JPH0251466A - Production of calcium phosphate molded body and calcium phosphate sintered body - Google Patents
Production of calcium phosphate molded body and calcium phosphate sintered bodyInfo
- Publication number
- JPH0251466A JPH0251466A JP63202783A JP20278388A JPH0251466A JP H0251466 A JPH0251466 A JP H0251466A JP 63202783 A JP63202783 A JP 63202783A JP 20278388 A JP20278388 A JP 20278388A JP H0251466 A JPH0251466 A JP H0251466A
- Authority
- JP
- Japan
- Prior art keywords
- calcium phosphate
- molded body
- molded
- slurry
- molding
- 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.)
- Pending
Links
- 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 title claims abstract description 40
- 239000001506 calcium phosphate Substances 0.000 title claims abstract description 38
- 229910000389 calcium phosphate Inorganic materials 0.000 title claims abstract description 35
- 235000011010 calcium phosphates Nutrition 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 238000000465 moulding Methods 0.000 claims abstract description 17
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 238000010304 firing Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 abstract description 10
- 229910052586 apatite Inorganic materials 0.000 abstract description 6
- 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 abstract description 6
- 210000000988 bone and bone Anatomy 0.000 abstract description 3
- 229910000391 tricalcium phosphate Inorganic materials 0.000 abstract description 3
- 235000019731 tricalcium phosphate Nutrition 0.000 abstract description 3
- 229940078499 tricalcium phosphate Drugs 0.000 abstract description 3
- 238000005336 cracking Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 210000004746 tooth root Anatomy 0.000 abstract 1
- XWKBMOUUGHARTI-UHFFFAOYSA-N tricalcium;diphosphite Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])[O-].[O-]P([O-])[O-] XWKBMOUUGHARTI-UHFFFAOYSA-N 0.000 abstract 1
- 238000000034 method Methods 0.000 description 18
- 239000002244 precipitate Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 208000005156 Dehydration Diseases 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 1
- 230000000035 biogenic effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 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 description 1
- 238000007493 shaping process Methods 0.000 description 1
Landscapes
- Materials For Medical Uses (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明はリン酸カルシウム成形体及びリン酸カルシウム
焼結体の製造方法に関する。さらに詳しくは、本発明は
スラリー状のリン酸カルシウムを湿式プレスにより脱水
、加圧成形するリン酸カルシウム成形体の製造方法及び
このようにして得られた成形体を焼成するリン酸カルシ
ウム焼結体の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a calcium phosphate molded body and a method for producing a calcium phosphate sintered body. More specifically, the present invention relates to a method for producing a calcium phosphate molded body by dehydrating and press-molding slurry-like calcium phosphate by wet pressing, and a method for producing a calcium phosphate sintered body by firing the molded body thus obtained.
従来の技術
近年、リン酸カルシウム焼結体は、人工骨材、人工歯根
などの生体材料として、その需要は益々増加の一途をた
どりつつある。リン酸カルシウムはこれを成形したのち
、焼成により、高強度の焼結体とされているが、この成
形方法としては、湿式沈殿法で得られたリン酸カルシウ
ムのゼラチン状沈殿物を成形型も兼ねる遠沈管に入れ、
分離し、そのまま乾燥して成形体とする方法（特開昭６
２４６９４９号公報）、ゼラチン状沈殿物を切断、造形
、成形して成形体とする方法（特公昭５９−４１９４６
号公報）などが知られている。しかし、いずれの場合も
、沈殿の生成条件により、成形体密度が変化するため、
通常ではその都度乾燥条件を変えなければならないし、
またこのようにしても一定の高密度体をコンスタントに
得ることが難しいという欠点を有する。また、得られた
成形体は水分量が多く軟質のため保形性が低い上に長時
間にわたる乾燥処理を免れず、しかも乾燥による収縮率
が２５〜５０％と大きいため、乾燥後ひびが入りやすく
、大型のものは作れないという欠点がある。さらに、遠
沈管を用いる場合は、形や大きさが制限されるのを免れ
ない。BACKGROUND OF THE INVENTION In recent years, the demand for calcium phosphate sintered bodies as biomaterials for artificial aggregates, artificial tooth roots, etc. has been steadily increasing. Calcium phosphate is molded and then fired to produce a high-strength sintered body. This molding method involves placing a gelatinous precipitate of calcium phosphate obtained by a wet precipitation method in a centrifuge tube that also serves as a mold. Get in,
A method of separating and drying as it is to form a molded body (Japanese Patent Application Laid-open No. 6
246949), a method of cutting, shaping and molding a gelatinous precipitate into a molded body (Japanese Patent Publication No. 59-41946)
Publication No.) etc. are known. However, in either case, the density of the compact changes depending on the conditions for forming the precipitate.
Normally, you have to change the drying conditions each time.
Further, even if this method is used, there is a drawback that it is difficult to constantly obtain a certain high-density body. In addition, the obtained molded product has a high moisture content and is soft, so it has poor shape retention and has to be dried for a long time.Moreover, the shrinkage rate due to drying is as high as 25-50%, so it cracks after drying. The drawback is that it is easy to make and cannot be made in large sizes. Furthermore, when using a centrifuge tube, the shape and size are inevitably limited.
他方、上記ゼラチン状沈殿物からの成形体を、成形圧３
００〜５０００ｋｇ／ ｃｍ２でラバープレスする方法
も知られているが（特開昭６２−１１３７５７号公報）
、乾燥物を粉砕しさらにプレス処理するという煩雑な操
作を要するのを免れない。On the other hand, the molded body made from the gelatinous precipitate was molded under a molding pressure of 3
A method of rubber pressing at 00 to 5000 kg/cm2 is also known (Japanese Unexamined Patent Publication No. 113757/1983).
However, it is unavoidable that complicated operations such as pulverizing the dried material and further press processing are required.
発明が解決しようとする課題
本発明は、このような従来の欠点を克服し、高品質のリ
ン酸カルシウム成形体及びリン酸カルシウム焼結体を簡
単に、かつ工業的に有利に製造する方法を提供すること
を目的としてなされたものである。Problems to be Solved by the Invention The present invention aims to overcome these conventional drawbacks and provide a method for easily and industrially advantageous manufacturing of high-quality calcium phosphate molded bodies and calcium phosphate sintered bodies. It was done for a purpose.
課題を解決するための手段
本発明者らは、リン酸カルシウム成形体及びリン酸カル
シウム焼結体の工業的に有利な製造方法を開発するため
に種々研究を重ねた結果、金型中で加圧と脱水を同時に
行うことができる、いわゆる湿式プレスをリン酸カルシ
ウムスラリーに適用することにより、その目的を達成し
うろことを見出し、この知見に基づいて本発明を完成す
るに至った。Means for Solving the Problems The present inventors have conducted various studies to develop an industrially advantageous manufacturing method for calcium phosphate molded bodies and calcium phosphate sintered bodies, and as a result, the present inventors have developed a method for pressurizing and dehydrating in a mold. It was discovered that the objective could be achieved by applying so-called wet pressing to calcium phosphate slurry, which can be carried out simultaneously, and based on this knowledge, the present invention was completed.
すなわち、本発明は、スラリー状のリン酸カルシウムを
湿式プレスにより脱水しながら、加圧成形することを特
徴とするリン酸カルシウム成形体の製造方法、及びスラ
リー状のリン酸カルシウムを湿式プレスにより脱水しな
がら、加圧成形したのち、得られた成形体を焼成するこ
とを特徴とするリン酸カルシウム焼結体の製造方法を提
供するものである。That is, the present invention provides a method for producing a calcium phosphate molded body, which is characterized in that a slurry of calcium phosphate is pressure-molded while being dehydrated by a wet press, and a method of producing a calcium phosphate molded body is characterized in that a slurry of calcium phosphate is pressure-molded while being dehydrated by a wet press. The present invention provides a method for producing a calcium phosphate sintered body, which is characterized in that the obtained molded body is then fired.
本発明で用いるリン酸カルシウムとしては、例えば、ア
パタイトやリン酸三カルシウムなどが挙げられ、このも
のは単独で用いてもよいし、また２種以上の混合物とし
て用いてもよい。アパタイトとしては、乾式法又は湿式
法による合成アパタイトでもよいし、各種を推動物の骨
、歯から回収された生体アパタイトでもよい。例えば、
乾式法としては、９００−１３００°Ｃの高温下の水蒸
気気流中でリン酸カルシウムと過剰のＣａＯを反応させ
る方法等が挙げられる。リン酸三カルシウムとしては、
α−リン酸三カルシウムやβ−リン酸三カルシウムなど
が挙げられる。Examples of the calcium phosphate used in the present invention include apatite and tricalcium phosphate, which may be used alone or as a mixture of two or more. The apatite may be synthetic apatite produced by a dry or wet method, or may be biogenic apatite recovered from the bones and teeth of various animals. for example,
Examples of the dry method include a method in which calcium phosphate and excess CaO are reacted in a steam stream at a high temperature of 900 to 1300°C. As tricalcium phosphate,
Examples include α-tricalcium phosphate and β-tricalcium phosphate.
本発明のリン酸カルシウム成形体を製造するには、先ず
、リン酸カルシウムのスラリーを調製する。このスラリ
ー濃度は５０〜９５％、好ましくは６０〜８７％とする
。このスラリーを湿式プレス金型に入れ、所要の成形圧
で加圧しながら、脱水する。この脱水処理は吸引脱水が
好ましく、吸引力を減圧条件等をコントロールすること
により調整することができ、この吸引力の程度に応じて
成形体の含水率を調整することができる。前記成形圧は
通常１０〜４０００ｋｇ／ ｃｍ”、好ましくは２０〜
３００、より好ましくは３０〜２００の範囲である。To manufacture the calcium phosphate molded article of the present invention, first, a slurry of calcium phosphate is prepared. The slurry concentration is 50-95%, preferably 60-87%. This slurry is placed in a wet press mold and dehydrated while being pressed at the required molding pressure. This dehydration treatment is preferably carried out by suction dehydration, and the suction force can be adjusted by controlling the vacuum conditions, etc., and the water content of the molded article can be adjusted depending on the degree of this suction force. The molding pressure is usually 10 to 4000 kg/cm", preferably 20 to 4000 kg/cm".
300, more preferably in the range of 30-200.
このようにして得たリン酸カルシウム成形体は必要に応
じて乾燥する。The calcium phosphate molded body thus obtained is dried if necessary.
本発明のリン酸カルシウム焼結体を製造するには、前記
リン酸カルシウム成形体の製造方法と同様な操作後、得
られた成形体を焼成することによって行われる。この際
の焼成温度は通常８００〜１５００℃、好ましくは１０
００−１４００°Ｃの範囲である。また、焼成時間は成
形体の種類や焼成温度等により異なるが、通常５分〜１
２時間、好ましくは３０分〜８時間の範囲である。The calcium phosphate sintered body of the present invention is produced by performing the same operations as in the method for producing the calcium phosphate molded body, and then firing the obtained molded body. The firing temperature at this time is usually 800 to 1500°C, preferably 10°C.
The range is 00-1400°C. The firing time varies depending on the type of compact and firing temperature, but is usually 5 minutes to 1 hour.
The time period is 2 hours, preferably 30 minutes to 8 hours.
次に添付図面に従って、本発明の実施態様の１例を説明
する。Next, one example of an embodiment of the present invention will be described according to the accompanying drawings.
先ず第１図ないし第４図は、本発明の一連の操作過程を
示す断面図であって、ダイス３と上バンチ１１下パンチ
２で形成された空隙部４に、射出ポンプ５を介して原料
スラリーＡを充てんする（第１図、第２図）。次に上バ
ンチｌと下バンチ２を操作してスラリーＡを押圧し、各
パンチに設けられたチャンネル６・・・及び各パンチの
スラリー接触面に取り付けられたフィルター７．７を介
して脱水しながら、加圧成形する（第３図）。最後に、
十分な強度が得られるまでリン酸カルシウムを固化させ
たのち、下バンチ２を押し上げてダイス３から成形体８
を取り出す（第４図）。 上記のチャンネル６は、上パ
ンチ１又は下パンチ２の一方のみに設けるだけでもよい
。First of all, FIGS. 1 to 4 are cross-sectional views showing a series of operating steps of the present invention, in which the raw material is injected into the cavity 4 formed by the die 3, the upper bunch 11, and the lower punch 2 via the injection pump 5. Fill with slurry A (Figures 1 and 2). Next, the slurry A is pressed by operating the upper bunch L and the lower bunch 2, and is dehydrated through the channels 6 provided in each punch and the filters 7 and 7 attached to the slurry contact surface of each punch. Pressure molding is carried out (Fig. 3). lastly,
After solidifying the calcium phosphate until sufficient strength is obtained, the lower bunch 2 is pushed up and the molded body 8 is released from the die 3.
Take out (Figure 4). The above-mentioned channel 6 may be provided only in either the upper punch 1 or the lower punch 2.
このようにして得た成形体を、常法に従って焼成すれば
、リン酸カルシウム焼結体を得ることができる。A calcium phosphate sintered body can be obtained by firing the molded body thus obtained according to a conventional method.
発明の効果
本発明方法によれば、成形体の水分量が少ないため、乾
燥時にほとんど収縮せず、ひびが入りにくく、大型の成
形体も作れるし、また乾燥時間が少なくてすみ、トータ
ルの成形時間が短縮されるし、さらにまた遠沈管による
ように形が限定されることがないし、しかも沈殿法など
の湿式法で得られたスラリーをそのまま脱水、高圧成形
することができ、従来のラバープレス法などの高圧成形
において前処理として不可欠な粉砕操作を要しないとい
う顕著な効果を奏する。Effects of the Invention According to the method of the present invention, since the moisture content of the molded product is small, it hardly shrinks during drying, is less likely to crack, large-sized molded products can be made, and the drying time is short, which improves overall molding. It saves time, and the shape is not limited as with centrifuge tubes. Furthermore, slurry obtained by wet methods such as precipitation can be dehydrated and high-pressure molded as is, and it does not require the use of conventional rubber presses. This has the remarkable effect of eliminating the need for a pulverization operation, which is essential as a pretreatment in high-pressure molding such as methods.
本発明の焼結体は、ち密、硬質で、優れた強度を有し、
構造物、特に人工歯根や人工骨用などのの生体構造物な
どとして好適に使用される。The sintered body of the present invention is dense, hard, and has excellent strength.
It is suitably used as structures, especially biological structures such as artificial tooth roots and artificial bones.
実施例 次に実施例によって本発明をさらに詳細に説明する。Example Next, the present invention will be explained in more detail with reference to Examples.
実施例１
湿式沈殿法により合成したヒドロキシアパタイトを、定
性ろ紙により脱水して、スラリー濃度７５％にした。得
られたスラリー３０ｙを金型（３０ｄｍｍ）に入れた。Example 1 Hydroxyapatite synthesized by a wet precipitation method was dehydrated using qualitative filter paper to give a slurry concentration of 75%. The obtained slurry 30y was placed in a mold (30 dmm).
金型のうすの上にフィルターを載置し、成形圧４００＃
ｇ／ ｃｒｙ”で成形しｔ；。この際、上パンチに設け
た吸引穴から水分を吸引した。Place the filter on top of the mold and set the molding pressure to 400#.
g/cry". At this time, water was sucked out from the suction hole provided in the upper punch.
このようにして得た成形体を１２０℃で８時間乾燥し、
成形密度１６ｙ／ｃ−の乾燥成形体を得た。乾燥時の収
縮率は０％であった。この乾燥成形体を１３００°Ｃで
２時間焼成し、焼結密度３．１０９／Ｃがの焼結体を得
た。The molded body thus obtained was dried at 120°C for 8 hours,
A dry molded body with a molded density of 16y/c- was obtained. The shrinkage rate during drying was 0%. This dry compact was fired at 1300°C for 2 hours to obtain a sintered body with a sintered density of 3.109/C.
実施例２
アバタイ）ＩＮ料を湿式振動ミルにより６０分間粉砕し
た。定性ろ紙により吸引脱水して、スラリー濃度８０％
にした。得られたスラリー１００ｇを金型（５０ｍｍｘ
５０ｍｍ）に入れ、吸引脱水しながら、成形圧２００
７２９／ ｃｒｓ２で成形した。Example 2 Avatai) IN material was ground for 60 minutes using a wet vibration mill. Suction dehydrated using qualitative filter paper to obtain a slurry concentration of 80%.
I made it. 100g of the obtained slurry was placed in a mold (50mm x
50 mm), and while dehydrating with suction, press 200 molding pressure.
Molded with 729/crs2.
このようにして得た成形体を５０°Ｃで２４時間乾燥し
、成形密度１−４９７ｃｍ３の乾燥成形体を得た。乾燥
時の収縮率は０％であった。この乾燥成形体を１３００
’ｃで２時間焼成し、焼結密度３．０５９／ｃ＋＋＋３
の焼結体を得た。The molded body thus obtained was dried at 50° C. for 24 hours to obtain a dry molded body with a molded density of 1-497 cm 3 . The shrinkage rate during drying was 0%. This dry molded body was heated to 1300
Sintered at 'c for 2 hours, sintered density 3.059/c+++3
A sintered body was obtained.
実施例３
アパタイト原料１００ｇに水３０ｇを混合し、混練機に
よりｌＯ分間混合した。得られたスラリーを金型Ｃ６Ｉ
ｍｍ）に入れ、吸引脱水しながら、成形圧６００ｋｇ／
ｃｍ”で成形し、成形密度１．６ｇ／ｃ＋＊”ノ成形
体を得た。Example 3 100 g of apatite raw material was mixed with 30 g of water and mixed for 10 minutes using a kneader. The obtained slurry was molded into mold C6I.
mm), and while dehydrating with suction, the molding pressure was 600 kg/
cm" to obtain a molded product with a molding density of 1.6 g/c++".
このようにして得た成形体を１２５０°Ｃで３時間焼成
し、焼結密度３−１３ｇ／ｃｍ’の焼結体を得た。The molded body thus obtained was fired at 1250°C for 3 hours to obtain a sintered body with a sintered density of 3-13 g/cm'.
第１図ないし第４図は本発明方法に従って湿式プレス機
を用いた成形工程の１例を示す断面図であり、図中１は
上パンチ、２は下パンチ、３はダイス、４は空隙部、５
は射出ポンプ、６はチャンネル、７はフィルター、８は
成形体、Ａは原料スラリーを示す。
第
図
第
図
第
図
第
図1 to 4 are cross-sectional views showing an example of a molding process using a wet press machine according to the method of the present invention, in which 1 is an upper punch, 2 is a lower punch, 3 is a die, and 4 is a gap. , 5
6 is an injection pump, 6 is a channel, 7 is a filter, 8 is a molded body, and A is a raw material slurry. Figure Figure Figure Figure Figure
Claims (1)
脱水しながら、加圧成形することを特徴とするリン酸カ
ルシウム成形体の製造方法。 ２ スラリー状のリン酸カルシウムを湿式プレスにより
脱水しながら、加圧成形したのち、得られた成形体を焼
成することを特徴とするリン酸カルシウム焼結体の製造
方法。[Scope of Claims] 1. A method for producing a calcium phosphate molded article, which comprises pressurizing and molding slurry-like calcium phosphate while dehydrating it using a wet press. 2. A method for producing a calcium phosphate sintered body, which comprises pressing and molding a slurry of calcium phosphate while dehydrating it using a wet press, and then firing the obtained molded body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63202783A JPH0251466A (en) | 1988-08-16 | 1988-08-16 | Production of calcium phosphate molded body and calcium phosphate sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63202783A JPH0251466A (en) | 1988-08-16 | 1988-08-16 | Production of calcium phosphate molded body and calcium phosphate sintered body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0251466A true JPH0251466A (en) | 1990-02-21 |
Family
ID=16463118
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63202783A Pending JPH0251466A (en) | 1988-08-16 | 1988-08-16 | Production of calcium phosphate molded body and calcium phosphate sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0251466A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108025983A (en) * | 2015-09-16 | 2018-05-11 | 株式会社索夫塞拉 | New burns till calcium phosphate formed body and its manufacture method |
-
1988
- 1988-08-16 JP JP63202783A patent/JPH0251466A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108025983A (en) * | 2015-09-16 | 2018-05-11 | 株式会社索夫塞拉 | New burns till calcium phosphate formed body and its manufacture method |
| EP3351519A4 (en) * | 2015-09-16 | 2019-05-22 | SofSera Corporation | Novel sintered calcium phosphate body and method for producing same |
| US10981832B2 (en) | 2015-09-16 | 2021-04-20 | Sofsera Corporation | Sintered calcium phosphate molded body and process for manufacturing the same |
| CN108025983B (en) * | 2015-09-16 | 2021-06-04 | 株式会社索夫塞拉 | Novel calcined calcium phosphate molded body and method for producing same |
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