CN105460912B - A kind of method that high-specific surface area hydroxyapatite is prepared using fish-bone - Google Patents
A kind of method that high-specific surface area hydroxyapatite is prepared using fish-bone Download PDFInfo
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- CN105460912B CN105460912B CN201510892186.0A CN201510892186A CN105460912B CN 105460912 B CN105460912 B CN 105460912B CN 201510892186 A CN201510892186 A CN 201510892186A CN 105460912 B CN105460912 B CN 105460912B
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- fish
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- hydroxyapatite
- surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Materials For Medical Uses (AREA)
Abstract
The invention discloses a kind of method that high-specific surface area hydroxyapatite is prepared using fish-bone.The present invention is raw material with fish-bone, and the fish-bone after cleaning dries 4 ~ 24 h at 70 ~ 90 DEG C, obtains dry fish-bone；The dry fish-bones of 1 ~ 10 g and 5 ~ 30 mL distilled water are mixed, and the h of hydro-thermal process 12 ~ 30 is carried out in 160 ~ 220 DEG C.The product that hydro-thermal reaction is obtained is filtered, washed, and it is 166.57m to be placed in 70 ~ 90 DEG C of 4 ~ 24 h of drying and obtain specific surface area2/ g hydroxyapatite.The present invention uses fish-bone as raw material hydro-thermal one-step synthesis high-specific surface area hydroxyapatite first, and raw material sources are abundant, resource utilization is high, technological process is simply efficient and economical and practical, green, have good industrial prospect and social benefit.
Description
Technical field
The invention belongs to the preparation field of hydroxyapatite, and in particular to one kind prepares high-specific surface area hydroxyl using fish-bone
The method of apatite.
Background technology
China's stock of fish enriches, fish processing industry high speed development.Fish-bone is the accessory substance of fish processing industry, in fish plus
In work, bone accounts for more than the 30% of fish weight in fish head and fish.Research shows, in fish-bone outside moisture removal, mainly by ash content（Mineral
Matter）, albumen and fat composition, ash composition highest in three, the content highest of calcium, phosphorus wherein in ash content.At present, Japan, U.S.
The aquatic products processing accessory substance of state can reach the degree that classified use is carried out according to its chemical composition and biochemical characteristic, and it is processed
The output value reaches several times to tens times of the flesh of fish.In the fish processing industry in China, fish-bone generally with other processing fents together by
Abandon or only as fertilizer, feed, cause to the wasting of resources and environmental pollution.
Hydroxyapatite（Hydroxyatite, chemical molecular formula Ca10(PO4)6(OH)2）It is any animal skeleton, tooth
Main mineral constituent, there is good biocompatibility and bioactivity and the binding ability excellent with human body bone.Hydroxy-apatite
Stone is white powder, belongs to hexagonal crystal system, and the structure channel in Crystal Structure of Hydroxyapatite imparts its good ion and handed over
Transsexual energy, and hydroxyapatite has loose structure, there is very big porosity, can adsorb and recycle in industrial wastewater
Contents of many kinds of heavy metal ion, fluorine ion, organic dye molecule, be a kind of sorbing material with very strong suction-operated, and hydroxyl
Apatite is good with environment compatibility, does not easily cause secondary pollution, is a kind of Novel ring that can be widely applied to environmental pollution improvement
Border sorbing material.
The common synthetic method of hydroxyapatite has the precipitation method, hydro-thermal method, Hydrolyze method, sol-gel process and solid phase to close
Into method etc..The raw material of preparation mainly has chemical raw material, animal skeleton, coral, shell, eggshell etc..The present invention with industrial production and
The fish-bone discarded in life is raw material, cheap and green, and hydroxyapatite is prepared from suitable preparation method,
The production cost of hydroxyapatite is not only reduced, and and can is recycled discarded fish-bone, is the high attached of fish-bone
The exploitation of value-added product provides new approach, so as to realize resource make full use of and sustainable development.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of easy, efficient, economy with industrial production
And the fish-bone discarded in life is the method that raw material prepares high-specific surface area hydroxyapatite, its raw material sources enriches, resource profit
High with rate, technological process is simple, efficiently, effectively reduces the cost for preparing high-specific surface area hydroxyapatite, and economical and practical,
It is green.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of method that high-specific surface area hydroxyapatite is prepared using fish-bone, it is comprised the following steps that：
The fish-bone discarded in life is collected, the fish-bone after cleaning dries 4 ~ 24h, be air-cooled to room by being warming up to 70 ~ 90 DEG C
The method of temperature obtains dry fish-bone；The dry fish-bones of 1 ~ 10g and 5 ~ 30mL distilled water are mixed and pour into polytetrafluoroethyllining lining not
Become rusty in steel reactor, be positioned over after being tamping in 160 ~ 220 DEG C of constant temperature ovens, 12 ~ 30h of hydro-thermal reaction；Hydro-thermal reaction is obtained
To product filtered, washed to neutrality, after be placed in 70 ~ 90 DEG C of 4 ~ 24h of drying and obtain high-specific surface area hydroxyapatite.
The fish-bone include one kind in the fish-bone of perch, carp, crucian, silver carp, bighead, black carp, grass carp and bream or
Person is a variety of.
Hydroxyapatite specific surface area made from a kind of method as described above is 166.57m2/g。
The remarkable advantage of the present invention is：
（1）The present invention is raw material using the fish-bone discarded in industrial production and life, cheap and green, choosing
Hydroxyapatite is prepared for suitable preparation method, reduces the production cost of hydroxyapatite；
（2）The present invention is recycled discarded fish-bone, is provided newly for the exploitation of the high value added product of fish-bone
Approach, so as to realize resource make full use of and sustainable development；
（3）Preparation process is modified without high-temperature calcination without surface, and prepared hydroxyapatite specific surface area is big, activity
By force；
（4）Preparation technology is simple, easily operated, is easy to promote.
Brief description of the drawings
The X ray diffracting spectrum of hydroxyapatite made from Fig. 1 embodiments 1, as can be seen from the figure hydroxyapatite is special
Levy diffraction maximum；
The scanning electron microscopy of hydroxyapatite made from Fig. 2 embodiments 1, as can be seen from the figure hydroxyapatite
It is more in 200nm, hole for graininess, size；
N2 adsorption/desorption curve of hydroxyapatite made from Fig. 3 embodiments 1, it can be seen that with nitrogen partial pressure
Increase, adsorbance gradually increase, and illustrate that its specific surface area is larger；
Hydroxyapatite BJH graph of pore diameter distribution made from Fig. 4 embodiments 1.It was found from figure, the average hole of hydroxyapatite
Footpath is in 200nm or so；
Fig. 5 is through the hydroxyapatite obtained by embodiment 1 and conventional hydroxy apatite to the Congo red solution of 80mg/L（CR）
Absorption situation comparison diagram.
Embodiment
In order that content of the present invention easily facilitates understanding, with reference to embodiment to of the present invention
Technical scheme is described further, but the present invention is not limited only to this.
Embodiment 1
The fish-bone discarded in life is collected, the fish-bone after cleaning is warming up to 80 DEG C by the first step, dries 9 h, is air-cooled to
The method of room temperature obtains dry fish-bone, and the dry fish-bones of 2.4g and 14mL distilled water are mixed and pour into the stainless of polytetrafluoroethyllining lining
In steel reactor, it is positioned over after being tamping in 200 DEG C of constant temperature ovens, hydro-thermal reaction 24h.The product that hydro-thermal reaction is obtained is taken out
Filter, wash to neutrality, after be placed in 80 DEG C of 9 h of drying and obtain high-specific surface area hydroxyapatite.
Embodiment 2
The fish-bone discarded in life is collected, the fish-bone after cleaning dries 24h, be air-cooled to room temperature by being warming up to 70 DEG C
Method obtains dry fish-bone；The dry fish-bones of 1g and 5mL distilled water are mixed to the stainless steel cauldron for pouring into polytetrafluoroethyllining lining
In, it is positioned over after being tamping in 160 DEG C of constant temperature ovens, hydro-thermal reaction 30h；The product that hydro-thermal reaction is obtained is filtered, washed
To neutrality, after be placed in 90 DEG C of drying 4h and obtain hydroxyapatite.
Embodiment 3
The fish-bone discarded in life is collected, the fish-bone after cleaning dries 4h, be air-cooled to the side of room temperature by being warming up to 90 DEG C
Method obtains dry fish-bone；The dry fish-bones of 10g and 30mL distilled water are mixed to the stainless steel cauldron for pouring into polytetrafluoroethyllining lining
In, it is positioned over after being tamping in 220 DEG C of constant temperature ovens, hydro-thermal reaction 12h；The product that hydro-thermal reaction is obtained is filtered, washed
To neutrality, after be placed in 90 DEG C of drying 4h and obtain hydroxyapatite.
Embodiment 4
Hydroxyapatite made from 25mg embodiments 1 is weighed respectively and conventional hydroxy apatite is placed in 50mL conical flasks,
It is separately added into the Congo red solution for the 80mg/L concentration that 25mL is prepared in advance.Conical flask be placed under constant temperature blender with magnetic force with
240rpm speed oscillation, centrifuged after the vibration 480min times and take its supernatant liquid, use ultraviolet-uisible spectrophotometer
Absorbance of the remaining Congo red solution of measure at maximum absorption band 497nm, utilizes Congo red Solutions Solution concentration before and after absorption
Difference, calculate hydroxyapatite to Congo red eliminating rate of absorption；It can be seen that hydroxyapatite produced by the present invention is compared to normal
Rule hydroxyapatite has good adsorption effect to Congo red solution, shows that it has high-specific surface area.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, it should all belong to the covering scope of the present invention.
Claims (1)
- A kind of 1. method that high-specific surface area hydroxyapatite is prepared using fish-bone, it is characterised in that：Collect what is discarded in life Fish-bone, the fish-bone after cleaning dry 9h, the method for being air-cooled to room temperature obtains dry fish-bone by being warming up to 80 DEG C；By the dry fishes of 2.4g The mixing of bone and 14mL distilled water is poured into the stainless steel cauldron of polytetrafluoroethyllining lining, and 200 DEG C of perseverances are positioned over after being tamping In warm baking oven, hydro-thermal reaction 24h；The product that hydro-thermal reaction obtains is filtered, washed to neutrality, after be placed in 80 DEG C of bakings Dry 9h obtains high-specific surface area hydroxyapatite；The specific surface area of obtained hydroxyapatite is 166.57m2/g。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510892186.0A CN105460912B (en) | 2015-12-08 | 2015-12-08 | A kind of method that high-specific surface area hydroxyapatite is prepared using fish-bone |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510892186.0A CN105460912B (en) | 2015-12-08 | 2015-12-08 | A kind of method that high-specific surface area hydroxyapatite is prepared using fish-bone |
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| Publication Number | Publication Date |
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| CN105460912A CN105460912A (en) | 2016-04-06 |
| CN105460912B true CN105460912B (en) | 2018-01-12 |
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| CN201510892186.0A Expired - Fee Related CN105460912B (en) | 2015-12-08 | 2015-12-08 | A kind of method that high-specific surface area hydroxyapatite is prepared using fish-bone |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109264690A (en) * | 2018-12-06 | 2019-01-25 | 湖南三友环保科技股份有限公司 | A method of purifying fish waste Central Plains form hydroxyapatite |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106082155B (en) * | 2016-06-07 | 2018-04-06 | 广西壮族自治区药用植物园 | The method that hydroxyapatite is prepared using fish-bone |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1915092A (en) * | 2006-05-23 | 2007-02-21 | 大连础明生物科技有限公司 | Active quick dissolving full valued bone powder, and preparation method |
| CN101987208A (en) * | 2009-08-03 | 2011-03-23 | 宁波大学 | Multi-phase large-aperture bone regeneration bracket material transformed from cuttlebone and preparation method thereof |
| CN102145193A (en) * | 2011-04-14 | 2011-08-10 | 李亚屏 | Cuttlebone conversion series porous biological ceramics |
| CN103112837A (en) * | 2013-03-18 | 2013-05-22 | 厦门大学 | Preparation method of nano-hydroxyapatite |
-
2015
- 2015-12-08 CN CN201510892186.0A patent/CN105460912B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1915092A (en) * | 2006-05-23 | 2007-02-21 | 大连础明生物科技有限公司 | Active quick dissolving full valued bone powder, and preparation method |
| CN101987208A (en) * | 2009-08-03 | 2011-03-23 | 宁波大学 | Multi-phase large-aperture bone regeneration bracket material transformed from cuttlebone and preparation method thereof |
| CN102145193A (en) * | 2011-04-14 | 2011-08-10 | 李亚屏 | Cuttlebone conversion series porous biological ceramics |
| CN103112837A (en) * | 2013-03-18 | 2013-05-22 | 厦门大学 | Preparation method of nano-hydroxyapatite |
Non-Patent Citations (2)
| Title |
|---|
| Biological hydroxyapatite obtained from fish bones;M. Boutinguiza etc.;《Materials Science and Engineering C》;20111203;第32卷;478-486 * |
| Extraction of pure natural hydroxyapatite from the bovine bones bio waste by three different methods;Nasser A.M.etc.;《Journal of materials processing technology》;20090401;第209卷(第7期);3408-3415 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109264690A (en) * | 2018-12-06 | 2019-01-25 | 湖南三友环保科技股份有限公司 | A method of purifying fish waste Central Plains form hydroxyapatite |
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