JPH04331719A - Method for synthesizing fine grain of hydroxyapatite and apparatus for synthesis - Google Patents
Method for synthesizing fine grain of hydroxyapatite and apparatus for synthesisInfo
- Publication number
- JPH04331719A JPH04331719A JP13052791A JP13052791A JPH04331719A JP H04331719 A JPH04331719 A JP H04331719A JP 13052791 A JP13052791 A JP 13052791A JP 13052791 A JP13052791 A JP 13052791A JP H04331719 A JPH04331719 A JP H04331719A
- Authority
- JP
- Japan
- Prior art keywords
- hydroxyapatite
- raw material
- solution
- material solution
- gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 229910052588 hydroxylapatite Inorganic materials 0.000 title claims abstract description 24
- 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 abstract description 24
- 238000000034 method Methods 0.000 title claims description 27
- 230000002194 synthesizing effect Effects 0.000 title claims description 9
- 238000003786 synthesis reaction Methods 0.000 title description 12
- 230000015572 biosynthetic process Effects 0.000 title description 11
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 25
- 230000005587 bubbling Effects 0.000 claims abstract description 14
- 239000012670 alkaline solution Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 12
- 239000010419 fine particle Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 238000007664 blowing Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 abstract description 11
- 239000011575 calcium Substances 0.000 abstract description 8
- 235000011007 phosphoric acid Nutrition 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 6
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 abstract description 5
- 239000007864 aqueous solution Substances 0.000 abstract description 5
- 239000001110 calcium chloride Substances 0.000 abstract description 5
- 235000011148 calcium chloride Nutrition 0.000 abstract description 5
- 229910001628 calcium chloride Inorganic materials 0.000 abstract description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 abstract description 3
- 229910052791 calcium Inorganic materials 0.000 abstract description 3
- 239000012159 carrier gas Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract 1
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 3
- 235000019700 dicalcium phosphate Nutrition 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 2
- 229910014497 Ca10(PO4)6(OH)2 Inorganic materials 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[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 VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 235000019731 tricalcium phosphate Nutrition 0.000 description 1
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 1
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明はヒドロキシアパタイト微
粒子の合成方法及び合成装置に関するものであり、詳し
くは微細で結晶性の良好な高純度ヒドロキシアパタイト
微粒子を合成するための方法及び装置に関するものであ
る。[Field of Industrial Application] The present invention relates to a method and apparatus for synthesizing fine hydroxyapatite particles, and more particularly to a method and apparatus for synthesizing fine, highly purified hydroxyapatite fine particles with good crystallinity. .
【０００２】0002
【従来の技術】ヒドロキシアパタイトの合成方法として
は、下記の４種類の方法が知られている。
■乾式法：Ｃａ３（ＰＯ４）２，ＣａＨＰＯ４，Ｃａ２
Ｐ２Ｏ７等を水蒸気中８００ ℃以上の高温下に固相反
応させる方法。
■湿式法：Ｈ３ＰＯ４，ＣａＣｌ２等を含有する原料溶
液をアルカリ水溶液中に供給して反応させる方法。
■水熱法：ＣａＨＰＯ４をオートクレーブ中で３００
℃以上、かつ数百気圧下に長時間反応させ、大きな結晶
を得る方法。
■固体−水系法：ＣａＨＰＯ４とＣａＣＯ３から溶解度
の小さいヒドロキシアパタイトを析出させる方法。BACKGROUND OF THE INVENTION The following four methods are known for synthesizing hydroxyapatite. ■Dry method: Ca3(PO4)2, CaHPO4, Ca2
A method in which P2O7, etc. are subjected to a solid phase reaction at high temperatures of 800°C or higher in steam. (2) Wet method: A method in which a raw material solution containing H3PO4, CaCl2, etc. is fed into an alkaline aqueous solution and reacted. ■Hydrothermal method: CaHPO4 in an autoclave at 300%
A method to obtain large crystals by reacting for a long time at temperatures above ℃ and under several hundred atmospheres. ■Solid-water method: A method in which hydroxyapatite with low solubility is precipitated from CaHPO4 and CaCO3.
【０００３】しかし上記方法の中で■及び■の方法は高
温高圧に耐える反応容器が必要であるため、設備費が高
くなるという欠点があり、■の方法は反応速度が遅いの
で、反応を完了させて収率を上げるためには高温で長時
間反応させる必要があるという欠点がある。However, among the above methods, methods (1) and (2) require a reaction vessel that can withstand high temperature and pressure, so they have the disadvantage of high equipment costs, and method (2) has a slow reaction rate, so it is difficult to complete the reaction. The drawback is that in order to increase the yield, it is necessary to carry out the reaction at high temperature for a long time.
【０００４】一方■の方法は特別な容器を必要とせず、
しかも反応速度の速い方法であるが、反応が急激に進む
傾向があり均一な合成環境を維持することが困難である
。そのため反応が不十分で未反応物が残る場合もあり、
Ｃａ／Ｐ＝１．６７ の化学量論比を均一に示す結晶を
再現性良く得ることが難しいという欠点がある。反応後
の熟成時間を長くして未反応物を少なくし、化学量論比
に近づけることも考えられるが、粒子径の不均一なもの
しか得られず、反応時間が長くなり生産性も低くなる。
そこで反応溶液濃度を低く抑えて上記問題を克服するこ
とも試みられているが、合成量が少なくなるので生産性
向上にはつながらない。また均一な合成雰囲気を得るた
めに、たとえば反応槽に取りつけた攪拌機の攪拌速度を
高くして均一に混合をすることが試みられるが、湿式法
での合成反応は非常な短時間で終了するのでその効果は
あまり期待できず、また攪拌動力が増加するとともに攪
拌装置が大きくなり合成装置も大型化する。更に合成は
不純物の混入を防ぐため密閉系で行われるが、攪拌速度
の増加により軸受部のシールが困難になるとともに磨耗
による不純物の混入が起こり、純粋なヒドロキシアパタ
イトの合成は難しい。On the other hand, method (①) does not require a special container;
Moreover, although this is a method with a fast reaction rate, the reaction tends to proceed rapidly and it is difficult to maintain a uniform synthesis environment. Therefore, the reaction may be insufficient and unreacted substances may remain.
A drawback is that it is difficult to obtain crystals uniformly exhibiting a stoichiometric ratio of Ca/P=1.67 with good reproducibility. It is possible to increase the aging time after the reaction to reduce the amount of unreacted substances and bring the ratio closer to the stoichiometric ratio, but this would only result in particles with non-uniform particle sizes, which would lengthen the reaction time and lower productivity. . Therefore, attempts have been made to overcome the above problem by keeping the concentration of the reaction solution low, but this does not lead to improved productivity because the amount of synthesis decreases. In addition, in order to obtain a uniform synthesis atmosphere, attempts are made to increase the stirring speed of a stirrer attached to the reaction tank to achieve uniform mixing, but the synthesis reaction in the wet method completes in a very short time. Not much effect can be expected, and as the stirring power increases, the stirring device becomes larger and the synthesis apparatus also becomes larger. Furthermore, the synthesis is carried out in a closed system to prevent the contamination of impurities, but the increase in stirring speed makes it difficult to seal the bearing part and the contamination of impurities due to wear occurs, making it difficult to synthesize pure hydroxyapatite.
【０００５】[0005]
【発明が解決しようとする課題】本発明は以上の様な状
況に鑑みてなされたものであって、湿式法を改良するこ
とによって、均一組成で粒子サイズの揃ったヒドロキシ
アパタイトを効率良く安価に合成できる方法を提供しよ
うとするものである。[Problems to be Solved by the Invention] The present invention has been made in view of the above circumstances, and it is an object of the present invention to efficiently and inexpensively produce hydroxyapatite with a uniform composition and uniform particle size by improving the wet method. The aim is to provide a method for synthesis.
【０００６】[0006]
【課題を解決するための手段】上記課題を解決すること
のできた本発明のヒドロキシアパタイト微粒子の合成方
法は、湿式法でヒドロキシアパタイト微粒子を合成する
にあたり、原料溶液をバブリング用気体によって搬送し
微細な液滴としてアルカリ溶液の入った反応槽内に均一
に供給すると共に、前記バブリング用気体の吹込みによ
って反応槽内を均一に攪拌することに要旨がある。また
上記方法を実施する上で好適な装置は特に制限されるも
のではないが、原料溶液を微細な液滴としてバブリング
用気体と共に供給できる装置を反応槽内の下部に有する
合成装置を用いることにより容易に実施することができ
る。[Means for Solving the Problems] The method for synthesizing hydroxyapatite fine particles of the present invention, which can solve the above problems, involves transporting a raw material solution by a bubbling gas to form fine particles when synthesizing hydroxyapatite fine particles by a wet method. The gist is to uniformly supply the alkaline solution as droplets into the reaction tank and to uniformly stir the inside of the reaction tank by blowing in the bubbling gas. Furthermore, there are no particular restrictions on suitable equipment for carrying out the above method, but by using a synthesis equipment that has a device in the lower part of the reaction tank that can supply the raw material solution in the form of fine droplets together with bubbling gas. It can be easily implemented.
【０００７】[0007]
【作用】本発明は湿式法の改良法であって、リン酸源（
例えばＨ３ＰＯ４）とカルシウム源（例えばＣａＣｌ２
）をＣａ／Ｐが化学量論比の１．６７になるように調合
した原料溶液を、バブリング用気体をキャリアガスとし
て搬送することにより、微細な液滴としてアルカリ水溶
液中へ供給されることとなったので、アルカリ溶液中へ
均一に供給することができる。その結果反応条件を均一
なものとすることができ、均一組成で且つ粒子サイズの
揃ったヒドロキシアパタイトを効率良く生成することが
できる。[Operation] The present invention is an improved method of the wet method, and is a phosphoric acid source (
e.g. H3PO4) and calcium sources (e.g. CaCl2).
) is prepared so that the Ca/P ratio is 1.67, and the raw material solution is supplied into the alkaline aqueous solution as fine droplets by transporting bubbling gas as a carrier gas. Therefore, it can be uniformly supplied into the alkaline solution. As a result, the reaction conditions can be made uniform, and hydroxyapatite with a uniform composition and uniform particle size can be efficiently produced.
【０００８】以下更に詳しく説明する。本発明の原料溶
液を調合する際に用いられる原料は特に限定されるもの
ではなく、通常用いられているリン酸源やカルシウム源
を適宜用いることができる。原料として例えばＣａＣｌ
２とＨ３ＰＯ４を用いた場合の反応式は下記のとおりで
ある。１０ＣａＣｌ２＋ ６Ｈ３ＰＯ４＋ ２０ＫＯＨ
→ Ｃａ１０（ＰＯ４）６（ＯＨ）２＋ ２０ＫＣｌ
＋１８Ｈ２Ｏ従ってＣａＣｌ２ １０モルに対して Ｈ
３ＰＯ４ ６モルを完全に反応させることにより、Ｃａ
／Ｐが化学量論比（１．６７）であるヒドロキシアパタ
イトを得ることができる。[0008] This will be explained in more detail below. The raw materials used when preparing the raw material solution of the present invention are not particularly limited, and commonly used phosphoric acid sources and calcium sources can be used as appropriate. For example, CaCl as a raw material
The reaction formula when using 2 and H3PO4 is as follows. 10CaCl2+ 6H3PO4+ 20KOH
→ Ca10(PO4)6(OH)2+ 20KCl
+18H2O Therefore, for 10 moles of CaCl2 H
By completely reacting 6 moles of 3PO4, Ca
Hydroxyapatite in which /P is the stoichiometric ratio (1.67) can be obtained.
【０００９】バブリングにより攪拌されたアルカリ溶液
中に、上記原料溶液を微細な液滴として供給することに
より、原料溶液は同一環境下に同一条件で添加されるこ
ととなり、また添加後直ちに反応が終了するので、粒子
径にバラツキが少なくしかも化学量論組成のヒドロキシ
アパタイト微粒子を効率良く製造することができる。By supplying the raw material solution as fine droplets into the alkaline solution stirred by bubbling, the raw material solution is added under the same environment and under the same conditions, and the reaction ends immediately after addition. Therefore, hydroxyapatite fine particles having a stoichiometric composition with little variation in particle size can be efficiently produced.
【００１０】上記目的を達成するためには、原料溶液は
粒子径をおよそ０．５ｍｍ 以下の微細な液滴とするこ
とが好ましい。液滴の粒子径が大き過ぎる場合には、得
られるヒドロキシアパタイト微粒子の粒子径にバラツキ
が出やすい。また原料溶液はバブリング用気体と共に供
給することにより、攪拌下に供給されることとなる。上
記の様な状態で供給するためには、孔径が０．５ｍｍ
以下の気泡発生装置によりバブリングさせつつ、噴出孔
より原料溶液を噴出させることにより容易に目的を達成
することができる。[0010] In order to achieve the above object, the raw material solution is preferably formed into fine droplets with a particle size of about 0.5 mm or less. If the particle size of the droplets is too large, the particle size of the obtained hydroxyapatite fine particles tends to vary. Moreover, by supplying the raw material solution together with the bubbling gas, it is supplied under stirring. In order to supply in the above condition, the hole diameter must be 0.5 mm.
The purpose can be easily achieved by ejecting the raw material solution from the ejection hole while bubbling with the following bubble generator.
【００１１】バブリング用気体としてはＮ２あるいは空
気などの気体を適宜用いることができるが、空気を用い
る場合には空気に含まれるＣＯ２を取り込んだアパタイ
トが合成される傾向があり、純粋なヒドロキシアパタイ
トを合成するためには、Ｎ２ガスを用いることが望まし
い。バブリング用気体および原料溶液の供給を調整する
ことにより、原料溶液の粒子径は調節可能である。種々
の実験結果より、気体の供給圧は１．０ 〜５．０ｋｇ
／ｃｍ２、好ましくは３．０ｋｇ／ｃｍ２、原料溶液の
供給圧は１．０ｋｇ／ｃｍ２以下、好ましくは０．５ｋ
ｇ／ｃｍ２に設定される。更に例えば図１に示される様
な２重管構造の内管部に気体が通り、外管部に原料溶液
が通る供給部を有する構造の反応装置を用いて実施する
ことにより、原料溶液は気体により混合されより均一な
状態となる。As the bubbling gas, a gas such as N2 or air can be used as appropriate, but when air is used, apatite that incorporates CO2 contained in the air tends to be synthesized, and pure hydroxyapatite is not produced. For synthesis, it is desirable to use N2 gas. By adjusting the supply of the bubbling gas and the raw material solution, the particle size of the raw material solution can be adjusted. According to various experimental results, the gas supply pressure is 1.0 to 5.0 kg.
/cm2, preferably 3.0kg/cm2, and the supply pressure of the raw material solution is 1.0kg/cm2 or less, preferably 0.5k
g/cm2. Furthermore, by carrying out the reaction using a reactor having a double-tube structure with a supply section where gas passes through the inner tube and where the raw material solution passes through the outer tube, as shown in FIG. The mixture is mixed into a more uniform state.
【００１２】以下実施例によって本発明をさらに詳述す
るが、下記実施例は本発明を制限するものではなく、前
・後記の趣旨を逸脱しない範囲で変更実施することはす
べて本発明の技術範囲に包含される。[0012] The present invention will be explained in more detail with reference to examples below, but the following examples do not limit the present invention, and all modifications and implementations without departing from the spirit of the preceding and following descriptions are within the technical scope of the present invention. included in
【００１３】[0013]
【実施例】実施例１〜３
ＣａＣｌ２とＨ３ＰＯ４とを２．５ リットルの２５℃
の純粋あるいはイオン交換水中に下記表１に示す所定量
を溶解し原料溶液とした。ＫＯＨ を１７．５リットル
の７０℃の純水あるいはイオン交換水中に表１に示す所
定量を溶解しアルカリ溶液とした。[Example] Examples 1 to 3 2.5 liters of CaCl2 and H3PO4 at 25°C
A predetermined amount shown in Table 1 below was dissolved in pure or ion-exchanged water to prepare a raw material solution. A predetermined amount of KOH shown in Table 1 was dissolved in 17.5 liters of 70°C pure water or ion-exchanged water to obtain an alkaline solution.
【００１４】[0014]
【表１】[Table 1]
【００１５】反応に用いた装置を図１に示す。原料溶液
２は、ステンレスの密閉容器に入れ０．５ｋｇ／ｃｍ２
で加圧して前記アルカリ水溶液１中に液滴化して添加し
た。二重管構造のチューブ４から構成された原料供給部
は、アルカリ溶液の入った反応槽３の底部に浸漬した。
二重管構造のチューブの内管にはＮ２ガスを１〜５ｋｇ
／ｃｍ２で加圧して供給し、外管には原料溶液を供給し
た。その結果原料溶液はＮ２ガスとともに、二重管構造
のチューブの外管の表面に設けられた０．５ｍｍ 以下
の大きさのノズル孔５よりアルカリ溶液中に微細な液滴
として供給された。The apparatus used for the reaction is shown in FIG. Raw material solution 2 is placed in a stainless steel airtight container at a density of 0.5 kg/cm2.
The mixture was pressurized to form droplets into the alkaline aqueous solution 1 and added. A raw material supply section composed of a tube 4 having a double pipe structure was immersed in the bottom of a reaction tank 3 containing an alkaline solution. 1 to 5 kg of N2 gas is added to the inner tube of the double tube structure.
/cm2, and the raw material solution was supplied to the outer tube. As a result, the raw material solution was supplied as fine droplets into the alkaline solution together with N2 gas through a nozzle hole 5 with a size of 0.5 mm or less provided on the surface of the outer tube of the double tube structure.
【００１６】反応容器は、恒温水槽を用い７０℃にコン
トロールして合成をおこなった。酸性溶液を全量供給後
、約一時間７０℃で熟成を行った。反応後の懸濁液から
上澄み液を抜き取り、中和洗浄して乾燥させた後、合成
物を粉末Ｘ線回折により同定したところ、純粋なヒドロ
キシアパタイトが合成されていた。図２にＸ線回折ピー
クパターンを示す。また、ＩＣＰ 発光分光分析により
Ｃａ／Ｐが１．６７の化学量論比のヒドロキシアパタイ
トであることを確認した。更に懸濁液を透過型電子顕微
鏡（ＴＥＭ）により観察した結果、０．０５〜０．１０
μｍ の微細で均一なサイズのヒドロキシアパタイトで
あった。[0016] The reaction vessel was controlled at 70°C using a constant temperature water bath for synthesis. After supplying the entire amount of the acidic solution, aging was performed at 70° C. for about one hour. After the supernatant liquid was extracted from the suspension after the reaction, neutralized, washed, and dried, the synthesized product was identified by powder X-ray diffraction, and it was found that pure hydroxyapatite had been synthesized. Figure 2 shows the X-ray diffraction peak pattern. Further, it was confirmed by ICP emission spectrometry that it was hydroxyapatite with a stoichiometric ratio of Ca/P of 1.67. Furthermore, as a result of observing the suspension using a transmission electron microscope (TEM), it was found that the suspension was 0.05 to 0.10.
It was hydroxyapatite with a fine and uniform size of μm.
【００１７】[0017]
【発明の効果】本発明は以上の様に構成されており、化
学量論比で粒子径のそろったヒドロキシアパタイト粉末
を効率よく生産できる方法を提供することができるよう
になった。[Effects of the Invention] The present invention is constructed as described above, and it has become possible to provide a method for efficiently producing hydroxyapatite powder having a stoichiometric ratio and uniform particle diameters.
【図１】（Ａ）は本発明合成装置の概略説明図、（Ｂ）
は原料供給部の平面図、（Ｃ）は（Ｂ）のＡより見た二
重管構造のチューブの断面図である。FIG. 1: (A) is a schematic explanatory diagram of the synthesis apparatus of the present invention, (B)
2 is a plan view of the raw material supply section, and FIG. 2C is a cross-sectional view of a tube with a double tube structure as seen from A in FIG.
【図２】実施例で得られたヒドロキシアパタイトのＸ線
回折ピークパターンを示す図である。FIG. 2 is a diagram showing an X-ray diffraction peak pattern of hydroxyapatite obtained in an example.
１ アルカリ水溶液 ２ 原料溶液 ３ 反応槽 ４ 二重管構造のチューブ ５ ノズル孔 ６ 原料供給部 1 Alkaline aqueous solution 2 Raw material solution 3 Reaction tank 4. Double tube structure tube 5 Nozzle hole 6 Raw material supply department
Claims (2)
を合成するにあたり、原料溶液をバブリング用気体によ
って搬送し微細な液滴としてアルカリ溶液の入った反応
槽内に均一に供給すると共に、前記バブリング用気体の
吹込みによって反応槽内を均一に攪拌することを特徴と
するヒドロキシアパタイト微粒子の合成方法。Claim 1: When synthesizing hydroxyapatite fine particles by a wet method, a raw material solution is transported by a bubbling gas and uniformly supplied as fine droplets into a reaction tank containing an alkaline solution, and the bubbling gas is A method for synthesizing hydroxyapatite fine particles characterized by uniformly stirring the inside of a reaction tank by blowing.
グ用気体と共に供給できる装置を反応槽内の下部に有す
ることを特徴とするヒドロキシアパタイト微粒子の合成
装置。2. An apparatus for synthesizing fine hydroxyapatite particles, comprising a device at the lower part of a reaction tank that can supply a raw material solution in the form of fine droplets together with a bubbling gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13052791A JPH04331719A (en) | 1991-05-02 | 1991-05-02 | Method for synthesizing fine grain of hydroxyapatite and apparatus for synthesis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13052791A JPH04331719A (en) | 1991-05-02 | 1991-05-02 | Method for synthesizing fine grain of hydroxyapatite and apparatus for synthesis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04331719A true JPH04331719A (en) | 1992-11-19 |
Family
ID=15036433
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13052791A Withdrawn JPH04331719A (en) | 1991-05-02 | 1991-05-02 | Method for synthesizing fine grain of hydroxyapatite and apparatus for synthesis |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04331719A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| USRE39196E1 (en) | 1997-01-16 | 2006-07-18 | Massachusetts Institute Of Technology | Nanocrystalline apatites and composites, prostheses incorporating them, and method for their production |
| JP2013006145A (en) * | 2011-06-23 | 2013-01-10 | Central Research Institute Of Electric Power Industry | Mist generator |
-
1991
- 1991-05-02 JP JP13052791A patent/JPH04331719A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| USRE39196E1 (en) | 1997-01-16 | 2006-07-18 | Massachusetts Institute Of Technology | Nanocrystalline apatites and composites, prostheses incorporating them, and method for their production |
| USRE41584E1 (en) | 1997-01-16 | 2010-08-24 | Massachusetts Institute Of Technology | Nanocrystalline apatites and composites, prostheses incorporating them, and method for their production |
| USRE43661E1 (en) | 1997-01-16 | 2012-09-18 | Massachusetts Institute Of Technology | Nanocrystalline apatites and composites, prostheses incorporating them, and method for their production |
| USRE44820E1 (en) | 1997-01-16 | 2014-04-01 | Massachusetts Institute Of Technology | Nanocrystalline apatites and composites, prostheses incorporating them, and methods of their production |
| USRE46275E1 (en) | 1997-01-16 | 2017-01-17 | Massachusetts Institute Of Technology | Nanocrystalline apatites and composites, prostheses incorporating them, and method for their production |
| JP2013006145A (en) * | 2011-06-23 | 2013-01-10 | Central Research Institute Of Electric Power Industry | Mist generator |
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|---|---|---|---|
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