JPH09141387A - Phosphate-based investment compound composition for dental purpose - Google Patents

Phosphate-based investment compound composition for dental purpose

Info

Publication number
JPH09141387A
JPH09141387A JP7322429A JP32242995A JPH09141387A JP H09141387 A JPH09141387 A JP H09141387A JP 7322429 A JP7322429 A JP 7322429A JP 32242995 A JP32242995 A JP 32242995A JP H09141387 A JPH09141387 A JP H09141387A
Authority
JP
Japan
Prior art keywords
investment material
phosphate
dental
weight
tetrafluoroethylene resin
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
JP7322429A
Other languages
Japanese (ja)
Other versions
JP3529523B2 (en
Inventor
Kenichi Iiyama
賢一 飯山
Koichi Mamada
浩一 侭田
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.)
G C KK
GC Corp
Original Assignee
G C KK
GC Corp
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 G C KK, GC Corp filed Critical G C KK
Priority to JP32242995A priority Critical patent/JP3529523B2/en
Publication of JPH09141387A publication Critical patent/JPH09141387A/en
Application granted granted Critical
Publication of JP3529523B2 publication Critical patent/JP3529523B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Abstract

PROBLEM TO BE SOLVED: To obtain a phosphate-based investment compd. compsn. for dental purpose with which the holding of stable performance is possible without the removal of fine particles out of the investment compd. by pneumatic transportation at the time of production of a phosphate-based investment compd. compsn. for dental purpose. SOLUTION: This phosphate-based investment compd. compsn. is prepd. by mixing 0.01 to 0.5 pts.wt. tetrafluoroetylene resin with 100 pts.wt. mixture composed of magnesium oxide and ammonium dihydrogenphosphate as binders and quartz and cristobalite as refractory materials and further, mixing 0.001 to 0.05 pts.wt. one or >=2 kinds anion based surfactants selected form the group consisting of alkyl benzene sulfonate and alkyl sulfonate therewith.

Description

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

【0001】[0001]

【発明の属する技術分野】本発明は、歯科精密鋳造に使
用される歯科用リン酸塩系埋没材組成物に関するもの
で、より詳細には四フッ化エチレン樹脂の微細粒子捕捉
効果により、埋没材の製造時に空気輸送される埋没材中
の微細粒子がサイクロン分離器で分離されて包装工程ま
で輸送されるので、安定した性能を保持し得る歯科用リ
ン酸塩系埋没材組成物を提供するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a dental phosphate-based investment material composition used in dental precision casting, and more specifically, to an investment material due to the effect of capturing fine particles of tetrafluoroethylene resin. The present invention provides a dental phosphate-based investment material composition capable of maintaining stable performance, since fine particles in the investment material that are pneumatically transported during the production of are separated by a cyclone separator and transported to the packaging process. Is.

【0002】[0002]

【従来の技術】歯科金属修復物は、ロストワックス法に
よる精密鋳造技術により修復物の形態をワックス材料で
形成し、それにスプルー線(溶融金属注入口)を付し、
これを歯科用埋没材で埋没し、この歯科用埋没材が硬化
した後にスプルー線を抜き取り、ワックスを焼却除去す
ることによって出来た空洞に溶融金属を注入する手順に
よって作製されている。特に歯科金属修復物は、欠損し
た歯牙の修復を目的として口腔内に装着して使用される
ため高い寸法精度が要求されており、高い寸法精度を有
する歯科金属修復物を得るためには歯科用埋没材の硬化
時及び加熱時の膨張を利用して金属の鋳造収縮を補償す
る必要がある。
2. Description of the Related Art Dental metal restorations are made of a wax material in the form of restorations by a precision casting technique using the lost wax method, and sprue wires (molten metal injection ports) are attached to the restorations.
It is produced by a procedure of burying this in a dental investment material, extracting the sprue wire after the dental investment material is hardened, and injecting molten metal into the cavity formed by burning and removing the wax. In particular, a dental metal restoration is required to have high dimensional accuracy because it is used by mounting it in the oral cavity for the purpose of repairing a missing tooth. It is necessary to compensate for casting shrinkage of the metal by utilizing the expansion of the investment material during hardening and heating.

【0003】そのためには、歯科用埋没材においては、
凝結時の膨張(凝結膨張値)及び加熱時の膨張(熱膨張
値)を厳密にコントロールし、常に安定した鋳造収縮の
補償が可能となるように調整されている必要がある。凝
結膨張値及び熱膨張値に影響を与える因子としては埋没
材粒子の粒度分布が重要なファクターとなっている。粒
度分布が異なると凝結膨張値,熱膨張値が変動し、それ
に伴い鋳造収縮を補償する能力が変化し、最終的には金
属修復物の寸法精度に影響が現れる。そのため歯科用埋
没材の粒度分布のコントロールは、歯科用埋没材の生産
において重要な管理項目となっている。
For that purpose, in the dental investment material,
It is necessary to strictly control expansion during condensation (condensation expansion value) and expansion during heating (thermal expansion value) so that stable casting shrinkage compensation is always possible. The particle size distribution of investment material particles is an important factor that affects the setting expansion value and the thermal expansion value. If the particle size distribution is different, the setting expansion value and the thermal expansion value will fluctuate, and the ability to compensate for casting shrinkage will change accordingly, and finally the dimensional accuracy of the metal restoration will be affected. Therefore, controlling the particle size distribution of dental investment materials is an important control item in the production of dental investment materials.

【0004】歯科用埋没材としては、石英及び/又はク
リストバライトなどの耐火材に結合材としてα−半水石
こうを混合した石こう系埋没材と、石英及び/又はクリ
ストバライトなどの耐火材に結合材として酸化マグネシ
ウムとリン酸二水素アンモニウムとを混合した耐熱性の
高いリン酸塩系埋没材との二種類が一般に使用されてい
る。溶融温度が1100℃を超える陶材焼付用合金や金属製
の義歯床などに用いるコバルトクロム合金などの鋳造に
は、歯科用石こう系埋没材では耐熱性が不足するため歯
科用リン酸塩系埋没材が主に使用されている。
As the dental investment material, a gypsum-based investment material in which a refractory material such as quartz and / or cristobalite is mixed with α-hemihydrate gypsum as a binding material, and a refractory material such as quartz and / or cristobalite as a binding material Two types are generally used: a phosphate-based investment material having high heat resistance, which is a mixture of magnesium oxide and ammonium dihydrogen phosphate. Dental gypsum-based investment materials lack sufficient heat resistance when casting porcelain baking alloys with a melting temperature of over 1100 ° C or cobalt-chromium alloys used for metal denture bases, etc. Wood is mainly used.

【0005】以下に、歯科用リン酸塩系埋没材の製造工
程の概略を示す。 耐火材(石英やクリストバライトなど)の粉砕工程。 粉砕された耐火材に、結合材としての酸化マグネシウ
ムとリン酸二水素アンモニウムとを加え、更に粉砕・混
合する工程。 粉砕・混合後に行う硬化時間や流動性、粒度などの調
整工程。 包装工程。 通常及びの工程はボールミルなどのバッチ処理装置
で実施される。の調整工程はミルからの排出前に実施
される。調整後ミルから排出された粉体はの包装工程
に移行される。包装工程に歯科用リン酸塩系埋没材を輸
送するには、一般には空気を利用した空気輸送装置が利
用される。
The outline of the manufacturing process of the dental phosphate-based investment material is shown below. Grinding process of refractory materials (quartz, cristobalite, etc.). A process of adding magnesium oxide and ammonium dihydrogen phosphate as a binder to the crushed refractory material, and further crushing and mixing. Adjustment process such as curing time, fluidity and particle size after crushing and mixing. Packaging process. Usually and the steps are carried out in a batch processing apparatus such as a ball mill. The adjustment process of (1) is performed before discharge from the mill. The powder discharged from the mill after adjustment is transferred to the packaging process. In order to transport the dental phosphate-based investment material in the packaging process, an air transportation device using air is generally used.

【0006】空気輸送装置とは空気の流れに粉体を混合
して輸送する装置であり、その方式としては圧送式と吸
引式とがある。どちらの方式でも最終的には粉体と空気
流とを分離する必要があり、この分離にはサイクロン分
離器が一般に使用されているが、このサイクロン分離器
において微細な粉末粒子が空気流と分離されずに空気流
に乗ってサイクロン分離器の空気排出口に設置されてい
るエアーバグフィルターに捕捉されて廃棄されたり、よ
り微細な粒子はエアーバグフィルターを通り抜けて大気
中に放出されてしまう現象が発生する。それによってミ
ル排出時の歯科用リン酸塩系埋没材の粒度分布と空気輸
送後の粒度分布が異なるという現象が起きている。その
結果、空気輸送後は、歯科用リン酸塩系埋没材中の微細
な粒子が輸送前と比較して減少しており、それによって
凝結膨張値,熱膨張値などの諸性質が変化してしまい、
歯科用リン酸塩系埋没材として期待された性能が発揮で
きないような不都合な現象が生じている。
The air transport device is a device for transporting a powder mixed with an air flow, and its system includes a pressure-feed type and a suction type. In either method, it is necessary to finally separate the powder and the air stream, and a cyclone separator is generally used for this separation.In this cyclone separator, fine powder particles are separated from the air stream. Instead of riding on the air flow, it is trapped by the air bag filter installed at the air outlet of the cyclone separator and discarded, or finer particles pass through the air bag filter and are released into the atmosphere. Occurs. This causes a phenomenon that the particle size distribution of the dental phosphate-based investment material when discharged from the mill is different from the particle size distribution after pneumatic transportation. As a result, after air transportation, the fine particles in the dental phosphate-based investment material decreased compared to before transportation, which caused changes in various properties such as condensation expansion value and thermal expansion value. Sisters,
An inconvenient phenomenon has occurred in which the performance expected as a dental phosphate-based investment material cannot be exhibited.

【0007】具体的には、歯科用リン酸塩系埋没材から
微細な粒子が除去されると凝結膨張値,熱膨張値共に低
下し、金属修復物の鋳造収縮を補償する能力が低下し、
結果として金属修復物は期待した寸法より小さくなり、
口腔内に装着した場合の適合性が悪化し、咀嚼機能の回
復が不十分となるばかりではなく二次う蝕などの重大な
臨床上の問題点の原因にもなる。また、微細な粒子が除
去されると歯科用リン酸塩系埋没材の硬化後の圧縮強さ
が低下し、埋没材が加熱中の熱応力を受けて鋳型割れが
起こり易くなり、その結果として鋳バリなどの鋳造欠陥
が発生し、臨床上での使用が不可能となる。
Specifically, when fine particles are removed from the dental phosphate-based investment material, both the setting expansion value and the thermal expansion value decrease, and the ability of compensating the casting shrinkage of the metal restoration decreases.
As a result, the metal restoration is smaller than expected,
The suitability when worn in the oral cavity is deteriorated, and not only is the recovery of the masticatory function insufficient, but it also causes serious clinical problems such as secondary caries. Further, when the fine particles are removed, the compressive strength of the dental phosphate-based investment material after curing is reduced, and the investment material is susceptible to thermal stress during heating to easily cause mold cracking. Casting defects such as casting burrs occur, making it impossible to use clinically.

【0008】空気輸送後に期待された性能が発揮される
ようにミルの混合・粉砕の条件を見い出せれば前記欠陥
の発生防止対策とはなり得るが、実際には空気輸送によ
って起きる粒度分布の変化(微細粒子がどの程度除去さ
れてしまうか)は常に一定ではないために、粒度分布の
変化を前以って見込んだミルの粉砕・混合の条件を見い
出すことは事実上は不可能である。また空気輸送後に歯
科用リン酸塩系埋没材の各種の特性の調整を実施するこ
とは困難であり、空気輸送中の粒度分布の変化は製品の
安定性、最終的には金属修復物の寸法精度の安定性とい
う面においては大きな問題となっている。
[0008] If the conditions of mixing and crushing of the mill can be found so that the expected performance can be exhibited after pneumatic transportation, it can be a measure for preventing the occurrence of the above defects, but in reality, the change in particle size distribution caused by pneumatic transportation. Since (how much fine particles are removed) is not always constant, it is practically impossible to find out the milling / mixing conditions of the mill that anticipate changes in the particle size distribution. In addition, it is difficult to adjust various properties of dental phosphate-based investment materials after pneumatic transportation, and the change in particle size distribution during pneumatic transportation is product stability, and ultimately the size of metal restorations. This is a big problem in terms of accuracy stability.

【0009】[0009]

【発明が解決しようとする課題】本発明は前記従来技術
の問題点を解決し、歯科用リン酸塩系埋没材のミル排出
から包装工程に粉体を空気輸送して取り出す場合に、微
細な粉末がサイクロン分離器で分離されずにサイクロン
分離器の空気排出口に設置されているエアーバグフィル
ターに捕捉されたり、このエアーバグフィルターを通り
抜けて大気中に放出されたりすることなく、最終的な埋
没材製品中に微細な粉末が残留して期待される性能が安
定して得られ、常に寸法精度の高い金属修復物を得るこ
とができる歯科用リン酸塩系埋没材組成物を開発するこ
とを課題とする。
SUMMARY OF THE INVENTION The present invention solves the problems of the prior art described above, and when powder is pneumatically taken out from a mill discharge of a dental phosphate-based investment material to a packaging step, a fine powder is taken out. The powder is not separated by the cyclone separator and is not trapped by the air bag filter installed at the air outlet of the cyclone separator, or passes through this air bag filter and is not released into the atmosphere. To develop a dental phosphate-based investment material composition capable of stably obtaining the expected performance with fine powder remaining in the investment material product and always obtaining a metal restoration with high dimensional accuracy. Is an issue.

【0010】[0010]

【課題を解決するための手段】本発明者らは上記課題を
解決すべく鋭意研究の結果、結合材としての酸化マグネ
シウムとリン酸二水素アンモニウム、耐火材としての石
英とクリストバライトとから構成される粉末状歯科用リ
ン酸塩系埋没材組成物に、微細粉末捕捉材としての四フ
ッ化エチレン樹脂を所定量混合すれば、それが有する微
粒子捕捉作用により埋没材の微細粒子が空気輸送の最終
段階に設置されているサイクロン分離器で確実に空気と
分離されるので、常に安定した性能を保持した歯科用リ
ン酸塩系埋没材組成物を得ることができ、更にこの歯科
用リン酸塩系埋没材組成物にアルキルベンゼンスルフォ
ン酸塩,アルキル硫酸塩から成る群より選出される1種
又は2種以上の陰イオン系界面活性剤を混合すれば練和
操作性が改善されることを究明したのでる。
Means for Solving the Problems As a result of intensive studies to solve the above-mentioned problems, the present inventors composed of magnesium oxide and ammonium dihydrogen phosphate as binders, and quartz and cristobalite as refractory materials. If a powdered dental phosphate-based investment material composition is mixed with a predetermined amount of tetrafluoroethylene resin as a fine powder capturing material, the fine particles of the investment material have the fine particles of the investment material in the final stage of pneumatic transportation. Since it is reliably separated from air by the cyclone separator installed in the plant, it is possible to obtain a dental phosphate-based investment material composition that always maintains stable performance. If one or more anionic surfactants selected from the group consisting of alkylbenzene sulfonates and alkyl sulfates are mixed with the material composition, the kneading operability is improved. Out was to investigate that.

【0011】[0011]

【発明の実施の形態】即ち、本発明に係る歯科用リン酸
塩系埋没材組成物は、 a)結合材としての酸化マグネシウムとリン酸二水素ア
ンモニウム、 b)耐火材としての石英とクリストバライト、から構成
される混合物100重量部に対し、四フッ化エチレン樹脂
0.01〜0.5重量部が混合された第1の発明と、 a)結合材としての酸化マグネシウムとリン酸二水素ア
ンモニウム、 b)耐火材としての石英とクリストバライト、から構成
される混合物100重量部に対し、四フッ化エチレン樹脂
0.01〜0.5重量部と、アルキルベンゼンスルフォン酸
塩,アルキル硫酸塩から成る群より選ばれた1種又は2
種以上の陰イオン系界面活性剤0.001〜0.05重量部とが
混合された第2の発明とから成るものである。
BEST MODE FOR CARRYING OUT THE INVENTION That is, a dental phosphate-based investment material composition according to the present invention comprises a) magnesium oxide and ammonium dihydrogen phosphate as binders, b) quartz and cristobalite as refractory materials, 100 parts by weight of a mixture composed of tetrafluoroethylene resin
1st invention in which 0.01 to 0.5 parts by weight are mixed, and a) 100 parts by weight of a mixture composed of magnesium oxide and ammonium dihydrogen phosphate as a binder, b) quartz and cristobalite as a refractory material , Tetrafluoroethylene resin
0.01 to 0.5 parts by weight and one or two selected from the group consisting of alkylbenzene sulfonate and alkyl sulfate.
The second invention in which 0.001 to 0.05 parts by weight of one or more anionic surfactants are mixed.

【0012】水溶液中で四フッ化エチレンを重合する
と、微細な粒子状の四フッ化エチレンの樹脂が得られ
る。この微細な樹脂の分子鎖は、分子間凝集力が低く、
僅かな圧縮・剪断応力を受けることにより微細な蜘蛛の
巣状の繊維になる。この蜘蛛の巣状の繊維となった四フ
ッ化エチレン樹脂が埋没材中の微細な粒子を捕捉するの
で、埋没材粒子を空気輸送した場合にサイクロン分離器
で微細な粒子だけが空気と分離されずに選択的にサイク
ロン分離器の空気排出口に設置されているエアーバグフ
ィルターに捕捉されたり、このエアーバグフィルターを
通り抜けて大気中に放出されたりすることが防止される
のである。
By polymerizing ethylene tetrafluoride in an aqueous solution, a fine particulate resin of tetrafluoroethylene is obtained. The molecular chains of this fine resin have low intermolecular cohesive force,
It becomes fine cobweb-shaped fibers by receiving a slight compressive and shearing stress. Since the tetrafluoroethylene resin, which has become a cobweb-like fiber, captures the fine particles in the investment material, when the investment material particles are transported by air, only the fine particles are separated from the air by the cyclone separator. Instead, it is selectively prevented from being trapped by the air bag filter installed at the air outlet of the cyclone separator or being released through the air bag filter into the atmosphere.

【0013】具体的には、歯科用リン酸塩系埋没材の製
造中に耐火材及び結合材の粉砕の過程でミルの中に微細
な四フッ化エチレン樹脂を添加し、ミルによる剪断・圧
縮応力を四フッ化エチレン樹脂にも負荷するのである。
四フッ化エチレン樹脂は、分子鎖の主鎖のC−C結合は
強固であるがそれに対して他の分子鎖に対する分子間引
力は極端に小さいため、剪断・圧縮応力を負荷された四
フッ化エチレン分子は微細に繊維化する。この繊維が埋
没材中の微細な耐火材,結合材の粒子を絡み付くような
状態で捕捉する。この現象は走査型電子顕微鏡の観察結
果でも確認され、このことにより外観上では埋没材粒子
が凝集しているような効果を示すが、これは通常の粒子
を造粒する操作により起こる微粒子の緻密な凝集とは異
なり、微細な繊維の網目に微細粒子が捕捉された状態で
の軽度の粉体の凝集であるため歯科用リン酸塩系埋没材
としての特性に影響を与えることは生じない。
Specifically, during the production of a dental phosphate-based investment material, a fine tetrafluoroethylene resin is added to the mill during the process of crushing the refractory material and the binder, and shearing / compression is performed by the mill. The stress is also applied to the tetrafluoroethylene resin.
In the tetrafluoroethylene resin, the C—C bond of the main chain of the molecular chain is strong, but on the other hand, the intermolecular attractive force to other molecular chains is extremely small. Ethylene molecules are finely fibrillated. This fiber traps the particles of the fine refractory material and the binder in the investment material in a entangled state. This phenomenon was also confirmed by the results of observation with a scanning electron microscope, and this shows the effect that the investment material particles are agglomerated in appearance, but this is due to the fineness of fine particles caused by the operation of granulating ordinary particles. Unlike such agglomeration, it does not affect the characteristics of the dental phosphate-based investment material because it is a light powder agglomeration in the state where fine particles are captured in the fine fiber mesh.

【0014】四フッ化エチレン樹脂の微細な繊維に捕捉
された埋没材中の微細粒子は、空気輸送中においても四
フッ化エチレン樹脂と凝集している状態を維持し続ける
ので、空気輸送の最終段階に設置されているサイクロン
分離器で空気と分離されるため、微細な粒子だけが選択
的にサイクロン分離器の空気排出口に設置されているエ
アーバグフィルターに捕捉されたり、このエアーバグフ
ィルターを通り抜けて大気中に放出されたりすることが
防止される。これにより埋没材中の微細な粒子が除去さ
れることなく埋没材中に含有されるため、四フッ化エチ
レン樹脂を添加していない埋没材のように空気輸送後の
埋没材の特性値、特に凝結膨張値,熱膨張値が低下した
り、硬化後の圧縮強さが低下するような現象が防止でき
るのである。
Since the fine particles in the investment material trapped in the fine fibers of the tetrafluoroethylene resin continue to be in the state of aggregating with the tetrafluoroethylene resin even during the pneumatic transportation, the final state of the pneumatic transportation. Since it is separated from the air by the cyclone separator installed at the stage, only fine particles are selectively captured by the air bag filter installed at the air outlet of the cyclone separator, or this air bag filter is used. It is prevented from passing through and being released into the atmosphere. As a result, since the fine particles in the investment material are contained in the investment material without being removed, the characteristic values of the investment material after pneumatic transportation, such as the investment material without addition of tetrafluoroethylene resin, especially It is possible to prevent such phenomena that the setting expansion value and the thermal expansion value decrease and the compression strength after curing decreases.

【0015】この混合される四フッ化エチレン樹脂の添
加量が0.01重量部未満では、歯科用リン酸塩系埋没材の
微細粒子の捕捉作用が不十分で空気輸送による微細粒子
の喪失を防止する効果が十分に発揮されず、その結果と
して埋没材の重要な性質である凝結膨張値及び熱膨張値
が不安定になる。この理由から四フッ化エチレン樹脂の
添加量の下限を0.01重量部と規定した。
If the amount of the mixed tetrafluoroethylene resin is less than 0.01 parts by weight, the action of capturing the fine particles of the dental phosphate-based investment material is insufficient and the loss of the fine particles due to air transportation is prevented. The effect is not sufficiently exerted, and as a result, the settling expansion value and the thermal expansion value, which are important properties of the investment material, become unstable. For this reason, the lower limit of the amount of tetrafluoroethylene resin added is defined as 0.01 parts by weight.

【0016】また、四フッ化エチレン樹脂の添加量の上
限を0.5重量部とした理由は、以下の通りである。四フ
ッ化エチレン樹脂は前述した通り剪断・圧縮応力を負荷
されると微細に繊維化するが、添加量が埋没材に対して
過剰になると微細な粒子の捕捉作用だけでなくより大き
な粒子に対しても作用し、粉末が顆粒状に凝集する現象
が生じる。ミルから埋没材粉末を排出する工程は、ミル
の蓋を開けてミルを回転させながら排出口から落下する
粉末をホッパーで受けることにより行われるが、埋没材
粒子が過剰な四フッ化エチレン樹脂により顆粒状に凝集
しているとミルの排出口から排出される粉末量が減少
し、その結果として排出時間が可及的に増大する。また
ミルからの排出時の回転によっても、ミル内に残留した
埋没材は粉砕を受け続けるが、ミル粉砕の効率は粉末の
量とミル玉の相対的な割合で決定され、ミル玉の割合が
大きくなるほど粉砕効率は指数級数的に増大するためミ
ルからの排出時間が長くなることにより、ミルから最終
的に排出される粉末は最初に排出された粉末と比較して
粉砕が非常に過剰となって性質も全く異なってしまい、
粉砕後の調整が無意味となってしまう。このような理由
からミルからの排出時間の限度を鑑みて四フッ化エチレ
ン樹脂の添加量の上限を0.5重量部と規定した。
The reason why the upper limit of the amount of the tetrafluoroethylene resin added is set to 0.5 part by weight is as follows. As mentioned above, tetrafluoroethylene resin finely fibrillates when subjected to shearing / compressive stress, but if the amount of addition is excessive with respect to the investment material, it not only captures fine particles but also larger particles. Even if it works, a phenomenon occurs in which the powder aggregates into a granular shape. The step of discharging the investment material powder from the mill is performed by opening the lid of the mill and receiving the powder falling from the discharge port while rotating the mill with the hopper. Agglomeration in the form of granules reduces the amount of powder discharged from the outlet of the mill, and as a result, discharge time is increased as much as possible. Also, the investment material remaining in the mill continues to be pulverized by the rotation at the time of discharge from the mill, but the efficiency of mill pulverization is determined by the amount of powder and the relative proportion of mill balls, and the proportion of mill balls is As the grinding efficiency increases exponentially as the size increases, the discharge time from the mill becomes longer, and the powder finally discharged from the mill is extremely excessively ground compared with the powder discharged first. The nature is completely different,
Adjustment after crushing becomes meaningless. For this reason, the upper limit of the addition amount of the tetrafluoroethylene resin is defined as 0.5 part by weight in view of the limit of the discharge time from the mill.

【0017】第2の発明では、前記の第1の発明の組成
に加えてアルキルベンゼンスルフォン酸塩,アルキル硫
酸塩から成る群より選ばれる1種又は2種以上の陰イオ
ン系界面活性剤を0.001〜0.05重量部添加するものであ
るが、その理由を以下に述べる。
In the second invention, in addition to the composition of the first invention, 0.001 to 0.001 of one or more anionic surfactants selected from the group consisting of alkylbenzene sulfonates and alkyl sulfates is added. The reason for adding 0.05 part by weight is as follows.

【0018】四フッ化エチレン樹脂は撥水性が非常に強
く、これを含有する埋没材を練和液で練和した場合に
「埋没材と練和液とのなじみ」と称する使用上の操作感
に悪影響を与える。具体的には粉末と液の濡れ性が悪化
し、短時間で粉末と液との混合ができず、液の上に粉末
が浮いている状態になり、練和操作を行い難くなる。こ
の性質は、埋没材自体の性能・性質には直接には影響を
与えないが、練和性などの使用時の操作性に問題を生ず
る。この問題点を解決するために、四フッ化エチレン樹
脂の添加による練和時の「練和液とのなじみ」の悪化す
る現象を陰イオン系界面活性剤を添加し、粉末と液との
濡れ性を改善して練和性の向上を図ったのが第2の発明
である。
The tetrafluoroethylene resin has a very strong water repellency, and when the investment material containing the same is kneaded with a kneading solution, a feeling of operation in use called "familiarity between the investment material and the kneading solution" is obtained. Adversely affect. Specifically, the wettability of the powder and the liquid deteriorates, the powder and the liquid cannot be mixed in a short time, and the powder floats on the liquid, making it difficult to perform the kneading operation. Although this property does not directly affect the performance and properties of the investment material itself, it causes a problem in operability during use such as kneading property. In order to solve this problem, we added an anionic surfactant to prevent the phenomenon of "familiarity with the kneading liquid" at the time of kneading by adding tetrafluoroethylene resin, and wetting the powder with the liquid. The second aspect of the present invention aims to improve the compatibility and the kneadability.

【0019】上記の理由により陰イオン系界面活性剤を
添加するのであるが、非イオン系界面活性剤では四フッ
化エチレン樹脂の添加による「練和液とのなじみ」の性
質低下を改善するには多量の添加が必要であり、その結
果として埋没材の硬化物の圧縮強さの低下の傾向を示
し、溶融金属の流入時に鋳造圧力により鋳型の破損を招
くので望ましくない。アルキルベンゼンスルフォン酸
塩,アルキル硫酸塩は非イオン系界面活性剤に比べて少
量で「練和液とのなじみ」の改善が認められ、埋没材硬
化物の圧縮強さの低下も認められないので好ましい。
The anionic surfactant is added for the above reason, but the nonionic surfactant is effective in improving the property deterioration of "compatibility with the kneading liquid" due to the addition of the tetrafluoroethylene resin. Requires a large amount of addition, and as a result tends to lower the compressive strength of the cured product of the investment material, and causes the mold to break due to the casting pressure when the molten metal flows in, which is not desirable. Alkylbenzene sulfonate and alkyl sulphate are preferable because they improve the "familiarity with the kneading liquid" in a small amount compared with nonionic surfactants, and the compression strength of the cured investment material is not reduced. .

【0020】陰イオン系界面活性剤であるアルキルベン
ゼンスルフォン酸塩としてはドデシルベンゼンスルフォ
ン酸ナトリウムなどが使用され、アルキル硫酸塩として
はラウリル硫酸ナトリウム,ラウリル硫酸カリウム,ミ
リスチル硫酸ナトリウム,セチル硫酸ナトリウム,ステ
アリル硫酸ナトリウムなどが使用される。
Sodium dodecylbenzene sulfonate is used as the alkylbenzene sulfonate which is an anionic surfactant, and sodium lauryl sulfate, potassium lauryl sulfate, sodium myristyl sulfate, sodium cetyl sulfate and stearyl sulfate are used as the alkyl sulfate. Sodium is used.

【0021】陰イオン系界面活性剤の添加量は、0.001
重量部以上であれば「練和液とのなじみ」の改善が確認
されたので添加量の下限を0.001重量部と規定した。一
方、上限を0.05重量部と規定したのは、添加量が多くな
るほど、練和時の「練和液とのなじみ」は向上するが、
或る添加量を超えると埋没材の重要な特性である「凝結
時間」,「保存安定性」,「圧縮強さ」に影響を与える
ことが確認されたことによるものである。特に「圧縮強
さ」の低下は鋳造時の鋳バリ等の鋳造欠陥の原因とな
り、実用上埋没材の特性に悪影響を与えない添加量は0.
05重量部であることが実験で検証されたので陰イオン系
界面活性剤の添加量の上限を0.05重量部と規定した。
The amount of the anionic surfactant added is 0.001
If the amount is more than the weight part, improvement in "familiarity with the kneading liquid" was confirmed, so the lower limit of the addition amount was defined as 0.001 part by weight. On the other hand, the upper limit is defined as 0.05 parts by weight, the larger the amount added, the more "compatibility with the kneading liquid" at the time of kneading,
This is because it was confirmed that if the amount of addition exceeds a certain level, it affects important properties of the investment material, namely "setting time", "storage stability" and "compressive strength". In particular, the decrease in `` compressive strength '' causes casting defects such as casting burrs during casting, and the addition amount that does not adversely affect the properties of the investment material in practice is 0.
Since it was verified by experiments that the amount was 05 parts by weight, the upper limit of the addition amount of the anionic surfactant was defined as 0.05 parts by weight.

【0022】[0022]

【実施例】以下、本発明の実施例と比較例を挙げ本発明
を更に詳細に説明する。実施例1〜10は表1に示した
組成で、比較例1〜9は表3に示した組成で、結合材と
して酸化マグネシウムとリン酸二水素アンモニウムを、
耐火材として石英とクリストバライトを使用し、また実
施例1〜10,比較例3〜9では四フッ化エチレン樹脂
を配合したものであり、更に実施例6〜10,比較例7
〜9では陰イオン系界面活性剤を添加したものである。
EXAMPLES The present invention will be described in more detail with reference to Examples and Comparative Examples of the present invention. Examples 1 to 10 have the compositions shown in Table 1, Comparative Examples 1 to 9 have the compositions shown in Table 3, magnesium oxide and ammonium dihydrogen phosphate as binders,
Quartz and cristobalite were used as the refractory material, and in Examples 1 to 10 and Comparative Examples 3 to 9, tetrafluoroethylene resin was blended. Further, Examples 6 to 10 and Comparative Example 7 were used.
In Nos. 9 to 9, an anionic surfactant was added.

【0023】表2及び表4に示す各特性試験は、以下の
方法により行った。具体的には内容量100リットルの試
験配合用ボールミルを用いて埋没材の総重量を50Kgとし
たスケールによる粉砕・混合を行った。初めに耐火材で
ある石英とクリストバライトと場合によってはそれに加
えて微細粒子捕捉材である四フッ化エチレン樹脂の粉末
をミルに投入して耐火材が所定の粒度分布を示すまで粉
砕した。その後、結合材である酸化マグネシウムとリン
酸二水素アンモニウムを、場合によってはそれに加えて
陰イオン系界面活性剤をミルに投入し粉砕・混合を行い
凝結時間・流動性の調整を行った後にミルから排出し、
ホッパーに貯蔵した。四フッ化エチレン樹脂の粉末は、
耐火材及び結合材の粉砕・混合工程で剪断・圧縮応力を
負荷されて微細な繊維状となって埋没材の微細粒子を捕
捉している。ホッパーに貯蔵した埋没材の中から特性試
験用として1Kgずつランダムに5回サンプリングし合計
で5Kgの試料を採取し、残りの45Kgの埋没材を空気輸送
装置で空気輸送を行い、空気輸送により埋没材の微細な
粒子がどの程度喪失され、それによって埋没材の各特性
にどのような影響が現れるかの検証を行った。空気輸送
後のサンプルも輸送前と同様に1Kgずつランダムに5Kg
のサンプリングを行い試料とした。
The characteristic tests shown in Tables 2 and 4 were carried out by the following methods. Specifically, the test compounding ball mill having an internal capacity of 100 liters was used to perform crushing and mixing on a scale with the total weight of the investment material being 50 kg. First, the refractory material such as quartz and cristobalite and, in some cases, a powder of tetrafluoroethylene resin, which is a fine particle capturing material, were charged into a mill and ground until the refractory material exhibited a predetermined particle size distribution. After that, magnesium oxide and ammonium dihydrogen phosphate, which are binders, and, if necessary, an anionic surfactant are added to the mill, and the mixture is pulverized and mixed to adjust the setting time and fluidity, and then the mill. Discharged from the
Stored in hopper. The powder of tetrafluoroethylene resin is
Shear and compression stresses are applied in the crushing and mixing process of refractory materials and binders to form fine fibrous materials that capture the fine particles of the investment material. From the investment material stored in the hopper, 1 kg of each is randomly sampled 5 times for a characteristic test and a total of 5 kg is sampled. The remaining investment material of 45 kg is pneumatically transported by an air transportation device and buried by air transportation. It was verified how much fine particles of the wood were lost, and what kind of effect it had on the properties of the investment material. Samples after air transportation are 5 kg randomly, 1 kg each, as before transportation.
Was sampled and used as a sample.

【0024】それぞれの試料は、JIS T 6601「歯科鋳造
用石こう系埋没材」に定められた方法に準じて、空気輸
送前と空気輸送後の埋没材の特性を測定した。また微細
粒子の喪失の程度は、島津製作所社製の粒度分布計「SA
LD1100型」を使用し、測定レンジBで自動測定して、1.
9μm以下の粒子の体積パーセントを比較することにより
行った。鋳造体の適合精度の評価方法は、ニッシン社製
のA.D.A.No.2試験体のMOD模型に、通法に従ってワック
スパターンを作製し、それぞれの埋没材で埋没し、練和
開始から60分後から加熱を開始し、150分で800℃まで昇
温して30分間係留し、鋳型を800℃均一な状態にした
後、歯科用遠心鋳造機を用いてジーシー社製の歯科陶材
焼付用金合金「商品名:ジーセラボンドタイプIIゴー
ルドハード」を鋳造し、鋳造体掘り出し後にJIS#240メ
ッシュのアルミナ粉末によるサンドブラスト処理を施
し、焼付いた埋没材や酸化被膜を除去してMOD模型に戻
し模型との浮き上がり量を投影機を用いて測定し、その
大小で適合精度を評価した。それぞれの特性値は空気輸
送前,空気輸送後のそれぞれ1Kgずつ採取した試料で測
定した繰り返し5回の平均値であり、データのバラツキ
の程度は標準偏差で表現した。
The characteristics of each sample were measured according to the method specified in JIS T 6601 "Gypsum-based investment material for dental casting" before and after pneumatic transportation. In addition, the degree of loss of fine particles is determined by the particle size distribution analyzer “SA” manufactured by Shimadzu Corporation.
LD1100 type "is used, and the measurement range B is automatically measured.
This was done by comparing the volume percentage of particles below 9 μm. As for the evaluation method of the fitting accuracy of the cast body, a wax pattern was prepared according to the usual method on the MOD model of ADA No. 2 test body manufactured by Nissin Co., embedded with each investment material, and heated 60 minutes after the start of kneading After the temperature is raised to 800 ° C in 150 minutes and moored for 30 minutes, the mold is brought to a uniform state of 800 ° C, and a dental centrifugal casting machine is used to make a dental porcelain baking gold alloy made by GC. "Product name: Gicerabond Type II Gold Hard" is cast, and after digging out the cast body, sandblasting with JIS # 240 mesh alumina powder is performed, and the burned investment material and oxide film are removed and returned to the MOD model. The amount of uplift was measured using a projector, and the matching accuracy was evaluated based on its size. Each characteristic value is an average value of repeated 5 times measured with a sample of 1 kg each before and after pneumatic transportation, and the degree of data variation is expressed by standard deviation.

【0025】[0025]

【表1】 [Table 1]

【0026】[0026]

【表2】 [Table 2]

【0027】[0027]

【表3】 [Table 3]

【0028】[0028]

【表4】 [Table 4]

【0029】四フッ化エチレン樹脂の添加による微細粒
子捕捉効果の確認は、表1の組成及び表2の特性値から
明らかである。実施例1〜10は微細粒子捕捉材として
四フッ化エチレン樹脂が0.01から0.5重量部添加されて
いる。表2の特性値から明らかなように空気輸送前と空
気輸送後では凝結膨張,熱膨張や圧縮強さの値は空気輸
送時に僅かながらも微粉末が喪失するので低下する傾向
が確認された。一方、バラツキの程度を表す標準偏差は
やや増大する場合もあれば反対に減少する時もある。し
かしながら、これらの特性値の低下及びバラツキの変化
は歯科用リン酸塩系埋没材として最も重要な性質である
鋳造体の鋳造精度に対しては影響を与えず、両者間に統
計的な有意な差は確認されず、どちらも同様な鋳造精度
を有していた。このことから実施例1〜10において
は、四フッ化エチレン樹脂を埋没材に添加したボールミ
ルによる粉砕工程において、四フッ化エチレン樹脂が繊
維化し埋没材中の耐火材であるクリストバライトや石英
の微細粒子、及び結合材であるリン酸二水素アンモニウ
ムとマグネシアの微細粒子を捕捉する効果を発揮し、空
気輸送前と空気輸送後との間には物理的な特性の差違は
生ずることなく、その結果として実用上において最も重
要な特性である鋳造精度の低下は確認されず本発明の効
果が確認できた。
Confirmation of the effect of trapping fine particles by the addition of the tetrafluoroethylene resin is clear from the composition of Table 1 and the characteristic values of Table 2. In Examples 1 to 10, 0.01 to 0.5 parts by weight of tetrafluoroethylene resin is added as a fine particle capturing material. As is clear from the characteristic values in Table 2, it was confirmed that before and after pneumatic transportation, the values of setting expansion, thermal expansion and compressive strength tended to decrease due to a slight loss of fine powder during pneumatic transportation. On the other hand, the standard deviation, which indicates the degree of variation, may increase slightly or, on the contrary, decrease. However, the decrease in these characteristic values and the variation in the variations do not affect the casting accuracy of the cast body, which is the most important property as a dental phosphate-based investment material, and there is a statistically significant difference between the two. No difference was confirmed, and both had similar casting accuracy. From these facts, in Examples 1 to 10, fine particles of cristobalite or quartz, which are the refractory material in the investment material, are formed into fibers of the ethylene tetrafluoride resin in the pulverization process by the ball mill in which the investment material is added with the tetrafluoroethylene resin. , And the effect of capturing fine particles of the binding material ammonium dihydrogen phosphate and magnesia, and there is no difference in physical properties between before and after pneumatic transportation, and as a result, The effect of the present invention could be confirmed without any deterioration in casting precision, which is the most important characteristic in practical use.

【0030】一方、比較例1及び2では、組成的には実
施例1及び2と四フッ化エチレン樹脂以外は同様である
が、比較例1及び2では四フッ化エチレン樹脂が添加さ
れていないため空気輸送中に微細な粒子が喪失してしま
い、その結果として空気輸送前と空気輸送後では表4か
ら明らかなように特性値に差異が生じている。具体的に
は、鋳造体の寸法精度に影響を及ぼす特性である凝結膨
張値及び熱膨張値が、空気輸送前と空気輸送後では輸送
前の値に比べ輸送後の値が低下しており、このことによ
り鋳造体の適合精度が低下している。それに加えて大き
な問題点はバラツキの程度を示す標準偏差の値が大きく
なっている現象である。このことから比較例1及び2の
埋没材を用いて鋳造した場合には鋳造精度が悪化するこ
とと、鋳造精度のバラツキが生じ易くなる。膨張値が低
下することによる鋳造精度の悪化は、他の臨床上の対策
(鋳造用リングの内側に裏層するライナーの厚み,材質
などの選択など)により或る程度の解決は可能である
が、バラツキが大きくなることの対策は臨床上のテクニ
ックでは解決不可能であり、臨床上の使用に大きな問題
点となる。
On the other hand, in Comparative Examples 1 and 2, the composition is the same as in Examples 1 and 2 except for the tetrafluoroethylene resin, but in Comparative Examples 1 and 2, no tetrafluoroethylene resin is added. Therefore, fine particles are lost during pneumatic transportation, and as a result, characteristic values are different before and after pneumatic transportation as shown in Table 4. Specifically, the condensation expansion value and the thermal expansion value, which are the characteristics that affect the dimensional accuracy of the cast body, the value after transportation is lower than the value before transportation before and after pneumatic transportation, This reduces the fitting accuracy of the cast body. In addition to that, a big problem is a phenomenon that the value of the standard deviation showing the degree of variation is large. For this reason, when casting is performed using the investment material of Comparative Examples 1 and 2, the casting precision deteriorates and the casting precision easily varies. The deterioration of the casting precision due to the decrease in the expansion value can be solved to some extent by other clinical measures (selection of the thickness and material of the liner backing the inside of the casting ring, etc.). However, the countermeasure against the large variation cannot be solved by the clinical technique, which is a big problem in the clinical use.

【0031】同様に四フッ化エチレン樹脂の添加量が本
発明の範囲の下限未満である比較例3及び4では、実施
例3及び4と比較して空気輸送前であれば実施例と差異
は確認されないが、空気輸送後では適合精度において適
合精度の低下とバラツキの上昇が確認され、四フッ化エ
チレン樹脂添加の効果は発揮されていない。
Similarly, in Comparative Examples 3 and 4 in which the amount of tetrafluoroethylene resin added is less than the lower limit of the range of the present invention, there is a difference from Examples 3 and 4 before pneumatic transportation. Although not confirmed, a decrease in conformity accuracy and an increase in conformity were confirmed after pneumatic transportation, and the effect of the addition of tetrafluoroethylene resin was not exhibited.

【0032】四フッ化エチレン樹脂の添加量が本発明の
上限を超えた例が比較例5,6,8及び9である。四フ
ッ化エチレン樹脂は撥水性が特に強い物質であり、添加
量が0.8〜1.0重量部で且つ練和操作性向上のための陰イ
オン系界面活性剤を配合していない比較例5と比較例6
では練和操作性が極端に悪化して通常の歯科における埋
没材の練和方法では練和不可能であり、特性の測定も不
可能であった。また陰イオン系界面活性剤を添加した比
較例8及び9では練和操作性の評価は「良好」であった
が、四フッ化エチレン樹脂が過剰に添加されたことによ
り埋没材をミルから排出する工程で埋没材の粉末同士が
凝集する現象が起きて排出口から排出される量が減少
し、排出のためのミルの回転が残留した埋没材を粉砕
し、過剰粉砕になり更に凝集が進行し、ミルからの排出
が遅れるという悪循環が発生し、排出の初期と排出の最
後では粉末の特性、特に凝結膨張,熱膨張などの差異が
大きくなり、空気輸送以前に埋没材のバラツキを生じ
た。また排出に要する時間が長くなり、実際の操業は不
可能となった。また過剰粉砕により凝結膨張と熱膨張値
が大きくなり過ぎて鋳造精度の悪化を来たしている試験
体も存在した。以上の結果より、排出時の時間と排出時
の回転による粉砕の問題から四フッ化エチレン樹脂の添
加量の上限が0.5重量部であることが確認できた。
Examples in which the addition amount of the tetrafluoroethylene resin exceeds the upper limit of the present invention are Comparative Examples 5, 6, 8 and 9. The tetrafluoroethylene resin is a substance having a particularly strong water repellency, the addition amount thereof is 0.8 to 1.0 part by weight, and the anionic surfactant for improving the kneading operability is not blended. 6
In this case, the kneading operability was extremely deteriorated, and it was impossible to knead with the usual method of kneading the investment material in dentistry, and it was also impossible to measure the characteristics. In Comparative Examples 8 and 9 in which an anionic surfactant was added, the kneading operability was evaluated as “good”, but the investment material was discharged from the mill due to the excessive addition of the tetrafluoroethylene resin. In the process, the phenomenon that the investment material powders agglomerate with each other reduces the amount discharged from the discharge port, and the rotation of the mill for discharging crushes the remaining investment material and causes excessive crushing and further aggregation. However, there was a vicious cycle in which the discharge from the mill was delayed, and the characteristics of the powder, especially condensation expansion and thermal expansion, became large at the beginning of the discharge and at the end of the discharge, causing variations in the investment material before pneumatic transportation. . In addition, the time required for discharge became longer, and the actual operation became impossible. In addition, there was also a test piece in which the setting expansion and the thermal expansion value became too large due to excessive pulverization and the casting precision deteriorated. From the above results, it was confirmed that the upper limit of the addition amount of the tetrafluoroethylene resin is 0.5 parts by weight due to the problem of pulverization due to the time of discharging and the rotation during discharging.

【0033】また、表1の実施例1〜4において、撥水
性の強い物質である四フッ化エチレン樹脂が埋没材に添
加された場合に、0.1重量部までの添加量であれば陰イ
オン系界面活性剤が埋没材に配合されてなくとも「練和
液とのなじみ」の性質は「普通」の評価であった。この
「普通」の評価は、具体的には現行の歯科用リン酸塩系
埋没材製品と比較したもので、「良好」とは現行の製品
より評価が高く、「普通」とは現行製品と同等であるこ
とを示している。実施例4では四フッ化エチレン樹脂の
添加量が0.3重量部まで上昇すると「練和液とのなじ
み」が低下傾向を示して「やや難」の評価となる。「や
や難」の評価の具体的な意味は、実用上では練和するこ
とができるが、現行の製品よりは「練和液とのなじみ」
が悪く、それによって練和性が劣ることを示している。
実施例5の四フッ化エチレン樹脂の添加量が0.5重量部
になると練和性は低下したが、臨床ではかろうじて使用
可能という状態であった。
Further, in Examples 1 to 4 of Table 1, when a tetrafluoroethylene resin, which is a highly water-repellent substance, is added to the investment material, if the addition amount is up to 0.1 part by weight, The property of "familiar with the kneading liquid" was evaluated as "normal" even if the surfactant was not mixed in the investment material. This “ordinary” rating is specifically compared to the current dental phosphate-based investment material product, “good” is higher than the current product, and “ordinary” is the current product. It shows that they are equivalent. In Example 4, when the amount of the tetrafluoroethylene resin added increased to 0.3 parts by weight, the "familiarity with the kneading liquid" showed a tendency to decrease and the evaluation was "slightly difficult". The specific meaning of the evaluation of "somewhat difficult" is that it can be mixed in practice, but it is "familiar with the mixing liquid" rather than the current product.
Indicates that the blendability is poor and that the blending is poor.
When the amount of the tetrafluoroethylene resin added in Example 5 was 0.5 parts by weight, the miscibility was lowered, but it was barely usable in clinical use.

【0034】リン酸塩系埋没材に、強い撥水性を有する
四フッ化エチレン樹脂を添加することにより練和性が低
下することは上述の通りであるが、実施例6〜10はこ
の特性を改良するために陰イオン系の界面活性剤を添加
したものであり、陰イオン系界面活性剤を添加すること
により練和操作性の向上が確認された。具体的には、実
施例1と実施例6との比較において、配合上での差異は
陰イオン系界面活性剤の添加の有無だけであるが、実施
例1では練和操作性の評価が「普通」であるが、実施例
6では「良好」となる。同様に、実施例2と実施例7と
の比較において陰イオン系界面活性剤の添加の有無によ
り表1から判るように練和操作性に差が生じるが、表2
から判るように凝結膨張,熱膨張,圧縮強さ,1.9μm以
下の粒子の体積などの特性に加えて埋没材として最も重
要な特性である適合精度においては陰イオン系界面活性
剤の添加による影響は確認されなかった。
As described above, the addition of a tetrafluoroethylene resin having strong water repellency to the phosphate-based investment material reduces the kneading property, but Examples 6 to 10 exhibit this characteristic. An anionic surfactant was added for improvement, and it was confirmed that the kneading operability was improved by adding the anionic surfactant. Specifically, in the comparison between Example 1 and Example 6, the only difference in formulation is the presence or absence of the addition of an anionic surfactant, but in Example 1, the evaluation of the kneading operability was " It is "normal" but is "good" in Example 6. Similarly, in the comparison between Example 2 and Example 7, there is a difference in kneading operability depending on whether or not an anionic surfactant is added, but Table 2
As can be seen from the above, in addition to properties such as condensation expansion, thermal expansion, compressive strength, and volume of particles of 1.9 μm or less, the accuracy of fitting, which is the most important property as an investment material, is affected by the addition of an anionic surfactant. Was not confirmed.

【0035】また陰イオン系界面活性剤の添加による効
果としては、実施例9及び10では四フッ化エチレン樹
脂がそれぞれ0.3重量部と0.5重量部とかなりの量が添加
されているが、練和操作性の評価は「良好」となった。
それに対して陰イオン系界面活性剤以外の組成は同じで
ある実施例4及び5では陰イオン系界面活性剤が配合さ
れていないため練和操作性の評価は「やや難」となって
いる。これらの実施例の比較により、陰イオン系界面活
性剤の添加量が0.05重量部までであれば物理的性質に大
きな影響を及ぼすことはないことが確認された。
As an effect of adding an anionic surfactant, in Examples 9 and 10, 0.3 parts by weight and 0.5 parts by weight of tetrafluoroethylene resin were added, respectively, which were considerable amounts. The operability was evaluated as “good”.
On the other hand, in Examples 4 and 5 having the same composition other than the anionic surfactant, the kneading operability was evaluated as “somewhat difficult” because no anionic surfactant was blended. By comparing these examples, it was confirmed that if the amount of the anionic surfactant added was up to 0.05 parts by weight, the physical properties were not significantly affected.

【0036】また、陰イオン系界面活性剤の添加量の下
限を0.001重量部と規定した根拠は以下の通りである。
比較例7では四フッ化エチレン樹脂が0.5重量部添加さ
れており練和操作性は「やや難」である。四フッ化エチ
レン樹脂を0.5重量部添加した例としては比較例7の他
に実施例5及び実施例10があるが、実施例10では陰
イオン系界面活性剤が0.05重量部添加されており練和操
作性の評価は「良好」である。それに対して、実施例5
は陰イオン系界面活性剤が配合されておらず評価は「や
や難」である。比較例7では陰イオン系界面活性剤が0.
0007重量部添加されているが同様に「やや難」であり、
陰イオン系界面活性剤の添加効果は確認されなかった。
一方、実施例1と実施例6を比較すると、組成の違いは
陰イオン系界面活性剤の有無だけで、その添加量も0.00
1重量部であるが、練和操作性に対する効果は明確に現
われており、評価が「普通」から「良好」になった。以
上の理由により、練和操作性の向上に対する陰イオン系
界面活性剤の添加の下限を0.001重量部と規定した。
The basis for defining the lower limit of the addition amount of the anionic surfactant as 0.001 part by weight is as follows.
In Comparative Example 7, 0.5 part by weight of tetrafluoroethylene resin was added, and the kneading operability was “slightly difficult”. As an example of adding 0.5 parts by weight of tetrafluoroethylene resin, there are Example 5 and Example 10 in addition to Comparative Example 7. In Example 10, 0.05 part by weight of an anionic surfactant was added. The sum operability is evaluated as "good". On the other hand, Example 5
No anionic surfactant was added, and the evaluation is "somewhat difficult". In Comparative Example 7, the anionic surfactant was 0.
[0007] Although added in parts by weight, it is also "slightly difficult",
The effect of adding the anionic surfactant was not confirmed.
On the other hand, comparing Example 1 and Example 6, the difference in composition is only the presence or absence of an anionic surfactant, and the addition amount is 0.00
Although the amount was 1 part by weight, the effect on the kneading operability was clearly shown, and the evaluation was changed from “normal” to “good”. For the above reasons, the lower limit of the addition of the anionic surfactant for improving the kneading operability is defined as 0.001 part by weight.

【0037】陰イオン系界面活性剤の添加量の上限を0.
05重量部と規定した根拠は以下の通りである。比較例8
及び比較例9の四フッ化エチレン樹脂の添加量は0.8〜
1.0重量部と本発明の上限を超えているが、陰イオン系
界面活性剤の添加量も0.1〜0.2重量部と本発明の上限を
超えているために練和操作性の評価は「良好」である。
しかしながら、陰イオン系界面活性剤の過剰な添加は特
性値の中で、圧縮強さを大きく低下させる。また表2に
は示されていないが、リン酸塩系埋没材として重要な性
質である凝結時間を遅延させるという臨床上において大
きな欠陥をもたらす。圧縮強さの低下は鋳型の強度を低
下させ鋳造時の溶融金属の流入による圧力によって鋳型
が破損し、鋳バリの発生という致命的な鋳造欠陥の主要
因となるため避けなければならない現象である。鋳バリ
の発生しない圧縮強さの値は、従来からの実験及び経験
により4.0MPa以上あれば良いという結論があり、比較例
8及び9ではこの値を下回っているために鋳造体の中に
鋳バリの欠陥を有する試験体が確認された。それ以外の
鋳型で作製した試験体には鋳バリの発生は皆無であった
ためこの理論は正しいと考えられる。以上の実験結果よ
り陰イオン系界面活性剤の添加量の上限を圧縮強さから
鑑みて、且つ安全性を考慮して0.05重量部と規定した。
The upper limit of the amount of anionic surfactant added is set to 0.
The basis for defining 05 parts by weight is as follows. Comparative Example 8
And the addition amount of the tetrafluoroethylene resin of Comparative Example 9 is 0.8 to
Although it exceeds 1.0 part by weight and the upper limit of the present invention, the addition amount of the anionic surfactant is also 0.1 to 0.2 parts by weight and exceeds the upper limit of the present invention, and therefore the evaluation of the kneading operability is “good”. Is.
However, excessive addition of the anionic surfactant significantly reduces the compressive strength among the characteristic values. Although not shown in Table 2, it causes a serious clinical defect that the setting time, which is an important property as a phosphate-based investment material, is delayed. A decrease in compressive strength is a phenomenon that must be avoided because it decreases the strength of the mold and causes the mold to break due to the pressure caused by the inflow of molten metal during casting, which is a major cause of fatal casting defects such as the formation of casting burrs. . It has been concluded from conventional experiments and experience that the value of the compressive strength at which casting burrs do not occur should be 4.0 MPa or more, and in Comparative Examples 8 and 9, the value is below this value, and therefore, it is cast in a cast body. A test body having a burr defect was confirmed. It is considered that this theory is correct because there were no casting burrs in the test pieces produced by other molds. From the above experimental results, the upper limit of the amount of the anionic surfactant added was defined as 0.05 parts by weight in view of the compressive strength and in consideration of safety.

【0038】[0038]

【発明の効果】以上に詳述した如く、本発明に係る歯科
用リン酸塩系埋没材組成物は、結合材としての酸化マグ
ネシウムとリン酸二水素アンモニウムと耐火材としての
石英とクリストバライトから構成される混合物に四フッ
化エチレン樹脂を添加し、粉砕工程において四フッ化エ
チレン樹脂を微細な繊維化することにより、埋没材中の
微細粒子を捕捉し埋没材の空気輸送工程における埋没材
中の微細粒子の喪失を防止することができるので、その
結果として凝結膨張,熱膨張などの各特性値が安定した
歯科用リン酸塩系埋没材が得られ、寸法精度高い歯科金
属修復物の製作が可能となったのである。
As described above in detail, the dental phosphate-based investment material composition according to the present invention comprises magnesium oxide and ammonium dihydrogen phosphate as a binder, and quartz and cristobalite as a refractory material. The tetrafluoroethylene resin is added to the mixture to be mixed, and the fine particles of the tetrafluoroethylene resin are made into fine fibers in the crushing step to capture the fine particles in the investment material and Since it is possible to prevent the loss of fine particles, as a result, a dental phosphate-based investment material with stable characteristic values such as setting expansion and thermal expansion can be obtained, and it is possible to manufacture a dental metal restoration with high dimensional accuracy. It has become possible.

【0039】また、撥水性の高い四フッ化エチレン樹脂
を添加することによる練和操作性の悪化に対しては、ア
ルキルベンゼンスルフォン酸塩,アルキル硫酸塩から成
る群より選ばれる1種又は2種以上の陰イオン系界面活
性剤を添加することにより上記の問題を解決することが
可能となった。そして付随効果として、四フッ化エチレ
ン樹脂を添加し、粉砕工程で繊維化することによる微細
粒子捕捉効果により鋳型作製時の埋没材の練和操作時に
埋没材中の微細粒子の飛散を防止する効果も得られた。
As for the deterioration of the kneading operability due to the addition of the tetrafluoroethylene resin having high water repellency, one or more selected from the group consisting of alkylbenzene sulfonates and alkyl sulfates. It has become possible to solve the above problems by adding the anionic surfactant. And as an attendant effect, the effect of preventing the scattering of fine particles in the investment material during the kneading operation of the investment material at the time of the mold preparation by the addition effect of tetrafluoroethylene resin and the effect of capturing fine particles by fiberizing in the crushing process Also got.

【0040】前記したような種々の効果を有する本発明
に係る歯科用リン酸塩系埋没材組成物の歯科分野に貢献
する価値は非常に大きなものである。
The value of the dental phosphate-based investment material composition according to the present invention having various effects as described above is extremely great for contributing to the field of dentistry.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】a)結合材としての酸化マグネシウムとリ
ン酸二水素アンモニウム、 b)耐火材としての石英とクリストバライト、から構成
される混合物100重量部に対し、四フッ化エチレン樹脂
0.01〜0.5重量部が混合されていることを特徴とする歯
科用リン酸塩系埋没材組成物。
1. A tetrafluoroethylene resin based on 100 parts by weight of a mixture composed of a) magnesium oxide and ammonium dihydrogen phosphate as a binder, b) quartz and cristobalite as a refractory material.
A dental phosphate-based investment material composition, characterized in that 0.01 to 0.5 parts by weight are mixed.
【請求項2】a)結合材としての酸化マグネシウムとリ
ン酸二水素アンモニウム、 b)耐火材としての石英とクリストバライト、から構成
される混合物100重量部に対し、四フッ化エチレン樹脂
0.01〜0.5重量部と、アルキルベンゼンスルフォン酸
塩,アルキル硫酸塩から成る群より選ばれる1種又は2
種以上の陰イオン系界面活性剤0.001〜0.05重量部とが
混合されていることを特徴とする歯科用リン酸塩系埋没
材組成物。
2. A tetrafluoroethylene resin based on 100 parts by weight of a mixture composed of a) magnesium oxide and ammonium dihydrogen phosphate as a binder, b) quartz and cristobalite as a refractory material.
0.01 to 0.5 parts by weight and one or two selected from the group consisting of alkylbenzene sulfonate and alkyl sulfate.
A dental phosphate-based investment material composition, wherein 0.001 to 0.05 parts by weight of one or more anionic surfactants are mixed.
JP32242995A 1995-11-17 1995-11-17 Dental phosphate investment composition Expired - Lifetime JP3529523B2 (en)

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JP3529523B2 JP3529523B2 (en) 2004-05-24

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1319668C (en) * 2005-09-16 2007-06-06 海南三箭科技开发有限公司 Cast powder for casting high melting point metal and its usage
EP1867316A1 (en) * 2006-06-13 2007-12-19 GC Corporation Phosphate-based dental investing material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS50111890A (en) * 1974-02-12 1975-09-02
JPS62212255A (en) * 1986-03-12 1987-09-18 而至歯科工業株式会社 Low-dust powdery dental gypsum composition
JPH04200950A (en) * 1990-11-30 1992-07-21 Nisshin:Kk Molding material for casting metal having high melting point
JPH0558834A (en) * 1990-10-11 1993-03-09 Degussa Ag Water-soluble nondusty burying material and its manufacturing process
JPH06336409A (en) * 1993-05-27 1994-12-06 Taisei Shika Kogyo Kk Quick-heating embedding material composition

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS50111890A (en) * 1974-02-12 1975-09-02
JPS62212255A (en) * 1986-03-12 1987-09-18 而至歯科工業株式会社 Low-dust powdery dental gypsum composition
JPH0558834A (en) * 1990-10-11 1993-03-09 Degussa Ag Water-soluble nondusty burying material and its manufacturing process
JPH04200950A (en) * 1990-11-30 1992-07-21 Nisshin:Kk Molding material for casting metal having high melting point
JPH06336409A (en) * 1993-05-27 1994-12-06 Taisei Shika Kogyo Kk Quick-heating embedding material composition

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1319668C (en) * 2005-09-16 2007-06-06 海南三箭科技开发有限公司 Cast powder for casting high melting point metal and its usage
EP1867316A1 (en) * 2006-06-13 2007-12-19 GC Corporation Phosphate-based dental investing material

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