CN106730027B - A kind of preparation method of bone cement microballoon - Google Patents
A kind of preparation method of bone cement microballoon Download PDFInfo
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- CN106730027B CN106730027B CN201611003353.2A CN201611003353A CN106730027B CN 106730027 B CN106730027 B CN 106730027B CN 201611003353 A CN201611003353 A CN 201611003353A CN 106730027 B CN106730027 B CN 106730027B
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- bone cement
- microballoon
- slurry
- calcium
- liquid
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- 239000002639 bone cement Substances 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002002 slurry Substances 0.000 claims abstract description 47
- 230000003075 superhydrophobic effect Effects 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000007921 spray Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229920002313 fluoropolymer Polymers 0.000 claims abstract description 16
- 239000004811 fluoropolymer Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 84
- 235000011132 calcium sulphate Nutrition 0.000 claims description 44
- 239000001175 calcium sulphate Substances 0.000 claims description 22
- 239000011521 glass Substances 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 17
- 210000000988 bone and bone Anatomy 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 12
- MWKXCSMICWVRGW-UHFFFAOYSA-N calcium;phosphane Chemical compound P.[Ca] MWKXCSMICWVRGW-UHFFFAOYSA-N 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- 238000002513 implantation Methods 0.000 claims description 9
- -1 perfluoroethylene-propylene Chemical group 0.000 claims description 9
- 230000003068 static effect Effects 0.000 claims description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000004411 aluminium Substances 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 claims description 7
- 239000004568 cement Substances 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims description 6
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 claims description 6
- 239000004137 magnesium phosphate Substances 0.000 claims description 6
- 229910000157 magnesium phosphate Inorganic materials 0.000 claims description 6
- 229960002261 magnesium phosphate Drugs 0.000 claims description 6
- 235000010994 magnesium phosphates Nutrition 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 230000003993 interaction Effects 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- 239000011505 plaster Substances 0.000 claims description 3
- 238000000634 powder X-ray diffraction Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 239000003595 mist Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 10
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- 239000011737 fluorine Substances 0.000 claims 1
- 229910052731 fluorine Inorganic materials 0.000 claims 1
- 230000002209 hydrophobic effect Effects 0.000 claims 1
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 238000007711 solidification Methods 0.000 claims 1
- 230000008023 solidification Effects 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000004005 microsphere Substances 0.000 description 9
- 239000001506 calcium phosphate Substances 0.000 description 7
- 229910000389 calcium phosphate Inorganic materials 0.000 description 7
- 235000011010 calcium phosphates Nutrition 0.000 description 7
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 7
- 230000007547 defect Effects 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000007812 deficiency Effects 0.000 description 3
- 238000002242 deionisation method Methods 0.000 description 3
- 235000012424 soybean oil Nutrition 0.000 description 3
- 239000003549 soybean oil Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 206010005949 Bone cancer Diseases 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 208000027205 Congenital disease Diseases 0.000 description 1
- 208000029767 Congenital, Hereditary, and Neonatal Diseases and Abnormalities Diseases 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 206010039203 Road traffic accident Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000011132 hemopoiesis Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
Classifications
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/025—Other specific inorganic materials not covered by A61L27/04 - A61L27/12
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
- B05D1/04—Processes for applying liquids or other fluent materials performed by spraying involving the use of an electrostatic field
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2202/00—Metallic substrate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2506/00—Halogenated polymers
- B05D2506/10—Fluorinated polymers
Abstract
A kind of method of bone cement microballoon preparation, comprising the following steps: 1) using the fluoropolymer solutions of solvent configuration low-surface-energy, recycle electron spray that fluoropolymer is deposited on metallic conduction plate surface and form super-hydrophobic coat；2) bone cement and deionized water or solidify liquid are mixed well, configures bone cement slurry；3) bone cement slurry is quantitatively pipetted using liquid-transfering gun, and is dripped in super hydrophobic base, is stood at room temperature, after the complete self-curing of bone cement, obtains bone cement microballoon；Bone cement slurry by pipetting different volumes may be implemented to prepare various sizes of bone cement microballoon；With raw material availability height, the characteristics of microballoon good fluidity simple and easy to operate and prepared.
Description
Technical field
The invention belongs to inorganic bio preparation technical fields, and in particular to a kind of preparation method of bone cement microballoon.
Background technique
Bone is the bracket of human body, is responsible for the critical functions such as load-bearing, hematopoiesis and limb motion.However, with population old-age group
Aggravation, traffic accident, the appearance of bone tumour and the congenital disorders of change result in serious bone defect problem, because
This, it is significant for repairing bone defect to develop novel bone renovating material.
Inorganic bone cement is a kind of common bone renovating material, and this kind of material, which has, meets water or other water soluble solid agent
Can self-curing carry out the bone tissue of repair deficiency at block materials.Bone cement, which is processed into microballoon, to be had many advantages, such as, it can be with
Closely packed mode is filled in bone defect position, especially highly effective to the bone defect of some irregular, difficult fillings；Microballoon
Between gap be conducive to growing into for cambium and new vessels, and then the formation of new bone tissue can be accelerated；In addition, bone cement
Microballoon has excellent anti-disintegration after the molding of self-curing process in water, thus can give full play to its filling and mechanics branch
Support effect.Ye Jiandong etc. using by antiphase emulsifiable method prepare calcium phosphate bone cement microballoon (" a kind of self-setting calcium phosphate micro spheres and
Preparation method and application ", application number 201010188511.2), specific method is by gelatin/polysaccharide gum solidify liquid and calcium phosphate
Bone cement is deployed into slurry, then slurry is stirred in soybean oil and forms lotion, and is removed by the way of acetone and ethyl alcohol cleaning
Soybean oil is removed, and obtains wet calcium phosphate microsphere；It is then conserved aquation 2-7 days in climatic chamber, finally obtains calcium phosphate bone
Cement microballoon.This preparation method is extremely complex, long preparation period, in addition also introduces that soybean oil, acetone, ethyl alcohol etc. are toxic to be had
Harmful chemical substance；Bone cement huge number, in addition to calcium phosphate bone cement, there are also calcium sulfate bone cement, calcium silicon substrate bone cement, phosphorus
Sour magnesium bone cement etc., these bone cements all have potential application in Bone Defect Repari method, however this preparation method is only fitted
It is used to prepare calcium phosphate bone cement, the universality of this method is lower, and applicable surface is relatively narrow.These exactly above-mentioned disadvantages, limit
Application of this method in bio-medical field.
Summary of the invention
To overcome above-mentioned the deficiencies in the prior art, the purpose of the present invention is to provide a kind of sides of bone cement microballoon preparation
Method, there is raw material to utilize at the deficiencies of overcoming traditional preparation method complicated, poor using poisonous and harmful organic solvent and universality
The characteristics of rate is high, microballoon good fluidity simple and easy to operate and prepared.
To achieve the above object, the technical solution that the present invention just has is: a kind of method of bone cement microballoon preparation, including with
Lower step:
1) fluoropolymer solutions are configured using solvent, recycles electron spray that low-surface-energy macromolecule fluoropolymer sinks
Product forms super-hydrophobic coat in metallic conduction plate surface；
2) bone cement and deionized water or solidify liquid are mixed well, configures bone cement slurry；
3) the bone cement slurry quantitatively pipetted using liquid-transfering gun, and drip in super hydrophobic base, it stands at room temperature, to bone cement
After complete self-curing, bone cement microballoon is obtained；Bone cement slurry by pipetting different volumes may be implemented to prepare different sizes
Bone cement microballoon.
The concentration of fluoropolymer solutions described in step 1) be 0.010~0.100g/mL, solvent using dehydrated alcohol,
N,N-dimethylformamide or tetrahydrofuran.
The solvent is dehydrated alcohol.
Electron spray described in step 1) uses electrostatic spray, relevant parameter are as follows: flow velocity is 0.8~1.5mL/h, and voltage is
6.00~16.00 kV, collecting distance is 4~8cm, and acquisition time is 10~60min.
Metallic conduction plate described in step 1) is as receiver, using copper sheet, iron plate, aluminium sheet or stainless steel plate.
Bone cement described in step 2 uses half-H 2 O calcium sulphate, magnesium phosphate cement, calcium phosphorus base bone cement or calcium silicon substrate bone
Cement, preferred bone cement are half-H 2 O calcium sulphate.
Solidify liquid described in step 2 is ten water dobell's solutions or sodium radio-phosphate,P-32 solution.
The liquid-solid ratio of bone cement slurry described in step 2 is 0.1~3mL/g.
The volume that bone cement slurry is pipetted described in step 3) is 1~100 μ L.
The curing time at room temperature of bone cement slurry described in step 3) is 5~60min.
The beneficial effects of the present invention are:
Advantage is the present invention compared with prior art: 1) strong to water and aqueous solidify liquid using super hydrophobic surface
Repulsive interaction makes bone cement slurry be solidified into the microballoon of almost spherical in super hydrophobic surface in conjunction with bone cement self-curing characteristic,
Raw material availability can be effectively improved；2) preparation condition is mild, easy to operate, simple and easy to do, reproducible, and universality is strong；3)
Thus obtained microsphere morphological rules, size is uniform, and size is controllable, good fluidity, can better filling bone defects position.
Detailed description of the invention
Fig. 1 is the preparation flow schematic diagram of calcium sulfate microballoon of the present invention.
Fig. 2 is the stereoscan photograph and contact angle photo on super-hydrophobic coat surface obtained by electrostatic spray of the present invention.
Fig. 3 is the digital photograph figure of 1 calcium sulfate microballoon of the embodiment of the present invention.
Fig. 4 is the pure half-H 2 O calcium sulphate powder of the embodiment of the present invention 1 and calcium sulfate microballoon X ray diffracting spectrum.A: pure half water
Calcium sulfate powder, b: calcium sulfate microballoon.
Specific embodiment
Technical solution of the present invention will be clearly and completely described below.The embodiment described is only the present invention
A part of the embodiment, instead of all the embodiments.
Embodiment 1
A kind of bone cement method for preparing microsphere, comprising the following steps:
1) fluoropolymer being dissolved in dehydrated alcohol, configuration concentration is the solution of 0.044g/mL, 4h is stirred at room temperature, to
After polymer is completely dissolved, stop stirring, it is stand-by in implantation glass syringe after static 15min；Glass syringe is fixed on
On syringe pump, syringe needle connects the anode of high-voltage power supply；Using aluminium sheet as receiver, and connect cathode；Start to carry out electrostatic spray, obtain
To super-hydrophobic coat；Parameter during electrostatic spray is as follows: flow velocity 1.0mL/h, voltage 10.00kV, collects distance and is
5cm, acquisition time 30min；
2) it weighs 0.3g half-H 2 O calcium sulphate powder and is placed in perfluoroethylene-propylene beaker bottom, add the deionization of 0.45mL
Water is uniformly mixed immediately, forms uniform slurry, is configured to the half-H 2 O calcium sulphate slurry that liquid-solid ratio is 1.5mL/g；
3) it is dripped on the super-hydrophobic coat prepared by step 1) using the slurry that liquid-transfering gun pipettes 10 μ L, due to super-hydrophobic
Strong repulsive interaction of the surface to half-H 2 O calcium sulphate slurry, to form the microballoon of almost spherical；Then because of half-H 2 O calcium sulphate
The calcium sulfate microballoon of curing molding can be obtained after 30min for self-curing characteristic, collects, saves at room temperature.The calcium sulfate being prepared
Microballoon is by X-ray powder diffraction it is found that the ingredient for including in calcium sulfate microballoon has dead plaster, half-H 2 O calcium sulphate and two water
Calcium sulfate.
Fig. 1 is the preparation process schematic diagram of calcium sulfate microballoon, can understand from figure and get information about preparation process.
Fig. 2 is the stereoscan photograph and contact angle photo on super-hydrophobic coat surface obtained by electrostatic spray, it can be seen that institute
Prepares coating has ultra-hydrophobicity.
Fig. 3 is the digital photograph of calcium sulfate microballoon, and as can be seen from the figure prepared calcium sulfate microballoon size is uniform, closely
Like spherical shape.
Fig. 4 is the X-ray powder diffraction pattern of pure half-H 2 O calcium sulphate powder and calcium sulfate microballoon, it can be seen from the figure that
It include dead plaster, half-H 2 O calcium sulphate and calcium sulphate dihydrate in calcium sulfate microballoon.
Embodiment 2
A kind of bone cement method for preparing microsphere, comprising the following steps:
1) fluoropolymer is dissolved in dehydrated alcohol, configuration concentration is the solution of 0.015g/mL, stirs 4h at room temperature；To
After polymer is completely dissolved, stop stirring, static 15min will be stand-by in solution implantation glass syringe；By glass syringe
It is fixed on syringe pump, syringe needle connects the anode of high-voltage power supply；Using iron plate as receiver, and connect cathode；Start to carry out electrostatic
It is spraying, obtain super-hydrophobic coat；Parameter during electrostatic spray is as follows: flow velocity 0.8mL/h, voltage 6.00kV, collects
Distance is 4cm, acquisition time 60min；
2) it weighs 0.3g half-H 2 O calcium sulphate powder and is placed in perfluoroethylene-propylene beaker bottom, add the deionization of 0.15mL
Water is uniformly mixed immediately, forms uniform slurry, is configured to the half-H 2 O calcium sulphate slurry that liquid-solid ratio is 0.5mL/g；
3) it is dripped on the super-hydrophobic coat prepared by step 1) using the slurry that liquid-transfering gun pipettes 5 μ L, then because of half water sulphur
The self-curing characteristic of sour calcium can obtain the calcium sulfate microballoon for being solidified into almost spherical after 15 min, collect, save at room temperature.
Embodiment 3
A kind of bone cement method for preparing microsphere, comprising the following steps:
1) fluoropolymer is dissolved in dehydrated alcohol, configuration concentration is the solution of 0.09g/mL, stirs 4h at room temperature；To poly-
After conjunction object is completely dissolved, stop stirring, static 15min will be stand-by in solution implantation glass syringe；Glass syringe is fixed
On syringe pump, syringe needle connects the anode of high-voltage power supply；Using copper sheet as receiver, and cathode is connected, carries out electrostatic spray, obtain
Super-hydrophobic coat；Parameter during electrostatic spray is as follows: flow velocity 1.5mL/h, voltage 16.00kV, collects distance and is
8cm, acquisition time 10min；
2) it weighs 0.3g half-H 2 O calcium sulphate powder and is placed in perfluoroethylene-propylene beaker bottom, add the deionization of 0.9mL
Water is uniformly mixed immediately, forms uniform slurry, is configured to the half-H 2 O calcium sulphate slurry that liquid-solid ratio is 3mL/g；
3) it is dripped on the super-hydrophobic coat prepared by step 1) using the slurry that liquid-transfering gun pipettes 90 μ L, then because of half water
The calcium sulfate microballoon of curing molding can be obtained after 60min for the self-curing characteristic of calcium sulfate, collects, saves at room temperature.
Embodiment 4
A kind of bone cement method for preparing microsphere, comprising the following steps:
1) fluoropolymer is dissolved in n,N-Dimethylformamide, configuration concentration is the solution of 0.04 g/mL, at room temperature
Stir 4h；After object to be polymerized is completely dissolved, stop stirring, static 15 min will be stand-by in solution implantation glass syringe；By glass
Glass syringe is fixed on syringe pump, and syringe needle connects the anode of high-voltage power supply；Using stainless steel plate as receiver, and connect cathode；
Start to carry out electrostatic spray, obtains super-hydrophobic coat；Parameter during electrostatic spray is as follows: flow velocity 1.0mL/h, voltage
For 10.00kV, collecting distance is 5 cm, acquisition time 30min；
2) it weighs 0.5g magnesium phosphate cement and is placed in perfluoroethylene-propylene beaker bottom, add the ten water boron of 0.075mL
Acid sodium solution is uniformly mixed immediately, forms uniform slurry, is configured to the magnesium phosphate cement that liquid-solid ratio is 0.15mL/g
Slurry；
3) it is dripped on the super-hydrophobic coat prepared by step 1) using the slurry that liquid-transfering gun pipettes 10 μ L, then because of magnesium phosphate
The self-curing characteristic of bone cement can obtain the magnesium phosphate cement microballoon for being solidified into almost spherical after 8min, collect, protect at room temperature
It deposits.
Embodiment 5
A kind of bone cement method for preparing microsphere, comprising the following steps:
1) fluoropolymer is dissolved in tetrahydrofuran, configuration concentration is the solution of 0.04g/mL, stirs 4h at room temperature；To
After polymer is completely dissolved, stop stirring, static 15min will be stand-by in solution implantation glass syringe；By glass syringe
It is fixed on syringe pump, syringe needle connects the anode of high-voltage power supply；Using aluminium sheet as receiver, and connect cathode；Start just electrostatic
It is spraying, obtain super-hydrophobic coat；Parameter during electrostatic spray is as follows: flow velocity 1.0mL/h, voltage 10.00kV, receives
Integrate distance as 5cm, acquisition time 30min；
2) it weighs 0.5g calcium phosphorus base bone cement and is placed in perfluoroethylene-propylene beaker bottom, the sodium phosphate for adding 0.2mL is molten
Liquid is uniformly mixed immediately, forms uniform slurry, is configured to the calcium phosphorus base bone cement slurry that liquid-solid ratio is 0.4mL/g；
3) it is dripped on the super-hydrophobic coat prepared by step 1) using the slurry that liquid-transfering gun pipettes 10 μ L, then because of calcium phosphorus
The self-curing characteristic of base bone cement can obtain the calcium phosphorus base bone cement microballoon for being solidified into almost spherical after 25min, collect, room temperature
Lower preservation.
Embodiment 6
A kind of bone cement method for preparing microsphere, comprising the following steps:
1) fluoropolymer is dissolved in dehydrated alcohol, configuration concentration is the solution of 0.04g/mL, stirs 4h at room temperature；To poly-
After conjunction object is completely dissolved, stop stirring, static 15min will be stand-by in solution implantation glass syringe；Glass syringe is consolidated
It is scheduled on syringe pump, syringe needle connects the anode of high-voltage power supply；Using aluminium sheet as receiver, and connect cathode.Start to carry out electrostatic
Mist obtains super-hydrophobic coat；Parameter during electrostatic spray is as follows: flow velocity 1.0mL/h, voltage 10.00kV, collects
Distance is 5cm, acquisition time 30min；
2) it weighs 0.3g calcium silicon substrate bone cement and is placed in perfluoroethylene-propylene beaker bottom, add the deionized water of 0.3mL,
It is uniformly mixed immediately, forms uniform slurry, be configured to the calcium silicon substrate bone cement slurry that liquid-solid ratio is 1.0mL/g；
3) it is dripped on the super-hydrophobic coat prepared by step 1) using the slurry that liquid-transfering gun pipettes 10 μ L, then because of calcium silicon
The self-curing characteristic of base bone cement can obtain the calcium silicon substrate bone cement microballoon for being solidified into almost spherical after 60min, collect, room temperature
Lower preservation.
Claims (9)
1. a kind of method of bone cement microballoon preparation, which comprises the following steps:
1) fluoropolymer solutions are configured using solvent, recycles electron spray that fluoropolymer is deposited on metallic conduction plate surface
Form super-hydrophobic coat；
2) bone cement and deionized water or solidify liquid are mixed well, configures bone cement slurry；
3) bone cement slurry is quantitatively pipetted using liquid-transfering gun, and is dripped in super hydrophobic base, is stood at room temperature, completely certainly to bone cement
After solidification, bone cement microballoon is obtained；Bone cement slurry by pipetting different volumes may be implemented to prepare various sizes of bone water
Mud microballoon；
Bone cement described in step 2 uses half-H 2 O calcium sulphate, magnesium phosphate cement, calcium phosphorus base bone cement or calcium silicon substrate bone cement；
Solidify liquid described in step 2 is ten water dobell's solutions or sodium radio-phosphate,P-32 solution.
2. a kind of method of bone cement microballoon preparation according to claim 1, which is characterized in that fluorine-containing described in step 1)
The concentration of polymer solution is 0.010~0.100g/mL, and solvent uses dehydrated alcohol, n,N-Dimethylformamide or tetrahydro furan
It mutters.
3. a kind of method of bone cement microballoon preparation according to claim 1, which is characterized in that EFI described in step 1)
Mist uses electrostatic spray, relevant parameter are as follows: flow velocity is 0.8~1.5mL/h, and voltage is 6.00~16.00 kV, collects distance
For 4~8cm, acquisition time is 10~60min.
4. a kind of method of bone cement microballoon preparation according to claim 1, which is characterized in that metal described in step 1)
Conductive plate is as receiver, using copper sheet, iron plate, aluminium sheet or stainless steel plate.
5. a kind of method of bone cement microballoon preparation according to claim 1, which is characterized in that bone cement described in step 2
The liquid-solid ratio of slurry is 0.1~3mL/g.
6. a kind of method of bone cement microballoon preparation according to claim 1, which is characterized in that pipette bone described in step 3)
The volume of cement slurry is 1~100 μ L；The curing time at room temperature of bone cement slurry described in step 3) is 5~60min.
7. a kind of method of bone cement microballoon preparation according to claim 1, which comprises the following steps:
1) fluoropolymer is dissolved in dehydrated alcohol, configuration concentration is the solution of 0.044g/mL, stirs 4h at room temperature, to be polymerized
After object is completely dissolved, stop stirring, it is stand-by in implantation glass syringe after static 15min；Glass syringe is fixed on injection
On pump, syringe needle connects the anode of high-voltage power supply；Using aluminium sheet as receiver, and connect cathode；Start to carry out electrostatic spray, be surpassed
Hydrophobic coating；Parameter during electrostatic spray is as follows: flow velocity 1.0mL/h, voltage 10.00kV, and collecting distance is 5cm,
Acquisition time is 30min；
2) it weighs 0.3g half-H 2 O calcium sulphate powder and is placed in perfluoroethylene-propylene beaker bottom, add the deionized water of 0.45mL,
It is uniformly mixed immediately, forms uniform slurry, be configured to the half-H 2 O calcium sulphate slurry that liquid-solid ratio is 1.5mL/g；
3) it is dripped on the super-hydrophobic coat prepared by step 1) using the slurry that liquid-transfering gun pipettes 10 μ L, due to super hydrophobic surface
Strong repulsive interaction to half-H 2 O calcium sulphate slurry, to form the microballoon of almost spherical；Then because half-H 2 O calcium sulphate is from admittedly
Change characteristic, the calcium sulfate microballoon of curing molding can be obtained after 30min, collects, save at room temperature.The calcium sulfate microballoon being prepared
By X-ray powder diffraction it is found that the ingredient for including in calcium sulfate microballoon has dead plaster, half-H 2 O calcium sulphate and sulfate dihydrate
Calcium.
8. a kind of method of bone cement microballoon preparation according to claim 1, which comprises the following steps:
1) fluoropolymer is dissolved in tetrahydrofuran, configuration concentration is the solution of 0.04g/mL, stirs 4h at room temperature；It is to be polymerized
After object is completely dissolved, stop stirring, static 15min will be stand-by in solution implantation glass syringe；Glass syringe is fixed
On syringe pump, syringe needle connects the anode of high-voltage power supply；Using aluminium sheet as receiver, and connect cathode；Start just electrostatic spray,
Obtain super-hydrophobic coat；Parameter during electrostatic spray is as follows: flow velocity 1.0mL/h, voltage 10.00kV, collects distance
For 5cm, acquisition time 30min；
2) it weighs 0.5g calcium phosphorus base bone cement and is placed in perfluoroethylene-propylene beaker bottom, add the sodium radio-phosphate,P-32 solution of 0.2mL, stand
It is uniformly mixed, forms uniform slurry, be configured to the calcium phosphorus base bone cement slurry that liquid-solid ratio is 0.4mL/g；
3) it is dripped on the super-hydrophobic coat prepared by step 1) using the slurry that liquid-transfering gun pipettes 10 μ L, then because of calcium phosphorus base bone
The self-curing characteristic of cement can obtain the calcium phosphorus base bone cement microballoon for being solidified into almost spherical after 25min, collect, protect at room temperature
It deposits.
9. a kind of method of bone cement microballoon preparation according to claim 1, which comprises the following steps:
1) fluoropolymer is dissolved in dehydrated alcohol, configuration concentration is the solution of 0.09g/mL, stirs 4h at room temperature；Object to be polymerized
After being completely dissolved, stop stirring, static 15min will be stand-by in solution implantation glass syringe；Glass syringe is fixed on note
It penetrates on pump, syringe needle connects the anode of high-voltage power supply；Using copper sheet as receiver, and cathode is connected, carries out electrostatic spray, obtain super thin
Water coating；Parameter during electrostatic spray is as follows: flow velocity 1.5mL/h, voltage 16.00kV, and collecting distance is 8cm,
Acquisition time is 10min；
2) it weighs 0.3g half-H 2 O calcium sulphate powder and is placed in perfluoroethylene-propylene beaker bottom, add the deionized water of 0.9mL, stand
It is uniformly mixed, forms uniform slurry, be configured to the half-H 2 O calcium sulphate slurry that liquid-solid ratio is 3mL/g；
3) it is dripped on the super-hydrophobic coat prepared by step 1) using the slurry that liquid-transfering gun pipettes 90 μ L, then because of sulfate hemihydrate
The calcium sulfate microballoon of curing molding can be obtained after 60min for the self-curing characteristic of calcium, collects, saves at room temperature.
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| CN101850133A (en) * | 2010-06-01 | 2010-10-06 | 华南理工大学 | Self-setting calcium phosphate micro spheres, method for preparing same and application thereof |
| CN102815697A (en) * | 2012-08-28 | 2012-12-12 | 中国科学院过程工程研究所 | Preparation method of graphene oxide microspheres |
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| CN101850133A (en) * | 2010-06-01 | 2010-10-06 | 华南理工大学 | Self-setting calcium phosphate micro spheres, method for preparing same and application thereof |
| CN102815697A (en) * | 2012-08-28 | 2012-12-12 | 中国科学院过程工程研究所 | Preparation method of graphene oxide microspheres |
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