JPH0265865A - Medical or dental curable composition - Google Patents

Medical or dental curable composition

Info

Publication number
JPH0265865A
JPH0265865A JP63218066A JP21806688A JPH0265865A JP H0265865 A JPH0265865 A JP H0265865A JP 63218066 A JP63218066 A JP 63218066A JP 21806688 A JP21806688 A JP 21806688A JP H0265865 A JPH0265865 A JP H0265865A
Authority
JP
Japan
Prior art keywords
powder
aqueous solution
curable composition
curing liquid
weight
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
JP63218066A
Other languages
Japanese (ja)
Other versions
JP2609909B2 (en
Inventor
Yasuharu Imai
康晴 今井
Yasuto Tanaka
靖人 田中
Kazuo Koyama
和男 小山
Osamu Matsuda
治 松田
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.)
Dai Nippon Toryo KK
Original Assignee
Dai Nippon Toryo KK
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 Dai Nippon Toryo KK filed Critical Dai Nippon Toryo KK
Priority to JP63218066A priority Critical patent/JP2609909B2/en
Publication of JPH0265865A publication Critical patent/JPH0265865A/en
Application granted granted Critical
Publication of JP2609909B2 publication Critical patent/JP2609909B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Abstract

PURPOSE:To eliminate the irritability to a living body by obtaining biocompatibility and adjusting the pH of a kneaded mixture to the vicinity of neutrality by using an aqueous solution of at least one kind of a salt selected from a group consisting of diammonium phosphate, ammonium oxalate, ammonium acetate and sodium hydrogen tartarate as a curing liquid. CONSTITUTION:In a composition consisting of a powder, which consists of 100pts.wt. of an alpha-tricalcium phosphate powder and 5-30pts.wt. of a iodoform powder, and a curing liquid, an aqueous solution of a salt constituting said curable composition contains 10-40wt.% of diammonium phosphate, 3-5wt.% of ammonium oxalate, 20-60wt.% of ammonium acetate or 3-5wt.% of sodium hydrogen tartarate. When the concn. of the aqueous solution is lower than this range, the curability and workability of the curable composition become inferior and, when said concn. is higher than said range, the solubility of a kneaded cured substance becomes large. As the curing liquid, an aqueous solution of polyalkylene glycol (concentration, 5-15wt.%) can be together used in order to improve kneading properties.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は医科用または歯科用硬化性組成物、特に覆軍材
や根管充填材等の歯髄に直接的に接触させて使用する材
料として好適な硬化性組成物に関するものである。
[Detailed Description of the Invention] [Industrial Application Field] The present invention is applicable to medical or dental curable compositions, particularly as materials used in direct contact with dental pulp, such as covering materials and root canal filling materials. The present invention relates to suitable curable compositions.

〔従来の技術及びその解決すべき課題〕医科用または歯
科用硬化性組成物として生体適合性を有するα−リン酸
三カルシウムを粉剤として使用したものが注目されてき
ており、この種の硬化性組成物には、硬化液としてポリ
アクリル酸、クエン酸、酒石酸等の酸の水溶液が主とし
て使用されている。
[Prior art and problems to be solved] A curable composition for medical or dental use that uses biocompatible α-tricalcium phosphate as a powder has been attracting attention. In the composition, an aqueous solution of an acid such as polyacrylic acid, citric acid, or tartaric acid is mainly used as a curing liquid.

しかしながら、これら酸水溶液を硬化液に使用すると硬
化性組成物のpHが低くなるため生体に対する刺激性を
有しているという問題点があった。
However, when these acid aqueous solutions are used as a curing liquid, the pH of the curable composition becomes low, which poses a problem in that it is irritating to living organisms.

それ故、歯髄に直接的に接触して使用する覆軍材、根管
充填材等の材料として使用するには問題があった。
Therefore, there are problems in using it as a material for covering materials, root canal filling materials, etc. that are used in direct contact with the dental pulp.

また、硬化液のpHの問題を解決するために、前記ポリ
アクリル酸、クエン酸、酒石酸等の酸に中性となる塩な
どを添加したものも開発されてきているが、このような
硬化液を使用した硬化性組成物は、崩壊率が高いという
問題点があった。
In addition, in order to solve the problem of the pH of the curing liquid, products in which neutral salts are added to acids such as polyacrylic acid, citric acid, and tartaric acid have been developed. The curable composition using the above had a problem of high disintegration rate.

本発明者等はこのような現状に鑑み、前記問題点を解消
すべく、鋭意検討した結果、生体適合性を有し、かつ生
体に対し刺激性がなく、また崩壊率の低い医科用または
歯科用硬化性組成物を見出し本発明に到ったものである
In view of the current situation, the inventors of the present invention have made extensive studies to solve the above problems, and have found a medical or dental product that is biocompatible, non-irritating to living organisms, and has a low disintegration rate. The present invention was achieved by discovering a curable composition for use in the present invention.

〔課題を解決するための手段〕[Means to solve the problem]

すなわち、本発明は、 α−リン酸三カルシウム粉末からなる粉剤と硬化液とか
らなる組成物において、前記硬化液がリン酸三アンモニ
ウム、蓚酸アンモニウム、酢酸アンモニウム及び酒石酸
水素す) IJウムからなる群から選ばれた少なくとも
一種の塩の水溶液であることを特徴とする医科用または
歯科用硬化性組成物に関するものである。
That is, the present invention provides a composition comprising a powder made of α-tricalcium phosphate powder and a hardening liquid, wherein the hardening liquid comprises a group consisting of triammonium phosphate, ammonium oxalate, ammonium acetate, and hydrogen tartrate. The present invention relates to a medical or dental curable composition, which is an aqueous solution of at least one salt selected from the following.

また、本発明はX線造影性が必要な場合、α−リン酸三
カルシウム粉末100重量部及びヨードホルム粉末5〜
30重量部からなる粉剤を使用した前記医科用または歯
科用硬化性組成物に関するものである。
In addition, in the present invention, when X-ray contrast properties are required, 100 parts by weight of α-tricalcium phosphate powder and 5 to 5 parts of iodoform powder are used.
The present invention relates to the medical or dental curable composition using a powder containing 30 parts by weight.

以下、本発明の詳細な説明する。The present invention will be explained in detail below.

本発明の硬化性組成物を構成する粉剤〔P〕はα−リン
酸三カルンウム粉末単独もしくはX線造影性を必要とす
る場合それとヨードホルム粉末とからなっている。
The powder [P] constituting the curable composition of the present invention consists of α-tricarunium phosphate powder alone or, if X-ray contrastability is required, it and iodoform powder.

前記α−リン酸三カルシウムは公知の方法で製造するこ
とが出来、たとえば次の方法により製造することができ
る。
The α-tricalcium phosphate can be produced by a known method, for example, by the following method.

即ち、T−ピロリン酸カルシウムと炭酸力ルンウムとを
等モル量で均一に混合し、十分に乾燥させた後1000
〜1400℃、好ましくは1250℃前後で約1時間焼
成し、得られる生成物を微粉砕して粒径100μm以下
の微粉末とすることによって得ることができる。他の方
法としては、リン酸水Nカルシウムニ水和物と炭酸カル
シウムを2対1のモル比で均一に混合した後、前記方法
とほぼ同一条件で焼成、粉砕して得ることもできる。
That is, calcium T-pyrophosphate and carbonate are uniformly mixed in equimolar amounts, thoroughly dried, and then heated to 1000 ml.
It can be obtained by calcining at ~1400°C, preferably around 1250°C for about 1 hour, and pulverizing the resulting product into a fine powder with a particle size of 100 μm or less. Another method is to uniformly mix N-calcium phosphate dihydrate and calcium carbonate at a molar ratio of 2:1, and then sinter and crush the mixture under substantially the same conditions as the above method.

粉末の粒径は好ましくは20μm以下である。The particle size of the powder is preferably 20 μm or less.

また、前記ヨードホルム粉末は、従来から通常この種の
用途に使用されているものが使用出来、該粉末の粒径は
、好ましくは10μm以下である。
Further, the iodoform powder that has been conventionally used for this type of application can be used, and the particle size of the powder is preferably 10 μm or less.

なお、ヨードホルム粉末の配合量は、α−リン酸三カル
シウム100重量部に対し、5〜30重量部、特に好ま
しくは15〜25重量部である。
The amount of iodoform powder to be blended is 5 to 30 parts by weight, particularly preferably 15 to 25 parts by weight, per 100 parts by weight of α-tricalcium phosphate.

ヨードホルム粉末の配合量が前記範囲より少な過ぎると
硬化性組成物のX線造影性が不足してくるので好ましく
なく、一方過剰になると相対的にα−リン酸三カルシウ
ムが少なくなるため硬化性が悪くなるので好ましくない
If the amount of iodoform powder blended is too small than the above range, the X-ray contrast properties of the curable composition will be insufficient, which is undesirable.On the other hand, if it is too much, the curability will decrease because the amount of α-tricalcium phosphate will be relatively small. I don't like it because it makes it worse.

本発明に使用する粉剤CP)は以上説明した通り、α−
リン酸三カルシウム粉末もしくはそれとヨードホルム粉
末からなっているが、さらに必要に応じ硫酸バリウム粉
末、塩基性炭酸ビスマス粉末、シリカ粉末、アルミナ粉
末、アパタイト粉末等を配合してもよい。
As explained above, the powder CP used in the present invention is α-
It consists of tricalcium phosphate powder or tricalcium phosphate powder and iodoform powder, but barium sulfate powder, basic bismuth carbonate powder, silica powder, alumina powder, apatite powder, etc. may be further blended as necessary.

本発明の硬化性組成物を構成する硬化液〔L〕はリン酸
三アンモニウム、蓚酸アンモニウム、酢酸アンモニウム
及び酒石酸水素すl−IJウムからなる群から選ばれた
少なくとも一種の塩の水溶液である。
The curing liquid [L] constituting the curable composition of the present invention is an aqueous solution of at least one salt selected from the group consisting of triammonium phosphate, ammonium oxalate, ammonium acetate, and sulfur hydrogen tartrate.

これらの塩の水溶液濃度は、リン酸三アンモニウムが1
0〜40重量%、好ましくは10〜20重量%;蓚酸ア
ンモニウムが3〜5重量%、好ましくは4〜5重量%;
酢酸アンモニウムが20〜60重量%、好ましくは30
〜50重量%;酒石酸水素す) IJウムが3〜5重量
%、好ましくは4〜5重量%が適当である。水溶液濃度
が前記範囲より小さいと硬化性組成物の硬化性、作業性
が悪くなる傾向にある。一方、前記範囲より大きいと練
和硬化物の溶解性が大きくなる傾向にある。
The concentration of these salts in aqueous solution is 1
0-40% by weight, preferably 10-20% by weight; 3-5% by weight of ammonium oxalate, preferably 4-5% by weight;
Ammonium acetate is 20-60% by weight, preferably 30%
~50% by weight; hydrogen tartrate) 3 to 5% by weight, preferably 4 to 5% by weight of IJum is suitable. If the concentration of the aqueous solution is lower than the above range, the curability and workability of the curable composition tend to deteriorate. On the other hand, if it is larger than the above range, the solubility of the kneaded and cured product tends to increase.

本発明にふいては、硬化液としてポリエチレングリコー
ノペポリプロピレングリコール等のポリアルキレングリ
コールの水溶液(水溶液濃度5〜15重量%)を練和性
等をよくするために併用することも可能である。さらに
必要に応じ増粘剤、界面活性剤等の各種添加剤を少量添
加することも可能である。
In the present invention, an aqueous solution (aqueous solution concentration of 5 to 15% by weight) of polyalkylene glycol such as polyethylene glycone polypropylene glycol can be used in combination as a curing liquid in order to improve kneading properties and the like. Furthermore, it is also possible to add small amounts of various additives such as thickeners and surfactants, if necessary.

本発明の硬化性組成物は以上説明した粉剤CP)と硬化
液CLIとからなり、それらを好ましくは〔P〕とCL
)の重量比CP〕/ CL、]が1.0〜2.0となる
割合で、使用直前に練和し使用に供される。
The curable composition of the present invention consists of the powder agent CP) and the curing liquid CLI as described above, preferably [P] and CL
) is kneaded and used immediately before use at a ratio such that the weight ratio CP]/CL,] is 1.0 to 2.0.

〔発明の効果〕〔Effect of the invention〕

本発明の硬化性組成物は、化学的に歯の成分に近い、α
−リン酸三カルシウムを使用しているため生体適合性が
あり、また練和物のpHも中性付近にあり、生体に対す
る刺激性もなく、さらに崩壊率も小さい。それ故覆軍材
や根管充填材として好適であり、また覆軍材や根管充填
材として要求される練和物の適度な動粘性、操作性、硬
化性、封鎖性等の性状を満足しており、画期的な硬化性
組成物といえる。
The curable composition of the present invention has α
- Since it uses tricalcium phosphate, it is biocompatible, and the pH of the kneaded product is near neutral, so it is not irritating to living organisms and has a low disintegration rate. Therefore, it is suitable as a covering material and root canal filling material, and also satisfies the properties such as appropriate kinematic viscosity, operability, hardening properties, and sealing properties of the kneaded material required for covering material and root canal filling material. It can be said to be a revolutionary curable composition.

〔実施例〕〔Example〕

以下、本発明を実施例により更に詳細に説明する。 Hereinafter, the present invention will be explained in more detail with reference to Examples.

実施例1〜6及び比較例1〜3 公知の方法によりγ−ピロリン酸カルシウムと炭酸カル
シウムを等モル混合し、焼成してα−リン酸三カルシウ
ムを合成し、粉砕して300メツシユの篩を通過させて
、所定の粒度のα−リン酸三カルシウム粉末を得た。
Examples 1 to 6 and Comparative Examples 1 to 3 γ-Calcium pyrophosphate and calcium carbonate were mixed in equimolar amounts by a known method, baked to synthesize α-tricalcium phosphate, and pulverized to pass through a 300-mesh sieve. In this way, α-tricalcium phosphate powder with a predetermined particle size was obtained.

このようにして得られたα−リン酸三カルシウム粉末(
α−TCPという)を使用して第1表に示す他の粉末成
分CP〕と混合し、JIS−T6602の方法に準拠し
て第1表に示す硬化液〔L〕と練和した。(表中の数値
は重量部を示す。)かくして調製した練和物の崩壊率、
表面pH及びX線造影性を調べ、その結果を第1表下段
に示した。
The α-tricalcium phosphate powder thus obtained (
α-TCP) was mixed with other powder components CP shown in Table 1 and kneaded with the hardening liquid [L] shown in Table 1 according to the method of JIS-T6602. (The numbers in the table indicate parts by weight.) The disintegration rate of the kneaded product thus prepared,
The surface pH and X-ray contrast property were investigated, and the results are shown in the lower part of Table 1.

第1表の試験結果より明らかの通り、本発明の硬化性組
成物は、硬化物の表面pHが中性付近にあり、それ放生
体に対する刺激性がきわめて小さく、また崩壊率も小さ
く良好であった。
As is clear from the test results in Table 1, the curable composition of the present invention has a surface pH of the cured product near neutrality, has very little irritation to the release body, and has a low disintegration rate. Ta.

一方、硬化液にリン酸三アンモニウム水溶液を使用した
比較例1およびポリアクリル酸ナトリウム水溶液を使用
した比較例2は崩壊率が高く、またポリアクリル酸水溶
液を使用した比較例3は硬化物の表面pHが低く生体に
対する刺激性があり不適であった。
On the other hand, Comparative Example 1, which used triammonium phosphate aqueous solution as the curing liquid, and Comparative Example 2, which used sodium polyacrylate aqueous solution, had a high disintegration rate, and Comparative Example 3, which used polyacrylic acid aqueous solution, had a high disintegration rate. The pH was low and irritating to living organisms, making it unsuitable.

注6) 分子旧約3000の非イオン性ポリエチレングリコール
アクリル酸−イタコン酸共重合体(イタコン酸含有量3
5重量%)重合度2700〜7500 JIS  T−6602に準する。
Note 6) Nonionic polyethylene glycol acrylic acid-itaconic acid copolymer with a molecular age of approx. 3000 (itaconic acid content 3
5% by weight) Degree of polymerization 2700-7500 According to JIS T-6602.

粉剤[P]と硬化液CL]とを1分間均一に練和し、該
練和物を容器に入れ、その表面を平らにして濾紙をのせ
、練和開始150秒後に水を滴下し、濾紙を湿らせ、密
封24時間放置後、フラット型pH電極(ベックマン 
フラット型複合電極#39523S−502A)を濾紙
に接触させ練和物の表面pHを測定した。
Powder [P] and hardening liquid CL] were uniformly kneaded for 1 minute, the kneaded product was put into a container, the surface was flattened and a filter paper was placed on it, and 150 seconds after the start of kneading, water was added dropwise and the filter paper After moistening and sealing for 24 hours, use a flat pH electrode (Beckman
A flat type composite electrode #39523S-502A) was brought into contact with the filter paper to measure the surface pH of the kneaded product.

2mm厚の硬化物に80KV、200mへのX線を0.
02秒間照射し、X線フィルムを感光させ調べた。
A 2 mm thick cured product was exposed to X-rays at 80 KV and 200 m at 0.
The sample was irradiated for 02 seconds, and the X-ray film was exposed and examined.

Claims (2)

【特許請求の範囲】[Claims] (1)α−リン酸三カルシウム粉末からなる粉剤と硬化
液とからなる組成物において、前記硬化液がリン酸二ア
ンモニウム、蓚酸アンモニウム、酢酸アンモニウム及び
酒石酸水素ナトリウムからなる群から選ばれた少なくと
も一種の塩の水溶液であることを特徴とする医科用また
は歯科用硬化性組成物。
(1) A composition comprising a powder made of α-tricalcium phosphate powder and a hardening liquid, wherein the hardening liquid is at least one selected from the group consisting of diammonium phosphate, ammonium oxalate, ammonium acetate, and sodium hydrogen tartrate. A curable composition for medical or dental use, characterized in that it is an aqueous solution of a salt of.
(2)α−リン酸三カルシウム粉末100重量部及びヨ
ードホルム粉末5〜30重量部からなる粉剤と硬化液と
からなる組成物において、前記硬化液がリン酸二アンモ
ニウム、蓚酸アンモニウム、酢酸アンモニウム及び酒石
酸水素ナトリウムからなる群から選ばれた少なくとも一
種の塩の水溶液であることを特徴とする医科用または歯
科用硬化性組成物。
(2) A composition comprising a powder consisting of 100 parts by weight of α-tricalcium phosphate powder and 5 to 30 parts by weight of iodoform powder, and a curing liquid, wherein the curing liquid includes diammonium phosphate, ammonium oxalate, ammonium acetate, and tartaric acid. A curable composition for medical or dental use, which is an aqueous solution of at least one salt selected from the group consisting of sodium hydrogen.
JP63218066A 1988-08-31 1988-08-31 Medical or dental curable composition Expired - Lifetime JP2609909B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP63218066A JP2609909B2 (en) 1988-08-31 1988-08-31 Medical or dental curable composition

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP63218066A JP2609909B2 (en) 1988-08-31 1988-08-31 Medical or dental curable composition

Publications (2)

Publication Number Publication Date
JPH0265865A true JPH0265865A (en) 1990-03-06
JP2609909B2 JP2609909B2 (en) 1997-05-14

Family

ID=16714116

Family Applications (1)

Application Number Title Priority Date Filing Date
JP63218066A Expired - Lifetime JP2609909B2 (en) 1988-08-31 1988-08-31 Medical or dental curable composition

Country Status (1)

Country Link
JP (1) JP2609909B2 (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007197329A (en) * 2006-01-23 2007-08-09 Kuraray Medical Inc Calcium phosphate composition and method for producing the same
JP2012236854A (en) * 2012-08-10 2012-12-06 Kuraray Noritake Dental Inc Method for producing calcium phosphate composition
JP2017145195A (en) * 2016-02-15 2017-08-24 株式会社松風 Two-paste type root canal-filling sealer composition
JP2017145196A (en) * 2016-02-15 2017-08-24 株式会社松風 Root canal-filling sealer composition

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5988351A (en) * 1982-11-10 1984-05-22 科学技術庁無機材質研究所長 Production of apatite cement hardened body
JPS62153204A (en) * 1985-12-27 1987-07-08 Advance Res & Dev Co Ltd Root canal filling material for dental use
JPS62182146A (en) * 1985-10-11 1987-08-10 三井東圧化学株式会社 Hardenable material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5988351A (en) * 1982-11-10 1984-05-22 科学技術庁無機材質研究所長 Production of apatite cement hardened body
JPS62182146A (en) * 1985-10-11 1987-08-10 三井東圧化学株式会社 Hardenable material
JPS62153204A (en) * 1985-12-27 1987-07-08 Advance Res & Dev Co Ltd Root canal filling material for dental use

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007197329A (en) * 2006-01-23 2007-08-09 Kuraray Medical Inc Calcium phosphate composition and method for producing the same
JP2012236854A (en) * 2012-08-10 2012-12-06 Kuraray Noritake Dental Inc Method for producing calcium phosphate composition
JP2017145195A (en) * 2016-02-15 2017-08-24 株式会社松風 Two-paste type root canal-filling sealer composition
JP2017145196A (en) * 2016-02-15 2017-08-24 株式会社松風 Root canal-filling sealer composition

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JP2609909B2 (en) 1997-05-14

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