CN106362218A - Preparation method of porous alpha-TCP microballoon with anti-bacterial function - Google Patents

Preparation method of porous alpha-TCP microballoon with anti-bacterial function Download PDF

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CN106362218A
CN106362218A CN201610946615.2A CN201610946615A CN106362218A CN 106362218 A CN106362218 A CN 106362218A CN 201610946615 A CN201610946615 A CN 201610946615A CN 106362218 A CN106362218 A CN 106362218A
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microsphere
porous
tcp
preparation
gelatin
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CN106362218B (en
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于翔
徐茜
杨柳
张�浩
王娜
杨秀琴
宋会芬
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Hubei Xinyong Biological Environmental Protection Technology Co ltd
Jiuer Xi'an Intellectual Property Service Co ltd
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Henan Institute of Engineering
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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
    • A61L27/56—Porous materials, e.g. foams or sponges
    • 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
    • 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
    • A61L27/14—Macromolecular materials
    • A61L27/22—Polypeptides or derivatives thereof, e.g. degradation products
    • A61L27/222—Gelatin
    • 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
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/54—Biologically active materials, e.g. therapeutic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L89/00—Compositions of proteins; Compositions of derivatives thereof
    • 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
    • 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

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Dispersion Chemistry (AREA)
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Abstract

The invention discloses a preparation method of a porous alpha-TCP microballoon with an anti-bacterial function. The method comprises the following steps of (1) ball-milling monocalcium phosphate, calcium carbonate and zinc sulfate, uniformly mixing, and drying to prepare composite powder;(2) preparing a gelatin solution, preparing gelatin according to a certain proportion, uniformly mixing the gelatin and the composite powder, utilizing an electrostatic drop generation method for preparing a gelatin and composite powder microballoon;(3) sintering the gelatin and composite powder microballoon step by step to obtain the porous alpha-TCP microballoon with the anti-bacterial function. The method for preparing the porous alpha-TCP microballoon provided by the invention is simpler, the preparation efficiency is higher, and meanwhile, the porous alpha-TCP microballoon has higher porosity and has a certain anti-bacterial function, can be applicable to treatment of infected bone defects, and is wider in application prospect.

Description

A kind of preparation method of the porous α-tcp microsphere with antibacterial functions
Technical field
The invention belongs to bone defect healing field, particularly to a kind of porous α-tcp microsphere with antibacterial functions Simple preparation method and application.
Background technology
Bone is one of most important tissue of human body, and it can play protection intracorporeal organ, provides attachment for muscle, produces blood The effect of liquid cell.At present, due to human body because wound, aging, motion, inflammation, tumor and the marrow caused by congenital malformation scorching, The orthopaedic disease patients such as bone tuberculosis, infectious Cranial defect are countless, and the health giving people class brings great harm, always A difficult problem on Orthopedic Clinical.Bone renovating material is can to substitute or repair human body disease damage osseous tissue and realize regeneration function one kind newly The material of type is therefore, very big to the requirement of bone renovating material.The material of application bone defect healing is varied at present, wherein α Type tricalcium phosphate (α-tcp) bone material has good effect, and application is relatively broad, compared with other carrier materials, α-tcp In addition to the biocompatibility with height, can temporarily moulding and self-curing, and there is degradability, osteogenic activity and solidification process etc. The advantages of warm nature, therefore obtain the extensive concern of international material circle and medical circle.
Further, since Cranial defect would generally be along with the generation of inflammation during repairing, the method commonly used at present is Oral antibiotic, or in wound site intramuscular injection antibiotic.But, long-term oral or intramuscular injection antibiotic can make patient produce How permanently effective for antibiotic is therefore acted on the Hot Contents that affected part has also become current research by the problem of drug resistance.Mesh Anti-inflammation class medicine is exactly mixed by most method of front employing with bone renovating material, allows medicament to uniformly release Put, but, simple is mixed into the effect being difficult to play slow release in bone renovating material by medicine.At present, for α-tcp, adopt α-tcp is exactly prepared into porous microsphere by most methods, then adsorbs antibacterials in porous α-tcp microsphere, thus Reach the effect of slow release.The method of α-tcp porous microsphere preparation at present mainly has extrusion molding, Drop Condensation method, microemulsion method, mesh Front these methods adopting are all prepared by material based on α-tcp, and these methods are complex, relatively costly.
Content of the invention
In order to solve some shortcomings existing for current bone impairment renovation material, and porous α-tcp microspheres are relatively For complicated problem, the present invention provides a kind of preparation method of the porous α-tcp microsphere with antibacterial functions, will prepare first α- The raw material of tcp is that inorganic antiseptic is compound with macromolecule is prepared into microsphere, is then passed through gradient sintering and is prepared into porous microsphere, leads to Cross the gas that the reaction of itself formed and macromolecule decompose led to space so that antibacterial porous α-tcp microsphere have higher Porosity.
For solving above-mentioned technical problem, the present invention employs the following technical solutions:
A kind of preparation method of the porous α-tcp microsphere with antibacterial functions, step is as follows:
(1) dalcium biphosphate and Calcium Carbonate are added in ethanol solution, are subsequently adding zinc sulfate, ball milling, sucking filtration, vacuum is done Dry, obtain cah2po4And caco3Composite granule；
(2) composite granule is added in gelatin solution, is uniformly mixing to obtain mixed solution, will be mixed using micro-injection pump molten Liquid is clamp-oned in low temperature coagulating bath, simultaneously applied voltage on the syringe needle of micro-injection pump, obtains the compound of gelatin and composite granule Microsphere, after washing with alcohol, is vacuum dried at normal temperatures；
(3) dried complex microsphere is put in high temperature sintering furnace and be sintered, obtain with antibacterial work(after being cooled to room temperature Porous α-tcp the microsphere of energy.
In described step (1) ratio of dalcium biphosphate and the amount of the material of Calcium Carbonate is 2.13:1；The material of zinc sulfate Amount account for dalcium biphosphate and Calcium Carbonate total material amount 1% ~ 5%.
In described step (1), the time of ball milling is 0.5-1h.
In described step (1), the mass fraction of gelatin solution is 15%-35%, and gelatin is 1:1- with the mass ratio of composite granule 1:2.5.
In described step (2), the injection rate of micro-injection pump is 20-50ml/h, is carried on micro-injection pump syringe needle Voltage is 5-20kv.
Sintering procedure in described step (3) is: wherein sintering procedure is: with the ramp of 2-10 DEG C/min to 500 DEG C, be incubated 0.5-1h, then according to the ramp of 2-10 DEG C/min is to 800 DEG C, after insulation 1-2h slow cooling to room temperature, so Afterwards again by high temperature sintering furnace with the ramp of 2-10 DEG C/min to 1350 DEG C, insulation 2-3h after, be rapidly decreased to room temperature.
The porous microsphere being obtained using the preparation method of the described porous α-tcp microsphere with antibacterial functions, hole It is interconnected, porosity is 30-60%.
It is applied to using the porous microsphere that the preparation method of the described porous α-tcp microsphere with antibacterial functions is obtained The treatment of various sizes of infectivity Cranial defect.
Beneficial effects of the present invention: 1, the present invention is not added with any organic solvent during preparation, thus will not Defective material remains, material has good biocompatibility；2nd, the method for present invention preparation porous α-tcp microsphere is more simple Single, so that manufacturing cycle is greatly shortened, improve preparation efficiency, and the porous microsphere porosity being obtained is higher, can make drug loading Greatly improve；3rd, the present invention directly inorganic antiseptic is added in porous α-tcp microsphere during preparation, makes antibacterial Scattered more uniform in microsphere, the slow-release time of antibacterial can be made to extend, so that the utilization rate of medicine is greatly improved, improve The therapeutic effect of Cranial defect.
Specific embodiment
With reference to specific embodiment, the present invention will be further described.It should be understood that following examples are merely to illustrate this Invention can make one according to the content of foregoing invention not for limiting the scope of the present invention, the person skilled in the art in this field Nonessential improvement and adjustment a bit.
Embodiment 1
The preparation method step of the porous α-tcp microsphere with antibacterial functions of the present embodiment is as follows:
(1) by 73.2g(0.426mol) calcium hydrogen phosphate (cahpo4·2h2O) and 20g(0.2mol) Calcium Carbonate (caco3) be added to In ethanol solution, it is subsequently adding 1.0g(0.006mol) zinc sulfate (znso4), ball milling 0.5h, sucking filtration, vacuum drying, obtain cah2po4And caco3Composite granule；
(2) 15g gelatin is added in 100ml water and is configured to gelatin solution, then above-mentioned for 15g composite granule is added to gelatin In solution, after stirring, obtain mixed solution, using micro-injection pump, mixed solution is clamp-oned by temperature with the speed of 20ml/h It is about the voltage that 5kv is applied in 4 DEG C of water on syringe needle simultaneously, the gelatin obtaining utilizes second with the complex microsphere of composite granule After alcohol is washed, it is vacuum dried at normal temperatures；
(3) complex microsphere obtained above is put in high temperature sintering furnace and be sintered, wherein sintering procedure is: with 2 DEG C/min Ramp to 500 DEG C, and be incubated 0.5h, then according to the ramp of 2 DEG C/min is to 800 DEG C, slowly drop after insulation 1h Warm to room temperature, then again by high temperature sintering furnace with the ramp of 2 DEG C/min to 1350 DEG C, after insulation 2h, rapid lower the temperature, cooling Obtain the porous α-tcp microsphere with antibacterial functions to room temperature, record the porosity of porous α-tcp microsphere using bet method It is about 54.5%.
Embodiment 2
The preparation method step of the porous α-tcp microsphere with antibacterial functions of the present embodiment is as follows:
(1) by 73.2g(0.426mol) calcium hydrogen phosphate (cahpo4·2h2O) and 20g(0.2mol) Calcium Carbonate (caco3) be added to In ethanol solution, it is subsequently adding 3.0g(0.018mol) zinc sulfate (znso4), ball milling 1h, sucking filtration, vacuum drying, obtain cah2po4And caco3Composite granule；
(2) 35g gelatin is added in 100ml water and is configured to gelatin solution, then above-mentioned for 87.5g composite granule is added to bright In sol solution, after stirring, obtain mixed solution, with the speed of 50ml/h, mixed solution is clamp-oned using micro-injection pump low The voltage of 20kv, in warm coagulating bath, is applied on syringe needle simultaneously, the gelatin obtaining utilizes ethanol with the complex microsphere of composite granule After being washed, it is vacuum dried at normal temperatures；
(3) complex microsphere obtained above is put in high temperature sintering furnace and be sintered, wherein sintering procedure is: with 10 DEG C/min Ramp to 500 DEG C, and be incubated 1h, then according to the ramp of 10 DEG C/min is to 800 DEG C, slow cooling after insulation 2h To room temperature, then again by high temperature sintering furnace with the ramp of 10 DEG C/min to 1350 DEG C, after insulation 3h, rapid lower the temperature, cooling Obtain the porous α-tcp microsphere with antibacterial functions to room temperature, record the porosity of porous α-tcp microsphere using bet method It is about 31.8%.
Embodiment 3
The preparation method step of the porous α-tcp microsphere with antibacterial functions of the present embodiment is as follows:
(1) by 73.2g(0.426mol) calcium hydrogen phosphate (cahpo4·2h2O) and 20g(0.2mol) Calcium Carbonate (caco3) be added to In ethanol solution, it is subsequently adding 5.0g zinc sulfate (znso4) (0.030mol), ball milling 1h, sucking filtration, vacuum drying, obtain cah2po4And caco3Composite granule；
(2) 25g gelatin is added in 100ml water and is configured to gelatin solution, then above-mentioned for 50g composite granule is added to gelatin In solution, after stirring, obtain mixed solution, using micro-injection pump, mixed solution is clamp-oned by low temperature with the speed of 30ml/h The voltage of 15kv, in coagulating bath, is applied on syringe needle simultaneously, the gelatin obtaining is entered using ethanol with the complex microsphere of composite granule After row washing, it is vacuum dried at normal temperatures；
(3) complex microsphere obtained above is put in high temperature sintering furnace and be sintered, wherein sintering procedure is: with 5 DEG C/min Ramp to 500 DEG C, and be incubated 1h, then according to the ramp of 5 DEG C/min is to 800 DEG C, slow cooling after insulation 2h To room temperature, then again by high temperature sintering furnace with the ramp of 5 DEG C/min to 1350 DEG C, after insulation 3h, rapid lower the temperature, be cooled to Obtain the porous α-tcp microsphere with antibacterial functions after room temperature, using the porosity that bet method records porous α-tcp microsphere be 43.7%.
Embodiment 4
The preparation method step of the porous α-tcp microsphere with antibacterial functions of the present embodiment is as follows:
(1) by 73.2g(0.426mol) calcium hydrogen phosphate (cahpo4·2h2O) and 20g(0.2mol) Calcium Carbonate (caco3) be added to In ethanol solution, it is subsequently adding 3.0g zinc sulfate (znso4) (0.018mol), ball milling 0.5h, sucking filtration, vacuum drying, obtain cah2po4And caco3Composite granule；
(2) 25g gelatin is added in 100ml water and is configured to gelatin solution, then above-mentioned for 50g composite granule is added to gelatin In solution, after stirring, obtain mixed solution, using micro-injection pump, mixed solution is clamp-oned by low temperature with the speed of 40ml/h The voltage of 20kv, in coagulating bath, is applied on syringe needle simultaneously, the gelatin obtaining is entered using ethanol with the complex microsphere of composite granule After row washing, it is vacuum dried at normal temperatures；
(3) complex microsphere obtained above is put in high temperature sintering furnace and be sintered, wherein sintering procedure is: with 5 DEG C/min Ramp to 500 DEG C, and be incubated 1h, then according to the ramp of 5 DEG C/min is to 800 DEG C, slow cooling after insulation 2h To room temperature, then again by high temperature sintering furnace with the ramp of 5 DEG C/min to 1350 DEG C, after insulation 2h, rapid lower the temperature, be cooled to Obtain the porous α-tcp microsphere with antibacterial functions after room temperature, using the porosity that bet method records porous α-tcp microsphere be 44.3%.
Ultimate principle and principal character and the advantages of the present invention of the present invention have been shown and described above.The skill of the industry The simply explanation it should be appreciated that the present invention is not restricted to the described embodiments, described in above-described embodiment and description for the art personnel The principle of the present invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these Changes and improvements both fall within scope of the claimed invention.Claimed scope by appending claims and Its equivalent thereof.

Claims (8)

1. a kind of preparation method of the porous α-tcp microsphere with antibacterial functions is it is characterised in that step is as follows:
(1) dalcium biphosphate and Calcium Carbonate are added in ethanol solution, are subsequently adding zinc sulfate, ball milling, sucking filtration, vacuum is done Dry, obtain cah2po4And caco3Composite granule；
(2) composite granule is added in gelatin solution, is uniformly mixing to obtain mixed solution, will be mixed using micro-injection pump molten Liquid is clamp-oned in low temperature coagulating bath, simultaneously applied voltage on the syringe needle of micro-injection pump, obtains the compound of gelatin and composite granule Microsphere, after washing with alcohol, is vacuum dried at normal temperatures；
(3) dried complex microsphere is put in high temperature sintering furnace and be sintered, obtain with antibacterial work(after being cooled to room temperature Porous α-tcp the microsphere of energy.
2. the porous α-tcp microsphere with antibacterial functions according to claim 1 preparation method it is characterised in that: In described step (1) ratio of dalcium biphosphate and the amount of the material of Calcium Carbonate is 2.13:1；The amount of the material of zinc sulfate accounts for phosphorus Acid dihydride calcium and the 1% ~ 5% of the amount of Calcium Carbonate total material.
3. the porous α-tcp microsphere with antibacterial functions according to claim 1 preparation method it is characterised in that: In described step (1), the time of ball milling is 0.5-1h.
4. the porous α-tcp microsphere with antibacterial functions according to claim 1 preparation method it is characterised in that: In described step (1), the mass fraction of gelatin solution is 15%-35%, and gelatin is 1:1-1:2.5 with the mass ratio of composite granule.
5. the porous α-tcp microsphere with antibacterial functions according to claim 1 preparation method it is characterised in that: In described step (2), the injection rate of micro-injection pump is 20-50ml/h, and the voltage being carried on micro-injection pump syringe needle is 5- 20kv.
6. the porous α-tcp microsphere with antibacterial functions according to claim 1 preparation method it is characterised in that: Sintering procedure in described step (3) is: wherein sintering procedure is: with the ramp of 2-10 DEG C/min to 500 DEG C, insulation 0.5-1h, then according to the ramp of 2-10 DEG C/min is to 800 DEG C, after insulation 1-2h, slow cooling, to room temperature, then will again High temperature sintering furnace after insulation 2-3h, is rapidly decreased to room temperature with the ramp of 2-10 DEG C/min to 1350 DEG C.
7. it is obtained using the preparation method of the arbitrary described porous α-tcp microsphere with antibacterial functions of claim 1 ~ 6 Porous microsphere it is characterised in that: described porous microsphere hole is interconnected, porosity be 30-60%.
8. it is obtained using the preparation method of the arbitrary described porous α-tcp microsphere with antibacterial functions of claim 1 ~ 6 Porous microsphere is applied to the treatment of various sizes of infectivity Cranial defect.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108178656A (en) * 2018-01-11 2018-06-19 江西理工大学 A kind of high porosity porous ceramics microballoon and preparation method thereof
CN114225094A (en) * 2021-11-17 2022-03-25 丽水市中心医院 Gelatin composite embolism microsphere containing nano calcium carbonate, preparation method thereof and drug-loaded embolism microsphere

Citations (1)

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Publication number Priority date Publication date Assignee Title
US20040076685A1 (en) * 2002-07-11 2004-04-22 Merck Patent Gmbh Method of preparing porous calcium phosphate morsels and granules via gelatin processing

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
US20040076685A1 (en) * 2002-07-11 2004-04-22 Merck Patent Gmbh Method of preparing porous calcium phosphate morsels and granules via gelatin processing

Non-Patent Citations (1)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108178656A (en) * 2018-01-11 2018-06-19 江西理工大学 A kind of high porosity porous ceramics microballoon and preparation method thereof
CN108178656B (en) * 2018-01-11 2020-10-20 江西理工大学 High-porosity porous ceramic microsphere and preparation method thereof
CN114225094A (en) * 2021-11-17 2022-03-25 丽水市中心医院 Gelatin composite embolism microsphere containing nano calcium carbonate, preparation method thereof and drug-loaded embolism microsphere

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