CN112206346A - Magnetic biological glass bone cement and preparation method thereof - Google Patents

Magnetic biological glass bone cement and preparation method thereof Download PDF

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Publication number
CN112206346A
CN112206346A CN202011045055.6A CN202011045055A CN112206346A CN 112206346 A CN112206346 A CN 112206346A CN 202011045055 A CN202011045055 A CN 202011045055A CN 112206346 A CN112206346 A CN 112206346A
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bioglass
magnetic
bone cement
liquid
powder
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李朝阳
崔永顺
刘春芳
李梦霞
吕维加
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Shandong Mantak Biomedical Engineering Co ltd
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Shandong Mantak Biomedical Engineering Co ltd
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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
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02—Inorganic materials
    • A61L27/10—Ceramics or glasses
    • 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
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02—Inorganic materials
    • A61L27/12—Phosphorus-containing materials, e.g. apatite
    • 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
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/14—Macromolecular materials
    • A61L27/16—Macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • 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
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • 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
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/54—Biologically active materials, e.g. therapeutic substances
    • 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
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/58—Materials at least partially resorbable by the body
    • 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
    • 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/412—Tissue-regenerating or healing or proliferative agents

Abstract

The invention relates to the technical field of bone cement, in particular to magnetic bioglass bone cement and a preparation method thereof. The magnetic biological glass bone cement mainly comprises the following raw materials in percentage by mass: powder: 45-89% of polyacrylate, 10-50% of magnetic bioglass and 1-5% of benzoyl peroxide; liquid: 0.5 to 5 percent of N, N-dimethyl-p-toluidine, 0.05 to 2 percent of hydroquinone and 93 to 99.45 percent of methyl methacrylate. According to the invention, strontium element replaces calcium element to prepare strontium-based bioglass, ferroferric oxide is introduced into the strontium-based bioglass to endow the bioglass with certain magnetic guidance, the prepared magnetic bioglass is compounded with PMMA to obtain magnetic bioglass bone cement, the bone cement can enhance osteogenesis activity after being implanted into a defect part, the temperature of the bone cement can be controlled, tissues are not damaged, the targeted temperature control is realized, the sterilization and bacteriostasis effects are realized, and the degradation and absorption can be realized.

Description

Magnetic biological glass bone cement and preparation method thereof
Technical Field
The invention relates to the technical field of bone cement, in particular to magnetic bioglass bone cement and a preparation method thereof.
Background
Bone cement is a common name of bone cement, and is a medical material used for orthopedic surgery. The biological bone cement forms two systems in the development process: acrylic resin bone cement (PMMA) with poor biocompatibility and calcium phosphate bone cement with good biocompatibility.
At present, the most widely used bone cement in clinical application is acrylic resin bone cement. It has the advantages of high mechanical strength, fast curing speed, etc., but it also has significant defects, such as: (1) the curing temperature is too high, and tissues are damaged; (2) the elastic modulus is 4-40 times of that of the spongy bone of the vertebral body, and excessively high elastic modulus leads to excessive increase of the hardness of the formed vertebral body and stress concentration, so that the adjacent vertebral body is compressed and fractured again; (3) lack of biological activity, can not degrade and absorb, exist in the vertebral body in the form of foreign matter for a long time, etc.; (4) the high temperature generated when the bone cement is cured improves inflammation at the patient site, but since the temperature is gradually lowered to the same temperature as the body temperature after the bone cement is cured, the effect is not sustained.
Chinese patent application CN109621013A discloses a composite bone cement with low heat release and high bioactivity and a preparation method thereof, wherein the composite bone cement is prepared by mixing 40-80% of solid-phase powder and 10-50% of liquid-phase powder. The solid phase powder comprises graphene, polymethyl methacrylate and hydroxyapatite, and the liquid phase comprises methyl methacrylate, hydroquinone and N, N-dimethyl-p-toluidine. The composite bone cement of the technology has good injectability and bioactivity, and the addition of the graphene with the ultrahigh specific surface area ensures that the reaction heat of the obtained PMMA bone cement is gradually released in the use process, so that the surrounding bone tissues are not damaged, the polymerization heat release temperature of the composite bone cement is reduced in the curing process, and the requirements of filling and repairing bone defects can be met. But the graphene is high in manufacturing cost, the sawtooth edges of the graphene nanoparticles are very sharp and strong, the graphene nanoparticles can be easily punctured into human skin and cell membranes of immune cells, the graphene has potential harm to human beings and other animals, the graphene is used as a raw material, vascular ingrowth and body fluid circulation are not facilitated, and potential safety hazards exist.
Disclosure of Invention
The invention aims to provide magnetic bioglass bone cement and a preparation method thereof, which overcome the defects of the prior art, and compound the magnetic bioglass and the bone cement to form the bone cement with magnetic regulation, wherein the magnetic bioglass improves the mechanical property of the bone cement, enhances the bioactivity of the bone cement, endows the bone cement with certain magnetism, can regulate and control the bone cement in a targeted manner, controls the temperature of the bone cement by hysteresis heating to obtain the antibacterial and bacteriostatic effects of the bone cement, accelerates the healing of bones, has good degradation performance and is beneficial to the ingrowth of blood vessels and the circulation of body fluid.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the magnetic biological glass bone cement mainly comprises the following raw materials in percentage by mass:
powder:
45% -89% of polyacrylate;
10% -50% of magnetic bioglass;
1 to 5 percent of benzoyl peroxide;
liquid:
0.5 to 5 percent of N, N-dimethyl-p-toluidine;
0.05 to 2 percent of hydroquinone;
93-99.45% of methyl methacrylate;
the adding ratio of the powder to the liquid is (1-3) g:1 ml.
Preferably, the magnetic bioglass bone cement mainly comprises the following raw materials in percentage by mass:
powder:
63% of polyacrylate;
35% of magnetic bioglass;
2% of benzoyl peroxide;
liquid:
3% of N, N-dimethyl-p-toluidine;
1% of hydroquinone;
96% of methyl methacrylate;
the adding ratio of the powder to the liquid is 2g:1 ml.
Preferably, SiO in the magnetic bioglass2：SrO：Fe3O4：Na2O：P2O5The molar percentage of (40-50): (20-40): (10-20): (10-20): (1-10).
More preferably, SiO in the magnetic bioglass2：SrO：Fe3O4：Na2O：P2O5The mole percentage of (A) is 40:20:15:15: 10.
preferably, the SrO can be partially replaced by CaO, with a maximum replacement mole percentage of 20%.
A preparation method of magnetic bioglass bone cement comprises the following preparation steps:
(1) weighing silicon dioxide, strontium carbonate, ferroferric oxide, sodium carbonate and phosphorus pentoxide powder, wherein SiO is2：SrO：Fe3O4：Na2O：P2O5The molar percentage of (40-50): (20-40): (10-20): (10-20): (1-10), stirring and mixing for 30-60 min;
(2) putting the powder mixture uniformly mixed in the step (1) into a zirconia crucible, controlling the temperature rise rate of a sintering furnace to be 5-8 ℃/min, controlling the reaction temperature to be 1300-1600 ℃, and controlling the reaction time to be 4-8 h to prepare a bioglass liquid;
(3) after the reaction in the step (2) is finished, pouring the prepared bioglass liquid into an ethanol solution for cooling and dispersing, sintering and drying at 600-800 ℃ for 1-3 h after cooling, and performing ball milling to obtain magnetic bioglass;
(4) weighing magnetic bioglass, polyacrylate and benzoyl peroxide according to specified mass percentage, uniformly mixing to obtain magnetic bioglass bone cement powder, weighing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate according to specified mass percentage, and uniformly mixing to obtain bone cement liquid;
(5) according to the powder-liquid ratio (1.5-2.5) g:1mL of bone cement liquid is added into the magnetic bioglass bone cement powder, and the magnetic bioglass bone cement is obtained after uniform stirring and solidification.
Preferably, Fe in said step (1)3O4The particle size distribution range of (B) is 5-200 nm.
Preferably, the volume fraction of the ethanol solution is 10-40%.
The bioglass has good biological activity and can be firmly and chemically combined with bone formation, and Hench proves that the bioglass has good biological activity and bone repair function through basic research, animal experiments and clinical experimental observation for nearly 20 years. Although many studies on bioglass are available, the studies on the simultaneous modification of magnetic guidance and biological activity of bioglass are less, and particularly, the replacement studies on a bioglass system by a melting method are rarely reported.
Ferroferric oxide is a magnetic black crystal, also called magnetic iron oxide. Strontium (Sr) is one of the essential trace elements for human body, and accounts for about 0.01% of bone mass. Sr, like other trace elements, has the functions of maintaining normal functions in vivo, preventing dental caries and enhancing bone strength.
The inventor of the invention replaces calcium element in bioglass with strontium element with osteoinductivity, introduces ferroferric oxide, endows bioglass with certain magnetic guidance, reconstructs components of bioglass by a melting method, replaces the strontium element, can further enhance the biological activity and structural stability of bioglass, endows certain osteoinductivity, adds the prepared magnetic bioglass into bone cement, enhances the biological activity of the bone cement, endows the bone cement with certain osteoinductivity and magnetic guidance, further can regulate and control the bone cement in a targeted manner, controls the temperature of the bone cement through hysteresis heating, obtains the antibacterial and bacteriostatic effects of the bone cement, and accelerates bone healing.
The invention has the beneficial effects that: compared with the prior art, the magnetic bioglass bone cement and the preparation method thereof have the following advantages: preparing strontium-based bioglass by replacing calcium with strontium, introducing ferroferric oxide into the strontium-based bioglass to endow the bioglass with certain magnetic guidance, and compounding the prepared magnetic bioglass with PMMA to prepare magnetic bioglass bone cement; strontium in the magnetic bioglass can play a developing role, and after the magnetic bioglass is implanted into a defect part, the release of strontium elements can enhance osteogenic activity and accelerate bone healing; the temperature of the bone cement can be controlled, and the targeted temperature control is achieved on the premise of not damaging tissues, so that the effects of sterilization and bacteriostasis are achieved; can be degraded and absorbed, and is beneficial to vascular ingrowth and body fluid circulation.
Detailed Description
Example 1
The magnetic biological glass bone cement and the preparation method thereof are disclosed, wherein the magnetic biological glass bone cement comprises the following components in percentage by mass: the powder is 50% of magnetic bioglass, 45% of polyacrylate and 5% of benzoyl peroxide, and the liquid is 99.45% of methyl methacrylate, 0.05% of hydroquinone and 0.5% of N, N dimethyl p-toluidine; in magnetic bioglass, SiO2:SrO:Fe3O4:Na2O:P2O5Is 45:20:20:10: 5.
The preparation method of the magnetic bioglass bone cement comprises the following steps:
(1) weighing silicon dioxide, strontium carbonate, ferroferric oxide, sodium carbonate and phosphorus pentoxide powder, wherein SiO is2:SrO:Fe3O4:Na2O:P2O5Is 45:20:20:10:5, mixed for 60min, Fe3O4The particle size distribution range of (A) is 5-200 nm;
(2) putting the powder mixture uniformly mixed in the step (1) into a zirconia crucible, controlling the temperature rise rate of a sintering furnace to be 8 ℃/min, controlling the reaction temperature to be 1300 ℃ and the reaction time to be 8h, and preparing biological glass liquid;
(3) after the reaction in the step (2) is finished, pouring the prepared bioglass liquid into an ethanol solution with the volume fraction of 20%, cooling, dispersing, sintering and drying at 800 ℃ for 1h after cooling, and performing ball milling to obtain magnetic bioglass;
(4) weighing and uniformly mixing the magnetic bioglass, the polyacrylate and the benzoyl peroxide according to the specified mass percentage; obtaining magnetic bioglass bone cement powder, weighing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate according to specified mass percentage, and uniformly mixing to obtain bone cement liquid;
(5) adding the bone cement liquid into the magnetic bioglass bone cement powder according to the powder-liquid ratio of 1g to 1mL, uniformly stirring and curing to obtain the magnetic bioglass bone cement.
Example 2
The magnetic biological glass bone cement and the preparation method thereof are disclosed, wherein the magnetic biological glass bone cement comprises the following components in percentage by mass: the powder is 40% of magnetic bioglass, 57% of polyacrylate and 3% of benzoyl peroxide, and the liquid is 95% of methyl methacrylate, 1% of hydroquinone and 4% of N, N dimethyl p-toluidine; in magnetic bioglass, SiO2:SrO:Fe3O4:Na2O:P2O5The molar percentage of (A) is 40:20:20:15: 5.
The preparation method of the magnetic bioglass bone cement comprises the following steps:
(1) weighing silicon dioxide, strontium carbonate, ferroferric oxide, sodium carbonate and phosphorus pentoxide powder, wherein SiO is2:SrO:Fe3O4:Na2O:P2O5Is 40:20:20:15:5, mixed for 30min, Fe3O4The particle size distribution range of (A) is 5-200 nm;
(2) putting the powder mixture uniformly mixed in the step (1) into a zirconia crucible, controlling the temperature rise rate of a sintering furnace to be 5 ℃/min, controlling the reaction temperature to be 1600 ℃, and controlling the reaction time to be 4h to prepare biological glass liquid;
(3) after the reaction in the step (2) is finished, pouring the prepared bioglass liquid into 10 volume percent ethanol solution for cooling and dispersing, sintering and drying for 2h at 700 ℃ after cooling, and performing ball milling to obtain magnetic bioglass;
(4) weighing and uniformly mixing magnetic bioglass, polyacrylate and benzoyl peroxide in fixed mass percentage to obtain magnetic bioglass bone cement powder, weighing and uniformly mixing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate in specified mass percentage to obtain bone cement liquid;
(5) adding the bone cement liquid into the magnetic bioglass bone cement powder according to the powder-liquid ratio of 2g to 1mL, uniformly stirring and curing to obtain the magnetic bioglass bone cement.
Example 3
The magnetic biological glass bone cement and the preparation method thereof are disclosed, wherein the magnetic biological glass bone cement comprises the following components in percentage by mass: the powder is 35% of magnetic bioglass, 63% of polyacrylate and 2% of benzoyl peroxide, and the liquid is 96% of methyl methacrylate, 1% of hydroquinone and 3% of N, N-dimethyl-p-toluidine; in magnetic bioglass, SiO2:SrO:Fe3O4:Na2O:P2O5The molar percentage of (A) is 40:20:15:15: 10.
The preparation method of the magnetic bioglass bone cement comprises the following steps:
(1) weighing silicon dioxide, strontium carbonate, ferroferric oxide, sodium carbonate and phosphorus pentoxide powder, wherein SiO is2:SrO:Fe3O4:Na2O:P2O5Is 40:20:15:15:10, mixed for 45min, Fe3O4The particle size distribution range of (A) is 5-200 nm;
(2) putting the powder mixture uniformly mixed in the step (1) into a zirconia crucible, controlling the temperature rise rate of a sintering furnace to be 6 ℃/min, controlling the reaction temperature to be 1550 ℃ and the reaction time to be 6h, and preparing a bioglass liquid;
(3) after the reaction in the step (2) is finished, pouring the prepared bioglass liquid into 30 volume percent ethanol solution for cooling and dispersing, sintering and drying for 3h at 600 ℃ after cooling, and performing ball milling to obtain magnetic bioglass;
(4) weighing and uniformly mixing magnetic bioglass, polyacrylate and benzoyl peroxide in specified mass percentage to obtain magnetic bioglass bone cement powder, weighing and uniformly mixing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate in specified mass percentage to obtain bone cement liquid;
(5) adding the bone cement liquid into the magnetic bioglass bone cement powder according to the powder-liquid ratio of 2g to 1mL, uniformly stirring and curing to obtain the magnetic bioglass bone cement.
Example 4
The magnetic biological glass bone cement and the preparation method thereof are disclosed, wherein the magnetic biological glass bone cement comprises the following components in percentage by mass: the powder comprises 30 percent of magnetic bioglass, 67.5 percent of polyacrylate and 2.5 percent of benzoyl peroxide, and the liquid comprises 97.4 percent of methyl methacrylate, 0.1 percent of hydroquinone and 2.5 percent of N, N-dimethyl-p-toluidine; in magnetic bioglass, SiO2:SrO:Fe3O4:Na2O:P2O5The molar percentage of (A) is 40:30:10:10: 10.
The preparation method of the magnetic bioglass bone cement comprises the following steps:
(1) weighing silicon dioxide, strontium carbonate, ferroferric oxide, sodium carbonate and phosphorus pentoxide powder, wherein SiO is2:SrO:Fe3O4:Na2O:P2O5Is 40:30:10:10, mixed for 60min, Fe3O4The particle size distribution range of (A) is 5-200 nm;
(2) putting the powder mixture uniformly mixed in the step (1) into a zirconia crucible, controlling the temperature rise rate of a sintering furnace to be 5 ℃/min, controlling the reaction temperature to be 1500 ℃, and controlling the reaction time to be 7h to prepare biological glass liquid;
(3) after the reaction in the step (2) is finished, pouring the prepared bioglass liquid into an ethanol solution with 20% volume fraction for cooling and dispersing, sintering and drying for 2h at 700 ℃ after cooling, and performing ball milling to obtain magnetic bioglass;
(4) weighing and uniformly mixing magnetic bioglass, polyacrylate and benzoyl peroxide in specified mass percentage to obtain magnetic bioglass bone cement powder, weighing and uniformly mixing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate in specified mass percentage to obtain bone cement liquid;
(5) adding the bone cement liquid into the magnetic bioglass bone cement powder according to the powder-liquid ratio of 2g to 1mL, uniformly stirring and curing to obtain the magnetic bioglass bone cement.
Example 5
The magnetic biological glass bone cement and the preparation method thereof are disclosed, wherein the magnetic biological glass bone cement comprises the following components in percentage by mass: the powder comprises 20 percent of magnetic bioglass, 77.5 percent of polyacrylate and 2.5 percent of benzoyl peroxide, and the liquid comprises 97.8 percent of methyl methacrylate, 0.2 percent of hydroquinone and 2 percent of N, N-dimethyl-p-toluidine; in magnetic bioglass, SiO2:SrO:Fe3O4:Na2O:P2O5In a molar ratio of 42:24:18:10: 6.
The preparation method of the magnetic bioglass bone cement comprises the following steps:
(1) weighing silicon dioxide, strontium carbonate, ferroferric oxide, sodium carbonate and phosphorus pentoxide powder, wherein SiO is2:SrO:Fe3O4:Na2O:P2O5Is 42:24:18:10:6, mixed for 60min, Fe3O4The particle size distribution range of (A) is 5-200 nm;
(2) putting the powder mixture uniformly mixed in the step (1) into a zirconia crucible, controlling the temperature rise rate of a sintering furnace to be 5 ℃/min, controlling the reaction temperature to be 1400 ℃ and the reaction time to be 8h, and preparing biological glass liquid;
(3) after the reaction in the step (2) is finished, pouring the prepared bioglass liquid into 40 volume percent ethanol solution for cooling and dispersing, sintering and drying for 2h at 800 ℃ after cooling, and performing ball milling to obtain magnetic bioglass;
(4) weighing and uniformly mixing magnetic bioglass, polyacrylate and benzoyl peroxide in specified mass percentage to obtain magnetic bioglass bone cement powder, weighing and uniformly mixing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate in specified mass percentage to obtain bone cement liquid;
(5) adding the bone cement liquid into the magnetic bioglass bone cement powder according to the powder-liquid ratio of 2g to 1mL, uniformly stirring and curing to obtain the magnetic bioglass bone cement.
Example 6
The magnetic biological glass bone cement and the preparation method thereof are disclosed, wherein the magnetic biological glass bone cement comprises the following components in percentage by mass: the powder is 10% of magnetic bioglass, 89% of polyacrylate and 1% of benzoyl peroxide, and the liquid is 93% of methyl methacrylate, 2% of hydroquinone and 5% of N, N dimethyl p-toluidine; in magnetic bioglass, SiO2:SrO:Fe3O4:Na2O:P2O5The molar percentage of (A) is 40:28:14:10: 8.
The preparation method of the magnetic bioglass bone cement comprises the following steps:
(1) weighing silicon dioxide, strontium carbonate, ferroferric oxide, sodium carbonate and phosphorus pentoxide powder, wherein SiO is2:SrO:Fe3O4:Na2O:P2O5Is 40:28:14:10:8, mixed for 60min, Fe3O4The particle size distribution range of (A) is 5-200 nm;
(2) putting the powder mixture uniformly mixed in the step (1) into a zirconia crucible, controlling the temperature rise rate of a sintering furnace to be 6 ℃/min, controlling the reaction temperature to be 1350 ℃ and controlling the reaction time to be 7h, and preparing biological glass liquid;
(3) after the reaction in the step (2) is finished, pouring the prepared bioglass liquid into an ethanol solution with 20% volume fraction for cooling and dispersing, sintering and drying for 2h at 700 ℃ after cooling, and performing ball milling to obtain magnetic bioglass;
(4) weighing and uniformly mixing magnetic bioglass, polyacrylate and benzoyl peroxide in fixed mass percentage to obtain magnetic bioglass bone cement powder, weighing and uniformly mixing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate in specified mass percentage to obtain bone cement liquid;
(5) adding the bone cement liquid into the magnetic bioglass bone cement powder according to the powder-liquid ratio of 3g to 1mL, uniformly stirring and curing to obtain the magnetic bioglass bone cement.
Test example 1 compression resistance test
The magnetic bioglass bone cement prepared in examples 1 to 6 was filled in a sample preparation mold, and after curing, samples having a diameter of 6.0mm and a length of 12mm were obtained, and the samples were subjected to a compressive strength test on a universal mechanical testing machine, respectively, and the test results are shown in table 1:
TABLE 1
Figure BDA0002707738460000091
As can be seen from Table 1, the bone cements prepared in examples 1 to 6 of the present invention have excellent compression resistance.
Test example 2 degradation test
Filling the magnetic bioglass bone cement prepared in examples 1-6 into a sample preparation mold, solidifying to obtain a sample with the diameter of 6.0mm and the length of 12mm, drying the sample at 37 ℃, respectively weighing the initial weight Xn of the dried sample prepared in examples 1-6, respectively soaking the samples prepared in examples 1-6 into a simulated human body fluid according to the ratio of the solid to the liquid of 1g/30ml, respectively, taking out the samples after soaking for 30 days, measuring the weight Xm of the sample after drying at 37 ℃, and measuring the weight loss rate L of the material as (Xn-Xm)/Xn x 100%, wherein the measurement results are shown in Table 2:
TABLE 2
Test items Example 1 Example 2 Example 3 Example 4 Example 5 Example 6
Weight loss ratio (%) 7.36％ 8.83％ 8.92％ 7.69％ 7.91％ 8.39％
The invention relates to a method for preparing a high-porosity polymethyl methacrylate bone cement, which is characterized in that common polymethyl methacrylate bone cement (PMMA) is not degradable, magnetic bioglass and PMMA are compounded, and the bioglass is rapidly degraded to obtain the bone cement with high porosity, so that the prepared magnetic bioglass bone cement can be degraded and the degradation meets the actual requirements of clinical tests.
Test example 3 curing time and curing temperature test
The magnetic bioglass bone cements prepared in examples 1 to 6 were cured at room temperature of 23 ℃ respectively, and the change in temperature of the surface portion of the bone cement was dynamically detected by a computer-controlled thermocouple-type temperature sensor puncture needle during the curing, and the test results are shown in table 3:
TABLE 3
Figure BDA0002707738460000101
As can be seen from Table 3, the magnetic bioglass bone cement prepared by the invention prolongs the curing time of the bone cement, and is beneficial to enhancing the sterilization and bacteriostasis effects in the curing process of the bone cement. The curing temperature of the magnetic bioglass bone cement prepared by the invention is lower than 57 ℃ in the curing process, and the defect that tissues are damaged due to overhigh curing temperature of the traditional PMMA bone cement can be effectively overcome. Test example 4 magnetic test and magnetocaloric performance test
The magnetic bioglass bone cement prepared in examples 1 to 6 was filled in a sample preparation mold to prepare a column having a length of 6mm and a diameter of 3mm, and the magnetism of the sample was measured by a vibration sample magnetometer.
The magnetic bioglass bone cement prepared in examples 1 to 6 was filled in a sample preparation mold to prepare a cylinder with a length of 9mm and a diameter of 9mm, a glass thermometer was inserted before curing, and after curing, the material was placed in a high-frequency induction coil with a frequency of 100kHz and a magnetic field size of 25KA. m-1And recording the temperature once every 5min, testing the temperature change of the sample along with the time under the alternating magnetic field, and observing the temperature rise capacity in the period.
The magnetic properties of the samples and the temperature-elevating ability of the samples are shown in Table 4:
TABLE 4
Figure BDA0002707738460000102
Figure BDA0002707738460000111
As can be seen from Table 4, the magnetic bioglass bone cements prepared in examples 1-6 have good temperature-raising and temperature-controlling capability under the alternating magnetic field.
The above embodiments are only specific examples of the present invention, and the protection scope of the present invention includes but is not limited to the product forms and styles of the above embodiments, and any suitable changes or modifications made by those skilled in the art according to the claims of the present invention shall fall within the protection scope of the present invention.

Claims (8)

1. The magnetic bioglass bone cement is characterized in that: the material mainly comprises the following raw materials in percentage by mass:
powder:
45% -89% of polyacrylate;
10% -50% of magnetic bioglass;
1 to 5 percent of benzoyl peroxide;
liquid:
0.5 to 5 percent of N, N-dimethyl-p-toluidine;
0.05 to 2 percent of hydroquinone;
93-99.45% of methyl methacrylate;
the adding ratio of the powder to the liquid is (1-3) g:1 ml.
2. The magnetic bioglass bone cement as defined in claim 1, wherein: the material mainly comprises the following raw materials in percentage by mass:
powder:
63% of polyacrylate;
35% of magnetic bioglass;
2% of benzoyl peroxide;
liquid:
3% of N, N-dimethyl-p-toluidine;
1% of hydroquinone;
96% of methyl methacrylate;
the adding ratio of the powder to the liquid is 2g:1 ml.
3. A magnetic bioglass bone cement as claimed in claim 1 or claim 2, wherein: SiO in the magnetic bioglass2：SrO：Fe3O4：Na2O：P2O5The molar percentage of (40-50): (20-40): (10-20): (10-20): (1-10).
4. A magnetic bioglass bone cement as claimed in claim 3, which is characterized in that: SiO in the magnetic bioglass2：SrO：Fe3O63：Na2O：P2O5The mole percentage of (A) is 40:20:15:15: 10.
5. a magnetic bioglass bone cement as claimed in claim 3, which is characterized in that: the SrO can be partially replaced by CaO, and the maximum replacement mole percentage is 20%.
6. The method for preparing magnetic bioglass bone cement according to claim 1, which is characterized in that: the preparation method comprises the following preparation steps:
(1) weighing silicon dioxide, strontium carbonate, ferroferric oxide, sodium carbonate and phosphorus pentoxide powder, wherein SiO is2：SrO：Fe3O4：Na2O：P2O5The molar percentage of (40-50): (20-40): (10-20): (10-20): (1-10), stirring and mixing for 30-60 min;
(2) putting the powder mixture uniformly mixed in the step (1) into a zirconia crucible, controlling the temperature rise rate of a sintering furnace to be 5-8 ℃/min, controlling the reaction temperature to be 1300-1600 ℃, and controlling the reaction time to be 4-8 h to prepare a bioglass liquid;
(3) after the reaction in the step (2) is finished, pouring the prepared bioglass liquid into an ethanol solution for cooling and dispersing, sintering and drying at 600-800 ℃ for 1-3 h after cooling, and performing ball milling to obtain magnetic bioglass;
(4) weighing magnetic bioglass, polyacrylate and benzoyl peroxide according to specified mass percentage, uniformly mixing to obtain magnetic bioglass bone cement powder, weighing N, N-dimethyl-p-toluidine, hydroquinone and methyl methacrylate according to specified mass percentage, and uniformly mixing to obtain bone cement liquid;
(5) according to the powder-liquid ratio (1.5-2.5) g:1mL of bone cement liquid is added into the magnetic bioglass bone cement powder, and the magnetic bioglass bone cement is obtained after uniform stirring and solidification.
7. The method for preparing a magnetic bioglass bone cement according to claim 6, which is characterized in that: fe in the step (1)3O4The particle size distribution range of (B) is 5-200 nm.
8. The method for preparing a magnetic bioglass bone cement according to claim 6, which is characterized in that: the volume fraction of the ethanol solution is 10-40%.
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