CN106390190A - Process for manufacturing alpha-tricalcium phosphate-alpha-calcium sulfate hemihydrates bone cement porous bracket through squashing method - Google Patents
Process for manufacturing alpha-tricalcium phosphate-alpha-calcium sulfate hemihydrates bone cement porous bracket through squashing method Download PDFInfo
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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
- A61L27/02—Inorganic materials
- A61L27/025—Other specific inorganic materials not covered by A61L27/04 - A61L27/12
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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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Abstract
The invention relates to a process for manufacturing an alpha-tricalcium phosphate-alpha-calcium sulfate hemihydrates bone cement porous bracket through a squashing method. The process comprises the following steps: mixing raw materials calcium hydrophosphate and calcium carbonate in molar ratio through a solid-solid reaction process, roasting the raw materials at a temperature ranging from 1250 DEG C to 1400 DEG C, and quickly cooling the raw materials to the room temperature, preparing alpha-TCP powder; putting calcium sulphate dehydrate into distilled water, adding sodium citrate and magnesium sulfate, heating reactants in certain proportion in a sealed container to 130 DEG C, reacting for 6 hours, filtering and drying to prepare alpha-CSH powder; and mixing alpha-TCP and alpha-CSH powder in a mass ratio from (9 to 1) to (5 to 5), taking soluble salt particles or sugar particles with particle diameter being 100 to 300mu m as a pore-foaming agent, sufficiently mixing powder, pressing and forming by use of a tablet press through a proper mould, soaking in 37DEG C water bath, removing the pore-foaming agent during curing, thereby preparing the bone cement porous bracket. According to the process, adopted raw materials are simple and the preparation process is easy, so that the process is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of method of biology medical material technical field, specifically a kind of α-TCP [type alpha tricalcium phosphate]
The preparation method of the bone cement porous support compound with α-CSH [α-half-H 2 O calcium sulphate], blend alpha-TCP, α-CSH powder and suitable
When filling porogen such as solubility salt grain, the sugared grain of ratio, by above-mentioned powder tablet machine in suitable mould compressing after
It is placed directly within solidification in water, dissolve porogen simultaneously, prepare the bone cement porous support that α-TCP and α-CSH is combined.
Background technology
Calcium phosphate bone cement possesses good biocompatibility and osteoinductive due to it, in artificial bone renovating material neck
Domain is widely used.During repairing bone injury, calcium phosphate bone cement has certain biology in vivo
Degradability, the calcium of material degradation release, P elements can furnish ample material for bone growth, are finally reached area of new bone and replace completely
Process for artificial bone.But clinical discovery, the degradation rate of calcium phosphate bone cement is excessively slow, usually with new bone growth speed not
Coupling, extends the healing time of bone trauma position on the contrary.Calcium sulfate bone class bone cement is also a kind of degradable artificial Bone Defect Repari
Material, possesses good biocompatibility and bone conductibility.Research shows, because α-CSH bone cement degradation in vivo is very fast,
With α-TCP compound use, the biological degradability of bone cement can be made to possess certain controllability, make the degradation speed of material and new bone life
Long speed more mate [Mao K, Cui F, Li J, et al, Journal of Biomaterials Applications,
2012].
As implantation class bone renovating material, the porous of bone cement can increase the surface area of material, on the one hand can be cell
Adhesion provides bigger area, contributes to cell adhesion, and allow vascular tissue's growth [Yao Jun, et al,
Biomaterials, 2005], be on the other hand conducive to material and body fluid to be fully contacted, accelerate the degraded of material.Traditional salt
Analysis method step is complicated, generally powder is shaped with porogen mixing post-reinforcing liquid, then leaches porogen, process is slow during pore
And pore uniform level not high it is impossible to batch production.
Content of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of α-TCP/ α-CSH Composite Bone with pressed disc method preparation
Cement porous support, possesses good porous and mechanical property, simultaneously preparation method is simple, is suitable for batch production.The present invention
Purpose be to provide a kind of preparation method of α-TCP/ α-CSH composite bone cement porous support so as to possess excellent performance
While, enormously simplify preparation process, suitable expanding production.
Pressed disc method prepares type alpha tricalcium phosphate/α-half-H 2 O calcium sulphate bone cement porous support it is characterised in that comprising following step
Suddenly：
（1）Using solid reaction process by raw material calcium hydrogen phosphate and Calcium Carbonate in molar ratio 2:After 1 is sufficiently mixed, in 1250-1400
DEG C calcining 2-4h be rapidly cooled to room temperature, prepares α-TCP powder, product is through wet ball grinding control particle diameter at 2-4 μm；By two water
Calcium sulfate 50g is placed in 150mL distilled water, adds sodium citrate 0.225g and magnesium sulfate 3g, the reactant of above ratio is close
Close vessel in heating heat filtering to 130 DEG C of reaction 6h and preparation α-CSH powder is dried；
（2）Above-mentioned α-TCP, α-CSH powder in mass ratio 9:1 to 5:5 mixing, with particle diameter for 100-300 μm of solubility salt grain or
Sugared grain is porogen, after powder is sufficiently mixed, compressing by suitable mould using tablet machine, in 37 DEG C of water-baths
Soak, remove porogen while solidification, prepare bone cement porous support.
Step（1）The raw material hybrid mode of described solid reaction process is the wet ball grinding for medium using dehydrated alcohol,
Rotating speed is 450rpm, and Ball-milling Time is 1-4h, and ratio of grinding media to material is mass ratio 3:1.
Step（2）The acquisition pattern of described salt grain or sugared grain is using mortar grinder or dry ball milling grinding and sieving,
Obtain the granule that particle diameter is 100-300 μm.
Step（2）The mixed proportion of described porogen is mass fraction 50-80%, and hybrid mode is dry ball milling.
Step（2）Described mould be diameter 6-10mm cylindrical die, in 37 DEG C of water-baths soak time be 24h with
On.
The purpose of the present invention is achieved through the following technical solutions：Mol ratio is 2:1 calcium hydrogen phosphate and Paris white
End is sufficiently mixed；Using solid reaction process, control reaction condition, prepare as α-TCP powder；By sulfate dihydrate calcium powder
It is scattered in pure water, add sodium citrate and magnesium sulfate as crystal modifier, reaction obtains α-CSH powder；Grind and sieve and obtain
The salt particle of size 100-300 μm or sugared granule, are sufficiently mixed in proportion and prepare bone water with α-TCP and α-CSH powder
Mud powder；Using tablet machine, above-mentioned powder is pressed into required form by particular mold, the demoulding is taken out and obtained artificial osseous granuleses；
This osseous granules is placed in pure water so as to abundant solidify, during being somebody's turn to do, filling porogen separates out completely simultaneously, is placed in 60 after taking-up
It is dried in DEG C baking oven, prepare α-TCP/ α-CSH composite bone cement porous support.
The present invention comprises the following steps：
1st, calcium hydrogen phosphate is mixed homogeneously with Calcium Carbonate, it is mol ratio 2:1.Described hybrid mode is the use of dehydrated alcohol to be mixed
Close the ball milling mixing of medium, rotating speed 450rpm, Ball-milling Time is 1-4h, mixed suspension removes ethanol by rotary evaporation
After put in 60 DEG C of baking ovens be dried.
2nd, dried calcium hydrogen phosphate and calcium carbonate mixture are calcined after 2-4h in 1250-1400 DEG C of stove and take out,
Rapidly cool down under air blast environment, obtain α-TCP powder, obtain the α-TCP powder of uniform particle diameter afterwards using the mode of wet ball grinding
End, its particle size range is at 2-4 μm.
3rd, calcium sulphate dihydrate 50g is placed in 150mL distilled water, adds sodium citrate 0.225g and magnesium sulfate 3g, close
Close vessel in heating to 130 DEG C of reaction 6h, after reaction terminates, rapid is fallen steam, mixed liquor is carried out heat filtering, is placed in 130
It is dried in DEG C baking oven, prepare α-CSH powder.
4th, sieve after crude salt grain or sugared grain grinding, screen out granule in 100-300 μ m for the size.Described grind
Mill mode can be using mortar grinder or dry ball milling.
5th, α-TCP, α-CSH, filler powder are mixed in proportion, the mass ratio of wherein α-TCP and α-CSH is 9:1
To 5:Between 5, the total mass ratio shared by implant is 50%-80%.Described hybrid mode is dry ball milling.
6th, using tablet machine, above-mentioned powder is pressed into required form by mould, the demoulding is taken out and obtained artificial osseous granuleses.
Described mould can be the cylinder of diameter 6-10mm.
7th, gained osseous granuleses are put in 37 DEG C of water-baths so as to abundant solidification removes filling porogen simultaneously, take out rearmounted
It is dried in 60 DEG C of baking ovens, prepare α-TCP/ α-CSH composite bone cement porous support.
It is an advantage of the current invention that：
1st, use α-CSH adjust α-TCP bone cement degradation cycle, porous support is prepared using pressed disc method simultaneously so as to
Degradation rate is more mated with new bone growth speed, and then promotes the healing of osseous tissue.
2nd, preparation method is simple, decreases the preparation of bone cement solidify liquid, raw materials used simple, is suitable to produce in a large number.
Brief description
Fig. 1, Fig. 2 are the SEM electron-microscope scanning results of bone cement porous support prepared by this technology, and pore size is 50-
300nm, microcosmic result display α-TCP, α-CSH have obtained good growth by the crystallization of sufficient hydration reaction.
Specific embodiment
Following examples are implemented premised on inventive technique scheme, give detailed embodiment and specific behaviour
Make process, but protection scope of the present invention is not limited to following embodiments.
Embodiment 1：
（1）Prepared by α-TCP powder：
In molar ratio 2:1 weighs Dicalcium Phosphate and calcium carbonate powder, the use of appropriate dehydrated alcohol is medium wet ball grinding, turns
Fast 400rpm, Ball-milling Time 4h, ball milling pearl and powder quality are than for 3:1.Raw material mixed liquor removes ethanol by rotary evaporation, puts
24h is dried in 60 DEG C of baking ovens.Dried powder is placed in Muffle furnace, takes out, in air blast environment after 1400 DEG C of calcining 2h
Under rapidly cool down.By the powder after cooling with dehydrated alcohol for medium wet ball grinding, rotating speed 400rpm, Ball-milling Time is 6h, ball
Mill pearl and powder quality ratio is for 4:1.Powder suspension is placed in fully dry in 80 DEG C of baking ovens, prepares α-TCP powder.
（2）Prepared by α-CSH：
Calcium sulphate dihydrate 50g is placed in 150mL distilled water, adds sodium citrate 0.225g and magnesium sulfate 3g, in hermetic container
In be heated to 130 DEG C of reaction 6h, after reaction terminates, rapid send out steam, mixed liquor is carried out heat filtering, is placed in 130 DEG C of baking ovens
Middle drying, prepares α-CSH powder.
Embodiment 2：
α-TCP prepared by embodiment 1, α-CSH powder in mass ratio 7:3 mixing, then press for 100-300 μm of salt grain with particle diameter
Mass ratio 5：5 mixing, obtain bone cement powder, above-mentioned powder are placed in the cylindrical die of a diameter of 6mm, using tablet machine
Fully it is compacted, be placed in 37 DEG C of water-baths after the demoulding and soak 24h removing salt grain, obtain bone cement porous support.Its SEM electron-microscope scanning is tied
As shown in Figure 1 and Figure 2, record its porosity is 46% to fruit, comprcssive strength 10MPa.
Embodiment 3;
α-TCP prepared by embodiment 1, α-CSH powder in mass ratio 7:3 mixing, then press for 100-300 μm of salt grain with particle diameter
Mass ratio 3:7 mixing, obtain bone cement powder, above-mentioned powder are placed in the cylindrical die of a diameter of 6mm, using tablet machine
Fully it is compacted, be placed in 37 DEG C of water-baths after the demoulding and soak 24h removing salt grain, obtain bone cement porous support.Recording its porosity is
83%, comprcssive strength 5MPa.
Claims (5)
1. pressed disc method prepares type alpha tricalcium phosphate/α-half-H 2 O calcium sulphate bone cement porous support it is characterised in that comprising following step
Suddenly：
（1）Using solid reaction process by raw material calcium hydrogen phosphate and Calcium Carbonate in molar ratio 2:After 1 is sufficiently mixed, in 1250-1400
DEG C calcining 2-4h be rapidly cooled to room temperature, prepares α-TCP powder, product is through wet ball grinding control particle diameter at 2-4 μm；By two water
Calcium sulfate 50g is placed in 150mL distilled water, adds sodium citrate 0.225g and magnesium sulfate 3g, the reactant of above ratio is close
Close vessel in heating heat filtering to 130 DEG C of reaction 6h and preparation α-CSH powder is dried；
（2）Above-mentioned α-TCP, α-CSH powder in mass ratio 9:1 to 5:5 mixing, with particle diameter for 100-300 μm of solubility salt grain or
Sugared grain is porogen, after powder is sufficiently mixed, compressing by suitable mould using tablet machine, in 37 DEG C of water-baths
Soak, remove porogen while solidification, prepare bone cement porous support.
2. pressed disc method prepares type alpha tricalcium phosphate/α-half-H 2 O calcium sulphate bone cement porous support, its feature according to claim 1
It is, step（1）The raw material hybrid mode of described solid reaction process is the wet ball grinding for medium, rotating speed using dehydrated alcohol
For 450rpm, Ball-milling Time is 1-4h, and ratio of grinding media to material is mass ratio 3:1.
3. pressed disc method prepares type alpha tricalcium phosphate/α-half-H 2 O calcium sulphate bone cement porous support, its feature according to claim 1
It is, step（2）The acquisition pattern of described salt grain or sugared grain is using mortar grinder or dry ball milling grinding and sieving, obtains
Particle diameter is 100-300 μm of granule.
4. pressed disc method prepares type alpha tricalcium phosphate/α-half-H 2 O calcium sulphate bone cement porous support, its feature according to claim 1
It is, step（2）The mixed proportion of described porogen is mass fraction 50-80%, and hybrid mode is dry ball milling.
5. pressed disc method prepares type alpha tricalcium phosphate/α-half-H 2 O calcium sulphate bone cement porous support, its feature according to claim 1
It is, step（2）Described mould is the cylindrical die of diameter 6-10mm, and in 37 DEG C of water-baths, soak time is more than 24h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107715171A (en) * | 2017-10-31 | 2018-02-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of medicine controlled releasing injectable type bone cement of fast degradation and products thereof and application |
| CN107970489A (en) * | 2017-11-29 | 2018-05-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Carry preparation method of injectable type bone cement of medicine organic phosphoric acid modified zirconia and products thereof and application |
| CN109331222A (en) * | 2018-09-21 | 2019-02-15 | 夏炜 | Bone renovating material and its preparation and the application of 3D porous support can be formed in situ |
| WO2019153794A1 (en) * | 2018-02-09 | 2019-08-15 | 华南理工大学 | Hollow porous spherical particle artificial bone, preparation method therefor and use thereof |
| CN110170073A (en) * | 2019-05-17 | 2019-08-27 | 江苏澳盛复合材料科技有限公司 | The preparation method and artifical bone's material of artifical bone's material |
| CN111790004A (en) * | 2020-06-17 | 2020-10-20 | 天津市康婷生物工程集团有限公司 | Preparation method of universal drug-loaded calcium-phosphorus cement porous scaffold |
| TWI767467B (en) * | 2020-12-22 | 2022-06-11 | 財團法人石材暨資源產業研究發展中心 | 3D Printed Compositions and Bone Implants |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107715171A (en) * | 2017-10-31 | 2018-02-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of medicine controlled releasing injectable type bone cement of fast degradation and products thereof and application |
| CN107970489A (en) * | 2017-11-29 | 2018-05-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Carry preparation method of injectable type bone cement of medicine organic phosphoric acid modified zirconia and products thereof and application |
| WO2019153794A1 (en) * | 2018-02-09 | 2019-08-15 | 华南理工大学 | Hollow porous spherical particle artificial bone, preparation method therefor and use thereof |
| US11077225B2 (en) | 2018-02-09 | 2021-08-03 | South China University Of Technology | Hollow porous spherical particle artificial bone as well as preparation method and application thereof |
| CN109331222A (en) * | 2018-09-21 | 2019-02-15 | 夏炜 | Bone renovating material and its preparation and the application of 3D porous support can be formed in situ |
| CN110170073A (en) * | 2019-05-17 | 2019-08-27 | 江苏澳盛复合材料科技有限公司 | The preparation method and artifical bone's material of artifical bone's material |
| CN110170073B (en) * | 2019-05-17 | 2022-05-06 | 江苏澳盛复合材料科技有限公司 | Method for producing material for artificial bone and material for artificial bone |
| CN111790004A (en) * | 2020-06-17 | 2020-10-20 | 天津市康婷生物工程集团有限公司 | Preparation method of universal drug-loaded calcium-phosphorus cement porous scaffold |
| TWI767467B (en) * | 2020-12-22 | 2022-06-11 | 財團法人石材暨資源產業研究發展中心 | 3D Printed Compositions and Bone Implants |
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