JPH06263415A - Production of spherical hydroxyapatite particle aggregate - Google Patents

Production of spherical hydroxyapatite particle aggregate

Info

Publication number
JPH06263415A
JPH06263415A JP9039793A JP9039793A JPH06263415A JP H06263415 A JPH06263415 A JP H06263415A JP 9039793 A JP9039793 A JP 9039793A JP 9039793 A JP9039793 A JP 9039793A JP H06263415 A JPH06263415 A JP H06263415A
Authority
JP
Japan
Prior art keywords
hydroxyapatite
slurry
spherical
particle aggregate
powder
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.)
Granted
Application number
JP9039793A
Other languages
Japanese (ja)
Other versions
JP2826938B2 (en
Inventor
Minoru Wakana
穣 若菜
Nobuyuki Matsuda
信之 松田
Fumihiro Kaji
文宏 鍛冶
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Taihei Chemical Industrial Co Ltd
Original Assignee
Taihei Chemical Industrial Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Taihei Chemical Industrial Co Ltd filed Critical Taihei Chemical Industrial Co Ltd
Priority to JP5090397A priority Critical patent/JP2826938B2/en
Publication of JPH06263415A publication Critical patent/JPH06263415A/en
Application granted granted Critical
Publication of JP2826938B2 publication Critical patent/JP2826938B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/048Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/281Sorbents specially adapted for preparative, analytical or investigative chromatography
    • B01J20/282Porous sorbents

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Materials For Medical Uses (AREA)
  • Cosmetics (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

PURPOSE:To attain excellent high temp. resistance and high strength with a well-ordered spherical shape by spray drying to sinter a slurry made of a hydroxyapatite particulate, a prescribed quantity of an inorganic deflocculant and water. CONSTITUTION:The slurry 50-150cps in viscosity (Brookfield type rotational viscometer) is obtained by blending 3-30wt.% hydroxyapatite which is a calcium phosphate compound having the composition of Ca10(PO4)6(OH)2, 0.01-2wt.% inorganic deflocculant such as water glass and water. Next, the slurry is sprayed from the upper part of a drying tower such as a spray drier, dried by hot air and taken out from the bottom of the drying tower to obtain a dried material. The spherical hydroxyapatite particle aggregate is obtained by sintering the dried material at >=500 deg.C.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、主として、クロマトグ
ラフィー充填剤、酵素等の生理活性物質の支持体、細胞
培養の支持体、化粧品材料等として使用される球状ヒド
ロキシアパタイト粒子集合体の新規な製造方法に関する
ものである。
FIELD OF THE INVENTION The present invention mainly relates to a novel aggregate of spherical hydroxyapatite particles used as a chromatographic packing material, a support for physiologically active substances such as enzymes, a support for cell culture, and a cosmetic material. The present invention relates to a manufacturing method.

【0002】[0002]

【従来の技術】従来から、球状のヒドロキシアパタイト
粒子集合体、及び、その製造方法は、よく知られてい
る。例えば、特開昭62−230607号公報には、濃
度0.1ないし20重量%のゲル状のヒドロキシアパタ
イトスラリーを100ないし200℃の気流中に噴霧
し、収集したものを、必要に応じて更に乾燥し、焼結し
て、1ないし10μmの粒径を有する球状のヒドロキシ
アパタイト粒子集合体を製造する方法が開示されてい
る。
2. Description of the Related Art Conventionally, spherical hydroxyapatite particle aggregates and a method for producing the same have been well known. For example, in JP-A-62-230607, a gel-like hydroxyapatite slurry having a concentration of 0.1 to 20% by weight is sprayed in an air stream of 100 to 200 ° C. and collected, and if necessary, further collected. A method for producing spherical hydroxyapatite particle aggregates having a particle size of 1 to 10 μm by drying and sintering is disclosed.

【0003】また、特開平2−180707号公報に
は、10ないし60重量%のヒドロキシアパタイト水性
スラリーを、室温以上に加温された傾斜した回転軸を有
する容器の上部に装填し、容器の回転とともにこのスラ
リーを回転させながら乾燥し、必要に応じて更に焼結し
て、20ないし5000μmの粒径を有するヒドロキシ
アパタイト粒子集合体を製造する方法が開示されてい
る。
Further, in JP-A-2-180707, 10 to 60% by weight of an aqueous slurry of hydroxyapatite is loaded on the upper part of a container having an inclined rotating shaft heated to room temperature or above, and the container is rotated. A method for producing a hydroxyapatite particle aggregate having a particle size of 20 to 5000 μm by drying the slurry while rotating and further sintering it as required is disclosed.

【0004】また、特開平2−180709号公報に
は、10〜80重量%の粒径10μm以下のヒドロキシ
アパタイト、及び、0.1〜10重量%のアルギン酸ナ
トリウム等の水溶性可凝固有機高分子化合物からなるス
ラリーを、ノズルから塩化カルシウム水溶液等の凝固浴
に滴下させて、球状カプセルを得、この球状カプセルを
焼成して、平均粒径2〜4000μmの粒径を有する球
状のヒドロキシアパタイト粒子集合体を製造する方法が
開示されている。
Further, JP-A-2-180709 discloses that 10 to 80% by weight of hydroxyapatite having a particle size of 10 μm or less and 0.1 to 10% by weight of a water-soluble coagulable organic polymer such as sodium alginate. A slurry of the compound is dropped from a nozzle into a coagulation bath such as an aqueous solution of calcium chloride to obtain spherical capsules, and the spherical capsules are fired to aggregate spherical hydroxyapatite particles having an average particle diameter of 2 to 4000 μm. A method of making a body is disclosed.

【0005】更に、特開平4−175213号公報に
は、1〜90重量%のヒドロキシアパタイト、0を越え
10重量%以下のポリアクリル酸アンモニウム等の水溶
性高分子分散剤からなるスラリーを、スプレードライヤ
ーに供給して、造粒乾燥して、ほぼ真球状で粒径10μ
m以下のヒドロキシアパタイト粒子集合体を製造する方
法が開示されている。
Further, in JP-A-4-175213, a slurry comprising a water-soluble polymer dispersant such as 1 to 90% by weight of hydroxyapatite and more than 0 and 10% by weight or less of ammonium polyacrylate is sprayed. It is supplied to a dryer, granulated and dried, and it is almost spherical and has a particle size of 10μ.
A method for producing hydroxyapatite particle aggregates of m or less is disclosed.

【0006】[0006]

【発明が解決しようとする課題】特開昭62−2306
07号公報に開示された球状ヒドロキシアパタイト粒子
集合体、及び、特開平2−180707号公報に開示さ
れたヒドロキシアパタイト粒子集合体は、スラリーの状
態から乾燥する過程で、ヒドロキシアパタイト粒子が単
純に塊になっただけのものであるので、焼成しても、粒
子集合体として高い強度のものは得られなかった。
Problems to be Solved by the Invention JP-A-62-2306
In the spherical hydroxyapatite particle aggregates disclosed in JP-A-07-2007 and the hydroxyapatite particle aggregates disclosed in JP-A-2-180707, hydroxyapatite particles simply aggregate in the process of drying from a slurry state. However, even if it was fired, a particle aggregate having a high strength could not be obtained.

【0007】また、特開平2−180709号公報に開
示された球状のヒドロキシアパタイト粒子集合体は、高
温で焼成しなければ、アルギン酸塩等の凝固性有機高分
子化合物がヒドロキシアパタイト粒子の接着剤として働
き、特開平4−175213号公報に開示された真球状
ヒドロキシアパタイト粒子集合体においても、高温で焼
成しなければ、ポリアクリル酸アンモニウム等の高分子
分散剤が、ある程度、ヒドロキシアパタイト粒子の接着
剤として働くことが予想さもさるが、高温で焼成すれ
ば、これらの有機高分子化合物の分解によって接着効果
が失われ、粒子集合体として高い強度のものが得られな
いばかりか、これらの有機化合物の分解・炭化等によっ
て粒子集合体を着色したり、有機化合物の劣化又は発泡
によって集合体粒子が破壊されたりするおそれがあっ
た。
Further, in the spherical hydroxyapatite particle aggregate disclosed in JP-A-2-180709, a coagulable organic polymer compound such as alginate serves as an adhesive for hydroxyapatite particles unless it is fired at a high temperature. In the spherical hydroxyapatite particle aggregate disclosed in Japanese Patent Laid-Open No. 4-175213, a polymer dispersant such as ammonium polyacrylate is, to some extent, an adhesive agent for hydroxyapatite particles unless it is baked at a high temperature. It is expected that it will work as a compound, but if it is baked at a high temperature, the adhesive effect will be lost due to the decomposition of these organic polymer compounds, and it will not be possible to obtain a particle aggregate having high strength, and also the organic compound Particle aggregates are colored by decomposition, carbonization, etc., or aggregate particles are caused by deterioration or foaming of organic compounds. There is a possibility that or be destroyed.

【0008】本発明が解決しようとする課題は、整った
球状の形状を有し、かつ、高温の焼成にも耐え、極めて
高い強度を有するヒドロキシアパタイト粒子集合体を製
造する方法を開発することにある。
[0008] The problem to be solved by the present invention is to develop a method for producing a hydroxyapatite particle aggregate having a regular spherical shape, withstanding high temperature firing and having extremely high strength. is there.

【0009】[0009]

【課題を解決するための手段】本発明者らは、前述の課
題を解決するために、主として、ヒドロキシアパタイト
微粒子3〜30重量%、無機解膠剤0.01〜2重量
%、及び、水からなるスラリーを、乾燥塔の上部から微
細液滴として噴霧し、乾燥し、必要に応じて、焼結する
ことを特徴とする球状ヒドロキシアパタイト粒子集合体
の製造方法を提案する。また、この方法においてヒドロ
キシアパタイトスラリーにベンガラ、カオリン、タルク
等の顔料を添加して複合化することにより有色顔料とし
ても使用できる。
In order to solve the above-mentioned problems, the inventors of the present invention have mainly used 3 to 30% by weight of hydroxyapatite fine particles, 0.01 to 2% by weight of an inorganic peptizer, and water. We propose a method for producing a spherical hydroxyapatite particle aggregate, which comprises spraying a slurry containing the above from the upper part of a drying tower as fine droplets, drying and, if necessary, sintering. Further, in this method, a pigment such as red iron oxide, kaolin, talc, etc. is added to the hydroxyapatite slurry to form a composite, which can be used as a colored pigment.

【0010】本発明におけるヒドロキシアパタイト微粒
子とは、Ca10(PO(OH)なる組成を有
するりん酸カルシウム化合物であり、水酸化カルシウム
水溶液とりん酸との反応、及び、塩化カルシウム等の水
溶性カルシウム塩の水溶液とりん酸もしくは水溶性りん
酸塩水溶液との反応等の溶液反応、又は、水蒸気下にお
けるりん酸カルシウムと炭酸カルシウムとの高温固相反
応等種々の方法により製造される。なお、本発明におけ
るヒドロキシアパタイト微粒子ついては、微細な結晶の
ものをうるために、溶液反応で得られたものが好まし
く、更に、特に純度の高いものうるためには、水酸化カ
ルシウム水溶液とりん酸との反応によって製造されたも
のが好ましい。
The hydroxyapatite fine particles in the present invention are a calcium phosphate compound having a composition of Ca 10 (PO 4 ) 6 (OH) 2, which reacts with an aqueous solution of calcium hydroxide and phosphoric acid, and calcium chloride and the like. It is produced by various methods such as a solution reaction such as a reaction between an aqueous solution of the water-soluble calcium salt of bisphenol and phosphoric acid or an aqueous solution of the water-soluble phosphate, or a high temperature solid-state reaction of calcium phosphate and calcium carbonate under steam. . The hydroxyapatite fine particles in the present invention are preferably those obtained by a solution reaction in order to obtain fine crystals, and further, in order to obtain particularly high purity, calcium hydroxide aqueous solution and phosphoric acid are used. What was manufactured by the reaction of is preferable.

【0011】本発明におけるスラリー中のヒドロキシア
パタイトの濃度は3〜30重量%であり、特に好ましい
範囲は5〜20重量%である。濃度が低いほど得られる
球状ヒドロキシアパタイト粒子の大きさが小さくなり、
濃度が高いほど得られる粒子が大きくなる。また、3重
量%未満であると噴霧乾燥の際の効率が悪くなるだけで
なく、球状の粒子が得難くあり、30重量%を超えると
均一な大きさの粒子が得難くなるだけでなく、得られた
粒子の形状もいびつになる。
The concentration of hydroxyapatite in the slurry of the present invention is 3 to 30% by weight, and a particularly preferred range is 5 to 20% by weight. The lower the concentration, the smaller the size of spherical hydroxyapatite particles obtained,
The higher the concentration, the larger the particles obtained. Further, if it is less than 3% by weight, not only the efficiency at the time of spray drying is deteriorated, but also it is difficult to obtain spherical particles, and if it exceeds 30% by weight, it becomes difficult to obtain particles having a uniform size. The shape of the obtained particles also becomes distorted.

【0012】本発明において使用される無機解膠剤は、
スラリー中のヒドロキシアパタイトのゲル化するのを防
止し、噴霧されるスラリーの流動性を維持して、噴霧さ
れる微細液滴の大きさを均一化するとともに、噴霧され
た微細液滴の形状を球形に維持するためのものである
が、更に、乾燥後の粉体の焼結の際、ヒドロキシアパタ
イトの融着剤としても作用するものが好ましい。このよ
うな無機解膠剤として、ヘキサメタりん酸ナトリウム、
水ガラス、シリカゾル、アルミナゾル等をあげることが
できる。
The inorganic peptizer used in the present invention is
It prevents the hydroxyapatite in the slurry from gelling, maintains the fluidity of the slurry to be sprayed, and makes the size of the sprayed fine droplets uniform, and also the shape of the sprayed fine droplets. Although it is for maintaining a spherical shape, it is preferable that it also acts as a fusing agent for hydroxyapatite during sintering of the powder after drying. As such an inorganic peptizer, sodium hexametaphosphate,
Examples thereof include water glass, silica sol, alumina sol and the like.

【0013】前述の組成の本発明におけるスラリーのB
型回転粘度計に粘度よるは、50〜150cpsの範囲
にあり、これを、スプレードライヤーのような乾燥塔の
上部から噴霧し、熱風により乾燥し、乾燥塔底部から取
り出したものを、500℃以上で焼結して、製品とす
る。
B of the slurry of the present invention having the aforementioned composition
The viscosity depends on the mold type rotational viscometer and is in the range of 50 to 150 cps. This is sprayed from the top of a drying tower such as a spray dryer, dried with hot air, and taken out from the bottom of the drying tower at 500 ° C. or higher. Sintered with to make a product.

【0014】[0014]

【作用】本発明に係わる方法により製造された球状ヒド
ロキシアパタイト粒子は、無機解膠剤によりヒドロキシ
アパタイトが均一に分散されているため、単に液滴とし
て球状の形状を有し、更に製品として球状の形状を有す
るだけでなく、有機高分子分散剤を使用した場合と異な
り焼成の際に着色、劣化、発泡等の問題がなく、充分に
焼成することができので、強度の高い粒子を得ることが
できる。更に、ヘキサメタりん酸ナトリウムのように解
膠剤の中に、焼成の際に融着剤として働くものがある場
合には、更に高い強度の粒子をえることができる。
The spherical hydroxyapatite particles produced by the method according to the present invention have a spherical shape as a droplet because the hydroxyapatite is uniformly dispersed by the inorganic peptizer, and the spherical hydroxyapatite particles have a spherical shape as a product. Not only does it have a shape, but unlike the case where an organic polymer dispersant is used, there is no problem of coloring, deterioration, foaming, etc. at the time of firing, and since it can be sufficiently fired, particles with high strength can be obtained. it can. Furthermore, when some of the deflocculants such as sodium hexametaphosphate function as a fusing agent during firing, particles having higher strength can be obtained.

【0015】[0015]

【実施例】【Example】

1. ヒドロキシアパタイトスラリーの製造 17.7重量%の水酸化カルシウム水溶液4.15l
に、10%りん酸5.85lを徐々に添加し、10重量
%ヒドロキシアパタイトスラリーを得た。このスラリー
の粘度は250cpsであった。
1. Production of hydroxyapatite slurry 4.15 l of 17.7 wt% calcium hydroxide aqueous solution
Then, 5.85 l of 10% phosphoric acid was gradually added to obtain a 10 wt% hydroxyapatite slurry. The viscosity of this slurry was 250 cps.

【0016】2. 球状ヒドロキシアパタイトの製造 〔実施例〕前述のヒドロキシアパタイトスラリーに0.
02重量%になるようにヘキサメタりん酸ナトリウムを
添加した。添加後のスラリーの粘度は150cpsであ
った。このスラリーを100kg/hrの流量で、回転
円盤型噴霧乾燥機に供給し、円盤回転数20000rp
m、熱風の入口温度350℃、出口温度130℃で乾燥
した。得られた粒子の平均直径は15μmであった。こ
れを500℃で焼結し、風力分級機(日本ニューマチッ
ク(株)製MDS型)で分級して粉体(以下「粉体1」
という)を得た。この粉体の平均直径は10μmであっ
た。
2. Production of Spherical Hydroxyapatite [Example] Into the hydroxyapatite slurry described above, 0.
Sodium hexametaphosphate was added so that it would be 02% by weight. The viscosity of the slurry after the addition was 150 cps. This slurry is supplied to a rotary disk type spray dryer at a flow rate of 100 kg / hr, and the disk rotational speed is 20000 rp.
m, the hot air inlet temperature was 350 ° C, and the outlet temperature was 130 ° C. The average diameter of the obtained particles was 15 μm. This is sintered at 500 ° C and classified by an air classifier (MDS type manufactured by Nippon Pneumatic Co., Ltd.) to obtain powder (hereinafter referred to as "powder 1").
I got). The average diameter of this powder was 10 μm.

【0017】〔比較例〕前述のヒドロキシアパタイトス
ラリーに何も添加せずに、そのまま実施例と同一の条件
で回転円盤型噴霧乾燥機に供給した。このスラリーの粘
度は250cpsであり、得られた粒子の平均直径は1
5μmであった。これを実施例と同一の条件で焼結し、
分級して粉体(以下「粉体2」という)を得た。この粉
体の平均直径は10μmであった。
Comparative Example Nothing was added to the above-mentioned hydroxyapatite slurry, and the slurry was directly supplied to a rotary disk type spray dryer under the same conditions as in the examples. The viscosity of this slurry is 250 cps and the average diameter of the obtained particles is 1
It was 5 μm. Sinter this under the same conditions as the example,
A powder (hereinafter referred to as "powder 2") was obtained by classification. The average diameter of this powder was 10 μm.

【0018】 3. 球状ヒドロキシアパタイトの形状試験 実施例で得られた粉体1と比較例で得られた粉体2の粒
度をレーザ回折式粒度分布測定装置(島津製作所(株)
製SALD−1100)により測定した。その結果は、
図1及び図2のとおりであった。また、粉体1と粉体2
の電子顕微鏡写真を電子顕微鏡写真装置(日立製作所
(株)製S−1300)により撮影した。その結果は、
図3及び図4のとおりであった。図1と図2とを比較
し、図3と図4とを比較しても明らかなように、本発明
に係わる粉体1は、強固に球状の形状を維持している
が、無機解膠剤を添加していない粉体2は、分級による
弱い物理的な力によっても壊れることが認められる。
3. Shape test of spherical hydroxyapatite The particle size of the powder 1 obtained in the example and the powder 2 obtained in the comparative example were measured by a laser diffraction type particle size distribution measuring device (Shimadzu Corporation).
SALD-1100 manufactured by SALD). The result is
The results are shown in FIGS. 1 and 2. Also, powder 1 and powder 2
The electron micrograph of was taken by an electron microscope photographic device (S-1300 manufactured by Hitachi, Ltd.). The result is
The results are shown in FIGS. 3 and 4. As is clear from comparison between FIG. 1 and FIG. 2 and comparison between FIG. 3 and FIG. 4, the powder 1 according to the present invention strongly maintains the spherical shape, It is recognized that the powder 2 to which the agent is not added is broken even by a weak physical force due to classification.

【0019】 4. 球状ヒドロキシアパタイトの強度試験 粉体1及び粉体2を、それぞれ、内径4.6mm 長さ
150mmのステンレススチールカラムにスラリー充填
法により充填した。この時の充填圧は500kg/cm
であった。充填後、それぞれ、カラムより粉体1及び
粉体2を取り出し、これらの粉体の粒度をレーザ回折式
粒度分布測定装置(島津製作所(株)製SALD−11
00)により測定した。その結果は、図5及び図6のと
おりであった。図1と図5、及び、図2と図6を比較し
ても明らかなように、本発明に係わる粉体1は、粒度が
殆ど変化していないのに対し、無機解膠剤を添加してい
ない粉体2は、カラムの充填の後において、粒子集合体
の崩壊が認められる。
[0019] 4. Strength Test of Spherical Hydroxyapatite Powder 1 and powder 2 were each packed in a stainless steel column having an inner diameter of 4.6 mm and a length of 150 mm by a slurry packing method. The filling pressure at this time is 500 kg / cm
It was 2 . After the packing, the powder 1 and the powder 2 are taken out from the column, and the particle size of these powders is measured by a laser diffraction particle size distribution analyzer (SALD-11 manufactured by Shimadzu Corporation).
00). The results are shown in FIGS. 5 and 6. As is clear from comparing FIG. 1 and FIG. 5 and FIG. 2 and FIG. 6, the powder 1 according to the present invention has almost no change in particle size, while the inorganic peptizer is added. In the powder 2 which is not present, the collapse of the particle aggregate is observed after the column is packed.

【0020】[0020]

【発明の効果】本発明に係わる球状ヒドロキシアパタイ
ト粒子集合体の製造方法は、前述のような構成と作用を
有するので、整った球状の形状と高い強度を有する球状
ヒドロキシアパタイト粒子集合体の製造を可能にするの
で、本発明に係わる製造方法によって得られた球状ヒド
ロキシアパタイト粒子集合体は、クロマトグラフィー充
填剤、酵素等の生理活性物質の支持体、細胞培養の支持
体、化粧品材料等として極めて優れた特性を有するもの
となる。
EFFECT OF THE INVENTION The method for producing spherical hydroxyapatite particle aggregates according to the present invention has the above-mentioned constitution and action, and therefore, the production of spherical hydroxyapatite particle aggregates having a regular spherical shape and high strength can be performed. The spherical hydroxyapatite particle aggregate obtained by the production method according to the present invention is extremely excellent as a chromatographic packing material, a support for physiologically active substances such as enzymes, a support for cell culture, a cosmetic material, etc. Have the following characteristics.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明に係わる球状ヒドロキシアパタイト粒子
集合体の粒度分布
FIG. 1 Particle size distribution of spherical hydroxyapatite particle aggregates according to the present invention

【図2】比較例に係わる球状ヒドロキシアパタイト粒子
集合体の粒度分布
FIG. 2 Particle size distribution of spherical hydroxyapatite particle aggregates according to Comparative Example

【図3】本発明に係わる球状ヒドロキシアパタイト粒子
集合体の電子顕微鏡写真
FIG. 3 is an electron micrograph of a spherical hydroxyapatite particle aggregate according to the present invention.

【図4】比較例に係わる球状ヒドロキシアパタイト粒子
集合体の電子顕微鏡写真
FIG. 4 is an electron micrograph of a spherical hydroxyapatite particle aggregate according to a comparative example.

【図5】カラムから取り出した本発明に係わる球状ヒド
ロキシアパタイト粒子集合体の粒度分布
FIG. 5: Particle size distribution of spherical hydroxyapatite particle aggregates according to the present invention taken out from a column

【図6】カラムから取り出した比較例に係わる球状ヒド
ロキシアパタイト粒子集合体の粒度分布
FIG. 6 is a particle size distribution of spherical hydroxyapatite particle aggregates according to a comparative example taken out from the column.

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 主として、ヒドロキシアパタイト微粒子
3〜30重量%、無機解膠剤0.01〜2重量%、及
び、水からなるスラリーを、乾燥塔の上部から微細液滴
として噴霧し、乾燥し、必要に応じて、焼結することを
特徴とする球状ヒドロキシアパタイト粒子集合体の製造
方法
1. A slurry mainly comprising 3 to 30% by weight of hydroxyapatite fine particles, 0.01 to 2% by weight of an inorganic peptizer, and water is sprayed as fine droplets from the upper part of a drying tower and dried. And a method for producing a spherical hydroxyapatite particle aggregate characterized by sintering, if necessary.
JP5090397A 1993-03-11 1993-03-11 Method for producing spherical hydroxyapatite particle aggregate Expired - Lifetime JP2826938B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP5090397A JP2826938B2 (en) 1993-03-11 1993-03-11 Method for producing spherical hydroxyapatite particle aggregate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP5090397A JP2826938B2 (en) 1993-03-11 1993-03-11 Method for producing spherical hydroxyapatite particle aggregate

Publications (2)

Publication Number Publication Date
JPH06263415A true JPH06263415A (en) 1994-09-20
JP2826938B2 JP2826938B2 (en) 1998-11-18

Family

ID=13997457

Family Applications (1)

Application Number Title Priority Date Filing Date
JP5090397A Expired - Lifetime JP2826938B2 (en) 1993-03-11 1993-03-11 Method for producing spherical hydroxyapatite particle aggregate

Country Status (1)

Country Link
JP (1) JP2826938B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011037120A1 (en) * 2009-09-28 2011-03-31 Hoya株式会社 Powder, process for production of powder, and adsorption device
JP2014509294A (en) * 2011-01-27 2014-04-17 シリム バーハド Method for simultaneously converting limestone into tricalcium phosphate and tetracalcium phosphate powders

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04175212A (en) * 1990-11-09 1992-06-23 Sekisui Plastics Co Ltd Method for wet synthesis of hydroxyapatite

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04175212A (en) * 1990-11-09 1992-06-23 Sekisui Plastics Co Ltd Method for wet synthesis of hydroxyapatite

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011037120A1 (en) * 2009-09-28 2011-03-31 Hoya株式会社 Powder, process for production of powder, and adsorption device
JP2011068539A (en) * 2009-09-28 2011-04-07 Hoya Corp Powder, method for producing powder, and adsorber
GB2487864A (en) * 2009-09-28 2012-08-08 Hoya Corp Powder, process for production of powder, and adsorption device
GB2487864B (en) * 2009-09-28 2015-07-29 Hoya Corp Powder, method of producing powder, and adsorption apparatus
JP2014509294A (en) * 2011-01-27 2014-04-17 シリム バーハド Method for simultaneously converting limestone into tricalcium phosphate and tetracalcium phosphate powders

Also Published As

Publication number Publication date
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