CN108863290A - A kind of preparation method of the phosphate bone cement composite material of the fiber containing CPP - Google Patents
A kind of preparation method of the phosphate bone cement composite material of the fiber containing CPP Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
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- C04B28/344—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders the phosphate binder being present in the starting composition solely as one or more phosphates
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- 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
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Abstract
The present invention relates to a kind of preparation methods of the phosphate bone cement composite material of fiber containing CPP, belong to medical repair materials technical field.The present invention is prepared for a kind of micro-sphere material with gelatin and chitosan, have the function of Drug controlled release, extend curative effect of medication, to improve the stability of drug, the adverse reaction of drug is reduced, while its own is with anti-inflammatory effect, gelatine-chitosan microballoon good biocompatibility, when gelatine-chitosan microballoon/calcium phosphate bone cement is in fluid environment, microballoon dissolves into liquid, and gelatin and chitosan can be slowly precipitated with liquid condition, wraps up entire bracket by gelatin and chitosan；It is three-dimensional netted, connection, microcellular structure in material cross-section of the present invention, micropore distribution is relatively uniform, these three-dimensional, connections, mesh space structure, are conducive to bone and cartilaginous tissue plays specific physiological function, and intensity is high, will not cause inflammatory reaction after implantation human body.
Description
Technical field
The present invention relates to a kind of preparation methods of the phosphate bone cement composite material of fiber containing CPP, belong to medical reparation
Field of material technology.
Background technique
Bone cement material is mainly used in the skeletal defect for the treatment of organism, can support affected part after filling up and hurts to avoid two degree
Evil.In general, bone cement include by the bone substitute materials pulvis formed and reconciliation aqua, in using it is preceding mixing make it
With mobility.The Nature comparison of fluid is easy to reach close filling, and must solidify in a short time and could prevent after being implanted into
Only destroyed by body fluid.Certainly, the structural strength after solidification also must support affected part to be just avoided that secondary injury enough.
Bone cement material is due to structural strength to be maintained, therefore the fresh importance for emphasizing porosity less.Bone water with hole
Mud material, cell can be allowed to be easy to attach for rough external surface and inner void can provide space and cell is allowed to grow, however hole
In the presence of the detraction for often therefore causing bone cement material structural strength after solidifying, therefore exploitation can take into account the bone water of intensity and porosity
Mud material has its necessity.
Being usually used in the substance in bone cement as bone substitute materials includes polymer, metal or salt, but poly- methyl-prop
E pioic acid methyl ester is not general bone ingredient, and bio-compatibility is poor compared with natural component, and can generate exothermic reaction when solidification, and easy pair
Affected part surrounding tissue impacts, therefore just has the bone cement developed using bone analogous components for material later.Use hydroxyl
Base apatite (one of bone important component), tricalcium phosphate and tetracalcium phosphate are main component, add growth factor and help bone
Bone growth.And use Dicalcium Phosphate and tricalcium phosphate that can form hydroxyapatite after mixing gradually in vivo as main component.
However above bone cement material hardening rate is slow, destroys after use vulnerable to body fluid and loses intensity and function, therefore further
Calcium sulfate is added to help to solidify.However since calcium sulfate just can not absorb or divide for organism immediately at bone cement implantation initial stage
Solution to provide material hole property is easy that osteocyte is made to be not easy to attach and lessen the curative effect.As previously mentioned, with hole
Bone cement material can allow cell to be easy to attach growth, and then help the generation of cytoplasm to improve therapeutic effect.
In recent years, people have developed a series of calcium phosphate bone cement products in succession to adapt to different human body hard tissue repair
It needs, the CPC bone cement developed at present is applied in clinical practice；However the generally existing brittleness of phosphoric acid salt material
Greatly, intensity it is low, with new bone growth rate mismatch, implantation human body after cause inflammatory reaction the disadvantages of, make its application range by
Larger limitation.
Summary of the invention
The technical problems to be solved by the invention：For the generally existing brittleness of phosphoric acid salt material is big, intensity is low and new bone
The problem of the disadvantages of growth rate mismatches, causes inflammatory reaction after implantation human body, provide a kind of phosphate of fiber containing CPP
The preparation method of bone-cement composite material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that：
（1）It is in 2% acetic acid solution that Chitosan powder, which is dissolved in mass fraction, and it is that 1.5% chitosan-acetic acid is molten that mass fraction, which is made,
Mass fraction is that 15% gelatin solution and atoleine are preheated to 50 DEG C by liquid, and the mass fraction after must preheating is 15% gelatin
Solution and preheated atoleine, the mass fraction after mass fraction is 1.5% chitosan-acetic acid solution and is preheated is 15%
Gelatin solution is uniformly mixed, and obtains mixed liquor A；
（2）In mass ratio 1: 10 compound emulsifying agent is added in atoleine, obtains emulsion, in mass ratio 1: 5 drips mixed liquor A
It is added in emulsion, is stirred at room temperature, obtain mixed liquid B, by mixed liquid B centrifugal treating, obtain sediment, sediment petroleum ether, second
Pure and mild distilled water respectively washs 3 times, is ground into uniform powder after drying at room temperature, can obtain micro-sphere material；
（3）According to parts by weight, 50~60 parts of calcium phoshate bone cement powders, 10~15 parts of CPP fibers, 15~18 parts are weighed respectively
Micro-sphere material, 7~10 parts of ball milling calcium carbonate powders, 5~10 parts of ammonium hydrogen carbonate, 70~90 parts of distilled waters, by calcium phosphate bone cement
Powder and distilled water are mixed and stirred for uniformly, obtaining slurry, and CPP fiber, micro-sphere material, ball milling calcium carbonate powder are added in the slurry
And ammonium hydrogen carbonate, it stirs evenly, obtains mixture, inject the mixture into mold, foam and be dried, demould to obtain fiber containing CPP
Phosphate bone cement composite material.
Step（1）The mass fraction is that the mass fraction after 1.5% chitosan-acetic acid solution and preheating is 15% gelatin
The mass ratio of solution is 1: 1.
Step（2）The compound emulsifying agent is Span-80 the and Tween-80 mixture of mass ratio 1: 1.
Step（2）Described is stirred at room temperature as 2~3h is stirred at room temperature under 1500~2000r/min mixing speed.
Step（2）The centrifugal treating be to be centrifuged 7~14cm of radius, 1000~1500r/min of revolving speed centrifugation 5~
10min。
Step（3）The mold is that diameter is 8mm, the stainless steel cylinder mold of high 12mm.
Step（3）It is after foaming 68~72h in 40~50 DEG C, to take out juxtaposition that the foaming, which is dried to be placed in temperature,
Dry 40~48h in 30~40 DEG C of baking ovens.
The present invention is compared with other methods, and advantageous effects are：
（1）The present invention is prepared for a kind of micro-sphere material with gelatin and chitosan, and gelatin is the drop of main organic principle-collagen of bone
Solve product, and non-immunogenicity, biodegradability that chitosan has, biocompatibility, are the rare days of nature
Right polymer carrier is had the function of Drug controlled release, is extended curative effect of medication using chitosan microball entrapped drug,
To improve the stability of drug, the adverse reaction of drug is reduced, while its own is with anti-inflammatory effect, gelatine-chitosan is micro-
Ball good biocompatibility, when gelatine-chitosan microballoon/calcium phosphate bone cement is in fluid environment, microballoon dissolves into liquid, gelatin
It can be slowly precipitated with liquid condition with chitosan, wrap up entire bracket by gelatin and chitosan, be equivalent to and increase on bracket
Gelatine-chitosan coating, this coating can obviously increase the cell activity of timbering material；
（2）The present invention selects calcium phosphate bone cement as basis material, and calcium polyphosphate fiber is as reinforcing material, the carbonic acid of ball milling
Calcium powder is as bioactivity regulator, and using composite technology, the phosphate bone cement for preparing a kind of fiber containing CPP is multiple
Condensation material is three-dimensional netted, connection, microcellular structure in the cross section of the composite material, and fiber random distribution, micropore distribution is compared
Uniformly, these three-dimensional, connections, mesh space structure can provide suitable nutrient delivery item for histiocytic growth, breeding
Part, steric requirements and excretion give-and-take conditions, are conducive to bone and cartilaginous tissue plays specific physiological function, and intensity is high, implantation
It will not cause inflammatory reaction after human body.
Specific embodiment
It is in 2% acetic acid solution that Chitosan powder, which is dissolved in mass fraction, and it is 1.5% chitosan-acetic acid that mass fraction, which is made,
Mass fraction is that 15% gelatin solution and atoleine are preheated to 50 DEG C by solution, and the mass fraction after must preheating is 15% bright
Sol solution and preheated atoleine, by volume 1: 1 by mass fraction be 1.5% chitosan-acetic acid solution and preheating after
Mass fraction is uniformly mixed for 15% gelatin solution, obtains mixed liquor A；In mass ratio 1: 1 mixes Span-80 and Tween-80
It is even, obtain compound emulsifying agent；In mass ratio 1: 10 compound emulsifying agent is added in atoleine, obtains emulsion, and in mass ratio 1: 5 will
Mixed liquor A is added drop-wise in emulsion, and under 1500~2000r/min mixing speed, 2~3h is stirred at room temperature, and obtains mixed liquid B, will
To be centrifuged 7~14cm of radius, 1000~1500r/min of revolving speed is centrifuged 5~10min, obtains sediment, sediment stone mixed liquid B
Oily ether, ethyl alcohol and distilled water respectively wash 3 times, are ground into uniform powder after drying at room temperature, can obtain micro-sphere material；By weight
Number meter, weigh respectively 50~60 parts of calcium phoshate bone cement powders, 10~15 parts of CPP fibers, 15~18 parts of micro-sphere materials, 7~
10 parts of ball milling calcium carbonate powders, 5~10 parts of ammonium hydrogen carbonate, 70~90 parts of distilled waters, by calcium phoshate bone cement powder and distilled water
It is mixed and stirred for uniformly, obtaining slurry, CPP fiber, micro-sphere material, ball milling calcium carbonate powder and ammonium hydrogen carbonate is added in the slurry,
It stirs evenly, obtains mixture, injecting the mixture into diameter is 8mm, and the stainless steel cylinder mold of high 12mm, being placed in temperature is 40
Foamed after 68~72h in~50 DEG C, taking-up is placed in 30~40 DEG C of baking ovens dry 40~48h, demould the fiber containing CPP phosphorus
Hydrochlorate bone-cement composite material.
Example 1
It is in 2% acetic acid solution that Chitosan powder, which is dissolved in mass fraction, and it is 1.5% chitosan-acetic acid solution that mass fraction, which is made,
It is that 15% gelatin solution and atoleine are preheated to 50 DEG C by mass fraction, the mass fraction after must preheating is 15% gelatin solution
With preheated atoleine, mass fraction is 1.5% chitosan-acetic acid solution and the quality point after preheating by 1: 1 by volume
Number is that 15% gelatin solution is uniformly mixed, and obtains mixed liquor A；In mass ratio 1: 1 is uniformly mixed Span-80 and Tween-80, must answer
Co-emulsifier；In mass ratio 1: 10 compound emulsifying agent is added in atoleine, obtains emulsion, and in mass ratio 1: 5 by mixed liquor A
It is added drop-wise in emulsion, under 1500r/min mixing speed, 2h is stirred at room temperature, obtains mixed liquid B, by mixed liquid B to be centrifuged radius
7cm, revolving speed 1000r/min are centrifuged 5min, obtain sediment, sediment petroleum ether, ethyl alcohol and distilled water respectively wash 3 times, room temperature
It is ground into uniform powder after lower drying, micro-sphere material can be obtained；According to parts by weight, 50 parts of calcium phosphate bone cements are weighed respectively
Powder, 10 parts of CPP fibers, 15 parts of micro-sphere materials, 7 parts of ball milling calcium carbonate powders, 5 parts of ammonium hydrogen carbonate, 70 parts of distilled waters, by phosphoric acid
Calcium bone cement powder and distilled water are mixed and stirred for uniformly, obtaining slurry, and CPP fiber, micro-sphere material, ball milling carbon are added in the slurry
Sour calcium powder and ammonium hydrogen carbonate, stir evenly, and obtain mixture, and injecting the mixture into diameter is 8mm, the stainless steel cylinder of high 12mm
Mould, being placed in temperature is after foaming 68h in 40 DEG C, and taking-up is placed in 30 DEG C of baking ovens dry 40h, demoulds to obtain fiber containing CPP
Phosphate bone cement composite material.
Example 2
It is in 2% acetic acid solution that Chitosan powder, which is dissolved in mass fraction, and it is 1.5% chitosan-acetic acid solution that mass fraction, which is made,
It is that 15% gelatin solution and atoleine are preheated to 50 DEG C by mass fraction, the mass fraction after must preheating is 15% gelatin solution
With preheated atoleine, mass fraction is 1.5% chitosan-acetic acid solution and the quality point after preheating by 1: 1 by volume
Number is that 15% gelatin solution is uniformly mixed, and obtains mixed liquor A；In mass ratio 1: 1 is uniformly mixed Span-80 and Tween-80, must answer
Co-emulsifier；In mass ratio 1: 10 compound emulsifying agent is added in atoleine, obtains emulsion, and in mass ratio 1: 5 by mixed liquor A
It is added drop-wise in emulsion, under 1750r/min mixing speed, 2.5h is stirred at room temperature, obtains mixed liquid B, by mixed liquid B to be centrifuged half
Diameter 11cm, revolving speed 1250r/min are centrifuged 8min, obtain sediment, sediment petroleum ether, ethyl alcohol and distilled water respectively wash 3 times, room
It is ground into uniform powder after the lower drying of temperature, micro-sphere material can be obtained；According to parts by weight, 55 parts of calcium phosphate bone water are weighed respectively
Mud powder, 13 parts of CPP fibers, 16 parts of micro-sphere materials, 9 parts of ball milling calcium carbonate powders, 7 parts of ammonium hydrogen carbonate, 80 parts of distilled waters, by phosphorus
Sour calcium bone cement powder and distilled water are mixed and stirred for uniformly, obtaining slurry, and CPP fiber, micro-sphere material, ball milling are added in the slurry
Calcium carbonate powder and ammonium hydrogen carbonate, stir evenly, and obtain mixture, and injecting the mixture into diameter is 8mm, the stainless steel circle of high 12mm
Cylinder mold, being placed in temperature is after foaming 70h in 45 DEG C, and taking-up is placed in 35 DEG C of baking ovens dry 44h, demoulds fine containing CPP
The phosphate bone cement composite material of dimension.
Example 3
It is in 2% acetic acid solution that Chitosan powder, which is dissolved in mass fraction, and it is 1.5% chitosan-acetic acid solution that mass fraction, which is made,
It is that 15% gelatin solution and atoleine are preheated to 50 DEG C by mass fraction, the mass fraction after must preheating is 15% gelatin solution
With preheated atoleine, mass fraction is 1.5% chitosan-acetic acid solution and the quality point after preheating by 1: 1 by volume
Number is that 15% gelatin solution is uniformly mixed, and obtains mixed liquor A；In mass ratio 1: 1 is uniformly mixed Span-80 and Tween-80, must answer
Co-emulsifier；In mass ratio 1: 10 compound emulsifying agent is added in atoleine, obtains emulsion, and in mass ratio 1: 5 by mixed liquor A
It is added drop-wise in emulsion, under 2000r/min mixing speed, 3h is stirred at room temperature, obtains mixed liquid B, by mixed liquid B to be centrifuged radius
14cm, revolving speed 1500r/min are centrifuged 10min, obtain sediment, sediment petroleum ether, ethyl alcohol and distilled water respectively wash 3 times, room
It is ground into uniform powder after the lower drying of temperature, micro-sphere material can be obtained；According to parts by weight, 60 parts of calcium phosphate bone water are weighed respectively
Mud powder, 15 parts of CPP fibers, 18 parts of micro-sphere materials, 10 parts of ball milling calcium carbonate powders, 10 parts of ammonium hydrogen carbonate, 90 parts of distilled waters, will
Calcium phoshate bone cement powder and distilled water are mixed and stirred for uniformly, obtaining slurry, and CPP fiber, micro-sphere material, ball are added in the slurry
Calcium carbonate powder and ammonium hydrogen carbonate are ground, stirs evenly, obtains mixture, injecting the mixture into diameter is 8mm, the stainless steel of high 12mm
Cylinder mold, being placed in temperature is after foaming 72h in 50 DEG C, and taking-up is placed in 40 DEG C of baking ovens dry 48h, demoulds containing CPP
The phosphate bone cement composite material of fiber.
The common phosphorus that the phosphate bone cement composite material of the fiber prepared by the present invention containing CPP and Shanghai company are produced
Barbiturates material is detected, specific testing result such as following table table 1：
Detection method：
Compressive strength determination：By in the mold of bone cement slurry filling Φ 10mm × 5mm, is taken out after 0.5h, be placed in 37 DEG C of water-baths
72h is conserved in pot, is tested using omnipotent mechanics machine, load 900N, pressing speed 1mm/min, pressure resistance is calculated
Degree, each component bone cement are all made of 5 Duplicate Samples, and calculated result is averaged；
Curing time measurement：The curing time of each bone cement sample is measured with similar Fred Gilmore needle indentation method, experiment repeats 5
It is secondary；
Anti-microbial property detection：The phosphate bone cement composite material of the fiber containing CPP is made to the cylindrical body of Φ 5mm × 2mm, is purchased from
The Escherichia coli (35218) and staphylococcus aureus (25923) of ATCC are used as strain, test each examination using plate inhibition zone method
The bacteriostasis property of sample, experiment are repeated 3 times.
The phosphate bone cement composite property of 1 fiber containing CPP of table characterizes
The phosphate bone cement composite material of the fiber prepared by the present invention containing CPP as shown in Table 1, compression strength is high, bio-compatible
Property is good, and bacteriostasis property is excellent, has a vast market value and application prospect.
Claims (7)
1. a kind of preparation method of the phosphate bone cement composite material of fiber containing CPP, it is characterised in that the specific steps are：
（1）It is in 2% acetic acid solution that Chitosan powder, which is dissolved in mass fraction, and it is that 1.5% chitosan-acetic acid is molten that mass fraction, which is made,
Mass fraction is that 15% gelatin solution and atoleine are preheated to 50 DEG C by liquid, and the mass fraction after must preheating is 15% gelatin
Solution and preheated atoleine, the mass fraction after mass fraction is 1.5% chitosan-acetic acid solution and is preheated is 15%
Gelatin solution is uniformly mixed, and obtains mixed liquor A；
（2）In mass ratio 1: 10 compound emulsifying agent is added in atoleine, obtains emulsion, in mass ratio 1: 5 drips mixed liquor A
It is added in emulsion, is stirred at room temperature, obtain mixed liquid B, by mixed liquid B centrifugal treating, obtain sediment, sediment petroleum ether, second
Pure and mild distilled water respectively washs 3 times, is ground into uniform powder after drying at room temperature, can obtain micro-sphere material；
（3）According to parts by weight, 50~60 parts of calcium phoshate bone cement powders, 10~15 parts of CPP fibers, 15~18 parts are weighed respectively
Micro-sphere material, 7~10 parts of ball milling calcium carbonate powders, 5~10 parts of ammonium hydrogen carbonate, 70~90 parts of distilled waters, by calcium phosphate bone cement
Powder and distilled water are mixed and stirred for uniformly, obtaining slurry, and CPP fiber, micro-sphere material, ball milling calcium carbonate powder are added in the slurry
And ammonium hydrogen carbonate, it stirs evenly, obtains mixture, inject the mixture into mold, foam and be dried, demould to obtain fiber containing CPP
Phosphate bone cement composite material.
2. a kind of preparation method of the phosphate bone cement composite material of fiber containing CPP according to claim 1, feature
It is：Step（1）The mass fraction is that the mass fraction after 1.5% chitosan-acetic acid solution and preheating is that 15% gelatin is molten
The mass ratio of liquid is 1: 1.
3. a kind of preparation method of the phosphate bone cement composite material of fiber containing CPP according to claim 1, feature
It is：Step（2）The compound emulsifying agent is Span-80 the and Tween-80 mixture of mass ratio 1: 1.
4. a kind of preparation method of the phosphate bone cement composite material of fiber containing CPP according to claim 1, feature
It is：Step（2）Described is stirred at room temperature as 2~3h is stirred at room temperature under 1500~2000r/min mixing speed.
5. a kind of preparation method of the phosphate bone cement composite material of fiber containing CPP according to claim 1, feature
It is：Step（2）The centrifugal treating be to be centrifuged 7~14cm of radius, 1000~1500r/min of revolving speed centrifugation 5~
10min。
6. a kind of preparation method of the phosphate bone cement composite material of fiber containing CPP according to claim 1, feature
It is：Step（3）The mold is that diameter is 8mm, the stainless steel cylinder mold of high 12mm.
7. a kind of preparation method of the phosphate bone cement composite material of fiber containing CPP according to claim 1, feature
It is：Step（3）It is after foaming 68~72h in 40~50 DEG C that the foaming, which is dried to be placed in temperature, and taking-up is placed in
Dry 40~48h in 30~40 DEG C of baking ovens.
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