CN101829358A - Preparation method of calcium phosphate ceramics/chitosan-hydroxyapatite composite coating porous material - Google Patents
Preparation method of calcium phosphate ceramics/chitosan-hydroxyapatite composite coating porous material Download PDFInfo
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Abstract
The invention provides a method for preparing a calcium phosphate ceramics/chitosan-hydroxyapatite composite coating porous material, which comprises steps of: selecting porous calcium phosphate ceramics with hole size of 300-600 microns and of a net-shaped hole structure, adding nano-hydroxyapatite in chitosan acetum with the mass percent of 0.5-5 percent to prepare a suspension, coating the surface of the porous calcium phosphate ceramics, and carrying out crosslinking process to obtain the calcium phosphate ceramics/chitosan-hydroxyapatite composite coating porous material, wherein the mass ratio of the hydroxyapatite to the chitosan in the chitosan-hydroxyapatite suspension is (6-1):(1-5). The invention has the technical scheme that a chitosan-hydroxyapatite coating is prepared on the porous calcium phosphate ceramics, thereby enhancing the surface bioactivity of the porous material; the coating is an organic-inorganic composite material and integrates the advantages of the chitosan and the hydroxyapatite, and the constitution of the surface of the material can be conveniently adjusted according to the actual need, thereby endowing the porous material with better combination property.
Description
Technical field
The present invention relates to be applied to the manufacturing process of the compound porous bone renovating material of organic and inorganic of biomedical sector, relate in particular to the method for preparing Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material.
Background technology
At present, in the bone defect repair, osteanagenesis is mainly undertaken by three kinds of fundamental mechanisms, and promptly bone conduction, osteogenesis and bone are induced.Bone conduction is meant that freshman bone tissue along the biocompatible materials surface or the hole growth of creeping, mainly occurs in material and host bone contact site, and its ossification is limited, and osteoconductive material only provides the biocompatibility interface for the new bone tissue migration; The skeletonization stem cell that osteogenesis is meant defect is in the bioactivity surface generation directed differentiation and the process of bringing out osteanagenesis; Bone is induced the process that mescenchymal stem cell is differentiated to form osseous tissue of not breaking up that is meant blood vessel migration on every side, and the material with osteoinductive usually can be at non-bony site skeletonization, as bringing out bone formation in subcutaneous or muscle.Hydroxyapatite (HA) and tricalcium phosphate (calcium phosphate biomaterial such as β-TCP), close with the main inorganic composition of vertebrates bone and tooth, have excellent biological compatibility, can be on the interface behind the implantable bone tissue chemical bonding very strong with bone formation, be applied clinical.Cavernous calcium phosphate bioceramic not only has excellent biological compatibility and unique may command degradation property, and has osteoinductive under certain conditions, thereby becomes one of focus of investigation of materials.
As bone tissue restoration, alternate material, always wish to have mechanical strength preferably again having the active while of good biological.The porous calcium phosphate bioceramic adopts the method preparation of high temperature sintering usually, and existing result of study shows that high temperature sintering can reduce the biological activity of material to a certain extent.Therefore, in actual fabrication process, for improving the biologic activity of material, hope can suitably reduce the sintering temperature of pottery, but the intensity of material often be cannot say for sure to demonstrate,prove; And the intensity in order to guarantee that material is higher, the normal again method that improves sintering temperature or prolong sintering time that adopts causes the material grains size to become big, and degree of crystallinity increases, and the result is that its biological activity descends.
For the calcium phosphate bioceramic that still can obtain having higher mechanical property when the lower temperature sintering, developed several different methods: 1. add the sintering aid acceleration of sintering; 2. use high-strength second carry out mutually toughness reinforcing; 3. pre-burning is toughness reinforcing; 4. rare earth is toughness reinforcing; 5. prepare crystal whisker toughened complex phase ceramic; 6. compound etc. with zirconium oxide, aluminium oxide.By said method, though can improve the mechanical property of Ca-P ceramic greatly, the biology performance to pottery produces certain negative effect simultaneously.After adding toughening sintering aid, form the vitrification sintering mostly, sintered body crystal grain is big, and bone conductibility and osteoinductive can reduce; The toughening sintering aid that has can bring some undesirable dephasigns; The composite reinforcing material that adds all is a bio-inert material usually, can not degrade in the practical application, will retain in vivo for a long time.
For fear of the defective that conventional high temperature furnace sintering brings, explore adopting different sintering process to prepare calcium phosphorus bioactive ceramics, as adopting microwave sintering, discharge plasma sintering etc.Although these methods can obtain having than normal sintering the porous ceramics of better combination property, pottery still will stand pyroprocess.As seen, mechanical property and the biological activity that improves bioceramic simultaneously is a pair of contradiction.
In order to remedy the deficiency of homogenous material, prepare biomaterial with better performance, in recent years, composite bone repairing material has obtained more research.Chitosan is a kind of natural biodegradable polysaccharide, its catabolite is a glucosamine, certain alkalescence is arranged, to human body and organize nontoxic, harmless, and have excellent biocompatibility, biodegradability, be ideal cell epimatrix material, can promote multiplely histiocyticly to stick and breed.Nanometer hydroxyapatite (nano-HA) is having bigger superiority aspect physicochemical property and biology except the characteristic with traditional HA.The porous support of nanometer hydroxyapatite and the compound preparation of chitosan, on the basis that keeps good biological performance, the intensity of material, toughness all obtain raising to a certain degree, but still have the technology instability, deficiency such as manufacturing cycle is long and composite materials property is on the low side.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, a kind of method for preparing Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material is provided, under the condition that is not changing existing technology, prepare and have the active porous bone repair material of good biological.
Purpose of the present invention is achieved through the following technical solutions:
The preparation method of Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material, characteristics are: select pore-size at 300～600 μ m, have the porous Ca-P ceramic of reticulated cell gap structure, in mass percent is to add nanometer hydroxyapatite in 0.5～5% the chitosan-acetic acid solution to make suspension, the porous Ca-P ceramic is carried out surface-coated, the mass ratio of hydroxyapatite and chitosan is (6～1) in chitosan-hydroxyapatite suspension: (1～5), through crosslinking Treatment, obtain Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material.
Further, the preparation method of above-mentioned Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material, at first, taking by weighing 0.5～5% the chitosan that accounts for the solution gross mass, to be dissolved in mass concentration be in 1～5% the acetum, to make chitosan-acetic acid solution;
Secondly, the mass ratio by hydroxyapatite and chitosan is (6～1): (1～5) takes by weighing the nanometer hydroxyapatite powder;
Then, the nanometer hydroxyapatite powder is joined in the chitosan-acetic acid solution, stir and obtain chitosan-hydroxyapatite suspension;
Then, pore-size is slowly immersed in chitosan-hydroxyapatite suspension at 300～600 μ m, porous Ca-P ceramic with reticulated cell gap structure, slowly propose after the submergence fully again, centrifugal treating in centrifuge is removed unnecessary suspension;
At last, after the porous material drying with coating, put into mass concentration and be 0.25～2.5% cross-linking agent solution crosslinking Treatment, clean, obtain Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material with dehydrated alcohol.
Further, the preparation method of above-mentioned Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material, wherein, the time of described crosslinking Treatment is 3～24h; Described cross-linking agent is any one in formaldehyde, glutaraldehyde, the Biformyl.
Again further, the preparation method of above-mentioned Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material, wherein, centrifuge speed is at 250～500 rev/mins during described centrifugal treating.
Substantive distinguishing features and obvious improvement that technical solution of the present invention is outstanding are mainly reflected in:
1. the present invention prepares chitosan-hydroxyapatite coating layer on porous calcium phosphorus ceramic matrix, has improved the surface bioactive of porous material;
2. matrix is the Ca-P ceramic with reticulated cell gap structure, can adopt existing prepared, wide accommodation; Coating is a composite organic-inorganic material, combines the advantage of chitosan and nanometer hydroxyapatite, and can adjust the composition of material surface according to actual needs easily, gives the porous material comprehensive performance;
3. coating is handled and is all carried out at room temperature, for medicine carrying, the composite growth factor of material are had laid a good foundation later on.
Description of drawings
Below in conjunction with accompanying drawing technical solution of the present invention is described further:
The SEM photo on the Ca-P ceramic surface of Fig. 1: embodiment 1;
The SEM photo on the Ca-P ceramics/chitosan of Fig. 2: embodiment 1-hydroxyapatite composite porous bone renovating material surface.
The specific embodiment
Mainly be subjected to the influence of its surface nature because of the biological activity of material, so, should on the basis that guarantees porous calcium phosphate bioceramic mechanical property, carry out suitable surface treatment to it, to improve the surface bioactive of material, make porous ceramics have excellent comprehensive performances.
The present invention prepares the method for Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material, select pore-size at 300～600 μ m, porous Ca-P ceramic with reticulated cell gap structure, in mass percent is to add the certain amount of nano hydroxyapatite in 0.5～5% the chitosan-acetic acid solution to make suspension, the porous Ca-P ceramic is carried out surface-coated, the mass ratio of hydroxyapatite and chitosan is (6～1) in chitosan-hydroxyapatite suspension: (1～5), through crosslinking Treatment, obtain Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material.On porous calcium phosphorus ceramic matrix, prepare chitosan-hydroxyapatite coating layer, to improve the surface bioactive of porous material.
Embodiment 1:
Taking by weighing the chitosan that accounts for solution gross mass 1%, to be dissolved in mass concentration be in 1% the acetum, to make chitosan-acetic acid solution;
By the mass ratio of hydroxyapatite and chitosan is to take by weighing the nanometer hydroxyapatite powder at 2: 1;
The nanometer hydroxyapatite powder is added in the chitosan-acetic acid solution, fully stir and obtain chitosan-hydroxyapatite suspension;
Pore-size is slowly immersed in chitosan-hydroxyapatite suspension at 300～600 μ m, porous Ca-P ceramic with reticulated cell gap structure, slowly proposes again after the submergence fully, in centrifuge in 400 rev/mins of centrifugal treating, to remove unnecessary suspension;
After the porous material drying of coating, put into mass concentration and be 0.25% glutaraldehyde solution cross-linking agent solution crosslinking Treatment 3h, clean with dehydrated alcohol then, obtain Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material.
Fig. 1 can show that the Ca-P ceramic surface is slick granule.Fig. 2 can show that after the processing, ceramic matrix is covered with composite coating, and coarse injustice becomes on microcosmic.After coating was handled, very big variation had taken place in the surface topography of ceramic material, and on the microcosmic, originally slick particle surface has applied hackly composite coating.
Embodiment 2:
Taking by weighing the chitosan that accounts for solution gross mass 5%, to be dissolved in mass concentration be in 3% the acetum, to make chitosan-acetic acid solution;
By the mass ratio of hydroxyapatite and chitosan is to take by weighing the nanometer hydroxyapatite powder at 1: 1;
The nanometer hydroxyapatite powder is added in the chitosan-acetic acid solution, fully stir and obtain chitosan-hydroxyapatite suspension;
Pore-size is slowly immersed in chitosan-hydroxyapatite suspension at 300～600 μ m, porous Ca-P ceramic with reticulated cell gap structure, slowly proposes again after the submergence fully, in centrifuge in 500 rev/mins of centrifugal treating, to remove unnecessary suspension;
After the porous material drying of coating, put into mass concentration and be 1.5% glyoxal solution cross-linking agent solution crosslinking Treatment 14h, clean with dehydrated alcohol then, obtain Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material.
Embodiment 3:
Taking by weighing the chitosan that accounts for solution gross mass 3%, to be dissolved in mass concentration be in 5% the acetum, to make chitosan-acetic acid solution;
By the mass ratio of hydroxyapatite and chitosan is to take by weighing the nanometer hydroxyapatite powder at 3: 5;
The nanometer hydroxyapatite powder is added in the chitosan-acetic acid solution, fully stir and obtain chitosan-hydroxyapatite suspension;
Pore-size is slowly immersed in chitosan-hydroxyapatite suspension at 300～600 μ m, porous Ca-P ceramic with reticulated cell gap structure, slowly proposes again after the submergence fully, in centrifuge in 450 rev/mins of centrifugal treating, to remove unnecessary suspension;
After the porous material drying of coating, put into mass concentration and be 2.5% formalin cross-linking agent solution crosslinking Treatment 24h, clean with dehydrated alcohol then, obtain Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material.
Embodiment 4:
Taking by weighing the chitosan that accounts for solution gross mass 0.5%, to be dissolved in mass concentration be in 1% the acetum, to make chitosan-acetic acid solution;
By the mass ratio of hydroxyapatite and chitosan is to take by weighing the nanometer hydroxyapatite powder at 1: 5;
The nanometer hydroxyapatite powder is added in the chitosan-acetic acid solution, fully stir and obtain chitosan-hydroxyapatite suspension;
Pore-size is slowly immersed in chitosan-hydroxyapatite suspension at 300～600 μ m, porous Ca-P ceramic with reticulated cell gap structure, slowly proposes again after the submergence fully, in centrifuge in 300 rev/mins of centrifugal treating, to remove unnecessary suspension;
After the porous material drying of coating, put into mass concentration and be 0.5% glutaraldehyde solution crosslinking Treatment 3h, clean with dehydrated alcohol then, obtain Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material.
Embodiment 5:
Taking by weighing the chitosan that accounts for solution gross mass 2%, to be dissolved in mass concentration be in 4% the acetum, to make chitosan-acetic acid solution;
By the mass ratio of hydroxyapatite and chitosan is to take by weighing the nanometer hydroxyapatite powder at 6: 1;
The nanometer hydroxyapatite powder is added in the chitosan-acetic acid solution, fully stir and obtain chitosan-hydroxyapatite suspension;
Pore-size is slowly immersed in chitosan-hydroxyapatite suspension at 300～600 μ m, porous Ca-P ceramic with reticulated cell gap structure, slowly proposes again after the submergence fully, in centrifuge in 250 rev/mins of centrifugal treating, to remove unnecessary suspension;
After the porous material drying of coating, put into mass concentration and be 1.25% glutaraldehyde solution cross-linking agent solution crosslinking Treatment 10h, clean with dehydrated alcohol then, obtain Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material.
In sum, the present invention prepares chitosan-hydroxyapatite coating layer on porous calcium phosphorus ceramic matrix, improved the surface bioactive of porous material; Matrix is the Ca-P ceramic with reticulated cell gap structure, can adopt existing prepared, wide accommodation; Coating is a composite organic-inorganic material, combines the advantage of chitosan and nanometer hydroxyapatite, and can adjust the composition of material surface according to actual needs easily, gives the porous material comprehensive performance; Coating is handled and is all carried out at room temperature, for medicine carrying, the composite growth factor of material are had laid a good foundation later on.
What need understand is: the above only is a preferred implementation of the present invention; for those skilled in the art; under the prerequisite that does not break away from the principle of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. the preparation method of Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material, it is characterized in that: select pore-size at 300～600 μ m, porous Ca-P ceramic with reticulated cell gap structure, in mass percent is to add nanometer hydroxyapatite in 0.5～5% the chitosan-acetic acid solution to make suspension, the mass ratio of hydroxyapatite and chitosan is (6～1) in chitosan-hydroxyapatite suspension: (1～5), the porous Ca-P ceramic is carried out surface-coated, through crosslinking Treatment, obtain Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material.
2. the preparation method of Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material according to claim 1 is characterized in that:
At first, taking by weighing the chitosan that accounts for solution gross mass 0.5～5%, to be dissolved in mass concentration be in 1～5% the acetum, to make chitosan-acetic acid solution;
Secondly, the mass ratio by hydroxyapatite and chitosan is (6～1): (1～5) takes by weighing the nanometer hydroxyapatite powder;
Then, the nanometer hydroxyapatite powder is joined in the chitosan-acetic acid solution, stir and obtain chitosan-hydroxyapatite suspension;
Then, pore-size is slowly immersed in chitosan-hydroxyapatite suspension at 300～600 μ m, porous Ca-P ceramic with reticulated cell gap structure, slowly propose after the submergence fully again, centrifugal treating in centrifuge is removed unnecessary suspension;
At last, after the porous material drying with coating, put into mass concentration and be 0.25～2.5% cross-linking agent solution crosslinking Treatment, clean, obtain Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material with dehydrated alcohol.
3. the preparation method of Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material according to claim 2, it is characterized in that: the time of described crosslinking Treatment is 3～24h.
4. the preparation method of Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material according to claim 2, it is characterized in that: described cross-linking agent is any one in formaldehyde, glutaraldehyde, the Biformyl.
5. the preparation method of Ca-P ceramics/chitosan-hydroxyapatite composite coating porous material according to claim 2 is characterized in that: centrifuge speed is at 250～500 rev/mins during described centrifugal treating.
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Cited By (8)
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| CN103272281A (en) * | 2013-05-30 | 2013-09-04 | 上海师范大学 | Carbon fiber-based hydroxyapatite/chitosan composite porous scaffold material and preparation method thereof |
| CN103272269A (en) * | 2013-05-30 | 2013-09-04 | 上海师范大学 | Hydroxyapatite/chitosan composite coating and preparation method thereof |
| CN103623463A (en) * | 2013-11-15 | 2014-03-12 | 无锡中科光远生物材料有限公司 | Preparation method of electrostatic spinning coating material for accelerating growth of bone tissues |
| CN103866368A (en) * | 2012-12-12 | 2014-06-18 | 北京纳通科技集团有限公司 | Calcium and phosphate salt biofilm layer and pulse electrochemistry modification method thereof |
| CN107890585A (en) * | 2017-10-31 | 2018-04-10 | 温州医科大学附属第二医院、温州医科大学附属育英儿童医院 | A kind of composite ceramics support and preparation method thereof |
| CN108404226A (en) * | 2018-05-25 | 2018-08-17 | 姜香 | A kind of preparation method of high-compatibility coating bracket material |
| CN110354818A (en) * | 2019-08-05 | 2019-10-22 | 泰州禾益新材料科技有限公司 | The hydroxy apatite-base composite material and preparation method of arsenic, fluorine in a kind of absorption water |
| CN113209382A (en) * | 2021-04-13 | 2021-08-06 | 浙江理工大学 | Three-dimensional reticular chitosan slow-release coating and preparation method thereof |
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| CN103866368A (en) * | 2012-12-12 | 2014-06-18 | 北京纳通科技集团有限公司 | Calcium and phosphate salt biofilm layer and pulse electrochemistry modification method thereof |
| CN103866368B (en) * | 2012-12-12 | 2016-04-06 | 北京纳通科技集团有限公司 | Calcium microcosmic salt biological membranous layer and pulse electrochemical method of modifying thereof |
| CN103272281A (en) * | 2013-05-30 | 2013-09-04 | 上海师范大学 | Carbon fiber-based hydroxyapatite/chitosan composite porous scaffold material and preparation method thereof |
| CN103272269A (en) * | 2013-05-30 | 2013-09-04 | 上海师范大学 | Hydroxyapatite/chitosan composite coating and preparation method thereof |
| CN103272281B (en) * | 2013-05-30 | 2014-10-29 | 上海师范大学 | Carbon fiber-based hydroxyapatite/chitosan composite porous scaffold material and preparation method thereof |
| CN103623463A (en) * | 2013-11-15 | 2014-03-12 | 无锡中科光远生物材料有限公司 | Preparation method of electrostatic spinning coating material for accelerating growth of bone tissues |
| CN107890585A (en) * | 2017-10-31 | 2018-04-10 | 温州医科大学附属第二医院、温州医科大学附属育英儿童医院 | A kind of composite ceramics support and preparation method thereof |
| CN108404226A (en) * | 2018-05-25 | 2018-08-17 | 姜香 | A kind of preparation method of high-compatibility coating bracket material |
| CN110354818A (en) * | 2019-08-05 | 2019-10-22 | 泰州禾益新材料科技有限公司 | The hydroxy apatite-base composite material and preparation method of arsenic, fluorine in a kind of absorption water |
| CN110354818B (en) * | 2019-08-05 | 2020-07-03 | 泰州禾益新材料科技有限公司 | Hydroxyapatite-based composite material for adsorbing arsenic and fluorine in water and preparation method thereof |
| CN113209382A (en) * | 2021-04-13 | 2021-08-06 | 浙江理工大学 | Three-dimensional reticular chitosan slow-release coating and preparation method thereof |
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Application publication date: 20100915 |