CN108721702A - A kind of preparation method of magnesium/l-lactic acid Composite Bone holder - Google Patents
A kind of preparation method of magnesium/l-lactic acid Composite Bone holder Download PDFInfo
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- CN108721702A CN108721702A CN201810695516.0A CN201810695516A CN108721702A CN 108721702 A CN108721702 A CN 108721702A CN 201810695516 A CN201810695516 A CN 201810695516A CN 108721702 A CN108721702 A CN 108721702A
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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
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
- A61L27/446—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with other specific inorganic fillers other than those covered by A61L27/443 or A61L27/46
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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
- A61L27/58—Materials at least partially resorbable by the body
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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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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a kind of preparation method of magnesium/l-lactic acid Composite Bone holder, this method is separated by solid-liquid separation after mixing l-lactic acid powder, magnesium dust and amphiphilic phosphatide powder by liquid phase, and solid obtains composite powder by dry and grinding；The composite powder prepares Composite Bone holder by Selective Laser Sintering.This method, which utilizes, has preferable binding ability between amphiphilic phosphatide and magnesium metal and l-lactic acid, the interface performance between magnesium metal and polymer l-lactic acid is improved, to improve the biological property and mechanical performance of magnesium/l-lactic acid Composite Bone holder.
Description
Technical field
The present invention relates to a kind of preparation methods of magnesium/l-lactic acid Composite Bone holder, more particularly to a kind of to utilize parents
Property phosphatide improve the method that magnesium and l-lactic acid binding performance prepare magnesium/l-lactic acid Composite Bone holder, belong to bone holder
Preparing technical field.
Background technology
L-lactic acid (PLLA) is the Typical Representative of clinical application biological degradation polyalcohol, since its source is renewable,
Synthesis is controllable, and mechanical performance and biocompatibility are well and as the hot spot of bone implant material research.Magnesium (Mg) due to its
Voluntarily it can degrade and absorb in human body, and there is good biomechanical compatibility with skeleton and cause more and more to close
Note.Therefore, Mg/PLLA composite materials may have both the advantages of two kinds of materials, and S.C.Cifuentes et al. are prepared for PLA/
Mg composite materials simultaneously have evaluated mechanical performance and hot property ([1] Cifuentes S C, Lieblich M, L ó pez F A, et
al.Effect of Mg content on the thermal stability and mechanical behaviour of
PLLA/Mg composites processed by hot extrusion.[J].Materials Science&
Engineering C,2017,72:18.；[2]Cifuentes S C,Frutos E,Benavente R,et
al.Assessment of mechanical behavior of PLA composites reinforced with Mg
micro-particles through depth-sensing indentations analysis[J].Journal of the
mechanical behavior of biomedical materials,2017,65:781-790.).Peng et al. are introduced
PLLA/Mg composite materials ([3] Peng Wan, Chen Yuan, the LiLi Tan, et that can be fully absorbed are prepared in Mg to PLLA
al.Fabrication and evaluation of bioresorbable PLLA/magnesium and PLLA/
magnesium fluoride hybrid composites for orthopedic implants[J].Composites
Science and Technology,2014,98:36-43.).On the basis of can be degradable, also have degradation property can
The features such as tune, degradation microenvironment acid-base neutralization.However metal Mg and polymer P LLA physicochemical properties differ greatly, cause Mg with
Stronger interface cohesion is hardly formed between PLLA, to reduce the mechanical property of composite material.
Invention content
During preparing the compound bone holder material of magnesium/l-lactic acid in the prior art, due to metal Mg and polymerization
Object PLLA physicochemical properties differ greatly, cause between the two Interface adhesive strength it is weak, to reduce the mechanical property of composite material
Can, the purpose of the invention is to provide a kind of using amphiphilic phosphatide simultaneously comprising polar hydrophilic group and nonpolarity parent
Oil base group, the method to improve polyether-ether-ketone and polyvinyl alcohol binding performance, this method utilize amphiphilic phosphatide and metal
There is preferable binding ability between magnesium and l-lactic acid, improves the interface performance between metal Mg and polymer P LLA, from
And obtain biological property and the better magnesium of mechanical performance/l-lactic acid Composite Bone holder.
To realize the above-mentioned technical purpose, the present invention provides a kind of preparation method of magnesium/l-lactic acid Composite Bone holder,
This method is separated by solid-liquid separation after mixing PLLA powder, Mg powder and amphiphilic phosphatide (PL) powder by liquid phase, and solid passes through
Dry and grinding, obtains composite powder；The composite powder prepares Composite Bone holder by Selective Laser Sintering.
Technical scheme of the present invention key is to improve the Interface adhesive strength between Mg and PLLA matrixes, PL using PL
Include simultaneously hydrophilic radical and hydrophobic group, there are preferable binding abilities between hydrophilic radical and Mg, and its is hydrophobic
Property carbochain tail and PLLA between there are preferable binding ability, PL play enhancing Mg and PLLA matrixes between binding ability work
With so as to which metal Mg particles are fixed and dispersed within well in PLLA matrixes, greatly increasing the power of Composite Bone holder
Performance is learned, the bioactivity of metal Mg is given full play to, improves the biological property of Composite Bone holder.
The PL of the present invention also acts as the effect for promoting Mg particles to disperse in the liquid phase, polar group in liquid phase mixed process
Group is adsorbed on Mg particle surfaces, and non-polar group is dispersed in organic solvent, can improve Mg particles in organic liquid phase
Dispersibility prevents Mg particles from being settled in liquid phase mixed process, while can obtain what Mg powder was uniformly mixed with PLLA powder
Mixed-powder.
Preferred scheme, the composite powder are grouped as by following mass percent group：PL1%~7%；Mg 2%~
14%；PLLA 79~97%.When PL is too low with respect to Mg contents, modification is not had to Mg, when PL is with respect to Mg too high levels,
Extra PL forms suspended particulate in liquid phase mixed process, can not act on Mg particles.
The grain size of preferred scheme, the PLLA powder is 1~3 μm, and fusing point is 178~180 DEG C.
Preferred scheme, the Mg powder diameters are 400~600nm, purity>99.9%.
Preferred scheme, the PL powder diameters are 3~15nm, and fusing point is 234~238 DEG C.
Preferred scheme is using stirring and ultrasonic disperse mode, the time of magnetic agitation in the liquid phase mixed process
40~60min, speed are 200~400r/min；The time of ultrasonic disperse is 10~30min, and temperature is 40~60 DEG C.
Preferred scheme, selective laser sintering technological parameter are：Laser power is 2.3~2.7W, sweep speed 100
~120mm/min, sweep span are 0.8~1.2mm, spot diameter is 0.3~0.7mm.
The method of the Mg/PLLA Composite Bone holders of the present invention, including following key step：
(1) PLLA, Mg and PL powder are weighed respectively in proportion, and three is mixed into beaker, is placed in absolute ethyl alcohol
Ultrasonic agitation obtains PLLA/Mg/PL suspension, then handles to obtain by magnetic agitation, filtering and freeze-day with constant temperature evenly dispersed
PLLA/Mg/PL mixed-powders；The content of amphiphilic PL and Mg is respectively 5wt.% and 10wt.% in the mixed-powder；Institute
The ultrasonic disperse time stated is 20min, and temperature is 50 DEG C, and the magnetic agitation time is 50min, magnetic stirring speed 300r/
min；
(2) preset powdering technique is used, mixed-powder is placed in selective laser sintering system, according to designed knot
Structure requirement, under conditions of laser power 2.5W, sweep speed 110mm/min, sweep span 1mm, spot diameter 0.5mm, profit
Composite powder is selectively scanned with laser.
Compared with the prior art, the good effect that technical solution of the present invention is brought：
1) present invention improves the binding ability between metal Mg and PLLA using PL, and PL includes hydrophobic carbochain tail and parent
The molecule head of water, there are preferable combination between hydrophilic molecule head and Mg, and hydrophobic carbochain tail and PLLA compatibilities
Preferably, to improve the Interface adhesive strength between Mg and PLLA by PL, the metal Mg disperses in PLLA matrixes point are realized
Cloth can preferably play the effect of Mg, the mechanical property of bone holder can not only be improved as reinforced phase, while metal Mg can be with
The Mg ions of generation can improve adherency, proliferation and the differentiation of osteoblast, improve the mechanical property of Composite Bone holder.
2) present invention prepares Composite Bone holder, it can be achieved that customizing external form using Selective Laser Sintering, and energy
Size, distribution and the connectivity of control hole.
3) Mg degrade the alkaline product to be formed can neutralize PLLA degradation acid product, reduce inflammation reaction.
Specific implementation mode
The specific implementation mode of the present invention is further described with reference to specific embodiment, but the content of the present invention is simultaneously
It is not limited to this.
Comparative example 1
Personalized shape is carried out to Composite Bone holder using Three-dimensional Design Software and inner porosity designs, will be designed
Three-dimensional data model import computer carry out hierarchy slicing processing, obtain each layer of section profile information.It weighs respectively
4.25 grams of PLLA powder, 0.75 gram of Mg powder, the two are sequentially added in the beaker equipped with 30ml absolute ethyl alcohols, through ultrasonic disperse
It is uniformly mixed with magnetic agitation.Mixing suspension is filtered using filter paper, it is dry in electric drying oven with forced convection, then to drying
Mixed-powder afterwards is ground, and the mixed-powder after grinding is placed in selective laser sintering system and is sintered experiment,
It is straight in laser power 2.5W, sweep speed 110mm/min, sweep span 1mm, hot spot according to pre-designed structural requirement
Under conditions of diameter 0.5mm, selectively sintered compound powder and PLLA/Mg Composite Bone holders are prepared using laser.It measures at this time
The tensile strength of compound bone holder material is 3.84MPa, compressive strength 21.31MPa.Illustrate in no addition PL powder,
Between metal Mg and PLLA combine it is poor, compressive strength is relatively low.
Embodiment 1
Personalized shape is carried out to Composite Bone holder using Three-dimensional Design Software and inner porosity designs, will be designed
Three-dimensional data model import computer carry out hierarchy slicing processing, obtain each layer of section profile information.It weighs respectively
4.25 grams of PLLA powder, 0.50 gram of Mg powder and 0.25 gram of PL powder, the burning equipped with 30ml absolute ethyl alcohols is sequentially added by three
In cup, it is uniformly mixed through ultrasonic disperse and magnetic agitation.Mixing suspension is filtered using filter paper, in electric drying oven with forced convection
It is dry, then the mixed-powder after drying is ground, the mixed-powder after grinding is placed in selective laser sintering system
In be sintered experiment, according to pre-designed structural requirement, in laser power 2.5W, sweep speed 110mm/min, scanning
Under conditions of spacing 1mm, spot diameter 0.5mm, selectively sintered compound powder and PLLA/Mg Composite Bones are prepared using laser
Holder.The tensile strength for measuring compound bone holder material at this time is 3.05MPa, compressive strength 101.24MPa.
Embodiment 2
Personalized shape is carried out to Composite Bone holder using Three-dimensional Design Software and inner porosity designs, will be designed
Three-dimensional data model import computer carry out hierarchy slicing processing, obtain each layer of section profile information.It weighs respectively
4.25 grams of PLLA powder, 0.63 gram of Mg powder and 0.12 gram of PL powder, the burning equipped with 30ml absolute ethyl alcohols is sequentially added by three
In cup, it is uniformly mixed through ultrasonic disperse and magnetic agitation.Mixing suspension is filtered using filter paper, in electric drying oven with forced convection
It is dry, then the mixed-powder after drying is ground, the mixed-powder after grinding is placed in selective laser sintering system
In be sintered experiment, according to pre-designed structural requirement, in laser power 2.5W, sweep speed 110mm/min, scanning
Under conditions of spacing 1mm, spot diameter 0.5mm, selectively sintered compound powder and PLLA/Mg Composite Bones are prepared using laser
Holder.The tensile strength for measuring compound bone holder material at this time is 3.44MPa, compressive strength 54.49MPa.
Embodiment 3
Personalized shape is carried out to Composite Bone holder using Three-dimensional Design Software and inner porosity designs, will be designed
Three-dimensional data model import computer carry out hierarchy slicing processing, obtain each layer of section profile information.It weighs respectively
4.25 grams of PLLA powder, 0.12 gram of Mg powder and 0.63 gram of PL powder, the burning equipped with 30ml absolute ethyl alcohols is sequentially added by three
In cup, it is uniformly mixed through ultrasonic disperse and magnetic agitation.Mixing suspension is filtered using filter paper, in electric drying oven with forced convection
It is dry, then the mixed-powder after drying is ground, the mixed-powder after grinding is placed in selective laser sintering system
In be sintered experiment, according to pre-designed structural requirement, in laser power 2.5W, sweep speed 110mm/min, scanning
Under conditions of spacing 1mm, spot diameter 0.5mm, selectively sintered compound powder and PLLA/Mg Composite Bones are prepared using laser
Holder.The tensile strength for measuring compound bone holder material at this time is 2.60MPa, compressive strength 63.51MPa.
Embodiment 5
Personalized shape is carried out to Composite Bone holder using Three-dimensional Design Software and inner porosity designs, will be designed
Three-dimensional data model import computer carry out hierarchy slicing processing, obtain each layer of section profile information.It weighs respectively
4.25 grams of PLLA powder, 0.50 gram of Mg powder and 0.25 gram of PL powder, the burning equipped with 30ml absolute ethyl alcohols is sequentially added by three
In cup, it is uniformly mixed through ultrasonic disperse and magnetic agitation.Mixing suspension is filtered using filter paper, in electric drying oven with forced convection
It is dry, then the mixed-powder after drying is ground, the mixed-powder after grinding is placed in selective laser sintering system
In be sintered experiment, according to pre-designed structural requirement, in laser power 2.3W, sweep speed 120mm/min, scanning
Under conditions of spacing 1mm, spot diameter 0.5mm, selectively sintered compound powder and PLLA/Mg Composite Bones are prepared using laser
Holder.The tensile strength for measuring compound bone holder material at this time is 2.87MPa, compressive strength 80.73MPa.
Embodiment 6
Personalized shape is carried out to Composite Bone holder using Three-dimensional Design Software and inner porosity designs, will be designed
Three-dimensional data model import computer carry out hierarchy slicing processing, obtain each layer of section profile information.It weighs respectively
4.25 grams of PLLA powder, 0.50 gram of Mg powder and 0.25 gram of PL powder, the burning equipped with 30ml absolute ethyl alcohols is sequentially added by three
In cup, it is uniformly mixed through ultrasonic disperse and magnetic agitation.Mixing suspension is filtered using filter paper, in electric drying oven with forced convection
It is dry, then the mixed-powder after drying is ground, the mixed-powder after grinding is placed in selective laser sintering system
In be sintered experiment, according to pre-designed structural requirement, in laser power 2.7W, sweep speed 100mm/min, scanning
Under conditions of spacing 1mm, spot diameter 0.5mm, selectively sintered compound powder and PLLA/Mg Composite Bones are prepared using laser
Holder.The tensile strength for measuring compound bone holder material at this time is 2.76MPa, compressive strength 76.54MPa.
Claims (5)
1. a kind of preparation method of magnesium/l-lactic acid Composite Bone holder, it is characterised in that：By PLLA powder, Mg powder and double
It after parent's property phosphatide powder is mixed by liquid phase, is separated by solid-liquid separation, solid obtains composite powder by dry and grinding；It is described compound
Powder prepares Composite Bone holder by Selective Laser Sintering.
2. a kind of preparation method of magnesium according to claim 1/l-lactic acid Composite Bone holder, it is characterised in that：Institute
Composite powder is stated to be grouped as by following mass percent group：
Amphiphilic phosphatidase 1 %~7%；
Mg2%~14%；
PLLA 79~97%.
3. a kind of preparation method of magnesium according to claim 1/l-lactic acid Composite Bone holder, it is characterised in that：
The grain size of the PLLA powder is 1~3 μm, and fusing point is 178~180 DEG C；
The Mg powder diameters are 400~600nm, purity>99.9%；
The amphiphilic phosphatide powder diameter is 3~15nm, and fusing point is 234~238 DEG C.
4. special according to a kind of preparation method of magnesium of claims 1 to 3 any one of them/l-lactic acid Composite Bone holder
Sign is：Using stirring and ultrasonic disperse mode in the liquid phase mixed process, the time of magnetic agitation is 40~60min, speed
Degree is 200~400r/min；The time of ultrasonic disperse is 10~30min, and temperature is 40~60 DEG C.
5. special according to a kind of preparation method of magnesium of claims 1 to 3 any one of them/l-lactic acid Composite Bone holder
Sign is：Selective laser sintering technological parameter is：Laser power is 2.3~2.7W, sweep speed be 100~120mm/min,
Sweep span is 0.8~1.2mm, spot diameter is 0.3~0.7mm.
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Cited By (2)
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| CN110384828A (en) * | 2019-06-18 | 2019-10-29 | 中南大学湘雅二医院 | A kind of magnetic method for carrying magnesium artificial bone and carrying magnesium artificial bone using 3D printing preparation magnetism |
| CN111558091A (en) * | 2020-05-19 | 2020-08-21 | 中南大学 | Antibacterial polymer-based bone scaffold containing silver-loaded carbon nanotubes and preparation method thereof |
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| CN111558091A (en) * | 2020-05-19 | 2020-08-21 | 中南大学 | Antibacterial polymer-based bone scaffold containing silver-loaded carbon nanotubes and preparation method thereof |
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| CN108721702B (en) | 2021-06-29 |
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