A dental water-hardening temporary filling material composition with excellent curability, ease of removal after hardening, and storage stability.

The dental water-hardening temporary filling material composition, with water-insoluble fine particles and balanced components, addresses the issues of slow hardening and stability, ensuring high curability and easy removal.

JP7860702B2Active Publication Date: 2026-05-18SHOFU INC
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Patent Information

Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Filing Date
2021-09-29
Publication Date
2026-05-18

AI Technical Summary

Technical Problem

Conventional dental water-hardening temporary fillings face issues with slow hardening, difficulty in removal after hardening, and decreased storage stability over time.

Method used

A dental water-hardening temporary filling material composition containing water-insoluble fine particles with a particle size of 0.1 μm or less, along with specific proportions of gypsum powder, organic solvent, and resin, enhances curability, removability, and storage stability.

Benefits of technology

The composition achieves high curability, excellent removability after hardening, and good storage stability without a decrease in curability over time.

✦ Generated by Eureka AI based on patent content.

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Abstract

To provide a hydraulic temporary sealing material composition for dentistry that satisfies each of high curability, excellent post-curing removability, and good storage stability to be used for the purpose of preventing food from entering the root canal, preventing bacterial infection of the treated area, and sealing a drug filled in the root canal, during the follow-up period after infected tooth material has been removed, for the duration of drug application, etc., when root canal treatment is performed in clinical dentistry by the sealing material being temporarily filled in and sealing a cavity or a root canal.SOLUTION: A hydraulic temporary sealing material composition for dentistry contains water-insoluble fine particles having a 50% particle size of 0.1 μm or less.SELECTED DRAWING: None
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Description

Technical Field

[0001] The present invention relates to a dental hydraulic temporary filling material composition.

Background Art

[0002] In dental clinics, when performing root canal treatment, during the observation period after removing infected dentin or the application period of drugs, etc., for the purpose of preventing the mixing of food into the root canal, preventing bacterial infection at the treatment site, sealing the drugs filled in the root canal, etc., a temporary seal is performed by temporarily filling a dental hydraulic temporary filling material into the cavity or root canal.

[0003] A dental hydraulic temporary filling material is a paste-like paste mainly composed of gypsum powder, which reacts with moisture such as saliva in the oral cavity and hardens after being filled into the cavity. After the end of the temporary sealing period, the hardened dental hydraulic temporary filling material is broken and removed. As such a dental hydraulic temporary filling material composition, those exemplified in Patent Document 1 or 2 are known.

Prior Art Documents

Patent Documents

[0004]

Patent Document 1

Patent Document 2

Summary of the Invention

Problems to be Solved by the Invention

[0005] Conventional dental water-hardening temporary fillings had the drawback of slow hardening, preventing them from functioning quickly after treatment. While it was possible to increase hardening speed by incorporating a high concentration of gypsum powder, the hardening component, this resulted in the hardened material becoming too hard and difficult to remove. Furthermore, even if the hardening speed was high initially, it would decrease over time after manufacturing. Thus, conventional dental water-hardening temporary fillings struggled to satisfy all three requirements: high hardening speed, excellent removeability after hardening, and good storage stability.

[0006] The present invention has been made in view of the above circumstances, and aims to provide a dental water-hardening temporary filling material composition that has high curability, excellent removeability after hardening, and good storage stability without a decrease in curability over time. [Means for solving the problem]

[0007] The above problems are solved by the present invention as described below. Specifically, the dental water-hardening temporary filling material composition of the present invention is characterized by containing water-insoluble fine particles with a particle size of 0.1 μm or less for 50% of the composition.

[0008] In one embodiment of the dental water-hardening temporary filling material composition of the present invention, it is preferable that the fine particles are not subjected to hydrophobic treatment.

[0009] Other embodiments of the dental water-hardening temporary filling material composition of the present invention preferably include gypsum powder, an organic solvent, and a resin.

[0010] In other embodiments of the dental water-hardening temporary filling material composition of the present invention, it is preferable that the composition contains 0.3 to 10% by mass of fine particles, 20 to 85% by mass of gypsum powder, 10 to 25% by mass of organic solvent, and 3 to 15% by mass of resin, relative to the total composition.

[0011] In another embodiment of the dental water-hardening temporary filling material composition of the present invention, it is preferable that the organic solvent is at least one selected from glycerin or its derivatives.

[0012] In another embodiment of the dental water-hardening temporary filling material composition of the present invention, it is preferable that the resin is at least one selected from vinyl acetate, vinyl chloride homopolymers, or copolymers thereof. [Effects of the Invention]

[0013] According to the present invention, it is possible to provide a dental water-hardening temporary filling material composition that has high curability, excellent removeability after hardening, and good storage stability without a decrease in curability over time. [Modes for carrying out the invention]

[0014] The dental water-hardening temporary filling material composition of the present invention is characterized by containing non-water-soluble fine particles with a particle size of 0.1 μm or less for 50% of the composition.

[0015] The non-water-soluble component (1) fine particles with a 50% particle size of 0.1 μm or less is a component that gives the dental water-hardening temporary filling material composition of the present invention high curability, excellent removalability after hardening, and good storage stability.

[0016] Component (1) The 50% particle size of the fine particles must be 0.1 μm or less, preferably 0.05 μm or less, and more preferably 0.02 μm or less. If the particle size exceeds 0.1 μm, not only will high curability not be obtained, but the curability may decrease over time, and good storage stability may not be achieved. In addition, the cured product may become harder than when no fine particles are included, and the removeability after curing may actually worsen.

[0017] Component (1) The fine particles must be water-insoluble. If water-soluble fine particles are used, the high curability, excellent post-curing removal properties, and good storage stability that are characteristic of the present invention may not be exhibited.

[0018] There are no particular restrictions on the constituent elements or crystal structure of the component (1) fine particles, and known fine particles can be used. In particular, it is preferable to use inorganic fine particles that do not swell easily in water or organic solvents and have high hardness.

[0019] Specific examples of the component (1) fine particles include, but are not limited to, aluminum oxide, silicon dioxide, titanium dioxide, magnesium oxide, zinc oxide, zirconium dioxide, bismuth oxide, yttrium oxide, aluminosilicate glass, borosilicate glass, soda-lime silicate glass, titania-silica glass, etc. These may be used in combination of two or more kinds. Among them, it is preferable to use aluminum oxide, silicon dioxide, titanium dioxide, and zinc oxide.

[0020] Although there is no particular limitation on whether or not the component (1) fine particles are surface-treated, it is preferable that they are not subjected to a hydrophobization treatment. By using fine particles having a hydrophilic surface, it becomes easier to exhibit high curability and good storage stability.

[0021] Although the content of the component (1) fine particles is not particularly limited, it is preferably within the range of 0.3 to 10% by mass, and more preferably within the range of 1 to 5% by mass with respect to the entire dental hydraulic temporary filling material composition. By setting the content of the component (1) fine particles to 0.3% by mass or more, high curability, excellent removability, and good storage stability can be surely exhibited. Also, by setting the content of the component (1) fine particles to 10% by mass or less, a paste property that is easy to handle can be maintained, and excessive curing expansion can be prevented.

[0022] There is no particular limitation on the shape of the component (1) fine particles, and any shape such as spherical, needle-like, plate-like, crushed, scaly, etc. can be used.

[0023] The gypsum powder of component (2) is a component that reacts and cures in the presence of water, and is a component that imparts curability to the dental hydraulic temporary filling material composition of the present invention. The gypsum powder in the present invention means calcium sulfate hemihydrate.

[0024] Although there is no particular limitation on the content of the (2) gypsum powder, it is preferably within the range of 20 to 85% by mass, and more preferably within the range of 40 to 75% by mass with respect to the entire dental hydraulic temporary filling material composition. By setting the content of the (2) gypsum powder to 20% by mass or more, high curability and good storage stability can be reliably exhibited. Further, by setting the content of the (2) gypsum powder to 85% by mass or less, excellent removability after curing can be more significantly exhibited.

[0025] There is no particular limitation on the 50% particle size of the (2) gypsum powder, and any particle size can be used so that it has an easy-to-handle paste property.

[0026] There is no particular limitation on the shape of the (2) gypsum powder, and any shape such as spherical, needle-shaped, plate-shaped, crushed, flaky, etc. can be used.

[0027] There is no particular limitation on the density of the (2) gypsum powder, and any density such as solid, hollow, porous, etc. can be used.

[0028] The (3) organic solvent is a component for pasting the dental hydraulic temporary filling material composition of the present invention.

[0029] The (3) organic solvent is not particularly limited as long as it does not react with the (2) gypsum powder, and known organic solvents can be used. However, from the viewpoint of storage stability, it is preferable to use an organic solvent with low volatility.

[0030] Specific examples of component (3) organic solvents include, but are not limited to, alcohols such as methanol, ethanol, propanol, isopropyl alcohol, isobutyl alcohol, ethylene glycol, low molecular weight polyethylene glycol, and glycerin; fatty acid esters such as ethyl acetate, butyl acetate, glycerin monoacetate, glycerin diacetate, glycerin triacetate, glycerin monomethacrylate, glycerin dimethacrylate, and glycerin monostearate; aliphatic hydrocarbons such as butane, pentane, and hexane; aromatic hydrocarbons such as benzene, toluene, and xylene; ketones such as methyl ethyl ketone and acetone; ethers such as diethyl ether; alkyl halides such as dichloromethane, chloroform, and carbon tetrachloride; organopolysiloxanes such as dimethylpolysiloxane and divinyldimethylpolysiloxane; and methacrylic acid esters such as methyl methacrylate, ethylene glycol dimethacrylate, and hydroxyethyl methacrylate. Two or more of these may be used in combination. Among these, it is preferable to use glycerin, glycerin monoacetate, glycerin diacetate, glycerin triacetate, glycerin monomethacrylate, glycerin dimethacrylate, glycerin monostearate, or glycerin derivatives thereof.

[0031] While there are no particular restrictions on the content of component (3) organic solvent, it is preferably in the range of 10 to 25% by mass of the total dental water-hardening temporary filling material composition, and more preferably in the range of 15 to 25% by mass. By setting the content of component (3) organic solvent to 10% by mass or more, the dental water-hardening temporary filling material composition of the present invention becomes an easy-to-handle paste, and good operability can be provided. Furthermore, by setting the content of component (3) organic solvent to 25% by mass or less, the stickiness of the paste can be reduced, and good operability can be provided.

[0032] Component (4) resin is a component that provides plasticity to the dental water-hardening temporary filling material composition of the present invention and adjusts the operability of the paste.

[0033] Component (4) The resin is not particularly limited as long as it is compatible with component (3) the organic solvent, and any known resin can be used.

[0034] Specific examples of component (4) resin include, but are not limited to, homopolymers and copolymers of vinyl acetate, vinyl chloride, acrylic acid, maleic acid, fumaric acid, and ethylene vinyl acetate copolymers. Two or more of these may be used in combination. Among these, it is preferable to use a homopolymer of vinyl acetate or vinyl chloride, or copolymers thereof.

[0035] While there are no particular restrictions on the content of component (4) resin, it is preferably in the range of 3 to 15% by mass, and more preferably in the range of 5 to 10% by mass, relative to the entire dental water-hardening temporary filling material composition. By setting the content of component (4) resin to 3% by mass or more, sufficient plasticity is imparted to the dental water-hardening temporary filling material composition of the present invention, and good handling properties can be achieved. Furthermore, by setting the content of component (4) resin to 15% by mass or less, high curability, excellent post-curing removal properties, and good storage stability without a decrease in curability over time can be more significantly achieved.

[0036] Furthermore, the dental water-hardening temporary filling material composition of the present invention may contain pigments, dyes, reaction modifiers, fillers, excipients, surfactants, antibacterial agents, ion-releasing agents, etc., to the extent that they do not impair the effects of the present invention. [Examples]

[0037] Examples and comparative examples of the present invention will be described below in detail, but the present invention is not limited to these examples.

[0038] (Details of the components used in the preparation of the dental water-hardening temporary filling material composition) Table 1 shows the components used in the preparation of the dental water-hardening temporary filling material compositions for the examples and comparative examples. The 50% particle size measurements for fine particles 1-5 and filling materials 1-6 are also included. The 50% particle size for fine particles 1-5 was calculated by image analysis of observations made with an electron microscope, while the 50% particle size for filling materials 1-6 was measured using a Nikkiso Microtrac MT3300.

[0039] (Preparation of dental water-hardening temporary filling material composition) According to the formulations shown in Table 2, each component was weighed and mixed in a kneading machine to prepare the dental water-hardening temporary filling material compositions for each example and comparative example. The evaluation methods for the dental water-hardening temporary filling material compositions shown in the examples and comparative examples are as follows.

[0040] (Hardening properties of dental water-hardening temporary filling material compositions) A dental water-hardening temporary filling material composition shown in the Examples and Comparative Examples was used to prepare a test specimen by filling a metal ring with an inner diameter of 15 mm and a height of 3 mm. This specimen was immersed in a 37°C constant temperature water bath so that only the bottom surface of the specimen was in contact with the water and left to stand for 30 minutes. After that, the specimen was removed from the constant temperature water bath and the water was removed. A Vicker needle weighing 100 gf and with a diameter of 1 mm was gently lowered from the top surface of the specimen, and the thickness of the hardened layer from the bottom surface of the specimen was measured and defined as the hardening property.

[0041] (Accelerated hardening properties of dental water-hardening temporary filling material compositions) The dental water-hardening temporary filling material compositions shown in the Examples and Comparative Examples were filled into plastic containers and subjected to accelerated curing tests by being left undisturbed for one month in a 50°C environment. After the accelerated curing test, each dental water-hardening temporary filling material composition was cured according to the method described above, and the thickness of the cured layer was measured and defined as the curability after the accelerated curing test.

[0042] (Attenuation rate) The curing decay rate obtained by accelerated testing was calculated using equation (1). (Formula 1) Attenuation rate = 100 × (curability - curability after accelerated test) / (curability)

[0043] (Removability of dental water-hardening temporary filling material compositions after hardening) The dental water-hardening temporary filling material compositions shown in the Examples and Comparative Examples were filled into simulated cavities formed in tooth models, and the models were immersed in water. After standing at room temperature for 3 days, the models were removed, and the moisture on the surface of the hardened dental water-hardening temporary filling material compositions was wiped off. The hardened compositions were removed from the simulated cavities using metal instruments, and a simulation of the removal of the hardened temporary filling material was performed. At this time, compositions that were moderately soft and easily removed were classified as "A", those that were somewhat hard but could be removed without problems were classified as "B", those that were hard and difficult to remove were classified as "C", and those that were very hard and difficult to remove were classified as "D".

[0044] (Evaluation results of the examples and comparative examples) Table 2 shows the evaluation results of the dental water-hardening temporary filling material compositions for each example and comparative example.

[0045] In Example 1, compared to Comparative Example 1, which did not contain component (1) fine particles, an improvement in curability was observed, and the decay rate was low at 24%. Furthermore, the cured composition was moderately soft and could be easily removed. Examples 2 to 5 are compositions prepared by changing the type of fine particles in Example 1 to fine particles 2 to 5. In Example 2, compared to Comparative Example 1, which did not contain component (1) fine particles, an improvement in curability was observed, and the decay rate was low at 15%. Furthermore, the cured composition was moderately soft and could be easily removed. In Examples 3 and 4, an improvement in curability was observed compared to Comparative Example 1, which did not contain component (1) fine particles. The decay rates were remarkably low at 3% and 9%, respectively, and there was almost no decrease in curability. Furthermore, the cured composition was moderately soft and could be easily removed. In Example 5, compared to Comparative Example 1, which did not contain component (1) fine particles, an improvement in curability was observed, and the decay rate was low at 18%. Furthermore, the cured composition was moderately soft and could be easily removed. Example 6 is a composition prepared using gypsum powder 2, instead of the gypsum powder used in Example 3. In Example 6, compared to Comparative Example 1, which did not contain component (1) fine particles, an improvement in curability was observed. The decay rate was remarkably low at 1%, and there was almost no decrease in curability. Furthermore, the cured composition was moderately soft and could be easily removed. Examples 7 to 12 are compositions prepared using organic solvents 1 to 3 and 5 to 7, respectively, instead of the organic solvents used in Example 3. In Examples 7-12, compared to Comparative Example 1, which did not contain component (1) fine particles, an improvement in curability was observed. The decay rate was remarkably low, less than 10%, and there was almost no decrease in curability. Furthermore, the cured composition was moderately soft and could be easily removed. Examples 13 and 14 are compositions prepared using resin 2 or 3 as the resin type in Example 3. In Examples 13 and 14, an improvement in curability was observed compared to Comparative Example 1, which did not contain component (1) fine particles. The decay rates were remarkably low at 2% and 3%, respectively, and there was almost no decrease in curability. Furthermore, the cured composition was moderately soft and could be easily removed. Examples 15 and 16 are compositions prepared by reducing the gypsum powder content in Example 3, increasing the content of other components, and incorporating filler 6. In Example 15, compared to Comparative Example 1, which did not contain component (1) fine particles, an improvement in curability was observed. The decay rate was remarkably low at 5%, and there was almost no decrease in curability. Furthermore, although the cured composition was slightly hard, it could be removed without any problems. In Example 16, compared to Comparative Example 1, which did not contain component (1) fine particles, an improvement in curability was observed. The decay rate was remarkably low at 1%, and there was almost no decrease in curability. Furthermore, the cured composition was moderately soft and could be easily removed. Example 17 is a composition prepared by reducing the gypsum powder content in Example 3 and replacing the reduced amount with filler 6. In Example 17, compared to Comparative Example 1, which did not contain component (1) fine particles, an improvement in curability was observed. The decay rate was remarkably low at 4%, and there was almost no decrease in curability. Furthermore, the cured composition was moderately soft and could be easily removed. Examples 18 and 19 are compositions prepared by increasing the gypsum powder content, decreasing the content of other components, and incorporating filler 6 compared to Example 3. In Example 18, compared to Comparative Example 1, which did not contain component (1) fine particles, an improvement in curability was observed. The decay rate was remarkably low at 9%, and almost no decrease in curability was observed. Furthermore, the cured composition was moderately soft and could be easily removed. In Example 19, compared to Comparative Example 1, which did not contain component (1) fine particles, an improvement in curability was observed, and the decay rate was low at 19%. Furthermore, although the cured composition was somewhat hard, it could be removed without any problems. Comparative Example 1 is a composition that does not contain the fine particles found in Example 1. In Comparative Example 1, the curing properties were lower compared to each example containing component (1) fine particles, and the decay rate was 40% or more. Furthermore, the cured composition was hard and difficult to remove. Comparative Examples 2-6 are compositions prepared by incorporating fillers 1-5, but without the fine particles found in Example 1. In Comparative Examples 2 and 3, the curability was lower compared to each example containing component (1) fine particles, and the decay rate was 40% or more. Furthermore, the cured composition was extremely hard and difficult to remove. In Comparative Examples 4-6, the curability was lower compared to each example containing component (1) fine particles, and the decay rate was 40% or more. Furthermore, the cured composition was hard and difficult to remove.

[0046] [Table 1]

[0047] [Table 2] [Industrial applicability]

[0048] According to the present invention, it is possible to provide a dental water-hardening temporary filling material composition that has high curability, excellent removeability after hardening, and good storage stability without a decrease in curability over time.

Claims

1. Component (1) Fine particles 0.3 to 10% by mass, Component (2) Gypsum powder 20-85% by mass, Component (3) Organic solvent 10 to 25% by mass, and Component (4) Resin 3-15% by mass A dental water-hardening temporary filling material composition comprising: The 50% particle size of the component (1) fine particles is 0.1 μm or less, and the component (1) fine particles are non-water soluble. The aforementioned component (1) fine particles are inorganic particles, The aforementioned component (2) gypsum powder is calcium sulfate hemihydrate, The aforementioned component (3) organic solvent is at least one selected from the group consisting of methanol, ethanol, propanol, isopropyl alcohol, isobutyl alcohol, ethylene glycol, polyethylene glycol, glycerin, ethyl acetate, butyl acetate, glycerin monoacetate, glycerin diacetate, glycerin triacetate, glycerin monomethacrylate, glycerin dimethacrylate, glycerin monostearate, butane, pentane, hexane, benzene, toluene, xylene, methyl ethyl ketone, acetone, diethyl ether, dichloromethane, chloroform, carbon tetrachloride, dimethylpolysiloxane, divinyldimethylpolysiloxane, methyl methacrylate, ethylene glycol dimethacrylate, and hydroxyethyl methacrylate. A dental water-hardening temporary filling material composition characterized in that the component (4) resin is a homopolymer of any of vinyl acetate, vinyl chloride, acrylic acid, maleic acid, and fumaric acid, two or more copolymers selected from the group consisting of vinyl acetate, vinyl chloride, acrylic acid, maleic acid, and fumaric acid, and at least one selected from the group consisting of ethylene vinyl acetate copolymer.

2. The dental water-hardening temporary filling material composition according to claim 1, characterized in that the surface of the fine particles of component (1) is not hydrophobic.

3. The dental water-hardening temporary filling material composition according to claim 1 or 2, wherein the component (3) organic solvent is at least one selected from the group consisting of glycerin, glycerin monoacetate, glycerin diacetate, glycerin triacetate, glycerin monomethacrylate, glycerin dimethacrylate, and glycerin monostearate.

4. The dental water-hardening temporary filling material composition according to any one of claims 1 to 3, wherein the component (4) resin is at least one selected from the group consisting of a homopolymer of vinyl acetate, a homopolymer of vinyl chloride, and a copolymer of vinyl acetate and vinyl chloride.