2 Application of material in preparation of hemostatic drug, wherein Mg 1-x R x B 2 R in (2) is calcium.
6. The Mg produced by the production process according to any one of claims 1 to 3 1-x R x B 2 Application of material in preparing medicine for promoting wound healing, wherein Mg 1-x R x B 2 The value of x in (2) is 0.
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