CN107382304A - A kind of Medical Compound Bioceramics material and preparation method thereof - Google Patents
A kind of Medical Compound Bioceramics material and preparation method thereof Download PDFInfo
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- CN107382304A CN107382304A CN201710650144.5A CN201710650144A CN107382304A CN 107382304 A CN107382304 A CN 107382304A CN 201710650144 A CN201710650144 A CN 201710650144A CN 107382304 A CN107382304 A CN 107382304A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/447—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on phosphates, e.g. hydroxyapatite
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
- C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
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Abstract
The invention provides a kind of Medical Compound Bioceramics material and preparation method thereof.Preparation method is as follows：（1）By hydroxyapatite, tricalcium phosphate, zirconium dioxide, sodium metasilicate, flaxseed gum, carboxymethyl chitosan and distilled water mixing and ball milling；（2）Glycolylurea epoxide resin and 3,3' diaminourea di-n-propylamine are added, is stirred 56 hours under the 200r/min of rotating speed 100；（3）Lecithin, silicone emulsion, polyoxypropylene ethylene oxide glycerin ether and polyethylene glycol are added, is put into after stirring in vacuum drying chamber and vacuumizes carry out defoaming treatment；（4）Green compact must be freezed by pouring into freezing apparatus for pouring；（5）It is put into sinter in sintering furnace after being freeze-dried and produces.The Medical Compound Bioceramics material of the present invention has good mechanical property, while has extraordinary biocompatibility again.
Description
Technical field
The present invention relates to biomedical materials field, and in particular to a kind of Medical Compound Bioceramics material and its preparation side
Method.
Background technology
With the development of material science, biomaterial is due to the spy for being repaired, being substituted and being regenerated to body tissue
Distinguished service energy, it has also become the important component in current biomedical engineering.Its research contents be related to material, medical physicses,
The subjects such as biochemistry and Modern High-Tech field.And bioceramic material is as a kind of lithotroph medical material, with
Biological tissue has good compatibility and excellent compatibility, the physicochemical properties stablized, can be sterilising and non-toxic etc.
Advantage, increasingly it is valued by people.It refers to be used as specific biology or a kind of ceramic material of physiological function, i.e., direct
Ceramic material for human body or biological, the medical, biochemistry related to human body etc..And it is the power for improving bioceramic material
The performances such as performance, stability and biocompatibility are learned, bioceramic material and other materials progress is compound, it is excellent so as to protrude its
Gesture, expand it and be applied to the focus developed for numerous enterprises and scholar's research.
The content of the invention
Technical problems to be solved：It is an object of the invention to provide a kind of Medical Compound Bioceramics material, has fine
Mechanical property, while there is extraordinary biocompatibility again.
Technical scheme：A kind of Medical Compound Bioceramics material, it is prepared by following component with parts by weight：Hydroxy-apatite
Stone 20-30 parts, tricalcium phosphate 10-20 parts, sodium metasilicate 1-2 parts, flaxseed gum 1-2 parts, glycolylurea epoxide resin 1-3 parts, titanium dioxide
Zirconium 0.5-1 parts, lecithin 1-2 parts, silicone emulsion 1-2 parts, polyoxypropylene ethylene oxide glycerin ether 1-2 parts, 3,3'- diaminourea two
Propylamine 1-3 parts, carboxymethyl chitosan 0.2-0.4 parts, polyethylene glycol 2-5 parts, distilled water 80-150 parts.
It is further preferred that a kind of described Medical Compound Bioceramics material, by following component with prepared by parts by weight and
Into：Hydroxyapatite 22-28 parts, tricalcium phosphate 12-17 parts, sodium metasilicate 1.2-1.8 parts, flaxseed gum 1.3-1.7 parts, glycolylurea ring
Oxygen tree fat 1.5-2.4 parts, zirconium dioxide 0.6-0.9 parts, lecithin 1.3-1.7 parts, silicone emulsion 1.2-1.8 parts, polyoxypropylene
It is ethylene oxide glycerin ether 1.2-1.7 parts, 3,3'- diaminourea di-n-propylamine 1.5-2.5 parts, carboxymethyl chitosan 0.25-0.35 parts, poly-
Ethylene glycol 3-4 parts, distilled water 100-130 parts.
The preparation method of above-mentioned Medical Compound Bioceramics material comprises the following steps：
（1）Hydroxyapatite, tricalcium phosphate, zirconium dioxide, sodium metasilicate, flaxseed gum, carboxymethyl chitosan and distilled water are mixed
Close, ball milling 24-30 hours are carried out in ball mill；
（2）Glycolylurea epoxide resin and 3,3'- diaminourea di-n-propylamine are added, 5-6 hours are stirred under rotating speed 100-200r/min；
（3）Lecithin, silicone emulsion, polyoxypropylene ethylene oxide glycerin ether and polyethylene glycol are added, after stirring 20-40 minutes
It is put into vacuum drying chamber and vacuumizes carry out defoaming treatment；
（4）Green compact must be freezed by pouring into freezing apparatus for pouring；
（5）It is put into after being freeze-dried in sintering furnace and carries out the sintering 3-4 hours at 550-650 DEG C of temperature and produce.
Further, step（1）Middle milling time is 26-28 hours.
Further, step（2）Middle rotating speed is 120-190r/min, and mixing time is 5.5 hours.
Further, step（5）Middle sintering temperature is 600 DEG C, and sintering time is 3.5 hours.
Beneficial effect：The present invention Medical Compound Bioceramics material there is good mechanical property, its compression strength and
Rupture strength highest respectively reaches 46.7MPa and 177MPa, while it has extraordinary biocompatibility, cytotoxicity again
Grade is only 0-1 levels.
Embodiment
Embodiment 1
A kind of Medical Compound Bioceramics material, it is prepared by following component with parts by weight：20 parts of hydroxyapatite, tricresyl phosphate
10 parts of calcium, 1 part of sodium metasilicate, 1 part of flaxseed gum, 1 part of glycolylurea epoxide resin, 0.5 part of zirconium dioxide, 1 part of lecithin, silicone emulsion
1 part, 1 part of polyoxypropylene ethylene oxide glycerin ether, 1 part of 3,3'- diaminourea di-n-propylamine, 0.2 part of carboxymethyl chitosan, polyethylene glycol
2 parts, 80 parts of distilled water.
The preparation method of above-mentioned Medical Compound Bioceramics material is：（1）By hydroxyapatite, tricalcium phosphate, titanium dioxide
Zirconium, sodium metasilicate, flaxseed gum, carboxymethyl chitosan and distilled water mix, and ball milling are carried out in ball mill 24 hours；（2）Add sea
Because of epoxy resin and 3,3'- diaminourea di-n-propylamines, stirred 5 hours under rotating speed 100r/min；（3）Add lecithin, emulsification silicon
Oil, polyoxypropylene ethylene oxide glycerin ether and polyethylene glycol, stirring is put into vacuumize in vacuum drying chamber after 20 minutes to be disappeared
Bubble processing；（4）Green compact must be freezed by pouring into freezing apparatus for pouring；（5）It is put into sintering furnace and is carried out in temperature after being freeze-dried
Sinter 3 hours and produce at 550 DEG C.
Embodiment 2
A kind of Medical Compound Bioceramics material, it is prepared by following component with parts by weight：22 parts of hydroxyapatite, tricresyl phosphate
12 parts of calcium, 1.2 parts of sodium metasilicate, 1.3 parts of flaxseed gum, 1.5 parts of glycolylurea epoxide resin, 0.6 part of zirconium dioxide, 1.3 parts of lecithin,
1.2 parts of silicone emulsion, 1.2 parts of polyoxypropylene ethylene oxide glycerin ether, 1.5 parts of 3,3'- diaminourea di-n-propylamine, carboxymethyl chitosan
0.25 part, 3 parts of polyethylene glycol, 100 parts of distilled water.
The preparation method of above-mentioned Medical Compound Bioceramics material is：（1）By hydroxyapatite, tricalcium phosphate, titanium dioxide
Zirconium, sodium metasilicate, flaxseed gum, carboxymethyl chitosan and distilled water mix, and ball milling are carried out in ball mill 26 hours；（2）Add sea
Because of epoxy resin and 3,3'- diaminourea di-n-propylamines, stirred 5.5 hours under rotating speed 120r/min；（3）Add lecithin, emulsification
Silicone oil, polyoxypropylene ethylene oxide glycerin ether and polyethylene glycol, stirring are put into vacuum drying chamber after 25 minutes and vacuumize progress
Defoaming treatment；（4）Green compact must be freezed by pouring into freezing apparatus for pouring；（5）It is put into sintering furnace and is carried out in temperature after being freeze-dried
Sinter 3.5 hours and produce at 600 DEG C of degree.
Embodiment 3
A kind of Medical Compound Bioceramics material, it is prepared by following component with parts by weight：25 parts of hydroxyapatite, tricresyl phosphate
15 parts of calcium, 1.5 parts of sodium metasilicate, 1.5 parts of flaxseed gum, 2 parts of glycolylurea epoxide resin, 0.75 part of zirconium dioxide, 1.5 parts of lecithin,
1.5 parts of silicone emulsion, 1.5 parts of polyoxypropylene ethylene oxide glycerin ether, 2 parts of 3,3'- diaminourea di-n-propylamine, carboxymethyl chitosan
0.3 part, 3.5 parts of polyethylene glycol, 115 parts of distilled water.
The preparation method of above-mentioned Medical Compound Bioceramics material is：（1）By hydroxyapatite, tricalcium phosphate, titanium dioxide
Zirconium, sodium metasilicate, flaxseed gum, carboxymethyl chitosan and distilled water mix, and ball milling are carried out in ball mill 27 hours；（2）Add sea
Because of epoxy resin and 3,3'- diaminourea di-n-propylamines, stirred 5.5 hours under rotating speed 150r/min；（3）Add lecithin, emulsification
Silicone oil, polyoxypropylene ethylene oxide glycerin ether and polyethylene glycol, stirring are put into vacuum drying chamber after 25 minutes and vacuumize progress
Defoaming treatment；（4）Green compact must be freezed by pouring into freezing apparatus for pouring；（5）It is put into sintering furnace and is carried out in temperature after being freeze-dried
Sinter 3.5 hours and produce at 600 DEG C of degree.
Embodiment 4
A kind of Medical Compound Bioceramics material, it is prepared by following component with parts by weight：28 parts of hydroxyapatite, tricresyl phosphate
17 parts of calcium, 1.8 parts of sodium metasilicate, 1.7 parts of flaxseed gum, 2.4 parts of glycolylurea epoxide resin, 0.9 part of zirconium dioxide, 1.7 parts of lecithin,
1.8 parts of silicone emulsion, 1.7 parts of polyoxypropylene ethylene oxide glycerin ether, 2.5 parts of 3,3'- diaminourea di-n-propylamine, carboxymethyl chitosan
0.35 part, 4 parts of polyethylene glycol, 130 parts of distilled water.
The preparation method of above-mentioned Medical Compound Bioceramics material is：（1）By hydroxyapatite, tricalcium phosphate, titanium dioxide
Zirconium, sodium metasilicate, flaxseed gum, carboxymethyl chitosan and distilled water mix, and ball milling are carried out in ball mill 28 hours；（2）Add sea
Because of epoxy resin and 3,3'- diaminourea di-n-propylamines, stirred 5.5 hours under rotating speed 190r/min；（3）Add lecithin, emulsification
Silicone oil, polyoxypropylene ethylene oxide glycerin ether and polyethylene glycol, stirring are put into vacuum drying chamber after 35 minutes and vacuumize progress
Defoaming treatment；（4）Green compact must be freezed by pouring into freezing apparatus for pouring；（5）It is put into sintering furnace and is carried out in temperature after being freeze-dried
Sinter 3.5 hours and produce at 600 DEG C of degree.
Embodiment 5
A kind of Medical Compound Bioceramics material, it is prepared by following component with parts by weight：30 parts of hydroxyapatite, tricresyl phosphate
20 parts of calcium, 2 parts of sodium metasilicate, 2 parts of flaxseed gum, 3 parts of glycolylurea epoxide resin, 1 part of zirconium dioxide, 2 parts of lecithin, silicone emulsion 2
Part, 2 parts of polyoxypropylene ethylene oxide glycerin ether, 3 parts of 3,3'- diaminourea di-n-propylamine, 0.4 part of carboxymethyl chitosan, polyethylene glycol 5
Part, 150 parts of distilled water.
The preparation method of above-mentioned Medical Compound Bioceramics material is：（1）By hydroxyapatite, tricalcium phosphate, titanium dioxide
Zirconium, sodium metasilicate, flaxseed gum, carboxymethyl chitosan and distilled water mix, and ball milling are carried out in ball mill 30 hours；（2）Add sea
Because of epoxy resin and 3,3'- diaminourea di-n-propylamines, stirred 6 hours under rotating speed 200r/min；（3）Add lecithin, emulsification silicon
Oil, polyoxypropylene ethylene oxide glycerin ether and polyethylene glycol, stirring is put into vacuumize in vacuum drying chamber after 40 minutes to be disappeared
Bubble processing；（4）Green compact must be freezed by pouring into freezing apparatus for pouring；（5）It is put into sintering furnace and is carried out in temperature after being freeze-dried
Sinter 4 hours and produce at 650 DEG C.
Comparative example 1
The present embodiment and the difference of embodiment 2 are not containing lecithin and silicone emulsion.Specifically：
A kind of Medical Compound Bioceramics material, it is prepared by following component with parts by weight：22 parts of hydroxyapatite, tricresyl phosphate
12 parts of calcium, 1.2 parts of sodium metasilicate, 1.3 parts of flaxseed gum, 1.5 parts of glycolylurea epoxide resin, 0.6 part of zirconium dioxide, polyoxypropylene oxidation
1.2 parts of Ethylene Glycol ether, 1.5 parts of 3,3'- diaminourea di-n-propylamine, 0.25 part of carboxymethyl chitosan, 3 parts of polyethylene glycol, distilled water
100 parts.
The preparation method of above-mentioned Medical Compound Bioceramics material is：（1）By hydroxyapatite, tricalcium phosphate, titanium dioxide
Zirconium, sodium metasilicate, flaxseed gum, carboxymethyl chitosan and distilled water mix, and ball milling are carried out in ball mill 26 hours；（2）Add sea
Because of epoxy resin and 3,3'- diaminourea di-n-propylamines, stirred 5.5 hours under rotating speed 120r/min；（3）Add polyoxypropylene oxidation
Ethylene Glycol ether and polyethylene glycol, stirring are put into vacuum drying chamber after 25 minutes and vacuumize carry out defoaming treatment；（4）Pour into cold
Green compact must be freezed by freezing apparatus for pouring；（5）It is put into sintering furnace that to carry out the sintering 3.5 at 600 DEG C of temperature small after being freeze-dried
When produce.
Rupture strength is determined using standard GB/T 6569-86.
Mtt assay detects cytotoxicity.
The partial properties index result table 1 below of Medical Compound Bioceramics material of the present invention, it will be seen that this material
With good mechanical property, its compression strength and rupture strength highest respectively reach 46.7MPa and 177MPa, while it is again
With extraordinary biocompatibility, cytotoxicity grade is only 0-1 levels.
The partial properties index of the Medical Compound Bioceramics material of table 1
| Name of product | Compression strength（MPa） | Rupture strength（MPa） | Cytotoxicity grade |
| Embodiment 1 | 46.3 | 174 | 0-1 |
| Embodiment 2 | 46.4 | 176 | 0-1 |
| Embodiment 3 | 46.6 | 177 | 0-1 |
| Embodiment 4 | 46.7 | 177 | 0-1 |
| Embodiment 5 | 46.6 | 176 | 0-1 |
| Comparative example 1 | 43.2 | 167 | 0-1 |
Claims (6)
- A kind of 1. Medical Compound Bioceramics material, it is characterised in that：It is prepared by following component with parts by weight：Hydroxy-apatite Stone 20-30 parts, tricalcium phosphate 10-20 parts, sodium metasilicate 1-2 parts, flaxseed gum 1-2 parts, glycolylurea epoxide resin 1-3 parts, titanium dioxide Zirconium 0.5-1 parts, lecithin 1-2 parts, silicone emulsion 1-2 parts, polyoxypropylene ethylene oxide glycerin ether 1-2 parts, 3,3'- diaminourea two Propylamine 1-3 parts, carboxymethyl chitosan 0.2-0.4 parts, polyethylene glycol 2-5 parts, distilled water 80-150 parts.
- A kind of 2. Medical Compound Bioceramics material according to claim 1, it is characterised in that：By following component with weight Part is prepared：Hydroxyapatite 22-28 parts, tricalcium phosphate 12-17 parts, sodium metasilicate 1.2-1.8 parts, flaxseed gum 1.3-1.7 Part, glycolylurea epoxide resin 1.5-2.4 parts, zirconium dioxide 0.6-0.9 parts, lecithin 1.3-1.7 parts, silicone emulsion 1.2-1.8 parts, Polyoxypropylene ethylene oxide glycerin ether 1.2-1.7 parts, 3,3'- diaminourea di-n-propylamine 1.5-2.5 parts, carboxymethyl chitosan 0.25- 0.35 part, polyethylene glycol 3-4 parts, distilled water 100-130 parts.
- A kind of 3. preparation method of Medical Compound Bioceramics material described in any one of claim 1 to 2, it is characterised in that： Comprise the following steps：（1）Hydroxyapatite, tricalcium phosphate, zirconium dioxide, sodium metasilicate, flaxseed gum, carboxymethyl chitosan and distilled water are mixed Close, ball milling 24-30 hours are carried out in ball mill；（2）Glycolylurea epoxide resin and 3,3'- diaminourea di-n-propylamine are added, 5-6 hours are stirred under rotating speed 100-200r/min；（3）Lecithin, silicone emulsion, polyoxypropylene ethylene oxide glycerin ether and polyethylene glycol are added, after stirring 20-40 minutes It is put into vacuum drying chamber and vacuumizes carry out defoaming treatment；（4）Green compact must be freezed by pouring into freezing apparatus for pouring；（5）It is put into after being freeze-dried in sintering furnace and carries out the sintering 3-4 hours at 550-650 DEG C of temperature and produce.
- A kind of 4. preparation method of Medical Compound Bioceramics material according to claim 3, it is characterised in that：The step Suddenly（1）Middle milling time is 26-28 hours.
- A kind of 5. preparation method of Medical Compound Bioceramics material according to claim 3, it is characterised in that：The step Suddenly（2）Middle rotating speed is 120-190r/min, and mixing time is 5.5 hours.
- A kind of 6. preparation method of Medical Compound Bioceramics material according to claim 3, it is characterised in that：The step Suddenly（5）Middle sintering temperature is 600 DEG C, and sintering time is 3.5 hours.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330285A (en) * | 2015-12-11 | 2016-02-17 | 华南协同创新研究院 | ZrO2-toughened bioactive ceramic powder material for 3D printing and preparation and application thereof |
| CN105481466A (en) * | 2015-12-11 | 2016-04-13 | 华南协同创新研究院 | ZrO2 toughened porous calcium phosphate biological ceramic material and preparation method and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330285A (en) * | 2015-12-11 | 2016-02-17 | 华南协同创新研究院 | ZrO2-toughened bioactive ceramic powder material for 3D printing and preparation and application thereof |
| CN105481466A (en) * | 2015-12-11 | 2016-04-13 | 华南协同创新研究院 | ZrO2 toughened porous calcium phosphate biological ceramic material and preparation method and application thereof |
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