CN1389503A - In-situ compounding process of synthesizing nano composite chitosan/hydroxyapatite material - Google Patents
In-situ compounding process of synthesizing nano composite chitosan/hydroxyapatite material Download PDFInfo
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- CN1389503A CN1389503A CN 02136031 CN02136031A CN1389503A CN 1389503 A CN1389503 A CN 1389503A CN 02136031 CN02136031 CN 02136031 CN 02136031 A CN02136031 A CN 02136031A CN 1389503 A CN1389503 A CN 1389503A
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- solution
- chitosan
- calcium
- hydroxyapatite
- ion
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- 238000000034 method Methods 0.000 title claims abstract description 20
- 229920001661 Chitosan Polymers 0.000 title claims description 37
- 229910052588 hydroxylapatite Inorganic materials 0.000 title claims description 25
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 title claims description 25
- 239000000463 material Substances 0.000 title abstract description 7
- 238000013329 compounding Methods 0.000 title description 2
- 238000011065 in-situ storage Methods 0.000 title description 2
- 239000002114 nanocomposite Substances 0.000 title 1
- 230000002194 synthesizing effect Effects 0.000 title 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 12
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 6
- 239000011159 matrix material Substances 0.000 claims description 11
- 239000011575 calcium Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- -1 phosphoric acid salt compound Chemical class 0.000 claims description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- 229940085991 phosphate ion Drugs 0.000 claims description 6
- 159000000007 calcium salts Chemical class 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical group [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 2
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 2
- 229940045641 monobasic sodium phosphate Drugs 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 150000003016 phosphoric acids Chemical class 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical group [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 150000004676 glycans Chemical class 0.000 abstract description 9
- 239000000203 mixture Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 5
- 229940003871 calcium ion Drugs 0.000 abstract 2
- 229910052586 apatite Inorganic materials 0.000 abstract 1
- 239000011365 complex material Substances 0.000 abstract 1
- 238000005259 measurement Methods 0.000 abstract 1
- 210000000988 bone and bone Anatomy 0.000 description 9
- 239000000758 substrate Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- MSWZFWKMSRAUBD-IVMDWMLBSA-N 2-amino-2-deoxy-D-glucopyranose Chemical compound N[C@H]1C(O)O[C@H](CO)[C@@H](O)[C@@H]1O MSWZFWKMSRAUBD-IVMDWMLBSA-N 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- MSWZFWKMSRAUBD-UHFFFAOYSA-N beta-D-galactosamine Natural products NC1C(O)OC(CO)C(O)C1O MSWZFWKMSRAUBD-UHFFFAOYSA-N 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229960002442 glucosamine Drugs 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 230000008467 tissue growth Effects 0.000 description 1
- 230000029663 wound healing Effects 0.000 description 1
Landscapes
- Materials For Medical Uses (AREA)
Abstract
The invention provides a new method of under the normal temperature and ordinary pressure preparing the shell glycan/the oxhydryl-apatite nano complex materials. The method includes: at first make up the calcium-ion solution and the phosphor-ion solution, then evenly mix the calcium-ion solution with the phosphor-ion solution and add the acetic acid into the mixture to form the solution, then dissolve the shell glycan into this solution, then inject the solution containing the shell glycan into the mould to shape and dry it. Adopting the method of the invention can assure that the particles of the oxhydryl-apetite disperse in the shell glycan base body at the nano measurement (20-100 nm), and the materials made by using the invention's method are transparent and yellowish, and their mechanical property obviously is improved.
Description
Technical field
The present invention relates to the compound method for preparing chitosan/hydroxyapatite nano matrix material of original position.
Background technology
(Chitosan CS) is a kind of natural biodegradable polysaccharide to chitosan, and its degraded product is for having weakly alkaline glucosamine, to human body and organize nontoxic, harmless.It also has natural pharmaceutical activity, anti-tumor activity, antiinflammation except having excellent biocompatibility, impaired biological physical efficiency is induced special cells, accelerates wound healing.
(Hydroxyapatite, chemical structural formula HA) are (Ca to hydroxyapatite
10(OH)
2(PO
4)
6), be the main component (containing 60～70%) of human body natural's bone, have the guided bone of fabulous biological activity and osseous tissue growth.Proved that the HA kind plants the growth of physical efficiency inducing peripheral osseous tissue, and formed firm Chemical bond with host bone.
Hydroxyapatite is joined the synosteosis ability that can improve chitosan/hydroxyapatite composite material in the glycan substrate, promote the damaged reparation of bone; At present, the method for preparing chitosan/hydroxyapatite composite material mainly contains in direct blend, lyophilize and the solidification liquid and solidifies.Generally all be that employing is a matrix with the hydroxyapatite, account for 60%～90% (weight), and chitosan mainly be as excipient, tackiness agent in this system.Add chitosan solution in hydroapatite particles, hydroapatite particles is modulated into mashed prod or paste, hydroxyapatite just can be by any plastotype like this.But final material still shows the biological ceramics performance, and promptly fragility is big, and flexural strength is low.And be that the composite degradation of matrix is very slow with the hydroxyapatite, do not match with the process of union of fracture.The matrix material of this method preparation a little less than the two interface binding power of hydroxyapatite and chitosan, causes material opaque in appearance because the hydroxyapatite dispersion is inhomogeneous, presents white; Aspect mechanical property, descend.Therefore how to guarantee that in hydroxyapatite homodisperse in the glycan substrate matrix that is dispersed in chitosan smaller with guaranteeing hydroapatite particles be emphasis and the difficult point problem for preparing this class material at present.
Summary of the invention
The purpose of this invention is to provide the compound method for preparing chitosan/hydroxyapatite nano matrix material of original position, this method can guarantee that hydroxyapatite is dispersed in the glycan substrate.
The inventive method may further comprise the steps:
1) presses hydroxyapatite Ca
10(OH)
2(PO
4)
6To choose suitable calcium salt and phosphoric acid salt compound concentration respectively be that ionic calcium soln and the concentration of 0.5Kg/L～4.0Kg/L is the phosphate ion solution of 0.35Kg/L～2.0Kg/L to the amount of calcium ion and phosphonium ion in the chemical formula;
2) ionic calcium soln and the phosphate ion solution of respectively getting 50ml～400ml mixes in container, adds a certain amount of acetate, is mixed with acetic acid concentration (by volume) and is 1～8% solution;
3) chitosan is dissolved in step 2) in the gained solution, be mixed with chitosan content (by weight) and be 2.5%～6% chitosan solution;
4) chitosan solution that takes a morsel injects mould and forms one deck inner membrance earlier, then chitosan solution is injected mould, putting it into concentration (by weight) again is in 3～10%NaOH solidification liquid and mold removal, after 2～5 hours the chitosan solution gel stick is put into the distilled water rinsing to neutral, put into 50～80 ℃ of drying in oven.
Among the present invention, said calcium salt can be calcium chloride, lime carbonate, nitrocalcite, and phosphoric acid salt can be SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate, dipotassium hydrogen phosphate.
The invention provides a kind of in (both under mild conditions) preparation chitosan/hydroxyapatite nano matrix material novel method under normal temperature, the normal pressure.This method can guarantee hydroapatite particles, and (20～100nm) are dispersed in the chitosan basal body with nano-scale, the transparent little Huang of material that makes with the inventive method, mechanical property obviously improves, can remain in the bone repair process in the hydroxyapatite calcium ion and phosphonium ion continues, steadily, from glycan substrate, discharge lentamente, avoided the burst release phenomenon.
Embodiment
Further specify the present invention below in conjunction with specific examples.
The compound method for preparing chitosan/hydroxyapatite nano matrix material of original position of the present invention may further comprise the steps:
1) presses hydroxyapatite Ca
10(OH)
2(PO
4)
6To choose suitable calcium salt and phosphoric acid salt compound concentration respectively be that ionic calcium soln and the concentration of 1.6Kg/L is the phosphate ion solution of 0.8Kg/L to the amount of calcium ion and phosphonium ion in the chemical formula;
2) ionic calcium soln and the phosphate ion solution of respectively getting 200ml mixes in container, adds a certain amount of acetate, is mixed with acetic acid concentration (by volume) and is 2% solution;
3) chitosan is dissolved in step 2) in the gained solution, be mixed with chitosan content (by weight) and be 4% chitosan solution;
4) chitosan solution that takes a morsel injects mould and forms one deck inner membrance earlier, then chitosan solution is injected mould, putting it into concentration again is in the 5%NaOH solidification liquid and mold removal, after 4 hours the chitosan solution gel stick is put into the distilled water rinsing to neutral, put into 70 ℃ of drying in oven.Make chitosan of the present invention/hydroxyapatite nano material, its color and luster: little Huang is transparent, flexural strength: 89 ± 4MPa, modulus in flexure: 3.5 ± 0.1Gpa.
The mechanical property that table 1 has provided several samples compares.Table 1
| Sample | Flexural strength (MPa) | Modulus in flexure (GPa) |
| Natural bone | ?22±0.8 | ?1.4±0.4 |
| Pure chitosan | ?94±12 | ?3.5±0.5 |
| Direct blend CS/HA=100/5 | ?68±2 | ?3.2±0.2 |
| The compound CS/HA=100/5 of original position | ?86±7 | ?3.4±0.1 |
By table 1 as seen, prepare the mechanical property height of the mechanical property of material with in-situ compounding process, and be higher than the mechanical property of natural bone far away than the preparation sample of blend.
Claims (2)
1. the compound method for preparing chitosan/hydroxyapatite nano matrix material of original position is characterized in that may further comprise the steps:
1) presses hydroxyapatite Ca
10(OH)
2(PO
4)
6To choose suitable calcium salt and phosphoric acid salt compound concentration respectively be that ionic calcium soln and the concentration of 0.5Kg/L～4.0Kg/L is the phosphate ion solution of 0.35Kg/L～2.0Kg/L to the amount of calcium ion and phosphonium ion in the chemical formula;
2) ionic calcium soln and the phosphate ion solution of respectively getting 50ml～400ml mixes in container, adds a certain amount of acetate, is mixed with acetic acid concentration (by volume) and is 1～8% solution;
3) chitosan is dissolved in step 2) in the gained solution, be mixed with chitosan content (by weight) and be 2.5%～6% chitosan solution;
4) chitosan solution that takes a morsel injects mould and forms one deck inner membrance earlier, then chitosan solution is injected mould, putting it into concentration (by weight) again is in 3～10%NaOH solidification liquid and mold removal, after 2～5 hours the chitosan solution gel stick is put into the distilled water rinsing to neutral, put into 50～80 ℃ of drying in oven.
2. the compound method for preparing chitosan/hydroxyapatite nano matrix material of original position according to claim 1 is characterized in that said calcium salt is calcium chloride, lime carbonate, nitrocalcite, and phosphoric acid salt is SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate, dipotassium hydrogen phosphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02136031 CN1203120C (en) | 2002-07-15 | 2002-07-15 | In-situ compounding process of synthesizing nano composite chitosan/hydroxyapatite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02136031 CN1203120C (en) | 2002-07-15 | 2002-07-15 | In-situ compounding process of synthesizing nano composite chitosan/hydroxyapatite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1389503A true CN1389503A (en) | 2003-01-08 |
| CN1203120C CN1203120C (en) | 2005-05-25 |
Family
ID=4748473
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02136031 Expired - Fee Related CN1203120C (en) | 2002-07-15 | 2002-07-15 | In-situ compounding process of synthesizing nano composite chitosan/hydroxyapatite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1203120C (en) |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1307253C (en) * | 2005-02-03 | 2007-03-28 | 徐放 | Chitosan water-retaining gel adhesive substrate materials and method for preparing same |
| CN1326574C (en) * | 2005-12-13 | 2007-07-18 | 天津大学 | Nanometer hydroxyapatite/chitosan/gelatin porous scaffold material and preparation method thereof |
| CN100381181C (en) * | 2005-10-21 | 2008-04-16 | 四川大学 | Step-degrdeable bioactive implanting material comprising growth promotion factor |
| CN100551451C (en) * | 2007-04-26 | 2009-10-21 | 山东大学 | Composite of a kind of repairing bone defect and preparation method thereof |
| CN101822961A (en) * | 2010-03-10 | 2010-09-08 | 武汉理工大学 | In situ preparation method of hydroxyapatite /chitosan core-shell nanospheres |
| WO2011035573A1 (en) * | 2009-09-28 | 2011-03-31 | 暨南大学 | Nanometer hydroxyapatite / natural polymer composite material, preparation method and use thereof |
| CN102276879A (en) * | 2010-06-11 | 2011-12-14 | 中国科学院合肥物质科学研究院 | Fibrous nano-hydroxyapatite/chitosan composite material and preparation method thereof |
| CN101352585B (en) * | 2008-07-31 | 2012-02-01 | 华南理工大学 | Method for preparing directionally arranged nano hydroxylapatite granule/chitosan stent |
| CN102397581A (en) * | 2011-11-21 | 2012-04-04 | 浙江大学 | Method for generating chitosan/calcium phosphate hybrid material by electrochemical method biomimetic mineralization |
| CN101301495B (en) * | 2008-06-03 | 2012-07-25 | 陕西科技大学 | Method for preparing bone screw biological compound material |
| CN101648036B (en) * | 2009-08-26 | 2012-10-03 | 天津大学 | Lamellar hydroxylapatite and chitosan nano composite material as well as preparation method and application thereof |
| CN103463680A (en) * | 2013-08-21 | 2013-12-25 | 吴江市英力达塑料包装有限公司 | Preparation process of medical implant material |
| CN105086319A (en) * | 2015-08-18 | 2015-11-25 | 中国科学院上海硅酸盐研究所 | Bionic-structure hydroxyapatite (Hap)/polymer composite material, and preparation method and application thereof |
| CN106512099A (en) * | 2016-11-24 | 2017-03-22 | 上海大学 | Chitosan-based bionic bone tissue engineering scaffold and production method thereof |
| CN108714251A (en) * | 2018-06-06 | 2018-10-30 | 浙江大学 | The method that two-step method prepares the chitosan-based synthetism plate material of high hydroxyapatite content |
| CN109549928A (en) * | 2017-09-26 | 2019-04-02 | 清华大学深圳研究生院 | A kind of compound microballoon of Chitosan-Thiolated Polymers/calcium carbonate and preparation method thereof |
| CN110172199A (en) * | 2019-06-25 | 2019-08-27 | 扬州大学 | A kind of preparation method of hydroxyapatite/ultra-high molecular weight polyethylene nano-complex |
-
2002
- 2002-07-15 CN CN 02136031 patent/CN1203120C/en not_active Expired - Fee Related
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1307253C (en) * | 2005-02-03 | 2007-03-28 | 徐放 | Chitosan water-retaining gel adhesive substrate materials and method for preparing same |
| CN100381181C (en) * | 2005-10-21 | 2008-04-16 | 四川大学 | Step-degrdeable bioactive implanting material comprising growth promotion factor |
| CN1326574C (en) * | 2005-12-13 | 2007-07-18 | 天津大学 | Nanometer hydroxyapatite/chitosan/gelatin porous scaffold material and preparation method thereof |
| CN100551451C (en) * | 2007-04-26 | 2009-10-21 | 山东大学 | Composite of a kind of repairing bone defect and preparation method thereof |
| CN101301495B (en) * | 2008-06-03 | 2012-07-25 | 陕西科技大学 | Method for preparing bone screw biological compound material |
| CN101352585B (en) * | 2008-07-31 | 2012-02-01 | 华南理工大学 | Method for preparing directionally arranged nano hydroxylapatite granule/chitosan stent |
| CN101648036B (en) * | 2009-08-26 | 2012-10-03 | 天津大学 | Lamellar hydroxylapatite and chitosan nano composite material as well as preparation method and application thereof |
| WO2011035573A1 (en) * | 2009-09-28 | 2011-03-31 | 暨南大学 | Nanometer hydroxyapatite / natural polymer composite material, preparation method and use thereof |
| CN101822961B (en) * | 2010-03-10 | 2012-06-27 | 武汉理工大学 | In situ preparation method of hydroxyapatite /chitosan core-shell nanospheres |
| CN101822961A (en) * | 2010-03-10 | 2010-09-08 | 武汉理工大学 | In situ preparation method of hydroxyapatite /chitosan core-shell nanospheres |
| CN102276879A (en) * | 2010-06-11 | 2011-12-14 | 中国科学院合肥物质科学研究院 | Fibrous nano-hydroxyapatite/chitosan composite material and preparation method thereof |
| CN102397581A (en) * | 2011-11-21 | 2012-04-04 | 浙江大学 | Method for generating chitosan/calcium phosphate hybrid material by electrochemical method biomimetic mineralization |
| CN103463680A (en) * | 2013-08-21 | 2013-12-25 | 吴江市英力达塑料包装有限公司 | Preparation process of medical implant material |
| CN105086319B (en) * | 2015-08-18 | 2018-05-08 | 中国科学院上海硅酸盐研究所 | Hydroxyapatite/polymer composite material with bionical construction and preparation method and application |
| CN105086319A (en) * | 2015-08-18 | 2015-11-25 | 中国科学院上海硅酸盐研究所 | Bionic-structure hydroxyapatite (Hap)/polymer composite material, and preparation method and application thereof |
| CN106512099A (en) * | 2016-11-24 | 2017-03-22 | 上海大学 | Chitosan-based bionic bone tissue engineering scaffold and production method thereof |
| CN106512099B (en) * | 2016-11-24 | 2019-07-23 | 上海大学 | Chitosan-based biotic bone tissue engineering stent and preparation method thereof |
| CN109549928A (en) * | 2017-09-26 | 2019-04-02 | 清华大学深圳研究生院 | A kind of compound microballoon of Chitosan-Thiolated Polymers/calcium carbonate and preparation method thereof |
| CN108714251A (en) * | 2018-06-06 | 2018-10-30 | 浙江大学 | The method that two-step method prepares the chitosan-based synthetism plate material of high hydroxyapatite content |
| CN110172199A (en) * | 2019-06-25 | 2019-08-27 | 扬州大学 | A kind of preparation method of hydroxyapatite/ultra-high molecular weight polyethylene nano-complex |
| CN110172199B (en) * | 2019-06-25 | 2022-03-01 | 扬州大学 | Preparation method of hydroxyapatite/ultra-high molecular weight polyethylene nano composite |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1203120C (en) | 2005-05-25 |
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