CN107899084A - A kind of bone cement and preparation method - Google Patents
A kind of bone cement and preparation method Download PDFInfo
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- CN107899084A CN107899084A CN201710994878.5A CN201710994878A CN107899084A CN 107899084 A CN107899084 A CN 107899084A CN 201710994878 A CN201710994878 A CN 201710994878A CN 107899084 A CN107899084 A CN 107899084A
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- electrospun fibers
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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
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
- A61L27/46—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with phosphorus-containing inorganic fillers
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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
- A61L27/58—Materials at least partially resorbable by the body
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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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 a kind of bone cement, the preparation method of the bone cement includes：1) preparation of calcium phosphate nano particle, 2) preparation of electrospun fibers, 3) preparation of solid phase components, 4) preparation of solidify liquid and 5) curing, the bone cement is strong with good toughness and higher compression strength, plasticity, with fast curing properties and good biocompatibility and biological degradability, solves the defects of traditional bone cement brittleness is big, compression strength is low, difficult degradation.
Description
Technical field
The present invention relates to a kind of biomaterial for medical purpose field, more particularly to a kind of bone cement and preparation method.
Background technology
Calcium phosphate bone cement is a kind of self-curing non-ceramic type phosphorus ash stone material.It is first by Brown and Chow from 1985
First develop the bone renovating material using phosphate as main component.By the research and development of twenties years, led in bone renovating material
Domain, can random-shaping simultaneously can under the conditions of body fluid quick self-curing, and cured product with it is inorganic in human normal bone tissue
Component is close, biocompatibility is good.Calcium phosphate bone cement has become important a member of biomedical material.
Simple calcium phosphate bone cement is generally only used for non-negative since the brittleness of its own is larger and compression strength deficiency
The reparation of the diaphysis in weight area, limits its clinical practice.To strengthen calcium phosphate bone cement, researchers are by calcium phosphate bone water
Biodegradable fiber is introduced in mud can improve the degradation property of bone cement, so that bone cement enhancing, toughness reinforcing.
Fiber particularly nanofiber is a kind of high orientation and the fiber of high intensity, has good mechanical performance.It is quiet
Electrical spinning method is the effective ways that directly can continuously prepare nanofiber at present, because its is simple to operate, the fiber of preparation
Diameter is relatively thin and receives significant attention.But the density and surface state due to macromolecular fibre and inorganic phosphate difference are very
Greatly, as shown in Figure 1, therefore in the case where directly mixing, most of two kinds of components of bone cement：Organic fiber 2 and calcium phosphate without
The compatibility of machine particle 1 is undesirable, often lead to interface adhesion it is poor, disperse non-uniform problem, it is difficult to play enhancing effect.
Therefore, the interface bond strength of a kind of composite fibre enhancing composite bone cement, fiber and bone cement is badly in need of in this area
Height, and composite bone cement intensity height, good toughness, plasticity is strong, cures rapidly, and degraded is fast, and what preferably satisfaction operation used wants
Ask.
The content of the invention
It is high, tough it is an object of the present invention to providing a kind of interface bond strength for overcome the deficiencies in the prior art
The good blended electrospun fibers of organic-inorganic of property.
The second object of the present invention is the preparation method for providing the blended electrospun fibers of above-mentioned organic-inorganic.
The third object of the present invention is to provide the above-mentioned bone cement for including the electrospun fibers.
The fourth object of the present invention is the preparation method for providing above-mentioned bone cement.
An object of the present invention adopts the following technical scheme that realization：
A kind of blended electrospun fibers of organic-inorganic, are scattered in solvent and calcium phosphate nanometer by degradable polymer
Particle is blended and is made；
The degradable polymer is Poly(D,L-lactide-co-glycolide, polylactic acid, polyglycolic acid, poly- hydroxy aliphatic
It is more than one or both of acid esters, makrolon, polycaprolactone and polyglycolic acid；The solvent of the degradable polymer is four
Hydrogen furans and/or dimethylformamide；
The calcium phosphate nano particle for tricalcium phosphate, tetracalcium phosphate, calcium octahate phosphate, calcium monohydrogen phosphate, hydroxyapatite,
It is more than one or both of calcium pyrophosphate, calcium metaphosphate and calcium dihydrogen phosphate；The particle diameter of the calcium phosphate nano particle is
100-1000nm。
Further, the solvent of the degradable polymer presses (1-2) for tetrahydrofuran with dimethylformamide：1 body
Product is than composition.
Further, the calcium phosphate nano particle be ball milling in absolute ethyl alcohol is scattered in by calcium phosphate material and
Into.
Further, the molecular weight of the degradable polymer is 8-10 ten thousand.
Further, the degradable polymer is Poly(D,L-lactide-co-glycolide, polylactic acid or polycaprolactone.
Further, the calcium phosphate nano particle is by tetracalcium phosphate, type alpha tricalcium phosphate, bata-tricalcium phosphate, phosphoric acid
Any two kinds in calcium dihydrogen, calcium monohydrogen phosphate, calcium phosphate are pressed (1-2):1 weight ratio mixing composition.
The second object of the present invention adopts the following technical scheme that realization：
The preparation method of the above-mentioned blended electrospun fibers of organic-inorganic, comprises the following steps：
1) degradable polymer is scattered in the solvent of 5-20 times of weight, vibrates homogeneous at a high speed, obtain degradable polymerization
The dispersion liquid of thing；
2) the calcium phosphate nanometer of 2.5-15% mass is added in the dispersion liquid of the degradable polymer obtained to step 1)
Particle, ultrasonic vibration homogeneous after vibrating at a high speed, carries out electrostatic spinning after defoaming, spinning solution extruded velocity is 0.1-5mL/h, electricity
Press as 10-20kv, collect distance 10-20cm.
Further, in step 1), the molecular weight of degradable polymer is 8-10 ten thousand.
Further, vibration uses rotational trajectory formula mode of oscillation, hunting speed 150-200rpm, duration of oscillation at a high speed
For 30min.
Further, in step 2), spinning solution extruded velocity is 0.5-1mL/h, voltage 12-15kv, collects distance
14-16cm。
The third object of the present invention adopts the following technical scheme that realization：
A kind of bone cement for including the blended electrospun fibers of above-mentioned organic-inorganic.
Further, the bone cement, further includes chitosan and citric acid.
The fourth object of the present invention adopts the following technical scheme that realization：
A kind of preparation method of bone cement, comprises the following steps：
1) preparation of calcium phosphate nano particle：Absolute ethyl alcohol is added to disperse calcium phosphate material, ball milling, sieves, dry；
The calcium phosphate material is tricalcium phosphate, tetracalcium phosphate, calcium octahate phosphate, calcium monohydrogen phosphate, hydroxyapatite, burnt phosphorus
It is more than one or both of sour calcium, calcium metaphosphate and calcium dihydrogen phosphate；
2) preparation of electrospun fibers：By degradable polymer in solvent homogeneous, add the calcium phosphate of step 1)
Type nano granular carries out homogeneous, carries out electrostatic spinning after standing defoaming, obtains electrospun fibers；The degradable polymer is poly-
Poly lactic coglycolic acid, polylactic acid, polyglycolic acid, polyhydroxyalkanoate, makrolon, polycaprolactone and poly- second
It is more than one or both of alkyd；The solvent is tetrahydrofuran and/or dimethylformamide；Spinning solution extruded velocity is
0.1-5mL/h, voltage 10-20kv, collects distance 10-20cm；
3) preparation of solid phase components：The electrospun fibers that step 2) is obtained are dried, and are cut short, the calcium phosphate with step 1)
Type nano granular presses 1:The weight ratio mixing of (10-100), obtains solid phase components；
4) preparation of solidify liquid：According to mass ratio it is (0-2) by chitosan, citric acid and water：(3-4)：100 ratio into
Row mixing, and it is sufficiently stirred obtained solidify liquid；
5) cure：The solidify liquid of the solid phase components of step 3) and step 4) is pressed into (1-2) g:The weight ratio mixing of 1mL, Gu
Change obtains bone cement.
Further, in step 1), the calcium phosphate nano particle is by tetracalcium phosphate, type alpha tricalcium phosphate, β-phosphoric acid
Any two kinds in tricalcium, calcium dihydrogen phosphate, calcium monohydrogen phosphate, calcium phosphate are pressed (1-2):1 weight ratio mixing composition.
Further, in step 2), the degradable polymer is Poly(D,L-lactide-co-glycolide, polylactic acid or poly-
Caprolactone.
Further, in step 2), the solvent presses (1-2) for tetrahydrofuran with dimethylformamide:1 volume ratio group
Into.
Further, in step 3), electrospun fibers are cut short into the length of 2-5cm.
Further, in step 3), the weight ratio of electrospun fibers and calcium phosphate nano particle is (0.5-0.8):
10。
Further, in step 4), the deacetylation of the chitosan is 70-100%, weight average molecular weight 2000-100
Ten thousand.
Further, in step 5), solidification temperature is 37 DEG C, solidification humidity 100%.
Compared with prior art, the beneficial effects of the present invention are：
1) the blended electrospun fibers of organic-inorganic provided by the invention, are by degradable polymer and calcium phosphate nanometer
Particle is blended to be obtained, and degradable polymer is carried out after concussion homogeneous plus after calcium phosphate type nano granular homogeneous using organic solvent
Ultrasonic wave added homogeneous again, it is finally blended to obtain the blended electrospun fibers of organic-inorganic, the blended obtained organic-inorganic of this method
Blended electrospun fibers, the bond strength of degradable polymer and calcium phosphate nano particle is high, toughness is strong, and plasticity is strong,
With preferable medical application prospect.
2) bone cement provided by the invention, its organic degradable polymer use planted agent with inorganic calcium phosphate type nano granular
The dual combination pattern of outer conjunction, the bond strength at its interface is high, the bone cement is had good toughness and higher pressure resistance
Degree, plasticity are strong, have fast curing properties and good biocompatibility and biological degradability, solve traditional bone cement
The defects of brittleness is big, compression strength is low, difficult degradation.
Brief description of the drawings
Fig. 1 is the bone cement structure diagram of the prior art；
The structure diagram of Fig. 2 present invention；
In figure, each reference numeral：1st, inorganic particle；2nd, organic fiber.
Embodiment
In the following, with reference to attached drawing and embodiment, the present invention is described further, it is necessary to which explanation is, not
Under the premise of afoul, new implementation can be formed between various embodiments described below or between each technical characteristic in any combination
Example.
The present invention provides a kind of blended electrospun fibers of organic-inorganic, is scattered in by degradable polymer in solvent and phosphorus
Sour calcium type nano granular is blended and is made；
The degradable polymer is Poly(D,L-lactide-co-glycolide, polylactic acid, polyglycolic acid, poly- hydroxy aliphatic
It is more than one or both of acid esters, makrolon, polycaprolactone and polyglycolic acid；The solvent of the degradable polymer is four
Hydrogen furans and/or dimethylformamide；
The calcium phosphate nano particle for tricalcium phosphate, tetracalcium phosphate, calcium octahate phosphate, calcium monohydrogen phosphate, hydroxyapatite,
It is more than one or both of calcium pyrophosphate, calcium metaphosphate and calcium dihydrogen phosphate；The particle diameter of the calcium phosphate nano particle is
100-1000nm。
The blended electrospun fibers of the organic-inorganic are a kind of endogenous organic and inorganic cospinning electrospun fibers, are had
Have that preferable bond strength is high, toughness is strong.
The preparation method of the blended electrospun fibers of the organic-inorganic, comprises the following steps：
1) degradable polymer is scattered in the solvent of 5-20 times of weight, vibrates homogeneous at a high speed, obtain degradable polymerization
The dispersion liquid of thing；
2) the calcium phosphate nanometer of 2.5-15% mass is added in the dispersion liquid of the degradable polymer obtained to step 1)
Particle, ultrasonic vibration homogeneous after vibrating at a high speed, carries out electrostatic spinning after defoaming, spinning solution extruded velocity is 0.1-5mL/h, electricity
Press as 10-20kv, collect distance 10-20cm.
The preparation method is to utilize organic degradable polymer homogeneous in solvent, then equal with calcium phosphate nano particle
Matter, it is final it is blended go out endogenous, blended electrospun fibers of organic-inorganic that bond strength is high, larger stress can be born, with
Body has preferable compatible.
The present invention also provides a kind of bone cement prepared using the blended electrospun fibers of above-mentioned organic-inorganic.
The preparation method of above-mentioned bone cement comprises the following steps：
1) preparation of calcium phosphate nano particle：Absolute ethyl alcohol is added to disperse calcium phosphate material, ball milling, sieves, dry；
The calcium phosphate material is tricalcium phosphate, tetracalcium phosphate, calcium octahate phosphate, calcium monohydrogen phosphate, hydroxyapatite, burnt phosphorus
It is more than one or both of sour calcium, calcium metaphosphate and calcium dihydrogen phosphate；
2) preparation of electrospun fibers：By degradable polymer in solvent homogeneous, add the calcium phosphate of step 1)
Type nano granular carries out homogeneous, carries out electrostatic spinning after standing defoaming, obtains electrospun fibers；The degradable polymer is poly-
Poly lactic coglycolic acid, polylactic acid, polyglycolic acid, polyhydroxyalkanoate, makrolon, polycaprolactone and poly- second
It is more than one or both of alkyd；The solvent is tetrahydrofuran and/or dimethylformamide；Spinning solution extruded velocity is
0.1-5mL/h, voltage 10-20kv, collects distance 10-20cm；
3) preparation of solid phase components：The electrospun fibers that step 2) is obtained are dried, and are cut short, the calcium phosphate with step 1)
Type nano granular presses 1:The weight ratio mixing of (10-100), obtains solid phase components；
4) preparation of solidify liquid：According to mass ratio it is (0-2) by chitosan, citric acid and water：(3-4)：100 ratio into
Row mixing, and it is sufficiently stirred obtained solidify liquid；
5) cure：The solidify liquid of the solid phase components of step 3) and step 4) is pressed into (1-2) g:The weight ratio mixing of 1mL, Gu
Change obtains bone cement.
What bone cement prepared by the present invention obtained is a kind of planted agent-outer bone cement for closing double action, embedding in organic fiber
The nano particle of calcium phosphate material is entered, hence it is evident that improve interface compatibility and improve interface bond strength, have the bone cement
Have that good toughness and higher compression strength, plasticity are strong, have fast curing properties and good biocompatibility and
Biological degradability, solves the defects of traditional bone cement brittleness is big, compression strength is low, difficult degradation.
Embodiment 1：
A kind of blended electrospun fibers of organic-inorganic, are made by following steps：
1) preparation of calcium phosphate nano particle：0.6g hydroxyapatite nanoparticles are weighed, in anhydrous ethanol medium
Ball milling mixing, after crossing 200 mesh sieves, dry 1h, obtains hydroxyapatite nanoparticle in 50 DEG C of baking ovens；
2) it is 2 the Poly(D,L-lactide-co-glycolide that 0.75g molecular weight is 8-10w to be scattered in 3.65g volume ratios:1
Tetrahydrofuran-dimethylformamide in the mixed solvent, 150rpm vibration homogeneous 30min, obtains the dispersion liquid of degradable polymer；
3) hydroxyapatite nano made from step 1) is added in the dispersion liquid of the degradable polymer obtained to step 2)
Particle, after 150rpm vibrates homogeneous 30min, ultrasonic vibration homogeneous 30min, carries out electrostatic spinning, spinning solution extrusion after defoaming
Speed is 0.5mL/h, and voltage 15kv, collects distance 15cm, obtains organic-inorganic blending electrospun fibers.
Embodiment 2：
A kind of blended electrospun fibers of organic-inorganic, are made by following steps：
1) preparation of calcium phosphate nano particle：0.4g hydroxyapatite nanoparticles are weighed, in anhydrous ethanol medium
Ball milling mixing, after crossing 200 mesh sieves, dry 1h, obtains hydroxyapatite nanoparticle in 50 DEG C of baking ovens；
2) it is 1 the polylactic acid that 0.5g molecular weight is 8-10w to be scattered in 4.1g volume ratios:1 tetrahydrofuran-dimethyl methyl
Acid amides in the mixed solvent, 150rpm vibration homogeneous 30min, at 40 DEG C place 24 it is small when after, again 150rpm vibrate homogeneous 30
Minute simultaneously stands 30 minutes, obtains the dispersion liquid of degradable polymer；
3) hydroxyapatite nano made from step 1) is added in the dispersion liquid of the degradable polymer obtained to step 2)
Particle, after 150rpm vibrations homogeneous 30min, ultrasonic vibration homogeneous 30min, stand to bubble after eliminating immediately using mixed liquor into
Row electrostatic spinning, spinning solution extruded velocity are 0.8mL/h, and voltage 13kv, collects distance 15cm, obtain organic-inorganic blending
Electrospun fibers.
Embodiment 3：
A kind of blended electrospun fibers of organic-inorganic, are made by following steps：
1) preparation of calcium phosphate nano particle：0.48g hydroxyapatite nanoparticles are weighed, in anhydrous ethanol medium
Ball milling mixing, after crossing 200 mesh sieves, dry 1h, obtains hydroxyapatite nanoparticle in 50 DEG C of baking ovens；
2) it is 4 the polylactic acid that 0.6g molecular weight is 8-10w to be scattered in 3.92g volume ratios:3 tetrahydrofuran-dimethyl
Formamide in the mixed solvent, 150rpm vibration homogeneous 30min, at 40 DEG C place 24 it is small when after, again 150rpm vibrate homogeneous
30 minutes and stand 30 minutes, obtain the dispersion liquid of degradable polymer；
3) hydroxyapatite nano made from step 1) is added in the dispersion liquid of the degradable polymer obtained to step 2)
Particle, after 150rpm vibrates homogeneous 30min, ultrasonic vibration homogeneous 30min, stands to bubble and carries out electrostatic spinning after eliminating, spin
Silk solution extruded velocity is 0.6mL/h, and voltage 14kv, collects distance 15cm, obtains organic-inorganic blending electrospun fibers.
Embodiment 4：
A kind of blended electrospun fibers of organic-inorganic, are made by following steps：
1) preparation of calcium phosphate nano particle：0.32g hydroxyapatite nanoparticles are weighed, in anhydrous ethanol medium
Ball milling mixing, after crossing 200 mesh sieves, dry 1h, obtains hydroxyapatite nanoparticle in 50 DEG C of baking ovens；
2) it is 4 the polylactic acid that 0.4g molecular weight is 8-10w to be scattered in 4.28g volume ratios:3 tetrahydrofuran-dimethyl
Formamide in the mixed solvent, 150rpm vibration homogeneous 30min, at 40 DEG C place 24 it is small when after, again 150rpm vibrate homogeneous
30 minutes and stand 30 minutes, obtain the dispersion liquid of degradable polymer；
3) hydroxyapatite nano made from step 1) is added in the dispersion liquid of the degradable polymer obtained to step 2)
Particle, after 150rpm vibrates homogeneous 30min, ultrasonic vibration homogeneous 30min, stands to bubble and carries out electrostatic spinning after eliminating, spin
Silk solution extruded velocity is 1mL/h, and voltage 12kv, collects distance 15cm, obtains organic-inorganic blending electrospun fibers.
Embodiment 5：
A kind of bone cement, is made by following steps：
1) preparation of calcium phosphate nano particle：Absolute ethyl alcohol is added to disperse 7g type alpha tricalcium phosphates and 3g calcium dihydrogen phosphates,
After crossing 200 mesh sieves, dry 1h, obtains calcium phosphate nano particle in 50 DEG C of baking ovens；
2) preparation of electrospun fibers：The organic-inorganic blending electrospun fibers that Example 1 obtains；
3) preparation of solid phase components：The electrospun fibers that step 2) obtains after dry 1h, are cut into 50 DEG C of baking ovens
The short-movie of 3mm long, takes 0.5g electrospun fibers short-movies, is uniformly mixed, obtains with the calcium phosphate nano particle that step 1) obtains
To the solid phase components of organic-inorganic blending electrospun fibers enhancing composite bone cement；
4) preparation of solidify liquid：By chitosan, citric acid and water according to mass ratio be 1：3：100 ratio is mixed,
And it is sufficiently stirred obtained solidify liquid；
5) cure：The solidify liquid of the solid phase components of step 3) and step 4) is pressed into 1.2g:The weight ratio mixing of 1mL, then
It is respectively filled in mould, is placed in 37 DEG C, cures in 100% humidity environment.Hardening time is 1h, its compression strength is dried after the demoulding
For 45.21MPa.
Embodiment 6：
A kind of bone cement, is made by following steps：
1) preparation of calcium phosphate nano particle：Add absolute ethyl alcohol to disperse 8g tetracalcium phosphates and 2g calcium monohydrogen phosphates, cross 200
After mesh sieve, dry 1h, obtains calcium phosphate nano particle in 50 DEG C of baking ovens；
2) preparation of electrospun fibers：The organic-inorganic blending electrospun fibers that Example 2 obtains；
3) preparation of solid phase components：The electrospun fibers that step 2) obtains after dry 1h, are cut into 50 DEG C of baking ovens
The short-movie of 3mm long, takes 0.8g electrospun fibers short-movies, is uniformly mixed, obtains with the calcium phosphate nano particle that step 1) obtains
To the solid phase components of organic-inorganic blending electrospun fibers enhancing composite bone cement；
4) preparation of solidify liquid：By chitosan, citric acid and water according to mass ratio be 1：4：100 ratio is mixed,
And it is sufficiently stirred obtained solidify liquid；
5) cure：The solidify liquid of the solid phase components of step 3) and step 4) is pressed into 1.5g:The weight ratio mixing of 1mL, then
It is respectively filled in mould, is placed in 37 DEG C, cures in 100% humidity environment.Hardening time is 1h, its compression strength is dried after the demoulding
For 49.35MPa.
Embodiment 7：
A kind of bone cement, is made by following steps：
1) preparation of calcium phosphate nano particle：Absolute ethyl alcohol is added to disperse 6g tetracalcium phosphates and 4g bata-tricalcium phosphates, mistake
After 200 mesh sieves, dry 1h, obtains calcium phosphate nano particle in 50 DEG C of baking ovens；
2) preparation of electrospun fibers：The organic-inorganic blending electrospun fibers that Example 3 obtains；
3) preparation of solid phase components：The electrospun fibers that step 2) obtains after dry 1h, are cut into 50 DEG C of baking ovens
The short-movie of 3mm long, takes 0.8g electrospun fibers short-movies, is uniformly mixed, obtains with the calcium phosphate nano particle that step 1) obtains
To the solid phase components of organic-inorganic blending electrospun fibers enhancing composite bone cement；
4) preparation of solidify liquid：By chitosan, citric acid and water according to mass ratio be 2：3：100 ratio is mixed,
And it is sufficiently stirred obtained solidify liquid；
5) cure：The solidify liquid of the solid phase components of step 3) and step 4) is pressed into 2g:The weight ratio mixing of 1mL, Ran Houfen
Do not insert in mould, be placed in 37 DEG C, cure in 100% humidity environment.Hardening time is 1h, its compression strength is dried after the demoulding and is
44.64MPa。
Embodiment 8：
A kind of bone cement, is made by following steps：
1) preparation of calcium phosphate nano particle：7g partially crystallized calcium phosphates and 3g calcium monohydrogen phosphates are added into absolute ethyl alcohol point
Dissipate, after crossing 200 mesh sieves, dry 1h, obtains calcium phosphate nano particle in 50 DEG C of baking ovens；
2) preparation of electrospun fibers：The organic-inorganic blending electrospun fibers that Example 4 obtains；
3) preparation of solid phase components：The electrospun fibers that step 2) obtains after dry 1h, are cut into 50 DEG C of baking ovens
The short-movie of 3mm long, takes 0.7g electrospun fibers short-movies, is uniformly mixed, obtains with the calcium phosphate nano particle that step 1) obtains
To the solid phase components of organic-inorganic blending electrospun fibers enhancing composite bone cement；
4) preparation of solidify liquid：By chitosan, citric acid and water according to mass ratio be 2：4：100 ratio is mixed,
And it is sufficiently stirred obtained solidify liquid；
5) cure：The solidify liquid of the solid phase components of step 3) and step 4) is pressed into 1.6g:The weight ratio mixing of 1mL, then
It is respectively filled in mould, is placed in 37 DEG C, cures in 100% humidity environment.Hardening time is 1h, its compression strength is dried after the demoulding
For 42.94MPa.
The above embodiment is only the preferred embodiment of the present invention, it is impossible to the scope of protection of the invention is limited with this,
The change and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed scope.
Claims (9)
1. a kind of preparation method of bone cement, it is characterised in that comprise the following steps：
1) preparation of calcium phosphate nano particle：Absolute ethyl alcohol is added to disperse calcium phosphate material, ball milling, sieves, dry；
The calcium phosphate material is tricalcium phosphate, tetracalcium phosphate, calcium octahate phosphate, calcium monohydrogen phosphate, hydroxyapatite, pyrophosphoric acid
It is more than one or both of calcium, calcium metaphosphate and calcium dihydrogen phosphate；
2) preparation of electrospun fibers：By degradable polymer, homogeneous, the calcium phosphate for adding step 1) are received in solvent
Rice grain carries out homogeneous, carries out electrostatic spinning after standing defoaming, obtains electrospun fibers；The degradable polymer is poly- breast
Acid-co-glycolic acid, polylactic acid, polyglycolic acid, polyhydroxyalkanoate, makrolon, polycaprolactone and polyethanol
It is more than one or both of acid；The solvent is tetrahydrofuran and/or dimethylformamide；Spinning solution extruded velocity is
0.1-5mL/h, voltage 10-20kv, collects distance 10-20cm；
3) preparation of solid phase components：The electrospun fibers that step 2) is obtained are dried, and are cut short, are received with the calcium phosphate of step 1)
Rice grain presses 1:The weight ratio mixing of (10-100), obtains solid phase components；
4) preparation of solidify liquid：According to mass ratio it is (0-2) by chitosan, citric acid and water：(3-4)：100 ratio is mixed
Close, and be sufficiently stirred obtained solidify liquid；
5) cure：The solidify liquid of the solid phase components of step 3) and step 4) is pressed into (1-2) g:The weight ratio mixing of 1mL, cures
To bone cement.
2. preparation method as claimed in claim 1, it is characterised in that in step 1), the calcium phosphate nano particle be by
Any two kinds in tetracalcium phosphate, type alpha tricalcium phosphate, bata-tricalcium phosphate, calcium dihydrogen phosphate, calcium monohydrogen phosphate, calcium phosphate are pressed (1-2):
1 weight ratio mixing composition.
3. preparation method as claimed in claim 1, it is characterised in that in step 2), the degradable polymer for polylactic acid-
Co-glycolic acid, polylactic acid or polycaprolactone.
4. preparation method as claimed in claim 1, it is characterised in that in step 2), the solvent is tetrahydrofuran and diformazan
Base formamide presses (1-2):1 volume ratio composition.
5. preparation method as claimed in claim 1, it is characterised in that in step 3), electrospun fibers are cut short into 2-5cm
Length.
6. preparation method as claimed in claim 1, it is characterised in that in step 3), electrospun fibers are received with calcium phosphate
The weight ratio of rice grain is (0.5-0.8):10.
7. preparation method as claimed in claim 1, it is characterised in that in step 4), the deacetylation of the chitosan is 70-
100%, weight average molecular weight is 2000-100 ten thousand.
8. preparation method as claimed in claim 1, it is characterised in that in step 5), solidification temperature is 37 DEG C, and solidification humidity is
100%.
A kind of 9. bone cement obtained such as claim 1-8 any one of them methods.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022134163A1 (en) * | 2020-12-25 | 2022-06-30 | 光华临港工程应用技术研发(上海)有限公司 | Calcium phosphate-based cement potting material and preparation method therefor |
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| CN1657483A (en) * | 2005-02-07 | 2005-08-24 | 武汉理工大学 | Preparation method of calcium phosphate composite bone cement |
| CN101128226A (en) * | 2004-11-24 | 2008-02-20 | 生物合成物有限公司 | Bioabsorbable composite material fiber |
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| CN103668940A (en) * | 2013-12-18 | 2014-03-26 | 华东理工大学 | Surface modification fiber-reinforced composite bone cement as well as preparation method and application thereof |
| CN103877621A (en) * | 2014-04-08 | 2014-06-25 | 广东药学院 | Electrospun fiber-reinforced calcium phosphate bone cement composite material and application thereof |
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| US6291547B1 (en) * | 1995-02-08 | 2001-09-18 | Materials Evolution And Development Usa Inc. | Bone cement compositions comprising fused fibrous compounds |
| CN101128226A (en) * | 2004-11-24 | 2008-02-20 | 生物合成物有限公司 | Bioabsorbable composite material fiber |
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| WO2022134163A1 (en) * | 2020-12-25 | 2022-06-30 | 光华临港工程应用技术研发(上海)有限公司 | Calcium phosphate-based cement potting material and preparation method therefor |
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