CN114569788A - PMMA composite bone cement powder and preparation method of PMMA composite bone cement - Google Patents
PMMA composite bone cement powder and preparation method of PMMA composite bone cement Download PDFInfo
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- CN114569788A CN114569788A CN202210077769.8A CN202210077769A CN114569788A CN 114569788 A CN114569788 A CN 114569788A CN 202210077769 A CN202210077769 A CN 202210077769A CN 114569788 A CN114569788 A CN 114569788A
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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
- A61L27/14—Macromolecular materials
- A61L27/16—Macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
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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
- A61L27/04—Metals or alloys
- A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
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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
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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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
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention relates to PMMA composite bone cement powder and a preparation method of PMMA composite bone cement, which are characterized by comprising the following steps: the PMMA composite bone cement is prepared by mixing and stirring the PMMA composite bone cement powder and a solvent when the PMMA composite bone cement is used, and the preparation method of the PMMA composite bone cement comprises the steps of drawing magnesium or magnesium alloy materials to prepare metal fibers, weighing and preparing PMMA powder and the solvent, preparing, screening, mixing and the like. The PMMA composite bone cement provided by the invention has excellent mechanical properties and excellent osteogenesis inducing capacity.
Description
Technical Field
The invention relates to the field of bone cement, in particular to PMMA composite bone cement powder added with magnesium or magnesium alloy fiber and a method for preparing bone cement by utilizing the PMMA composite bone cement powder.
Background
At present, PMMA (polymethyl methacrylate) bone cement widely applied to clinic is generally formed by mixing solid (PMMA, initiator, barium sulfate and the like) and liquid (MMA is mainly) at normal temperature and then curing, has better fluidity at the early stage of curing, and can be injected and implanted; the cured product has the advantages of good biomechanical characteristics, rapid forming and the like, so that the cured product can be rapidly developed in clinical application. However, since the PMMA composite bone cement cannot be degraded and lacks biological activity, the PMMA composite bone cement cannot be organically combined with host bone tissues, and after being implanted into a human body, the PMMA composite bone cement has poor fusion with surrounding bone tissues and is not beneficial to inducing the growth of the bone tissues; the long-term use of the implant can easily lead to the loosening and inflammation of the implant body, and the implant can fail to be implanted.
In order to increase the biological activity of PMMA bone cements, it is possible to add active components to PMMA, for example: the patent CN201410541808.0 discloses an akermanite/PMMA composite bone cement with an osteogenesis inducing function and a preparation method thereof, high-content akermanite powder not only maintains good mechanical properties of the bone cement, reduces polymerization temperature, but also improves the biological activity and biocompatibility of the bone cement, and can actively induce osteogenesis due to the contained elements of magnesium and silicon. However, the high content of akermanite ceramic particles is not good for the mechanical properties of PMMA, such as tensile property, bending resistance and the like.
Patent CN201910280988.4 discloses a bone cement with biological activity and a preparation method thereof, which is characterized in that heterogeneous bones are subjected to cell removal and immune component removal, then are ground into bone powder with a certain particle size, the bone powder is added into PMMA bone cement powder according to a certain proportion, the bone cement with the heat release temperature lower than 60 ℃ is prepared, and the biological active components of the bone cement are retained to the maximum extent. Although the addition of bone powder improves the bioactivity of PMMA bone cement, the mechanical properties of the bone cement are significantly reduced. Therefore, a modified material which can improve the bioactivity of the PMMA bone cement and can also improve the mechanical property of the PMMA bone cement is urgently needed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides PMMA composite bone cement powder, and the bone cement prepared from the PMMA composite bone cement powder has excellent mechanical properties.
The PMMA composite bone cement powder comprises magnesium or magnesium alloy fibers and PMMA powder, and the PMMA composite bone cement powder and a solvent are mixed and stirred when in use.
Further, the mass ratio of the magnesium or magnesium alloy fibers to the PMMA powder is 0.03-0.6: 2.
Further, in the PMMA composite bone cement powder, the particle size is at least 90% of the PMMA powder by mass; the diameter of the magnesium or magnesium alloy fiber is 0.05-0.09 mm.
The PMMA composite bone cement powder is added with a dispersant methyl cellulose, wherein the dispersant accounts for 1-3% by mass, and the viscosity is 400 mPa.s.
Further, the setting time of the PMMA composite bone cement powder after mixing is 15-25 min.
The invention also relates to a preparation method of the PMMA composite bone cement, which comprises the following steps: drawing fiber, namely drawing the magnesium or magnesium alloy material into slender metal fiber by using a drawing die; weighing and configuring PMMA powder and a solvent; preparing powder, namely adding the metal fibers and the PMMA powder into grinding equipment for mixing; sieving, namely sieving the mixed powder through a round hole sieve to obtain PMMA composite bone cement powder comprising magnesium or magnesium alloy fibers and the PMMA powder; mixing, namely mixing and stirring the PMMA composite bone cement powder and the solvent for use.
Further, the drawing fiber adopts a single drawing method, and the magnesium or magnesium alloy material passes through the multistage drawing die through tension force, so that the cross-sectional area of the magnesium or magnesium alloy material is gradually reduced.
Furthermore, the wire drawing die is designed with small holes, and the material of the wire drawing die is hard alloy or diamond.
Furthermore, the powder process adopts the equipment diameter respectively to be 2mm, 10mm, 20mm, and the mass ratio is 2 mm: 10 mm: and (3) grinding the mixture by a ball mill with grinding balls with the diameter of 20mm being 1:3:1 for 20-40 min, wherein the rotating speed of the ball mill can be set to be 100-150 r/min.
And further, in the mixing stage, the stirring time is 5-10 min.
The PMMA composite bone cement prepared by using the PMMA composite bone cement powder has excellent osteogenesis inducing capability, and the mechanical property of the PMMA composite bone cement is improved, so that the PMMA composite bone cement has a wider future in the field of bone repair materials.
Drawings
Fig. 1 is a schematic view of PMMA composite bone cement prepared using the powder according to the present invention.
Fig. 2 shows the compressive strength of PMMA composite bone cements with different magnesium fiber addition levels.
Detailed Description
The technical means adopted by the invention to achieve the predetermined object of the invention are further described below with reference to the drawings and the preferred embodiments of the invention.
The PMMA (polymethyl methacrylate) bone cement powder comprises the following components: magnesium or magnesium alloy fibers and PMMA powder. The mass ratio of the two is 0.03-0.6: 2.
The mass percentage of the PMMA powder with the particle size of 30-80 mu m in the PMMA composite bone cement powder is at least 90%, the too coarse particle size can lead the magnesium or magnesium alloy fiber to be unevenly dispersed in the PMMA composite bone cement, and the too fine particle size can lead the mechanical strength of the PMMA bone cement to be reduced. The PMMA powder comprises: 80-90% by mass of PMMA particles, 3-6% by mass of BPO (benzoyl peroxide) particles, 4-17% by mass of developer (zirconia) particles and 1-3% by mass of dispersant (methyl cellulose); the particle diameters of the PMMA particles, the BPO particles and the developing agent particles are all 20-100 mu m. The addition of the dispersing agent can uniformly disperse the magnesium or magnesium alloy fibers in the PMMA bone cement to avoid agglomeration.
The diameter of the magnesium or magnesium alloy fiber in the PMMA composite bone cement powder is 0.05-0.09 mm. If the magnesium or magnesium alloy fiber is too thin, the reinforcing effect cannot be achieved; if the magnesium or magnesium alloy fiber is too coarse, the magnesium or magnesium alloy fiber cannot be suspended and dispersed when the bone cement powder is mixed with a solvent, and is easy to precipitate, so that the magnesium or magnesium alloy fiber is agglomerated, and the reinforcing effect is affected.
When in use, the PMMA composite bone cement powder and a solvent are mixed and stirred, and are solidified after 15-25 min to form PMMA composite bone cement 2 with uniformly dispersed magnesium or magnesium alloy fibers 1 as shown in figure 1, wherein the mass ratio of the PMMA powder to the solvent is 2: 1.
The solvent comprises 93-97% by mass of MMA (methyl methacrylate) and 3-7% by mass of DMPT (dimethyl-p-toluidine). The mass ratio of the solvent to the PMMA powder was 1: 2.
The invention provides a preparation method for preparing PMMA composite bone cement 2, which comprises the following steps:
and S1, drawing the fiber, namely drawing the magnesium or magnesium alloy material into slender metal fiber by using a drawing die. The method adopts a single drawing method, and the magnesium or magnesium alloy material passes through a multistage wire drawing die through tension force, so that the cross section area of the magnesium or magnesium alloy material is gradually reduced to form metal fibers, wherein the metal fibers comprise short fibers with the length of 3-25 mm and long fibers with the length of more than 150 mm. Wherein the wire drawing die is provided with a plurality of small holes for magnesium or magnesium alloy materials to pass through, and the diameters of the small holes are gradually reduced. The advantage of the single drawing process is that metal fibers of uniform diameter can be obtained.
S2 PMMA powder and solvent are weighed and prepared.
S3, preparing powder, taking PMMA powder, adding the PMMA powder and metal fibers into a ball mill together, mixing and grinding for 20-40 min to form mixed powder, wherein the mixed powder comprises magnesium or magnesium alloy fiber 1 with the diameter of 0.05-0.09 mm and PMMA powder. The ball mill comprises grinding balls with diameters of 2mm, 10mm and 20mm respectively, the weight ratio of the grinding balls is 1:3:1, and the rotating speed of the ball mill is set to be 100-150 r/min. The process reduces the granularity of PMMA composite bone cement powder, and is beneficial to improving the mechanical strength of PMMA composite bone cement; on the other hand, the ball milling process can ensure that the magnesium or magnesium alloy fiber 1 and the magnesium-based composite powder are dispersed more uniformly, and the agglomeration of the magnesium or magnesium alloy fiber 1 is avoided.
And S4, screening, namely screening the mixed powder into PMMA composite bone cement powder by using a circular hole screen, wherein the PMMA composite bone cement powder comprises magnesium or magnesium alloy fiber 1 and PMMA powder. After sieving, the PMMA powder with the particle size of 30-80 mu m accounts for at least 90% (wt%).
S5, mixing the PMMA composite bone cement powder with a solvent when in use, stirring for 5-10 min to obtain a fluid, injecting the mixed fluid into a human body by using an injector, wherein the injection operation time is 5-10 min, and the fluid can be solidified into the PMMA composite bone cement 2 shown in figure 1 in the human body after 15-25 min.
The PMMA bone cement powder is modified by adding magnesium or magnesium alloy fibers, and as shown in figure 2, a statistical graph of the compressive strength of the solidified PMMA composite bone cement added with pure magnesium with different mass ratios, which is prepared by the preparation method, is shown in figure 2, wherein the mass ratios of PMMA, PMMA-Mg0.03, PMMA-Mg0.15, PMMA-Mg0.3, PMMA-Mg0.45 and PMMA-Mg0.6 respectively represent that the mass ratios of magnesium fibers, PMMA powder and solvent are 0:2:1, 0.03:2:1, 0.15:2:1, 0.3:2:1, 0.45:2:1 and 0.6:2:1 in sequence. It can be seen from the figure that the compressive strength of the modified PMMA composite bone cement is obviously stronger than that of the unmodified PMMA bone cement. With the increase of the content of the magnesium fiber, the biological activity and the osteogenesis capacity of the PMMA composite bone cement are continuously improved, but the mechanical property of the PMMA composite bone cement is increased firstly and then reduced, and the plasticity and the injectability are also deteriorated. Therefore, in the present invention, the mass ratio of the magnesium or magnesium alloy fibers 1, the PMMA powder and the solvent cannot exceed 0.6:2:1 at maximum, so that the magnesium or magnesium alloy fibers 1 can be uniformly dispersed in the PMMA bone cement. If the mass ratio exceeds 0.6:2:1, the magnesium or magnesium alloy fibers 1 are not uniformly dispersed, and the magnesium or magnesium alloy fibers 1 are agglomerated to cause the mechanical properties of the PMMA composite bone cement to be deteriorated.
The PMMA bone cement powder is modified by adding the magnesium or magnesium alloy fiber, and the modified PMMA composite bone cement prepared by utilizing the modified PMMA composite bone cement powder has excellent osteogenesis inducing capability, improves the mechanical property of the PMMA composite bone cement, and enables the PMMA composite bone cement to have a wider future in the field of bone repair materials.
The PMMA composite bone cement prepared by the present invention and the preparation method are further described by the following specific examples.
The first embodiment is as follows:
in the embodiment, 1.8g of pure magnesium fibers are used for modifying the PMMA bone cement, wherein the mass ratio of the pure magnesium fibers to the PMMA powder to the solvent is 0.03:2:1, the mass ratio of the PMMA powder with the particle size of 30-80 mu m is 91%, and the diameter of the pure magnesium fibers is 0.05 mm. The preparation method of this example is as follows:
A) and drawing the pure magnesium material into pure magnesium fiber with the length of 3mm by using a wire drawing die.
B) Weighing and preparing PMMA powder: 108g of PMMA, 7.2g of BPO, 4.8g of developer, and 3.6g of dispersant (methyl cellulose having a viscosity of 400 mPa.s) were weighed out; weighing, and mixing.
Weighing a solvent: weighing 57g of MMA, and 3g of DMPT; weighing, and mixing the two solutions.
C) The prepared PMMA powder and 1.8g of pure magnesium fibers are added into a ball mill and ground into mixed powder. The diameter weight ratio of the grinding balls refers to the ball mill in the preparation method, the rotating speed of the ball mill is set to be 100r/min, and the grinding time is set to be 30 min.
D) And screening the ground mixed powder by using a circular hole screen to prepare PMMA composite bone cement powder. After grinding and screening, the mass fraction of PMMA powder with the particle size of 30-80 mu m is 91%, and the diameter of the pure magnesium fiber is 0.05 mm.
E) Mixing the PMMA composite bone cement powder with a solvent, stirring for 5min, and standing for 15-25 min to form the PMMA composite bone cement.
As shown in FIG. 2, the compressive strength of the PMMA composite bone cement of the first example is 92MPa, which is improved by 7% compared with the compressive strength of the ordinary PMMA bone cement.
Example two:
in this example, 27g of pure magnesium fibers, which are used in the mass ratio of 0.45:2:1 to the PMMA powder and the solvent, are used to modify the PMMA bone cement, and the rest is the same as in the first example.
As shown in fig. 2, the compressive strength of the PMMA composite bone cement of the present embodiment is 171MPa, which is 99% higher than that of the ordinary PMMA bone cement, and the compressive strength reaches the maximum.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A PMMA composite bone cement powder is characterized by comprising: the PMMA composite bone cement powder is mixed with a solvent and stirred when in use.
2. The PMMA composite bone cement powder of claim 1, wherein the mass ratio of the magnesium or magnesium alloy fiber to the PMMA powder is 0.03-0.6: 2.
3. The PMMA composite bone cement powder of claim 1, wherein the mass ratio of the PMMA powder with a particle size of 30 to 80 μm in the PMMA composite bone cement powder is at least 90%, and the diameter of the magnesium or magnesium alloy fiber is 0.05 to 0.09 mm.
4. The PMMA composite bone cement powder of claim 1, wherein a dispersant methyl cellulose is added to the PMMA composite bone cement powder, the dispersant accounts for 1-3% by mass, and the viscosity is 400 mPa.s.
5. The PMMA composite bone cement powder of claim 1, wherein the setting time of the PMMA composite bone cement powder after mixing is 15-25 min.
6. A method for preparing PMMA composite bone cement comprising the PMMA composite bone cement powder according to any one of claims 1 to 5, comprising:
drawing fiber, namely drawing the magnesium or magnesium alloy material into slender metal fiber by using a drawing die;
weighing and configuring PMMA powder and a solvent;
preparing powder, namely adding the metal fibers and the PMMA powder into grinding equipment, mixing and grinding into mixed powder;
sieving, namely sieving the mixed powder by using a round hole sieve to obtain PMMA composite bone cement powder comprising magnesium or magnesium alloy fibers and the PMMA powder;
mixing, namely mixing and stirring the PMMA composite bone cement powder and the solvent for use.
7. The preparation method according to claim 6, wherein the drawn fiber is drawn by a single drawing method, and the magnesium or magnesium alloy material is drawn through the drawing die in multiple stages by tension, so that the cross-sectional area of the magnesium or magnesium alloy material is gradually reduced.
8. The preparation method according to claim 7, wherein the wire drawing die is designed with small holes, and the material of the wire drawing die is cemented carbide or diamond.
9. The method of claim 6, wherein the milling is performed by using a mill having a diameter of 2mm, 10mm, 20mm, and a mass ratio of 2 mm: 10 mm: and grinding the mixture by a ball mill with grinding balls with the diameter of 20mm being 1:3:1 for 20-40 min, wherein the rotating speed of the ball mill can be set to be 100-150 r/min.
10. The method according to claim 6, wherein the mixing step is carried out for 5 to 10 min.
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