CN105770988A - Bone repairing biological ceramic material based on 3D printing and preparation method thereof - Google Patents
Bone repairing biological ceramic material based on 3D printing and preparation method thereof Download PDFInfo
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- CN105770988A CN105770988A CN201610247006.8A CN201610247006A CN105770988A CN 105770988 A CN105770988 A CN 105770988A CN 201610247006 A CN201610247006 A CN 201610247006A CN 105770988 A CN105770988 A CN 105770988A
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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
- A61L27/18—Macromolecular materials obtained otherwise than 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
- A61L27/12—Phosphorus-containing materials, e.g. apatite
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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
- 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
- A61L27/56—Porous materials, e.g. foams or sponges
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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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- 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
- A61L2430/06—Materials or treatment for tissue regeneration for cartilage reconstruction, e.g. meniscus
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Abstract
A bone repairing biological ceramic material based on 3D printing is prepared from beta-tricalcium phosphate, hydroxyapatite and polylactic acid with the molecular weight being 100,000-120,000 and the viscosity being 0.79 dL/g-0.84 dL/g, and is of a three-dimensional grid structure with the porosity being 70%-90%, and the line diameter forming a grid is 100 micrometers to 300 micrometers. A preparation method comprises the steps that polylactic acid is dissolved in chloroform to prepare a solution with the mass concentration being 15-20%; beta-tricalcium phosphate and hydroxyapatite are added into the solution, and the mixture is stirred evenly and stably so that composite pulp can be obtained; the composite pulp is added into a 3D printing device to be printed, a precursor of the printed biological ceramic material is vacuumized so that chloroform can be fully volatized, and the product is obtained. The ceramic material is adjustable in degradation rate and good in mechanical performance and biocompatibility, can adapt to osteocyte and chondrocyte co-culture and composition of growth factors or micro-molecule polypeptides and can be used for simultaneous repairing of bones and cartilages.
Description
Technical field
The invention belongs to field of biomedical materials, be specifically related to the biology repaired for osteochondral defect printed based on 3D
Ceramic material, and relate to its preparation method.
Background technology
China causes numerous trauma fractures because of vehicle accident and work safety accident every year, adds bone tumor, ischemic femoral head
Property the orthopaedic disease such as downright bad, cause the Cranial defect case of more than 300 ten thousand.Clinically, due to autologous bone limited source, allograph bone
There is immunological rejection with bone-xenograft, and there is the defects such as potential transmission of pathogen danger, repair in the urgent need to research and development osseous tissue
Multiple material, is used for treating Cranial defect.Traditional timbering material and technology of preparing are difficult to high-volume and build different complicated bone
Repair materials, to meet the needs of individualized therapy clinically.The clinical bone tissue restoration timbering material needed to be applicable to not
With patient and different symptoms, its profile and microstructure because of people different because of disease.The clinical demand of this kind of individualized therapy
In the urgent need to having the timbering material of per-sonalization structures and performance.The rapid shapings such as 3 D-printing build the new technique of timbering material
Therefore obtain people more and more to pay close attention to.
Country's " " 12 " development plan guiding principle " is about accelerating to cultivate and clearly refer in the decision of development strategy new industry
Go out: accelerate research and development and the industrialization of the advanced biomedical engineering product such as armarium, medical material, promote large-scale development.
Medical apparatus and instruments and bio-medical material are developed and the attention of residing status in national economy by visible country.
Three-dimensional printing technology, is derived from rapid shaping (Rapid Prototyping, RP) technology, is rapidly to send out in the world today
One of manufacturing technology of exhibition.Rapid shaping is at computer-aided design and manufacturing technology, laser technology and material science and technology
Development, and with the combination of various forming techniques on the basis of occur a kind of new material processing technique, ultimate principle is
According to CAD, the modeling software such as UG, PROE carries out three-dimension modeling, and recycling Slice Software is cut into slices, and generates such as G generation
Code data, utilize laser, Numeric Control Technology accurately to be piled up by raw material, in the case of not having traditional moulds and fixture, quickly
Produce arbitrarily complicated shape and there is three-dimensional entity model or the part of certain function.Rapid shaping technique is applied to raw
The development of thing material is the inevitable outcome of material science and Developing Trends of Modern Manufacturing Technology, the appearance of rapid shaping technique, the most greatly
Shorten greatly the construction cycle of biomaterial, reduce R & D Cost, solve in clinical medicine invasive techniques in modern age one simultaneously
A science and technology difficult problem for the most great three-dimensional reconstruction.The particularly manufacture view at the artificial bone substitute of complicated shape is more aobvious
Its unique advantage is shown.Rapid shaping technique quickly accurate feature and develop into organizational structure personalization processing and provide
One good approach, can produce according to the requirement that patient is personalized and be applicable to the repairing of its particular/special requirement or transplant artificial limb,
Rapid shaping biomaterial manufacture is the result of material supply section subject and advanced manufacturing technology subject crossing, is also up-to-date technology progress
Inevitable outcome.
Summary of the invention
It is an object of the invention to provide a kind of Bone Defect Repari bioceramic material printed based on 3D and preparation method.This Bone Defect Repari
Bioceramic material degradation speed is adjustable, good biocompatibility, and adapts to bone chondrocyte co-cultivation and somatomedin
Or micromolecule polypeptide is compound, the repairing transplant of bone and cartilage can be carried out.
In the present invention, polylactic acid is abbreviated as PLA by some places, and nano-grade hydroxy apatite is abbreviated as nano-HA, β-phosphoric acid
DFP is abbreviated as β-TCP, and chloroform is abbreviated as CHCl3。
It is an object of the invention to be realized by below scheme:
A kind of Bone Defect Repari bioceramic material printed based on 3D, this bioceramic material is by bata-tricalcium phosphate, hydroxy-apatite
The polylactic acid that stone and molecular weight are 100,000-12 ten thousand, viscosity is 0.79dL/g-0.84dL/g is made, this bioceramic material
Structure be porosity be the three-dimensional mesh structure of 70%-90%, constitute grid line footpath be 100 μm-300 μm.
In the above-mentioned Bone Defect Repari bioceramic material printed based on 3D, it is preferable that described bata-tricalcium phosphate and hydroxyl phosphorus
The mass ratio of lime stone is 1:3-3:1, and in described bioceramic material, the weight/mass percentage composition of polylactic acid is 10%-90%.
In the above-mentioned Bone Defect Repari bioceramic material printed based on 3D, it is preferable that the granularity of described bata-tricalcium phosphate is little
In or equal to 12 μm, the granularity of described hydroxyapatite is less than or equal to 100nm.
The preparation method of above-mentioned Bone Defect Repari bioceramic material, this preparation method includes:
Polylactic acid is dissolved in chloroform and is configured to the solution that mass concentration is 15%-20%；
Joining in described solution by bata-tricalcium phosphate, hydroxyapatite, stirring to stable homogeneous prepares composite mortar；
Described composite mortar is added in the needle tubing of 3D printing device, parameter and the program of 3D printing device is set, print,
Obtaining the presoma of described bioceramic material, this presoma is placed in vacuum drying oven, evacuation makes chloroform fully volatilize,
Obtain described bioceramic material.
In the preparation method of above-mentioned Bone Defect Repari bioceramic material, it is preferable that described bata-tricalcium phosphate is by the following method
Prepare: first with Ca (OH)2And H3PO4For the former powder of Material synthesis beta-calcium phosphate, then former for this beta-calcium phosphate powder is passed through
800 DEG C of high-temperature roastings obtain beta-calcium phosphate powder body.
In the preparation method of above-mentioned Bone Defect Repari bioceramic material, it is preferable that also included before printing step compound
Slurry carries out the step being aged.
In the preparation method of above-mentioned Bone Defect Repari bioceramic material, it is preferable that the parameter arranging 3D printing device includes:
Work input air pressure 480KPa-580KPa is set, exports at 10-100psi according to air pressure during extruded velocity control work.
In the preparation method of above-mentioned Bone Defect Repari bioceramic material, it is preferable that described bata-tricalcium phosphate and hydroxy-apatite
The mass ratio of stone is 1:3-3:1, and in described bioceramic material, the weight/mass percentage composition of polylactic acid is 10%-90%.
In the preparation method of above-mentioned Bone Defect Repari bioceramic material, it is preferable that the granularity of described bata-tricalcium phosphate is less than
Or equal to 12 μm, the granularity of described hydroxyapatite is less than or equal to 100nm.
In the preparation method of above-mentioned Bone Defect Repari bioceramic material, it is preferable that described composite mortar is extruded at normal temperatures
Type.
Bone Defect Repari bioceramic material of the present invention two kinds of inorganic material bata-tricalcium phosphates and hydroxyapatite and the organic material of one
Material PLA is composited, and can regulate prepared bioceramic material by the ratio of regulation bata-tricalcium phosphate and hydroxyapatite
The degradation speed of material, PLA does not have cytotoxicity simultaneously, can improve the biology of prepared bioceramic material after crosslinking
The compatibility, the bioceramic material good mechanical properties prepared in addition.I.e. achieve advantage by the compound of three kinds of specified raw materials
Complementation, in conjunction with the architectural feature of institute's prepared material, cultivates for cell and somatomedin provides bionical biotic environment, energy
Adapt to the compound of bone chondrocyte co-cultivation and somatomedin or micromolecule polypeptide, can be used for osseocartilaginous repairing simultaneously.
Accompanying drawing explanation
Fig. 1 is the picture of the timbering material that embodiment 1 prepares.
Detailed description of the invention
Below by way of instantiation, the present invention will be further described.
Embodiment 1:
Taking 1.26gPLA, put in beaker, add stirrer, (analytical pure, Hengyang City is triumphant to suck CHCl3 with glue head dropper
Letter chemical reagent company limited) dropwise it is added drop-wise in beaker, instill 7.13g and stop, with sealed membrane, beaker bottle sealing being lived,
Then it is placed on agitator to stir to PLA and all dissolves, and adjust rotating speed solution bubble-free is produced, be configured to 15wt%
Clear solution A.Weighing 1.47g β-TCP and nano-HA the most respectively, join in solution A, stirring 1h is to homogeneous
Stable, obtain slurry B, slurry B is filled in pre-prepd needle tubing (EFD), with the rear end of ParafilmTM needle tubing
With the mouth of front end, still aging 24h, obtain slurry C.The high accuracy air-flotation type of pre-adjusted three-dimensional fine direct write motion
Automatically three-dimensional movement platform ABL10150 (Aerotech, U.S.A.), controls intelligence extrusion system EFD UltraTM2400 work
Making input air pressure 480KPa-580KPa, treat that after stably, air pressure is 550KPa, the air pressure output of operation controls
10-100psi, regulates and controls according to extruded velocity.Extrusion platform places frosted glass plate, in order to support product.
Using G code coding, set printing path, print 5 layers of 10mmx10mm, height is the porous of 0.75mm
Timbering material (presoma of bioceramic material), is positioned over vacuum drying oven, evacuation by obtained timbering material
(10-1Pa), the sheet glass of support is then sloughed.Chloroform is fully volatilized, obtains the timbering material (bioceramic being dried
Material), in timbering material, the content of PLA is 30wt%.
The timbering material that embodiment 1 prepares is as it is shown in figure 1, its structure is three-dimensional mesh structure.Optical microphotograph Microscopic observation,
Timbering material UNICOM is good, and stent diameter (constituting the line footpath of grid) is 150 μm.Observe under scanning electron microscope,
Frame material surface topography is coarse, and hydrometer method records its porosity and reaches 90%, is adapted to attachment and the somatomedin of osteocyte
With being combined of micromolecule polypeptide.
Embodiment 2:
Take 1.43gPLA, put in beaker, add stirrer, suck CHCl3 with glue head dropper and be dropwise added drop-wise in beaker,
Instill 8.10g to stop, with sealed membrane, beaker bottle sealing being lived, be then placed on agitator to stir to PLA and all dissolve,
And adjustment rotating speed makes solution bubble-free produce, it is configured to the clear solution A of 15wt%.Weigh 2.86g β-TCP the most respectively
And nano-HA, join in solution A, 1h is to stable homogeneous in stirring, obtains slurry B, is filled into by slurry B accurate in advance
In standby needle tubing (EFD), with rear end and the mouth of front end of ParafilmTM needle tubing, still aging 24h, obtain slurry C.
Automatic three-dimensional movement platform ABL10150 of high accuracy air-flotation type of pre-adjusted three-dimensional fine direct write motion
(Aerotech, U.S.A.), controls intelligence extrusion system EFD UltraTM2400 work input air pressure 480KPa-580KPa,
Treating that after stably, air pressure is 550KPa, the air pressure output of operation controls at 10-100psi, regulates and controls according to extruded velocity.
Extrusion platform places frosted glass plate, in order to support product.
Using G code coding, set printing path, it is 10 layers that printing obtains the number of plies, a diameter of 100 μm of support,
Initial diameter is 2.5mm, and maximum gauge is 10mm, spacing be the bottom surface of 0.5mm be circular timbering material (bioceramic material
The presoma of material), obtained timbering material is positioned over vacuum drying oven, evacuation (10-1Pa), then slough support
Sheet glass.Chloroform is fully volatilized, obtains the timbering material (bioceramic material) being dried, PLA in timbering material
Content be 20wt%.
Optical microphotograph Microscopic observation, timbering material UNICOM is good, and stent diameter is 100 μm.Observe under scanning electron microscope,
Timbering material surface topography is coarse, and hydrometer method records its porosity 85%, be adapted to the attachment of osteocyte and growth because of
Son is compound with micromolecule polypeptide.
Embodiment 3:
Take 1gPLA, put in beaker, add stirrer, suck CHCl with glue head dropper3Dropwise it is added drop-wise in beaker, instills
9g stops, and is lived by beaker bottle sealing with sealed membrane, is then placed on agitator to stir to PLA and all dissolves, and adjusts and turn
Speed makes solution bubble-free produce, and is configured to the clear solution A of 10wt%.Weigh 4.5g β-TCP and nano-HA the most respectively,
Joining in solution A, 1h is to stable homogeneous in stirring, obtains slurry B, slurry B is filled into pre-prepd needle tubing (EFD)
In, with rear end and the mouth of front end of ParafilmTM needle tubing, still aging 24h, obtain slurry C.Pre-adjusted three-dimensional
Automatic three-dimensional movement platform ABL10150 of the high accuracy air-flotation type (Aerotech, U.S.A.) of fine direct write motion, controls intelligence
Extrusion system EFD UltraTM2400 works input air pressure 480KPa-580KPa, treats that after stably, air pressure is 550KPa, work
Air pressure output when making controls at 10-100psi, regulates and controls according to extruded velocity.Frosted glass plate placed by extrusion platform,
In order to support product.
Using G code coding, set printing path, print 5 layers of 10mmx10mm, height is the porous of 0.75mm
Timbering material (presoma of bioceramic material), is positioned over vacuum drying oven, evacuation by obtained timbering material
(10-1Pa), the sheet glass of support is then sloughed.Chloroform is fully volatilized, obtains the timbering material (bioceramic being dried
Material), in timbering material PLA be content be 10wt%.
Optical microphotograph Microscopic observation, timbering material UNICOM is good, and stent diameter is 150 μm.Observe under scanning electron microscope,
Timbering material surface topography is coarse, and hydrometer method records its porosity 80%, be adapted to the attachment of osteocyte and growth because of
Son is compound with micromolecule polypeptide.
In above-described embodiment 1-3, the molecular weight of raw material PLA is 1.2 × 105, viscosity be 0.84dl/g, raw material β-TCP
Granularity be≤12 μm, the particle mean size of raw material nano-HA is 100nm, the mass ratio of raw material β-TCP and nano-HA
For 1:1.The experiment proved that, the ratio of regulation β-TCP and nano-HA can regulate the degraded of prepared bioceramic material
Speed, when the mass ratio of raw material β-TCP and nano-HA increases, the degradation speed of prepared bioceramic material reduces,
Otherwise, when the mass ratio of raw material β-TCP and nano-HA increases, the degradation speed of prepared bioceramic material increases.
Claims (10)
1. the Bone Defect Repari bioceramic material printed based on 3D, it is characterised in that: this bioceramic material is by β-phosphoric acid
The polylactic acid that DFP, hydroxyapatite and molecular weight are 100,000-12 ten thousand, viscosity is 0.79dL/g-0.84dL/g is made, should
The structure of bioceramic material be porosity be the three-dimensional mesh structure of 70%-90%, constitute grid line footpath be 100 μ
m-300μm。
2. the Bone Defect Repari bioceramic material printed based on 3D as claimed in claim 1, it is characterised in that: described β-
The mass ratio of tricalcium phosphate and hydroxyapatite is 1:3-3:1, the weight/mass percentage composition of polylactic acid in described bioceramic material
For 10%-90%.
3. the Bone Defect Repari bioceramic material printed based on 3D as claimed in claim 1, it is characterised in that: described β-
The granularity of tricalcium phosphate is less than or equal to 12 μm, and the granularity of described hydroxyapatite is less than or equal to 100nm.
4. the preparation method of Bone Defect Repari bioceramic material described in claim 1, it is characterised in that this preparation method includes:
Polylactic acid is dissolved in chloroform and is configured to the solution that mass concentration is 15%-20%；
Joining in described solution by bata-tricalcium phosphate, hydroxyapatite, stirring to stable homogeneous prepares composite mortar；
Described composite mortar is added in the needle tubing of 3D printing device, parameter and the program of 3D printing device is set, print,
Obtaining the presoma of described bioceramic material, this presoma is placed in vacuum drying oven, evacuation makes chloroform fully volatilize,
Obtain described bioceramic material.
5. the preparation method of Bone Defect Repari bioceramic material as claimed in claim 4, it is characterised in that described β-phosphoric acid
DFP prepares by the following method: first with Ca (OH)2And H3PO4For the former powder of Material synthesis beta-calcium phosphate, then by this β-
The former powder of calcium phosphate obtains beta-calcium phosphate powder body through 800 DEG C of high-temperature roastings.
6. the preparation method of Bone Defect Repari bioceramic material as claimed in claim 4, it is characterised in that: printing step it
Before also include step that composite mortar is aged.
7. the preparation method of Bone Defect Repari bioceramic material as claimed in claim 4, it is characterised in that 3D is set and prints
The parameter of equipment includes: arrange work input air pressure 480KPa-580KPa, defeated according to air pressure during extruded velocity control work
Go out at 10-100psi.
8. the preparation method of Bone Defect Repari bioceramic material as claimed in claim 4, it is characterised in that: described β-phosphoric acid
The mass ratio of DFP and hydroxyapatite is 1:3-3:1, and in described bioceramic material, the weight/mass percentage composition of polylactic acid is
10%-90%.
9. the preparation method of Bone Defect Repari bioceramic material as claimed in claim 4, it is characterised in that: described β-phosphoric acid
The granularity of DFP is less than or equal to 12 μm, and the granularity of described hydroxyapatite is less than or equal to 100nm.
10. the preparation method of Bone Defect Repari bioceramic material as claimed in claim 4, it is characterised in that: described composite pulp
Expect extrusion molding at normal temperatures.
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| CN106496977A (en) * | 2016-10-19 | 2017-03-15 | 深圳市艾科赛龙科技股份有限公司 | A kind of 3D printing poly-lactic acid material and preparation method thereof, Method of printing |
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