JP7284607B2 - Dental hydraulic temporary sealing material composition excellent in storage stability - Google Patents

Description

TECHNICAL FIELD The present invention relates to a dental hydraulic temporary sealing material composition having excellent storage stability. More particularly, the present invention relates to a dental hydraulic temporary sealing material composition which is excellent in initial hardening property and capable of reducing deterioration in hardening property over time.

When it is necessary to partially remove the dentin in the oral cavity due to caries, etc., it is generally possible to use a filling material such as a composite resin for dental fillings to restore the removed part of the dentin. Indirect restoration is performed by fabricating a prosthetic device that reproduces the shape of the tooth crown and attaching it to the site where the tooth substance has been removed using dental cement. In addition, when caries has progressed deep into the dentin and bacterial infection is observed in the dental pulp and root canals, root canal treatment such as pulpectomy and removal of infected tooth substance is performed. During these treatments, during the period before the prosthetic device is made, during the follow-up period after pulpectomy and removal of infected tooth material, and during the application of drugs, food may enter the cavity or root canal, or the treated area may become damaged. For the purpose of preventing bacterial infection and sealing drugs that have been inserted into the root canal, temporary sealing is performed to temporarily seal the cavity and root canal using a temporary filling material called temporary dental sealing material. ing.

Against this background, a temporary dental sealing material is required to have good sealing properties. In addition, if the temporary sealing material moves or deforms due to mastication after treatment, the sealing performance may be impaired. It needs to harden quickly and sufficiently in the oral cavity. On the other hand, the temporary dental sealant is a material intended to be removed during the course of treatment, so it must be easily removable without damaging the dentin around the application site.

Temporary sealing materials for dental use include temporary stoppers made of thermoplastic resins, dental cements such as eugenol cements, non-eugenol cements, and zinc phosphate cements, and dental resin-based temporaries containing polymerizable monomers and polymerization initiators. sealing materials, dental hydraulic temporary sealing materials containing calcium sulfate as a main component, and the like.

Temporary stoppers are used by heating the material to soften it and filling it into the cavity. While it is easy to fill and remove, it is a complicated work process because it requires heating and softening every time it is used. In addition, there is a problem that the sealing property of cavities is poor due to large shrinkage at the time of cooling and hardening.

Dental cement is used by kneading powder material and liquid material to form a paste and then filling it. Compared to temporary stoppers, there is less dimensional change during hardening, so it has good sealing properties for cavities. However, kneading the powder material and the liquid material is not only complicated, but also requires skill. Moreover, since the hardened body is hard, there is also a problem that it is difficult to remove.

Dental resin-based temporary sealing materials are hardened by the polymerization reaction of polymerizable monomers, and there are chemical polymerization types that polymerize and harden by mixing powder materials and liquid materials, and light that is excited by light of a specific wavelength. There is a photopolymerization type that polymerizes and cures by irradiating a composition containing a polymerization initiator with light. Since these compounds rapidly cure when the polymerization reaction starts, they have the advantage of being able to function at an early stage after the treatment.

On the other hand, hydraulic temporary sealing materials for dental use are putty-like pastes that are filled into cavities and harden by reacting with moisture such as saliva in the oral cavity, which eliminates the need for heating, kneading (mixing), and light irradiation. It has excellent operability. In addition, since calcium sulfate, which is the main component, has the property of expanding as it hardens, it is also excellent in sealing cavities.

Patent Document 1 discloses vinyl acetate, vinyl chloride, or a copolymer of both 10 to 35% by weight, ethyl alcohol 1 to 10% by weight, glycol acetate 1 to 10% by weight, zinc sulfate cement 5 to 30% by weight, and calcined gypsum. A hydraulic temporary sealing material is disclosed which is characterized by comprising a range of 30 to 65% by weight. It is disclosed that this hydraulic temporary sealing material adheres well to the cavity and can be easily removed from the tooth using an excavator or the like.

Patent Document 2 discloses A) 10 to 90% by weight of calcium sulfate, B) 5 to 40% by weight of vinyl acetate resin, C) 1 to 40% by weight of inorganic filler, D) 1 to 30% of alcohols having a boiling point of 110° C. or higher. % by weight, E) a hydraulic temporary sealing material characterized by comprising 0.001 to 5% by weight of a nonionic surfactant. This hydraulic temporary sealing material adheres to the paste surface without being repelled by water on the tooth surface due to the hydrophilic action of an organic solvent with moderate hydrophilicity and a nonionic surfactant. Moisture permeates and diffuses through the surface, increasing the initial hardening property. Furthermore, the hydrophilic effect is also effective for adhesion to the tooth substance, so the filling property in the oral cavity is improved. As a result, it is disclosed that the sequestering property is improved.

In Patent Document 3, component (1) hydraulic inorganic powder 65.0 to 85.0% by mass, component (2) organic solvent 10.0 to 25.0% by mass, component (3) resin 3.0 to 15.0% by mass. 0% by mass and 0.01 to 10.0% by mass of the component (4) sustained ion-releasing glass are disclosed. It is disclosed that this hydraulic temporary sealing material for dental use has high initial hardening property, and is expected to protect tooth structure such as strengthening tooth structure and inhibiting secondary caries by sustainably releasing various ions including fluoride ion. It is

However, these dental hydraulic temporary sealing materials have the disadvantage that the curability decreases over time. Therefore, when the patient touches or chews with the tongue, the temporary sealing material may move or deform, which may impair the sealing performance. Therefore, there is room for improvement in the storage stability of conventional hydraulic temporary sealing materials for dental use.

Japanese Patent Publication No. 38-2628 Japanese Unexamined Patent Application Publication No. 2011-213608 JP 2018-95573 A

Conventional hydraulic temporary sealing materials for dental use have the disadvantage that even if the initial hardening property is high, the hardening property decreases over time. If the temporary sealing material moves or deforms when the tooth or the opposing teeth come into contact with each other, a gap may be formed between the temporary sealing material and the tooth substance, which may impair the sealing performance. Accordingly, an object of the present invention is to provide a dental hydraulic temporary sealing material composition that reduces the decrease in curability over time.

In order to solve the above-mentioned problems, the inventors conducted intensive studies, and as a result, found that the decrease in curability over time can be reduced by blending quartz powder into the dental hydraulic temporary sealing material composition, and completed the present invention. came to.

That is, the present invention is a dental hydraulic temporary sealing material containing component (1) quartz powder, wherein the 50% particle size of component (1) quartz powder is preferably in the range of 3 to 500 μm. It is more preferable that the content of the quartz powder is in the range of 2.0 to 65.0 wt% with respect to the entire hydraulic temporary sealing material composition for dental use.

Further, the dental hydraulic temporary sealing material composition contains component (2) hydraulic inorganic powder,
Component (3) an organic solvent and component (4) resin are preferably included, and the content of these components (2) to (4) with respect to the entire dental hydraulic temporary sealing material composition is component (2) hydraulic inorganic powder 20.0 to 85.0 wt%,
Component (3) organic solvent 10.0 to 25.0 wt%, and component (4) resin 3.0 to 15.0 wt%
is more preferably included within the range of

Moreover, it is preferable that the component (2) hydraulic inorganic powder contains calcium sulfate. Furthermore, it is preferably calcium sulfate.

Moreover, it is preferable that the component (3) organic solvent contains glycerin or a derivative thereof. Furthermore, it is preferably glycerin or a derivative thereof.

Further, it is preferable that the component (4) resin contains at least one of vinyl acetate or vinyl chloride homopolymers or copolymers. Furthermore, it is preferably composed of at least one of vinyl acetate and vinyl chloride homopolymers and copolymers.

Since the hydraulic temporary sealing material composition for dental use of the present invention can reduce the decrease in curability over time, it stably exhibits high curability even after a long period of time from its production. Therefore, even if the patient's tongue or opposing teeth come into contact with the temporary sealing material applied in the oral cavity, the risk of deterioration of sealing performance due to deformation of the temporary sealing material can be reduced, contributing to the prevention of infection during the temporary sealing period. can.

TECHNICAL FIELD The present invention relates to a dental hydraulic temporary sealing material composition containing quartz powder.
Component (1) Quartz powder is a component that reduces the deterioration of the curability of the dental hydraulic temporary sealing material composition of the present invention over time.
Component (1) quartz powder is a powder mainly composed of crystals of silicon dioxide, and known quartz powder can be used without particular limitation.
Quartz has two types of crystal structures: low-temperature α-quartz and high-temperature β-quartz. In the component (1) quartz powder of the present invention, those having any crystal structure can be used without any limitation, and they can be mixed and used. From the viewpoint of quartz production, it is preferable to use α-quartz powder.

There are no particular restrictions on the method for producing the component (1) quartz powder, and various methods can be used, such as pulverizing and refining minerals mined from nature, or artificially producing amorphous silica by melting or synthesizing methods. It can be produced by crystallizing at Among them, the method of pulverizing and refining minerals mined from nature is preferable from the standpoint of ease of production and cost.

Although there is no particular limitation on the purity of the component (1) quartz powder, it is preferable to use a high-purity one with few impurities. That is, the purity as silicon dioxide is preferably 99.0% or more, more preferably 99.5% or more. In addition, the component (1) quartz powder may contain unavoidable impurities such as components derived from elements existing in the earth's crust such as iron, titanium and manganese, components derived from solvents in the synthesis process, and other components derived from manufacturing equipment. be.

The particle size of the component (1) quartz powder is not particularly limited, but the 50% particle size is preferably in the range of 3 to 500 μm, more preferably in the range of 30 to 300 μm. The particle size distribution range of the component (1) quartz powder is preferably 0.2 to 1000 μm.
The particle shape of the component (1) quartz powder is not particularly limited. be.

Although the content of component (1) quartz powder is not particularly limited, it is preferably 2.0 to 65.0 wt%, more preferably 2.0 to 30.0 wt%, relative to the entire dental hydraulic temporary sealing material composition. is more preferable. If the content of the component (1) quartz powder is less than 2.0 wt %, it may become difficult to exhibit the effect of reducing the decrease in curability over time. In addition, when the content of the component (1) quartz powder exceeds 65.0 wt%, the paste before hardening becomes very hard, which not only deteriorates the operability when filling a cavity or root canal, but also makes the paste of the present invention difficult. In some cases, the hydraulic temporary sealing material composition for dental use cannot be made into a paste.

The component (2) hydraulic inorganic powder is an inorganic powder that reacts and hardens in the presence of water, and is a component that imparts hardening properties to the hydraulic temporary sealing material composition for dental use of the present invention.

Component (2) hydraulic inorganic powder is not particularly limited as long as it is an inorganic powder that reacts and hardens in the presence of water, and known inorganic powders can be used.

Specific examples of the component (2) hydraulic inorganic powder include calcium sulfate, calcium silicate, calcium aluminate, hydraulic alumina and portland cement, among which calcium sulfate is preferred. Examples of calcium sulfate include α-type hemihydrate gypsum and β-type hemihydrate gypsum. Moreover, these may be used in combination of two or more kinds.

Although the particle size of the component (2) hydraulic inorganic powder is not particularly limited, the 50% particle size is preferably in the range of 0.01 to 100 μm, more preferably in the range of 0.1 to 50 μm. The shape of the component (2) hydraulic inorganic powder is not particularly limited, and any shape such as spherical, needle-like, plate-like, pulverized, and scale-like can be used.

Although the content of the component (2) hydraulic inorganic powder is not particularly limited, it is preferably 20.0 to 85.0% by weight, preferably 20.0 to 75.0% by weight, based on the entire dental hydraulic temporary sealing material composition. 0 wt % is more preferable. If the content of the component (2) hydraulic inorganic powder is less than 20.0 wt %, the initial curability may deteriorate. In addition, when the content of the component (2) hydraulic inorganic powder exceeds 85.0 wt%, the paste before hardening becomes very hard, and the operability when filling a cavity or root canal becomes worse. In some cases, the inventive hydraulic temporary sealing material composition cannot be made into a paste.

Component (3), the organic solvent, is a component for making the hydraulic temporary sealant composition for dental use of the present invention into a paste.

The component (3) organic solvent is not particularly limited as long as it is liquid at room temperature and does not react with the component (2) hydraulic inorganic 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.

Specific examples of the component (3) organic solvent include alcohols such as methanol, ethanol, propanol, isopropyl alcohol, isobutyl alcohol, ethylene glycol, low molecular weight polyethylene glycol, glycerin, ethyl acetate, butyl acetate, glycerin monoacetate, glycerin di Fatty acid esters such as acetate, glycerin triacetate, glycerin monomethacrylate, glycerin dimethacrylate, glycerin monostearate, aliphatic hydrocarbons such as butane, pentane, and hexane, aromatic hydrocarbons such as benzene, toluene, and xylene, methyl ethyl ketone, acetone, etc. ketones, ethers such as diethyl ether, alkyl halides such as dichloromethane, chloroform, and carbon tetrachloride, organopolysiloxanes such as dimethylpolysiloxane and divinyldimethylpolysiloxane, methacrylics such as methyl methacrylate, ethylene glycol dimethacrylate, and hydroxyethyl methacrylate. Examples include acid esters, and glycerin such as glycerin, glycerin monoacetate, glycerin diacetate, glycerin triacetate, glycerin monomethacrylate, glycerin dimethacrylate, glycerin monostearate, or a derivative thereof is preferably used. Moreover, these may be used in combination of two or more kinds.

Although the content of the component (3) organic solvent is not particularly limited, it is preferably 10.0 to 25.0 wt%, more preferably 10.0 to 20.0 wt%, relative to the entire dental hydraulic temporary sealing material composition. is more preferable. When the content of the component (3) organic solvent is less than 10.0 wt%, the paste before hardening becomes very hard, which not only deteriorates the operability when filling a cavity or root canal, but also prevents the dental treatment of the present invention. In some cases, the hydraulic temporary sealing material composition cannot be made into a paste. In addition, if the content of the component (3) organic solvent exceeds 25.0 wt%, the paste before hardening becomes soft and sticky, and the operability of filling a cavity or root canal deteriorates. , the initial curability may be poor.

Component (4) resin is a component for imparting plasticity to the dental hydraulic temporary sealing material composition of the present invention and for adjusting the operability of the paste.

The component (4) resin is not particularly limited as long as it is soluble in the component (3) organic solvent, and known resins can be used.

Specific examples of the component (4) resin include homopolymers and copolymers such as vinyl acetate, vinyl chloride, acrylic acid, maleic acid, and fumaric acid, and ethylene-vinyl acetate copolymers. It is preferable to use a homopolymer of vinyl or vinyl chloride, or a copolymer thereof. Moreover, these may be used in combination of two or more kinds.

Although the content of the component (4) resin is not particularly limited, it is preferably 3.0 to 15.0 wt% relative to the entire dental hydraulic temporary sealing material composition, and 5.0 to 10.0 wt%. It is even more preferable to have If the content of the component (4) resin is less than 3.0 wt%, the plasticity of the paste before hardening is lowered, and the operability of filling a cavity or root canal may be deteriorated. Moreover, when the content of the component (4) resin exceeds 15.0 wt%, the initial curability may be adversely affected.

Furthermore, the hydraulic temporary sealing material composition for dental use of the present invention may contain pigments, dyes, reaction modifiers, fillers, excipients, surfactants, antibacterial agents, ion release agents, etc., as long as they do not impair the effects of the present invention. can be added.

Examples and comparative examples of the present invention will be specifically described below, but the present invention is not limited to these examples.

(Details of Components Used for Preparation of Dental Hydraulic Temporary Sealing Material Composition)
Table 1 shows the components used in the preparation of the dental hydraulic temporary sealing material compositions of Examples and Comparative Examples.

The 50% particle size and X-ray diffraction pattern were measured for quartz powders 1 to 3 and two other fillers. Table 2 shows the measurement results of the 50% particle size, and FIGS. 1 to 5 show the measurement results of the X-ray diffraction pattern. The 50% particle size and X-ray diffraction pattern were measured by the following methods.
(50% particle size of quartz powders 1 to 3 and 2 other fillers)
It was measured using Microtrac MT3300 manufactured by Nikkiso Co., Ltd.
(X-ray diffraction patterns of quartz powders 1 to 3 and two other fillers)
It was measured using Rigaku Multiflex. Table 1 shows the measurement results.

(Preparation of dental hydraulic temporary sealing material composition)
According to the formulation shown in Table 1, each component was weighed and kneaded by a kneader to prepare hydraulic temporary sealing material compositions for dental use of each example and comparative example. Evaluation methods for the hydraulic temporary sealant compositions for dental use shown in Examples and Comparative Examples are as follows.
(Initial Curability of Dental Hydraulic Temporary Sealing Material Composition)
A metal ring having an inner diameter of 15 mm and a height of 3 mm was filled with the dental hydraulic temporary sealing material compositions of Examples and Comparative Examples to prepare test pieces. This was immersed in a constant temperature water bath at 37° C. so that only the bottom surface of the test piece was in contact with water, and allowed to stand still for 30 minutes. A Vicat needle weighing 100 gf and having a diameter of 1 mm was gently lowered from the top surface of the test piece to measure the thickness of the hardened layer from the bottom surface of the test piece.
(Curability after accelerated test of dental hydraulic temporary sealing material composition)
An accelerated test was performed by filling a plastic container with the hydraulic temporary sealing material compositions for dental use shown in Examples and Comparative Examples, and allowing the containers to stand in an environment of 70° C. for one month. Curability of each hydraulic temporary sealant for dental use after the accelerated test was evaluated in the same manner as the initial curability.
(Attenuation rate)
Curability attenuation rate by the accelerated test was calculated by the formula (1).
(Formula 1)
Attenuation rate = 100 x (initial curability - curability after accelerated test) / (initial curability)
(Hardness of dental hydraulic temporary sealing material composition)
A simulated cavity formed in a jaw model was filled with the dental hydraulic temporary sealing material compositions of Examples and Comparative Examples using a metal instrument to simulate a temporary sealing treatment. At this time, those having appropriate hardness that facilitated filling into the simulated cavity were evaluated as "appropriate", those that were slightly hard were evaluated as "hard", and those that were somewhat soft were evaluated as "soft".
(Evaluation results of Examples 1 to 7 and Comparative Examples 1 to 3)
Table 1 shows the evaluation results of the dental hydraulic temporary sealing material compositions shown in Examples 1 to 7 and Comparative Examples 1 to 3.
In Example 1, the initial curability was about 1 mm, the curability after the accelerated test was about 0.6 mm, and the attenuation rate was less than 40%. In addition, it had a moderate hardness that facilitates filling the simulated cavity.
Example 2 is a composition prepared by changing the type of component (1) quartz powder in Example 1 to quartz powder 2.
In Example 2, as in Example 1, the initial curability was about 1 mm, the curability after the accelerated test was about 0.6 mm, and the attenuation rate was less than 40%. In addition, it had a moderate hardness that facilitates filling the simulated cavity.
Example 3 is a composition prepared by changing the type of component (1) quartz powder in Example 1 to quartz powder 3.
In Example 3, the initial curability was about 1 mm, the curability after the accelerated test was about 0.5 mm, and the attenuation rate was less than 50%. In addition, it had a moderate hardness that facilitates filling the simulated cavity.
Examples 4 and 5 are compositions prepared by increasing the content of component (1) quartz powder 1 in Example 1 and decreasing the content of the other components.
In Example 4, as in Example 1, the initial curability was about 1 mm, the curability after the accelerated test was about 0.6 mm, and the attenuation rate was less than 40%. In addition, it had a moderate hardness that facilitates filling the simulated cavity.
In Example 5, very high curability was exhibited from the initial stage, and almost no decrease in curability was observed in the accelerated test, but it was found to be somewhat hard when filled into the simulated cavity.
Example 6 is a composition prepared by increasing the content of component (2) hydraulic inorganic powder in Example 1 and decreasing the content of component (3) organic solvent and component (4) resin. .
In Example 6, very high curability was exhibited from the initial stage, and almost no decrease in curability was observed in the accelerated test, but it was found to be somewhat hard when filled into the simulated cavity.
Example 7 is a composition prepared by reducing the content of component (2) hydraulic inorganic powder in Example 1 and increasing the content of component (3) organic solvent and component (4) resin. .
In Example 7, the initial curability was about 0.8 mm, the curability after the accelerated test was about 0.5 mm, and the attenuation rate was less than 40%. In addition, it had a moderate hardness that facilitates filling the simulated cavity.
Comparative Example 1 is a composition that does not contain the component (1) quartz powder in Example 1.
In Comparative Example 1, the initial curability was about 1 mm, the curability after the accelerated test was about 0.4 mm, and the attenuation rate was 60% or more. In addition, it had a moderate hardness that facilitates filling the simulated cavity.
Comparative Example 2 is a composition prepared by changing the component (1) quartz powder in Example 1 to component (5) other filler cristobalite powder.
Comparative Example 3 is a composition prepared by changing the component (1) quartz powder in Example 1 to component (5) other filler, amorphous silica powder.
In Comparative Examples 2 and 3, the initial curability was about 1 mm, the curability after the accelerated test was about 0.4 mm, and the attenuation rate was 60% or more. In addition, it had a moderate hardness that facilitates filling the simulated cavity.

According to the present invention, it is possible to provide a dental hydraulic temporary sealing material composition which is excellent in initial hardening property and can reduce deterioration in hardening property over time.

Claims (8)

Component (1) A dental hydraulic temporary sealing material composition characterized by containing quartz powder. 2. The dental hydraulic temporary sealing material composition according to claim 1, wherein said component (1) quartz powder has a 50% particle size in the range of 3 to 500 μm. Hydraulic temporary sealing for dental use according to claim 1 or 2, wherein the content of the component (1) quartz powder is in the range of 2.0 to 65.0 wt% with respect to the entire composition of hydraulic temporary sealing material for dental use. wood composition. The hydraulic temporary sealing material composition for dental use according to any one of claims 1 to 3 comprises component (2) a hydraulic inorganic powder,
A dental hydraulic temporary sealing material composition comprising component (3) an organic solvent and component (4) a resin. The content of the components (2) to (4) is 20.0 to 85.0 wt% of the component (2) hydraulic inorganic powder with respect to the entire dental hydraulic temporary sealing material composition,
Component (3) organic solvent 10.0 to 25.0 wt%, and component (4) resin 3.0 to 15.0 wt%
The dental hydraulic temporary sealing material composition according to any one of claims 1 to 4, comprising 6. The dental hydraulic temporary sealing material composition according to claim 4, wherein the component (2) the hydraulic inorganic powder contains calcium sulfate. 7. The method according to any one of claims 4 to 6, wherein the component (3) organic solvent contains at least one of glycerin, glycerin monoacetate, glycerin diacetate, glycerin triacetate, glycerin monomethacrylate, glycerin dimethacrylate and glycerin monostearate. The dental hydraulic temporary sealing material composition described. The dental hydraulic temporary sealing material according to any one of claims 4 to 7, wherein the component (4) resin contains at least one selected from vinyl acetate or vinyl chloride homopolymers and copolymers thereof. Composition.