CN103028143A - Preparation method of bone repairing material with magnetic-thermal therapy function - Google Patents
Preparation method of bone repairing material with magnetic-thermal therapy function Download PDFInfo
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- CN103028143A CN103028143A CN2013100002619A CN201310000261A CN103028143A CN 103028143 A CN103028143 A CN 103028143A CN 2013100002619 A CN2013100002619 A CN 2013100002619A CN 201310000261 A CN201310000261 A CN 201310000261A CN 103028143 A CN103028143 A CN 103028143A
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Abstract
The invention discloses a preparation method of a bone repairing material with a magnetic-thermal therapy function. The preparation method comprises the steps of preparing a ferric nitrate, zinc nitrate and citric acid mixed solution, mixing uniformly, adjusting pH to 4, obtaining a bright green magnetic zinc ferrite precursor solution, preparing a dicalcium silicate precursor with ethyl orthosilicate and calcium nitrate, adding a dicalcium silicate precursor solution to the bright green magnetic zinc ferrite precursor solution, stirring by thermostatic waterbath till green gel is formed, drying the green gel to dried gel, finally allowing the dried gel to be subjected to temperature programming and high-temperature rapid cooling, and obtaining the bone repairing material with the magnetic-thermal therapy function. The bone repairing material prepared by the method can repair bone defects caused by tumor cells, kills the residual tumor cells selectively by the action of thermal therapy, solves the problem that the bone defects caused by a cancer are recurrent at high proportion after simple repairing, better facilitates recovery of a patient, and improves life quality of the patient.
Description
Technical field
The present invention relates to a kind of preparation method with bone renovating material of magnetic thermotherapeutic function.
Background technology
Bone tumor scrapes or excises as main take operation at present, and operation is made every effort to thoroughly in order to avoid the residual tumor cell causes the recurrence of cancerating.Yet thoroughly removed because tumor cell is very difficult, so the postoperative patient relapse rate can be in any more.In order to reduce patient's Postoperative recurrent rate, improve Quality of Life, the related researcher has invented the bone renovating material with medicine carrying function, when making the bone reparation can by discharge slowly medicine progressively kill the residual tumor cell.By the method, patient's Postoperative recurrent rate has obtained obvious reduction.Regrettably, the most normal tissue cell of medicine of killing off tumor cells also can produce killing action at present, finds in the experiment, and in medicine kill tumor cell, the normal cell in the drug release scope also has been subject to very large damage.So, research and develop the novel focus that composite that the bone repair simultaneously can selective killing residual tumor cell just becomes present bone tumor type bone renovating material field that has.The magnetic thermotherapy can heat up in the target area circulation under the effect of extraneous alternating magnetic field, and then reaches the effect of thermotherapy as a kind of method in the thermotherapy.The method is according to the difference of tumor cell with heat tolerance between the normal cell, can the selectively killing tumor cell and do not damage normal tissue cell.Yet how with magnetic thermotherapy material with the effective combination of bone renovating material, preparation has the dummy of the two function concurrently, has limited research and the application of magnetic thermotherapy type bone renovating material.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with bone renovating material of magnetic thermotherapeutic function.Described bone renovating material with magnetic thermotherapeutic function is a kind of ferromagnetic iron oxysome/dicalcium silicate composite.After overcoming Patients with Bone Tumor tradition debridement, relapse rate remains high and the large problem of medicine for treating tumor thing toxic and side effects, satisfies the demand of the osseous tissue defect repair that is caused by tumor.
Concrete steps are:
(1) weight portion 0.5-1.5 part ferric nitrate, 0.5-1.5 part zinc nitrate and the mixing of 0.5-1.5 part citric acid are dissolved in the deionized water, be made into the solution that concentration is 5-20g/100mL, the magnetic agitation mix homogeneously, then use the pH value of ammonia regulator solution to be 4-6, obtain bright green solution and be the Zn ferrite precursor solution.
(2) parts by volume 0.5-1.5 part ethyl orthosilicate is joined in the deionized water, be made into the solution that volume fraction is 0.5-5%, the magnetic agitation mix homogeneously, then the pH value that adds the ammonia regulator solution is 4-6, aquation 20-40 minute, the lime nitrate that adds again weight portion 1.5-2.5 part obtains the dicalcium silicate precursor solution.
(3) the dicalcium silicate precursor solution that the Zn ferrite precursor solution that step (1) is made and step (2) make mixes, and the magnetic agitation mix homogeneously uses the pH value of ammonia regulator solution to be 4-6, forms green colloidal sol.
(4) 40-70 ℃ of drying of process removed free water to the colloidal sol that step (3) is obtained successively, a 100-150 ℃ drying is removed constitution water, finally obtains the rufous xerogel.
(5) xerogel that step (4) is obtained at first is positioned over interior 300-500 ℃ of Muffle furnace and ignites, and removes the organic facies in the xerogel; Then be warming up to 500-700 ℃ with 6-10 ℃/min, made the preliminary crystallization of Zn ferrite in constant temperature 1-4 hour; Then be warming up to 1000-1200 ℃ with 9-11 ℃/min, made the dicalcium silicate crystallization in constant temperature 4-6 hour and made Zn ferrite be converted into the ferromagnetism crystalline state, obtain the pitchy powder by the high temperature quenching at last, be the bone renovating material with magnetic thermotherapeutic function.
Described ethyl orthosilicate and ammonia are chemical pure.
Characteristics of the present invention:
(1) Zn ferrite presoma and dicalcium silicate presoma are mixed by solution state, avoided the problem of admixture of powder lack of homogeneity, realized the even distribution of ferrite composition in whole material.
(2) dry by stagewise, can fast and safely obtain the composite material precursor powder.
(3) by fractional crystallizaton, obtain the crystalline solid of Zn ferrite and dicalcium silicate, high temperature quenching has then obtained keeping the ferromagnetism Zn ferrite of high temperature crystallization attitude.
(4) the bone renovating material porosity of preparation is higher, reaches 50-80%; Be distributed with a large amount of micropores in the bone renovating material, mutually connect between the Kong Yukong; Particle diameter is 400-1000nm, and mean diameter is 700nm; The hot transfer power of magnetic is 7W/g, under the action of alternating magnetic field of 500Oe, 400kHz, can rise 30 ℃ from room temperature in 3-8 minute; Experimental result shows that this bone renovating material has good biocompatibility and osteoinductive in simulated body fluid experiment and the body.
The present invention is as a kind of Multifunctional bone repair materials, have good biocompatibility and osteoinductive, also has simultaneously the magnetic thermotherapeutic function, under the effect of extraneous alternating magnetic field, can selectively killing residual tumor cell and do not affect normal tissue cell, at the damaged clinical treatment of tumprigenicity bone huge potentiality are arranged.
Description of drawings
Fig. 1 is the process chart of the embodiment of the invention.
Fig. 2 is the XRD spectra of the composite of embodiment of the invention preparation.
Fig. 3 is the particle size distribution figure of the composite of embodiment of the invention preparation.
Fig. 4 is the surface topography electron scanning micrograph of composite after osteoblast is cultivated 1 day and 3 days of embodiment of the invention preparation, and a is 1 day; After b is 3 days.
The specific embodiment
Below in conjunction with concrete example the present invention is further elaborated, but the present invention is not limited to following examples.Described method is conventional method if no special instructions.Described raw material all can obtain from open commercial sources if no special instructions.
Embodiment:
(1) 8.95 gram Fe(NO3)39H2Os, 0.79 gram zinc nitrate hexahydrate and 5.26 gram citric acids mixing are dissolved in the deionized water, be made into the solution that concentration is 15g/100mL, the magnetic agitation mix homogeneously, then use the pH value to 4 of ammonia regulator solution, obtain the bright green solution of stable existence, i.e. the Zn ferrite precursor solution.
(2) 10 ml ethyl orthosilicates are joined in the deionized water, be made into volume fraction and be 3.5% solution, the magnetic agitation mix homogeneously, then the pH value to 4 that adds the ammonia regulator solution, 60 ℃ of aquations 30 minutes add calcium nitrate tetrahydrate 6 grams, obtain the dicalcium silicate precursor solution.
(3) the dicalcium silicate precursor solution with the Zn ferrite precursor solution of step (1) gained and step (2) gained mixes, the magnetic agitation mix homogeneously, and 60 ℃ of aquations 24 hours form green colloidal sol.
(4) colloidal sol that step (3) is obtained successively through 60 ℃ of dryings removed free water in 24 hours, 120 ℃ of dryings were removed constitution water in 24 hours, finally obtained the rufous xerogel.
(5) xerogel that step (4) is obtained at first is positioned over interior 300 ℃ of Muffle furnace and ignites, and removes the organic facies in the xerogel; Then be warming up to 600 ℃ with 8 ℃/min, constant temperature made the preliminary crystallization of Zn ferrite in 2 hours; Then be warming up to 1100 ℃ with 10 ℃/min, constant temperature made the dicalcium silicate crystallization in 5 hours and makes Zn ferrite be converted into the ferromagnetism crystalline state, obtained the pitchy powder by the high temperature quenching at last, was the bone renovating material with magnetic thermotherapeutic function.
Described ethyl orthosilicate and ammonia are chemical pure.
Claims (1)
1. preparation method with bone renovating material of magnetic thermotherapeutic function is characterized in that concrete steps are:
(1) weight portion 0.5-1.5 part ferric nitrate, 0.5-1.5 part zinc nitrate and the mixing of 0.5-1.5 part citric acid are dissolved in the deionized water, be made into the solution that concentration is 5-20g/100mL, the magnetic agitation mix homogeneously, then use the pH value of ammonia regulator solution to be 4-6, obtain bright green solution and be the Zn ferrite precursor solution;
(2) parts by volume 0.5-1.5 part ethyl orthosilicate is joined in the deionized water, be made into the solution that volume fraction is 0.5-5%, the magnetic agitation mix homogeneously, then the pH value that adds the ammonia regulator solution is 4-6, aquation 20-40 minute, the lime nitrate that adds again weight portion 1.5-2.5 part obtains the dicalcium silicate precursor solution;
(3) the dicalcium silicate precursor solution that the Zn ferrite precursor solution that step (1) is made and step (2) make mixes, and the magnetic agitation mix homogeneously uses the pH value of ammonia regulator solution to be 4-6, forms green colloidal sol;
(4) 40-70 ℃ of drying of process removed free water to the colloidal sol that step (3) is obtained successively, a 100-150 ℃ drying is removed constitution water, finally obtains the rufous xerogel;
(5) xerogel that step (4) is obtained at first is positioned over interior 300-500 ℃ of Muffle furnace and ignites, and removes the organic facies in the xerogel; Then be warming up to 500-700 ℃ with 6-10 ℃/min, made the preliminary crystallization of Zn ferrite in constant temperature 1-4 hour; Then be warming up to 1000-1200 ℃ with 9-11 ℃/min, made the dicalcium silicate crystallization in constant temperature 4-6 hour and made Zn ferrite be converted into the ferromagnetism crystalline state, obtain the pitchy powder by the high temperature quenching at last, be the bone renovating material with magnetic thermotherapeutic function;
Described ethyl orthosilicate and ammonia are chemical pure.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101367525A (en) * | 2008-09-19 | 2009-02-18 | 中国科学院上海硅酸盐研究所 | Sodium calcium silicate biological material, preparation method and uses thereof |
| US20100196514A1 (en) * | 2009-02-02 | 2010-08-05 | Chung Shan Medical University | Calcium silicate-based composite cement and methods for the preparation |
| CN102357260A (en) * | 2011-07-22 | 2012-02-22 | 四川大学 | Design and preparation method for novel calcium-magnesium-silicon multiphase bioactive ceramic, and use thereof |
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- 2013-01-03 CN CN2013100002619A patent/CN103028143A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101367525A (en) * | 2008-09-19 | 2009-02-18 | 中国科学院上海硅酸盐研究所 | Sodium calcium silicate biological material, preparation method and uses thereof |
| US20100196514A1 (en) * | 2009-02-02 | 2010-08-05 | Chung Shan Medical University | Calcium silicate-based composite cement and methods for the preparation |
| CN102357260A (en) * | 2011-07-22 | 2012-02-22 | 四川大学 | Design and preparation method for novel calcium-magnesium-silicon multiphase bioactive ceramic, and use thereof |
Non-Patent Citations (4)
| Title |
|---|
| 《Journal of Materials Science：Materials in Medicine》 20110108 Yumin Jiang etal. "Preparation of magnetic and bioactive calcium zinc iron silicon oxide composite for hyperthermia treatment of bone cancer and repair of bone defects" 第721-729页 1 第22卷, 第3期 * |
| 《中国陶瓷》 20011031 何新华 等 "Zn铁氧体-SiO2复合材料溶胶-凝胶制备工艺优化研究" 第16-19，31页 1 第37卷, 第5期 * |
| YUMIN JIANG ETAL.: ""Preparation of magnetic and bioactive calcium zinc iron silicon oxide composite for hyperthermia treatment of bone cancer and repair of bone defects"", 《JOURNAL OF MATERIALS SCIENCE：MATERIALS IN MEDICINE》 * |
| 何新华 等: ""Zn铁氧体-SiO2复合材料溶胶-凝胶制备工艺优化研究"", 《中国陶瓷》 * |
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Application publication date: 20130410 |