CN107362389A - A kind of calcium phosphate biological bone cement composite of CNT and graphene enhancing - Google Patents
A kind of calcium phosphate biological bone cement composite of CNT and graphene enhancing Download PDFInfo
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- CN107362389A CN107362389A CN201710456840.2A CN201710456840A CN107362389A CN 107362389 A CN107362389 A CN 107362389A CN 201710456840 A CN201710456840 A CN 201710456840A CN 107362389 A CN107362389 A CN 107362389A
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- bone cement
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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
- A61L27/08—Carbon ; Graphite
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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
Abstract
The invention discloses the calcium phosphate biological bone cement composite that a kind of CNT and graphene strengthen, it is made up of the component of following parts by weight：94.2 95 parts of α tricalcium phosphates, 4.8 5.2 parts of hydroxyapatite, 0.2 1 parts of graphene, 0.2 1 parts of CNT.In the present invention reinforcement of α tricalcium phosphate bone cements is used as by the use of graphene and CNT, the calcium phosphate biological bone cement composite of preparation has good intensity and biocompatibility, simultaneously, after microwave treatment, the setting time of calcium phosphate biological bone cement composite can significantly be shortened, and the further intensity for improving calcium phosphate biological bone cement composite.Available for the reparation of human body bone, replacement and the treatment of other orthopaedic diseases.Solve the problems, such as low intensity, poor toughness existing for calcium phosphate biological bone cement composite in the prior art.
Description
Technical field
The invention belongs to material science and biomedical crossing domain, and in particular to a kind of CNT and graphene increase
Strong calcium phosphate biological bone cement composite, more particularly to one kind is using type alpha tricalcium phosphate biological bone cement as matrix, with graphite
Alkene and CNT are calcium phosphate cement composite material of reinforcement and preparation method thereof.
Background technology
Type alpha tricalcium phosphate bone cement is one kind of calcium phosphate biological bone cement, has excellent bioactivity and bio-compatible
Property, it can be degraded in human body, be a kind of bone implant material with broad prospect of application.It is mainly by type alpha tricalcium phosphate and liquid phase
Composition, after solid phase and liquid phase mixing, congealing reaction occurs, forms a kind of material similar with porous ceramics, it is hard with human body
Tissue is (such as：Bone) compare, its poor toughness, low intensity.Further, since its presetting period, at 1 more than hour, and final setting time is grown
Up to several hours, therefore easily tissue is caused to be inflamed reaction.It is presently used for improving the method master of calcium phosphate biological bone cement
There are two aspects：First, its intensity is improved by reducing the porosity after solidifying, but this method makes the journey that its intensity improves
Spend limited, and the too small degradation time that can greatly extend calcium phosphate biological bone cement of the porosity；Second, pass through additional reinforcement
Material strengthens the intensity of calcium phosphate biological bone cement, and fiber is the most frequently used reinforcing material, as polymer fiber, carbon fiber,
Ceramic fibre etc., although being improved by the intensity of fiber calcium phosphate biological bone cement, compared with body bone tissue,
Intensity still differs larger, and the fiber of some biologically inerts can influence the activity of calcium phosphate biological bone cement.During for condensing
Between shortening, the method mainly taken at present for addition hydroxyapatite seed and coagulant, both approaches can effectively contract
The mechanical property of short calcium phosphate biological bone cement, wherein, being excessively added for hydroxyapatite can reduce calcium phosphate biological bone cement
Intensity.
In summary, in the prior art existing for calcium phosphate biological bone cement composite the problem of low intensity, poor toughness,
Still lack effective solution.
The content of the invention
For technical problem present in above-mentioned prior art, it is an object of the invention to provide a kind of CNT and graphite
The calcium phosphate biological bone cement composite of alkene enhancing.Using the mechanical property that graphene and CNT are excellent, by graphene
With reinforcement of the CNT as type alpha tricalcium phosphate bone cement, obtain a kind of not only with higher intensity but also with good biological
Type alpha tricalcium phosphate/graphene, the CNT calcium phosphate biological bone cement composite of performance.And utilize graphene and carbon nanometer
The absorption microwave property of pipe, by carrying out microwave treatment in calcium phosphate biological bone cement composite condensation process, make phosphoric acid
The setting time of calcium biological bone cement composite shortens, and intensity further improves.
In order to solve the above technical problems, the technical scheme is that：
A kind of calcium phosphate biological bone cement composite of CNT and graphene enhancing, by the component of following parts by weight
Composition：Type alpha tricalcium phosphate 94.2-95 parts, hydroxyapatite 4.8-5.2 parts, graphene 0.2-1 parts, CNT 0-1 parts.
Graphene and CNT have excellent mechanical property, using CNT and graphene as type alpha tricalcium phosphate bone
During the reinforcement of cement, the rupture strength and compression strength of type alpha tricalcium phosphate bone cement can be remarkably reinforced.But to carbon nanometer
The content requirement of pipe and graphene is strict, too high levels or too low is all difficult to play good enhancing effect.
Further, the calcium phosphate biological bone cement composite, is made up of the component of following parts by weight：Alpha-phosphate three
Calcium 94.2-95 parts, hydroxyapatite 4.8-5.2 parts, graphene 0.2-1 parts, CNT 0.2-1 parts.
Further, the calcium phosphate biological bone cement composite, is made up of the component of following parts by weight：Alpha-phosphate
DFP 94.2-95 parts, hydroxyapatite 4.8-5.2 parts, graphene 0.4-0.8 parts, CNT 0.4-0.8 parts.
Further, the calcium phosphate biological bone cement composite, is made up of the component of following parts by weight：Alpha-phosphate
DFP 94.2-95 parts, hydroxyapatite 4.8-5.2 parts, 0.6 part of graphene, 0.6 part of CNT.
Further, the graphene is redox graphene, granularity 0.55-3.74nm.
Redox graphene refer to by chemically or thermally the methods of not exclusively remove it is oxygen-containing in graphene oxide
A kind of two-dimentional carbon material obtained after functional group.
Further, the CNT is multi-walled carbon nanotube, its a diameter of 20-30nm.
The preparation method of above-mentioned calcium phosphate biological bone cement composite, comprises the following steps：
1) type alpha tricalcium phosphate, hydroxyapatite, graphene and CNT are weighed in proportion, mixing and ball milling, sieving, are obtained
Calcium phosphate biological bone cement composite material powder；
2) being well mixed material powder with water condenses mixture, and target composite is obtained after final set.
Microwave processes be well mixed for calcium phosphate biological bone cement composite powder with water solid-liquid after to final set
Continuation condensation stage after stage and final set, after microwave treatment, it is compound that calcium phosphate biological bone cement is greatly shortened
The setting time of material, and further increase the intensity of calcium phosphate biological bone cement composite.
Preferably, in step 2), after material powder is well mixed with water, into its local environment add microwave field until
Final set, after final set, in 24h, per 4h microwave treatment half an hour.
Further, in step 1), the rotating speed of ball milling is 350-450r/min, Ball-milling Time 4-6h.
Further, in step 1), the ball milling is dry grinding, without using ball-milling medium.
Further, in step 1), the powder after ball milling is crossed into 300 mesh sieves, obtains calcium phosphate biological bone cement composite wood
Expect material powder.
Further, in step 2), every gram of material powder is well mixed with 0.3-0.4ml water to be condensed.
Further, in step 2), the environment temperature of condensation is 36-38 DEG C, humidity 100%.Mainly simulate people
The environment of body, it is set to be condensed in similar human body environment, situation about can more reflect during its use.
Further, in step 2), the microwave frequency of microwave treatment is 0.43-2.45GHz, power 15-25W.
Further, in step 2), final set is measured using Gillmore crosspointer methods, when final set pin perpendicular to sample surfaces from
By sliding, it is impossible to reach final set when sample surfaces leave complete circular impression.
The calcium phosphate biological bone cement composite that above-mentioned preparation method is prepared.
Application of the above-mentioned calcium phosphate biological bone cement composite in bone repair and replacement.
A kind of calcium phosphate biological bone, it is prepared by above-mentioned calcium phosphate biological bone cement composite.
Beneficial effects of the present invention are：
In the present invention reinforcement of type alpha tricalcium phosphate bone cement, the calcium phosphate of preparation are used as by the use of graphene and CNT
Biological bone cement composite has good intensity and biocompatibility, meanwhile, after microwave treatment, can significantly it shorten
The setting time of calcium phosphate biological bone cement composite, and further raising calcium phosphate biological bone cement composite
Intensity.Available for the reparation of human body bone, replacement and the treatment of other orthopaedic diseases.
Brief description of the drawings
The Figure of description for forming the part of the application is used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its illustrate be used for explain the application, do not form the improper restriction to the application.
Fig. 1 is that calcium phosphate biological bone cement composite composition is type alpha tricalcium phosphate 94-95% without microwave treatment,
Hydroxyapatite 5%, graphene 0-1%, during CNT 0%, its rupture strength with graphene content change.
Fig. 2 is that calcium phosphate biological bone cement composite composition is type alpha tricalcium phosphate 94-95% without microwave treatment,
Hydroxyapatite 5%, graphene 0-1%, during CNT 0%, its compression strength with graphene content change.
Fig. 3 is that calcium phosphate biological bone cement composite composition is type alpha tricalcium phosphate 93.8- without microwave treatment
94.6%, hydroxyapatite 5%, graphene 0.2%, during CNT 0.2-1%, its rupture strength is with content of carbon nanotubes
Change.
Fig. 4 is that calcium phosphate biological bone cement composite composition is type alpha tricalcium phosphate 93.8- without microwave treatment
94.6%, hydroxyapatite 5%, graphene 0.2%, during CNT 0.2-1%, its compression strength is with content of carbon nanotubes
Change.
Fig. 5 is that calcium phosphate biological bone cement composite composition is type alpha tricalcium phosphate 94.2%, hydroxyapatite 5%, stone
Black alkene 0.2%, during CNT 0.6%, its rupture strength with microwave treatment time change.
Fig. 6 is that calcium phosphate biological bone cement composite composition is type alpha tricalcium phosphate 94.2%, hydroxyapatite 5%, stone
Black alkene 0.2%, during CNT 0.6%, its compression strength with microwave treatment time change.
Embodiment
It is noted that described further below is all exemplary, it is intended to provides further instruction to the application.It is unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
Embodiment 1
Calcium phosphate biological bone cement composite proportioning is (wt%)：Type alpha tricalcium phosphate 94.8%, hydroxyapatite 5%,
Graphene 0-1%, CNT 0%.
First, a certain amount of type alpha tricalcium phosphate, hydroxyapatite and graphene are weighed according to proportioning, is placed on ball grinder
In, with 400r/min ball milling 5h, 300 mesh sieves are crossed, obtain calcium phosphate biological bone cement composite material powder.Then by raw material
Powder is well mixed with distilled water with 0.35ml/g, is placed on temperature as 37 DEG C, humidity is to make it solidifying in 100% environment
Knot, the process do not have to microwave treatment.After 24h, the calcium phosphate biological bone cement composite that is condensed completely.
The calcium phosphate biological bone cement composite rupture strength is up to 11.6 ± 0.2MPa, referring to Fig. 1, pressure resistance
Degree is up to 59.3 ± 3.3MPa, referring to Fig. 2.Its presetting period is 13 ± 0.9min, and final setting time is 54 ± 2.1min.
Embodiment 2
Calcium phosphate biological bone cement composite proportioning is (wt%)：Type alpha tricalcium phosphate 94.2%, hydroxyapatite 5%,
Graphene 0.2%, CNT 0.2-1%.
First, a certain amount of type alpha tricalcium phosphate, hydroxyapatite and graphene are weighed according to proportioning, is placed on ball grinder
In, with 400r/min ball milling 5h, 300 mesh sieves are crossed, obtain calcium phosphate biological bone cement composite material powder.Then by raw material
Powder is well mixed with distilled water with 0.35ml/g, is placed on temperature as 37 DEG C, humidity is to make it solidifying in 100% environment
Knot, the process do not have to microwave treatment.After 24h, the calcium phosphate biological bone cement composite that is condensed completely.
The calcium phosphate biological bone cement composite rupture strength is up to 14.5 ± 0.2MPa, and referring to Fig. 3, compression strength can
Up to 86.5 ± 2.7MPa, referring to Fig. 4.Its presetting period is 7.7 ± 0.5min, and final setting time is 28.5 ± 1.0min.
Embodiment 3
Calcium phosphate biological bone cement composite proportioning is (wt%)：Type alpha tricalcium phosphate 94.2%, hydroxyapatite 5%,
Graphene 0.2%, CNT 0.2-1%.
First, a certain amount of type alpha tricalcium phosphate, hydroxyapatite and graphene are weighed according to proportioning, is placed on ball grinder
In, with 400r/min ball milling 5h, 300 mesh sieves are crossed, obtain calcium phosphate biological bone cement composite material powder.Then by raw material
Powder is well mixed with distilled water with 0.35ml/g, is placed on temperature as 37 DEG C, humidity is to make it solidifying in 100% environment
Knot, the process persistently use microwave treatment before final set, per 4h microwave treatment half an hour after final set.After 24h, condensed completely
Calcium phosphate biological bone cement composite.
The calcium phosphate biological bone cement composite rupture strength is up to 17.4 ± 0.2MPa, and referring to Fig. 5, compression strength can
Up to 104.5 ± 1.8MPa, referring to Fig. 6.Its presetting period is 7.2 ± 0.5min, and final setting time is 15.5 ± 1.2min.
It can be seen from the data of embodiment 1 and embodiment 2, when adding graphite in calcium phosphate biological bone cement composite
When alkene is without adding CNT, the performance of composite can be made to obtain a certain degree of raising.When same in the composite
When Shi Tianjia graphenes and CNT, compared to graphene is only added, it can become apparent from improving the intensity of composite, and
Test proves that while when adding graphene and CNT, the composite of preparation has more preferable biocompatibility.Root
Understand according to the data of embodiment 2 and embodiment 3, when increasing microwave field auxiliary condensation in preparation process, not only can substantially change
Kind initial set and final set speed, the intensity of the composite of preparation can also be significantly improved.
The preferred embodiment of the application is the foregoing is only, is not limited to the application, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. a kind of CNT and the calcium phosphate biological bone cement composite of graphene enhancing, it is characterised in that：By following heavy
Measure the component composition of part：Type alpha tricalcium phosphate 94.2-95 parts, hydroxyapatite 4.8-5.2 parts, graphene 0.2-1 parts, CNT
0-1 parts；
Preferably, the calcium phosphate biological bone cement composite, is made up of the component of following parts by weight：Type alpha tricalcium phosphate
94.2-95 parts, hydroxyapatite 4.8-5.2 parts, graphene 0.2-1 parts, CNT 0.2-1 parts；
Preferably, the calcium phosphate biological bone cement composite, is made up of the component of following parts by weight：Type alpha tricalcium phosphate
94.2-95 parts, hydroxyapatite 4.8-5.2 parts, graphene 0.4-0.8 parts, CNT 0.2-1 parts；
It is further preferred that the calcium phosphate biological bone cement composite, is made up of the component of following parts by weight：Alpha-phosphate three
Calcium 94.2-95 parts, hydroxyapatite 4.8-5.2 parts, 0.6 part of graphene, 0.6 part of CNT.
2. calcium phosphate biological bone cement composite according to claim 1 or 2, it is characterised in that：The graphene is
Redox graphene, granularity 0.55-3.74nm；
Preferably, the CNT is multi-walled carbon nanotube, its a diameter of 20-30nm.
3. the preparation method of any calcium phosphate biological bone cement composites of claim 1-2, it is characterised in that：Including such as
Lower step：
1) type alpha tricalcium phosphate, hydroxyapatite, graphene and CNT are weighed in proportion, mixing and ball milling, sieving, obtain phosphoric acid
Calcium biological bone cement composite material powder；
2) being well mixed material powder with water condenses mixture, and target composite is obtained after final set.
4. preparation method according to claim 3, it is characterised in that：In step 1), the rotating speed of ball milling is 350-450r/
Min, Ball-milling Time 4-6h；
Preferably, the ball milling is dry grinding, without using ball-milling medium.
Preferably, the powder after ball milling is crossed into 300 mesh sieves, obtains calcium phosphate biological bone cement composite material powder.
5. preparation method according to claim 3, it is characterised in that：In step 2), every gram of material powder and 0.3-0.4ml
Water is well mixed to be condensed；
Preferably, the environment temperature of condensation is 36-38 DEG C, humidity 100%.
6. preparation method according to claim 3, it is characterised in that：In step 2), material powder is well mixed with water
Afterwards, microwave field is added into its local environment up to final set, after final set, in 24h, per 4h microwave treatment half an hour.
7. preparation method according to claim 6, it is characterised in that：In step 2), the microwave frequency of microwave treatment is
0.43-2.45GHz, power 15-25W.
Preferably, final set is measured using Gillmore crosspointer methods, when final set pin freely slides perpendicular to sample surfaces, it is impossible in sample
Product surface reaches final set when leaving complete circular impression.
8. the calcium phosphate biological bone cement composite that any preparation methods of claim 4-7 are prepared.
9. application of the calcium phosphate biological bone cement composite in bone repair and replacement described in claim 8.
A kind of 10. calcium phosphate biological bone, it is characterised in that：It is prepared by above-mentioned calcium phosphate biological bone cement composite.
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