WO2023106519A1 - Dental impression material composition with excellent bubble control - Google Patents
Dental impression material composition with excellent bubble control Download PDFInfo
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- WO2023106519A1 WO2023106519A1 PCT/KR2022/007580 KR2022007580W WO2023106519A1 WO 2023106519 A1 WO2023106519 A1 WO 2023106519A1 KR 2022007580 W KR2022007580 W KR 2022007580W WO 2023106519 A1 WO2023106519 A1 WO 2023106519A1
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/90—Compositions for taking dental impressions
Definitions
- the present specification relates to a dental impression material composition having excellent bubble control.
- Impression materials are materials used when replicating intraoral shapes, and accuracy is important.
- an addition polymerization type silicone impression material that can accurately reproduce intraoral tissue and has little deformation and excellent mechanical strength is most popularly used.
- Recent addition polymerization type silicone impression materials include adding catalysts such as platinum and palladium capable of collecting hydrogen gas or including a waiting time of 30 minutes or more before pouring gypsum.
- catalysts such as platinum and palladium capable of collecting hydrogen gas or including a waiting time of 30 minutes or more before pouring gypsum.
- a waiting time of 30 minutes or more may cause inconvenience to the user, and hydrogen gas collection using a catalyst has a problem in that it is difficult to reliably solve the above problems due to limitations in the contact area and reaction rate with the catalyst. It is necessary to develop an impression material composition capable of minimizing the side effects caused by this.
- the description of the present specification is to solve the above-mentioned problems of the prior art, and one object of the present specification is to provide an impression material composition capable of solving the bubble problem while securing an appropriate curing time.
- V polydimethylsiloxane terminal is substituted with a vinyl group; And an organohydrogenpolysiloxane having a Si-H content of 3 to 4.5 mmol; a dental impression material composition comprising a is provided.
- the content of the V polydimethylsiloxane having the terminal substituted with a vinyl group may be 30 to 60 parts by weight, and the content of the organohydrogenpolysiloxane may be 5 to 10 parts by weight.
- the V polydimethylsiloxane whose terminal is substituted with a vinyl group, the first V polydimethylsiloxane having a 25 ° C viscosity of 100 to 500 cP, and the second V polydimethylsiloxane having a 25 ° C viscosity of 750 to 1500 cP Siloxane and 25 °C viscosity may include a third V polydimethylsiloxane of 5000 ⁇ 25000cP.
- the content of the first V polydimethylsiloxane is 10 to 15 parts by weight
- the content of the second V polydimethylsiloxane is 20 to 25 parts by weight
- the third V polydimethylsiloxane The content of may be 10 to 15 parts by weight.
- the ratio (Si-H/vinyl) of the vinyl content of the polydimethylsiloxane whose terminal is substituted with a vinyl group and the Si-H content of the organohydrogenpolysiloxane may be 1.5 to 3.
- the bubble area of the gypsum model cured in the dental impression material composition may be 20% or less.
- it may further include at least one selected from the group consisting of polydimethylsiloxane, a filler, a catalyst, and a curing retardant.
- 0 to 1 part by weight of the polydimethylsiloxane, 40 to 70 parts by weight of the filler, 0 to 2 parts by weight of the catalyst, and 0 to 1 part by weight of the curing retardant may be included.
- the catalyst may be platinum-based or palladium-based.
- the filler may be at least one selected from the group consisting of an inorganic filler and an amorphous synthetic filler.
- the impression material composition may have a curing time of 2 to 3 minutes at 37 ° C.
- FIG. 1 is a photograph of bubbles formed from an impression material composition according to an embodiment and a comparative example of the present specification.
- FIG. 2 is a graph showing the curing time of impression material compositions according to one embodiment and a comparative example of the present specification.
- FIG 3 is a graph showing the curing time according to accelerated aging of impression material compositions according to one embodiment and a comparative example of the present specification.
- a dental impression material composition according to one aspect of the present specification includes V polydimethylsiloxane substituted with a vinyl group at the terminal; and an organohydrogenpolysiloxane having a Si-H content of 3 to 4.5 mmol/g.
- V polydimethylsiloxane in which the terminal is substituted with a vinyl group may be represented by Formula 1 below.
- n may be 1 to 1000, but is not limited thereto. However, outside the above range, the viscosity increases excessively, and it may be difficult to implement desired characteristics.
- the impression material composition containing the V polydimethylsiloxane has excellent crosslinking properties and is advantageous in obtaining an impression through gypsum curing.
- the organohydrogenpolysiloxane may have a Si-H structure and react with the vinyl group of the V-polydimethylsiloxane. Hydrogen of the Si-H structure is added-polymerized with the double bond of the vinyl group to form a three-dimensional network structure, thereby suppressing relative movement between polymer chains and improving the long-term storage property of the impression material.
- the content of the Si-H structure may be controlled to 3 to 4.5 mmol/g.
- the Si-H structure is 3mmol/g, 3.1mmol/g, 3.2mmol/g, 3.3mmol/g, 3.4mmol/g, 3.5mmol/g, 3.6mmol/g , 3.7mmol/g, 3.8mmol/g, 3.9mmol/g, 4mmol/g, 4.1mmol/g, 4.2mmol/g, 4.3mmol/g, 4.4mmol/g, 4.5mmol/g or two of these values Those having a content in the range between can be used.
- a commercially available product can be used as the organohydrogenpolysiloxane, and the content of the Si-H structure can be specified according to the Si-H value of the commercially available product.
- the curing time may excessively increase, and if it exceeds 4.5 mmol / g, hydrogen gas is generated excessively, making it difficult to improve the bubble area even by the above method. .
- organohydrogenpolysiloxane may be represented by Formula 2 below.
- a dental impression material composition containing 30 to 60 parts by weight of the V polydimethylsiloxane whose terminal is substituted with a vinyl group and 5 to 10 parts by weight of the organohydrogenpolysiloxane can be used.
- the content of the V polydimethylsiloxane whose terminal is substituted with a vinyl group is, for example, 30 parts by weight, 32 parts by weight, 34 parts by weight, 36 parts by weight, 38 parts by weight, 40 parts by weight, 42 parts by weight, 44 parts by weight parts, 46 parts, 48 parts, 50 parts, 52 parts, 54 parts, 56 parts, 58 parts, 60 parts, or a range between two of these values. If the content of the V-polydimethylsiloxane is less than 30 parts by weight, the crosslinking time may be excessively long or additives such as fillers may easily aggregate, making it difficult to realize the level of elasticity required for the impression material. If the content of the V-polydimethylsiloxane exceeds 60 parts by weight, crosslinking is insufficient, resulting in deterioration in storage stability due to generation of air bubbles, and the shape may collapse when the impression body is taken.
- the content of the organohydrogenpolysiloxane is, for example, 5 parts by weight, 5.5 parts by weight, 6.0 parts by weight, 6.5 parts by weight, 7.0 parts by weight, 7.5 parts by weight, 8 parts by weight, 8.5 parts by weight, 9.0 parts by weight, 9.5 parts by weight, 10 parts by weight or a range between any two of these values. If the content of the organohydrogenpolysiloxane is out of the above range, crosslinking may be insufficiently performed, making it difficult to maintain the shape upon taking an impression body, or the crosslinking density may excessively increase, resulting in insufficient elasticity of the impression material.
- Viscosity in the present specification means a value measured at 25 °C with a viscometer. For example, it may be a value measured at a shear rate of 0.1 to 50 1/s by putting a sample of about 20 g in a cup & bob attachment at 25 ° C using an AR 2000ex rotational rheometer from TA Instruments.
- V polydimethylsiloxane One of the physical properties for confirming the characteristics of V polydimethylsiloxane is viscosity at 25°C.
- the V polydimethylsiloxane in which the terminal is substituted with a vinyl group one having a viscosity of 100 to 25000 cP at 25° C. may be used.
- the viscosity at 25 ° C. of the polydimethylsiloxane substituted with a vinyl group at the terminal is 100 cP, 150 cP, 200 cP, 250 cP, 300 cP, 350 cP, 400 cP, 450 cP, 500 cP, 550 cP, 600 cP, 650 cP, 700 cP, and 750 cP.
- the physical properties of the impression material can be more precisely controlled by using polydimethylsiloxanes having various viscosities together.
- the V polydimethylsiloxane whose terminal is substituted with a vinyl group includes 10 to 15 parts by weight of the first V polydimethylsiloxane having a viscosity of 100 to 500 cP at 25 ° C. and a second poly polydimethylsiloxane having a viscosity of 750 to 1500 cP at 25 ° C. 20 to 25 parts by weight of dimethylsiloxane and 10 to 15 parts by weight of 3 V polydimethylsiloxane having a viscosity of 5000 to 25000 cP at 25°C.
- the first V polydimethylsiloxane is, for example, 10 parts by weight, 10.5 parts by weight, 11 parts by weight, 11.5 parts by weight, 12 parts by weight, 12.5 parts by weight, 13 parts by weight, 13.5 parts by weight, 14 parts by weight, 14.5 parts by weight, 15 parts by weight, it may be included in the content of the range between the two values.
- the first V-polydimethylsiloxane is a low molecular weight component having a relatively low viscosity, and may impart fluidity to the impression material and increase crosslinking density.
- the second V polydimethylsiloxane is, for example, 20 parts by weight, 20.5 parts by weight, 21 parts by weight, 21.5 parts by weight, 22 parts by weight, 22.5 parts by weight, 23 parts by weight, 23.5 parts by weight, 24 parts by weight, It may be included in an amount of 24.5 parts by weight, 25 parts by weight or a range between these two values.
- the second V-polydimethylsiloxane is a component having a moderate viscosity, and may impart overall characteristics of the dental impression material composition.
- the 3-V polydimethylsiloxane is, for example, 10 parts by weight, 10.5 parts by weight, 11 parts by weight, 11.5 parts by weight, 12 parts by weight, 12.5 parts by weight, 13 parts by weight, 13.5 parts by weight, 14 parts by weight, It may be included in an amount of 14.5 parts by weight, 15 parts by weight or a range between these two values.
- the third V polydimethylsiloxane is a high molecular weight component having high viscosity, and can reduce the crosslinking density of the impression material.
- the ratio (Si-H/vinyl) of the Si-H content of the organohydrogenpolysiloxane and the vinyl content of the V-polydimethylsiloxane having the terminal substituted with a vinyl group may be 1.5 to 3.
- Si-H/vinyl can be 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3.0 or a range between two of these values. can If it is out of the above range, crosslinking may take an excessively long time, or air bubbles may be excessively generated on the surface when taking an impression.
- problems caused by hydrogen gas are improved while maintaining curing characteristics and storage stability of the dental impression material composition by adjusting the ratio of the first to third V polydimethylsiloxanes and the organohydrogenpolysiloxane. can do.
- the Si-H structure of the organohydrogenpolysiloxane can react with the vinyl group at the end of the V-polydimethylsiloxane
- the ratio of the content of the Si-H structure and the vinyl content of the V-polydimethylsiloxane is adjusted to obtain the impression material composition.
- the crosslinking density can be adjusted. If the crosslinking density of the impression material composition is excessively low, the tensile strength may be lowered or the impression material may be easily torn, and if the crosslinking density is excessively high, elasticity may be insufficient.
- the dental impression material composition includes V polydimethylsiloxane whose terminal is substituted with a vinyl group as a main component, but the Si-H content of the organohydrogenpolysiloxane is adjusted, and the viscosity is By controlling the ratio between different V polydimethylsiloxanes, storage stability, crosslinking density, and suppression of hydrogen gas formation can be achieved.
- the crosslinking density of the impression material composition may increase and the amount of hydrogen gas generated may increase.
- the crosslinking density of the impression material composition may decrease and the amount of hydrogen gas generated may decrease.
- the first V polydimethylsiloxane can increase the fluidity of the impression material composition, and the third V polydimethylsiloxane can improve storage stability of the impression material composition.
- bubble area is the area (%) of the area (%) in which bubbles are generated at the interface with the impression material after preparing five specimens of 30 mm wide ⁇ 30 mm long by pouring gypsum into the impression material composition and curing it. can mean average.
- storage stability may mean that the rate of change in the characteristics or shape of the impression material composition is small as the storage period is prolonged.
- the dental impression material composition can suppress the formation of air bubbles on the surface of the impression body by hydrogen gas generated in the crosslinking reaction.
- the bubble area of the gypsum model cured in the impression material composition may be 20% or less, for example, the bubble area is 20% or less, 19% or less, 18% or less, 17% or less, 16% or less, 15% or less, 14% or less, 13% or less, 12% or less, 11% or less, 10% or less, 9% or less, 8% or less, 7% or less, 6% or less, 5% or less, 4% or less, 3% or less, 2% Or less, 1% or less, 0% (if less than 1%, it is considered that no bubbles are generated), or a range between two values thereof, but is not limited thereto. If the bubble area of the dental composition exceeds the above range, a lot of bubbles are generated during impression taking using the impression material composition, and the accuracy of the impression body model may deteriorate.
- the dental impression material composition may further include at least one selected from the group consisting of polydimethylsiloxane, a chain extender, a silicone-based filler, a catalyst, and a curing retardant.
- polydimethylsiloxane 0 to 1 part by weight of the polydimethylsiloxane, 0 to 1 part by weight of the chain extender, 40 to 70 parts by weight of the silicone-based filler, 0 to 2 parts by weight of the catalyst, and 0 to 1 part by weight of the curing retardant.
- 0 to 1 part by weight of the polydimethylsiloxane 0 to 1 part by weight of the chain extender, 40 to 70 parts by weight of the silicone-based filler, 0 to 2 parts by weight of the catalyst, and 0 to 1 part by weight of the curing retardant.
- the addition of each component is optional, it may mean that it is not included in the case of 0 parts by weight.
- the polydimethylsiloxane which is not substituted with a vinyl end, may serve as an antifoaming agent.
- the polydimethylsiloxane may have a viscosity of 100 to 1000 cP at 25° C., but is not limited thereto.
- the content of the polydimethylsiloxane is, for example, 0 parts by weight, 0.001 parts by weight, 0.003 parts by weight, 0.005 parts by weight, 0.007 parts by weight, 0.01 parts by weight, 0.02 parts by weight, 0.03 parts by weight, 0.04 parts by weight, 0.05 parts by weight.
- the filler may be at least one selected from the group consisting of inorganic fillers and amorphous synthetic fillers.
- inorganic filler and the amorphous synthetic filler are used in combination, their weight ratio may be 40 to 60:3 to 10, respectively.
- the inorganic filler is added to realize the strength and excellent storage stability required for impression materials, and cristobalite, crystalline natural silica, barium aluminum silicate, strontium aluminum silicate, barium silicate glass, strontium silicate glass, borate aluminum silicate glass , Phosphate aluminum silicate glass, fluoroaluminosilicate glass, glass beads, calcium silicate, zirconium silicate and sodium aluminum silicate may include at least one selected from the group consisting of.
- the amorphous synthetic filler may serve as a reinforcing agent.
- the amorphous synthetic filler may be at least one selected from the group consisting of fumed silica, silica gel, precipitated silica, silica sol, and silicic acid.
- the content of the filler may be 40 to 70 parts by weight.
- the content of the filler is 40 parts by weight, 42 parts by weight, 44 parts by weight, 46 parts by weight, 48 parts by weight, 50 parts by weight, 52 parts by weight, 54 parts by weight, 56 parts by weight, 58 parts by weight, 60 parts by weight parts by weight, 62 parts by weight, 64 parts by weight, 66 parts by weight, 68 parts by weight, 70 parts by weight or a range between two of these values. If the content of the filler is less than 40 parts by weight, long-term storage may be difficult because it is not sufficiently dispersed in the impression material composition, and if it exceeds 70 parts by weight, strain may increase during long-term storage.
- the impression material composition may include cristobalite silica and fumed silica.
- Cristobalite silica is one of the silicate minerals, and it belongs to the tetragonal system at higher temperatures and the tetragonal system at lower temperatures around 268 ° C.
- the tetragonal one is called ⁇ -cristobalite and the tetragonal one is called ⁇ -cristobalite, and it may be common to use ⁇ -cristobalite as a filler.
- Fumed silica forms a three-dimensional structural bond, so when shear force acts on it, the mutual bond between silica molecules is easily broken, and it has a thixotropy property that changes into a sol-like form in a liquid state. Therefore, the flowability of the composition containing the fumed silica can be improved.
- Particles of fumed silica used as a filler are generally nano-sized and may be spherical. For example, fumed silica having an average particle size of 1 to 600 nm and a surface area of 5 to 600 m 2 /g may be used.
- the catalyst may be platinum-based or palladium-based.
- the catalyst may be platinum, a platinum compound, palladium, or a palladium compound.
- the catalyst not only shortens the reaction time, but also serves as a hydrogen adsorbent.
- the role as a hydrogen absorbent means to adsorb hydrogen gas generated during the manufacture of an impression body by pouring gypsum into the impression material composition, and as a result, it can help to obtain an accurate impression body model by suppressing the generation of air bubbles.
- the catalyst for example, 0 parts by weight, 0.001 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight Part, 1.0 part, 1.1 part, 1.2 part, 1.3 part, 1.4 part, 1.5 part, 1.6 part, 1.7 part, 1.8 part, 1.9 part, 2.0 part, or two of these It may be included in an amount in the range between. If the content of the catalyst exceeds 2 parts by weight, curing is performed excessively quickly, resulting in difficulty in obtaining an impression or suppression of bubble formation.
- the curing retardant may be used to control the working time.
- the curing retardant for example, 0 parts by weight, 0.001 parts by weight, 0.003 parts by weight, 0.005 parts by weight, 0.007 parts by weight, 0.01 parts by weight, 0.02 parts by weight, 0.03 parts by weight, 0.04 parts by weight, 0.05 parts by weight, 0.06 parts by weight, 0.07 parts by weight, 0.08 parts by weight, 0.09 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight part, 1.0 parts by weight or a range between two values thereof. If the content of the curing retardant exceeds 1 part by weight, it may act as an impurity.
- the shape of the dentition that is, the impression relief
- the shape of the dentition can be obtained by press-contacting the dentition and the base and maintaining the dentition until hardening.
- An impression body can be manufactured by pouring a plaster model into the impression relief and then curing it. Therefore, it is necessary to adjust the curing time to improve the usability of the impression material.
- the impression material composition 37 °C curing time may be 2 to 3 minutes, for example, 2 minutes, 2 minutes 10 seconds, 2 minutes 20 seconds, 2 minutes 30 seconds, 2 minutes 40 seconds, 2 minutes 50 seconds, 3 minutes or It may be a range between two of these values. If the curing time is out of the above range, the impression material is hardened before application to the oral cavity, or a push phenomenon occurs during curing, making it difficult to obtain an accurate impression.
- the impression material composition may further include at least one selected from the group consisting of a surfactant, an antioxidant, an anti-foaming agent, and a pigment, if necessary.
- a surfactant 0 to 2 parts by weight of the surfactant, 0 to 1 part by weight of the antioxidant, 0 to 1 part by weight of the defoaming agent, and 0 to 1 part by weight of the pigment may be included.
- the surfactant can improve wettability with teeth (the ability of each contacting surface to maintain contact) and reduce the amount of hydrogen gas generated.
- the surfactant is, for example, 0 parts by weight, 0.001 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight 1.0 parts by weight, 1.1 parts by weight, 1.2 parts by weight, 1.3 parts by weight, 1.4 parts by weight, 1.5 parts by weight, 1.6 parts by weight, 1.7 parts by weight, 1.8 parts by weight, 1.9 parts by weight, 2.0 parts by weight or two of these It can be included in the content of the range between the values. Outside of the above range, it may be difficult to control air bubbles through hydrogen generation, and it may be difficult to obtain an accurate impression body model due to low wettability with teeth when using the product.
- the surfactant is composed of a nonionic surfactant, sodium lauryl sulfate, monoglyceride sulfate, lauroyl sarcosine sodium, sucrose fatty acid ester, lauric acid diethanol amide, polyoxyethylene, trisiloxane ethoxylate, and fluorine-based surfactant. It may include one or more selected from the group, but is not limited thereto.
- the antioxidant a conventional antioxidant may be used to maintain physical properties for a long period of time.
- the antioxidant is, for example, 0 parts by weight, 0.001 parts by weight, 0.003 parts by weight, 0.005 parts by weight, 0.007 parts by weight, 0.01 parts by weight, 0.02 parts by weight, 0.03 parts by weight, 0.04 parts by weight, 0.05 parts by weight, 0.06 parts by weight parts by weight, 0.07 parts by weight, 0.08 parts by weight, 0.09 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight , 1.0 parts by weight or a range between these two values. If it is out of the above range, it may act as an impurity and it may be difficult to control the generation of bubbles and adjust the curing time.
- the defoaming agent for example, 0 parts by weight, 0.001 parts by weight, 0.003 parts by weight, 0.005 parts by weight, 0.007 parts by weight, 0.01 parts by weight, 0.02 parts by weight, 0.03 parts by weight, 0.04 parts by weight, 0.05 parts by weight, 0.06 parts by weight parts by weight, 0.07 parts by weight, 0.08 parts by weight, 0.09 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight , 1.0 parts by weight or may be included in the content of the range between the two values. If it is out of the above range, it may act as an impurity, making it difficult to store for a long time, or may not exhibit the effect of removing air bubbles.
- the pigment may be added to easily distinguish the color of the oral cavity when the impression material composition is applied in the oral cavity.
- the pigment is, for example, 0 parts by weight, 0.001 parts by weight, 0.003 parts by weight, 0.005 parts by weight, 0.007 parts by weight, 0.01 parts by weight, 0.02 parts by weight, 0.03 parts by weight, 0.04 parts by weight, 0.05 parts by weight, 0.06 parts by weight 0.07 parts by weight, 0.08 parts by weight, 0.09 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight, It may be included in an amount of 1.0 parts by weight or a range between these two values. If it is out of the above range, it may act as an impurity.
- the first polydimethylsiloxane, the second polydimethylsiloxane, and the third polydimethylsiloxane were mixed according to the Si-H/Vinyl values in Table 1 below, and the Si-H content in Table 1 below (manufacturer, Evonik) Organohydrogenpolysiloxane 7 parts by weight, polydimethylsiloxane 0.05 parts by weight, cristobalite silica 50 parts by weight, fumed silica 6.5 parts by weight, platinum catalyst 1 parts by weight, curing retardant 0.5 parts by weight, surfactant 1 weight part 0.5 part by weight of antioxidant, 0.5 part by weight of anti-foaming agent, and 0.5 part by weight of pigment were mixed using a vacuum stirrer, placed in an automixing cartridge, and rotated for 5 minutes at a rotational speed of 100 rpm using a centrifuge.
- a post impression material composition was prepared.
- Example 1 Example 2
- Bubble area (% Area) 32.5 1.2 14.4 - 37°C curing time 1 minute 33 seconds 2 minutes 2 seconds 1 minute 57 seconds 2 minutes 22 seconds
- the specimens manufactured using the impression material compositions of Examples showed a surface area of less than 15, ensuring the accuracy of the impression body model, and the curing time was 1 minute 50 It did not harden in a short time of more than a second, so it was excellent for taking accurate impressions.
- the specimen of Example 3 in which the Si-H content of the organohydrogenpolysiloxane was 3.2 mmol/g, did not generate bubbles, and the curing time was also 2 minutes and 22 seconds, indicating an appropriate curing time, not too short or long. This is considered to be due to the minimization of the role of hydrogen gas due to the optimum crosslinking chain length and crosslinking ratio through the control of Si—H content and Si—H/vinyl.
- the curing time in the oral cavity was measured using a rheometer.
- the accelerated aging result means the result of the storage stability of the impression material, and the smaller the change rate, the more stable and long-term storage is possible.
- Example 1 Example 2
- Example 3 Curing time after 0 years of acceleration 1 minute 33 seconds 2 minutes 2 seconds 1 minute 57 seconds 2 minutes 22 seconds Curing time after 1 year of acceleration 2 minutes 41 seconds 2 minutes 18 seconds 2 minutes 27 seconds 2 minutes 37 seconds Curing time after 2 years of acceleration 3 minutes 25 seconds 2 minutes 30 seconds 3 minutes 50 seconds 2 minutes 43 seconds Time of change (acceleration 2 years - acceleration 0 years) 1 minute 52 seconds 28 seconds 1 minute 53 seconds 21 seconds rate of change 120% 23% 97% 15%
- the impression material composition of Example showed a change rate of less than 100%, and in particular, the change rate of Example 3, which had the smallest surface area in FIG. 2, was 15%, which was the most excellent. There was no significant change despite storage, indicating excellent storage stability.
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Abstract
Disclosed is a dental impression composition comprising: vinyl group-terminated V polydimethylsiloxane; and organohydrogen polysiloxane having a Si-H content of 3-4.5mmol/g.
Description
본 명세서는 기포제어가 우수한 치과용 인상재 조성물에 관한 것이다. The present specification relates to a dental impression material composition having excellent bubble control.
인상재는 구강 내 형상을 복제할 때 사용하는 재료로서 정확성이 중요하다. 근래에는 구강 내 조직을 정확하게 재현할 수 있으면서 변형이 적고 기계적 강도가 우수한 부가중합형 실리콘 인상재가 가장 대중적으로 사용되고 있다.Impression materials are materials used when replicating intraoral shapes, and accuracy is important. In recent years, an addition polymerization type silicone impression material that can accurately reproduce intraoral tissue and has little deformation and excellent mechanical strength is most popularly used.
하지만 이런 부가중합형 실리콘 인상재는 많은 장점에도 불구하고 인상재를 경화시키는 재료 중 가교제라는 오르가노하이드로겐폴리실록산과 말단이 비닐기로 치환된 폴리다이메틸실록산이 반응하면서 부산물로 수소기체가 발생하게 된다. 이러한 수소기체로 인해 경화 후 구강 모델을 만들기 위해 석고를 붓게 되면 부정확한 모델을 만들게 되거나, 장기 보관에 부적합할 수 있다.However, in spite of many advantages of this addition polymerization type silicone impression material, hydrogen gas is generated as a by-product as organohydrogenpolysiloxane, which is a crosslinking agent, and polydimethylsiloxane whose terminal is substituted with a vinyl group react among the materials for curing the impression material. When gypsum is poured to make an oral model after curing due to such hydrogen gas, an inaccurate model may be made or it may be unsuitable for long-term storage.
최근 부가중합형 실리콘 인상재는 상기와 같은 문제점을 최소화하기 위해 수소가스를 포집할 수 있는 백금 및 팔라듐 등의 촉매를 첨가하거나 석고를 붓기 전 30분 이상의 대기시간을 포함하도록 하고 있다. 다만, 30분 이상의 대기시간은 사용자의 불편함을 초래할 수 있으며, 촉매를 이용한 수소가스 포집은 촉매와의 접촉면적과 반응속도의 한계로 전술한 문제를 확실하게 해결하기 힘든 문제가 있어, 수소가스로 인한 부작용을 최소화할 수 있는 인상재 조성물을 개발하는 것이 필요하다.In order to minimize the above-described problems, recent addition polymerization type silicone impression materials include adding catalysts such as platinum and palladium capable of collecting hydrogen gas or including a waiting time of 30 minutes or more before pouring gypsum. However, a waiting time of 30 minutes or more may cause inconvenience to the user, and hydrogen gas collection using a catalyst has a problem in that it is difficult to reliably solve the above problems due to limitations in the contact area and reaction rate with the catalyst. It is necessary to develop an impression material composition capable of minimizing the side effects caused by this.
본 명세서의 기재사항은 전술한 종래 기술의 문제점을 해결하기 위한 것으로, 본 명세서의 일 목적은 적절한 경화 시간을 확보하면서도 기포문제를 해결할 수 있는 인상재 조성물을 제공하는 것이다.The description of the present specification is to solve the above-mentioned problems of the prior art, and one object of the present specification is to provide an impression material composition capable of solving the bubble problem while securing an appropriate curing time.
일 측면에 따르면 말단이 비닐기로 치환된 V폴리다이메틸실록산; 및 Si-H 함량이 3~4.5mmol인 오르가노하이드로겐폴리실록산;을 포함하는, 치과용 인상재 조성물이 제공된다.According to one aspect V polydimethylsiloxane terminal is substituted with a vinyl group; And an organohydrogenpolysiloxane having a Si-H content of 3 to 4.5 mmol; a dental impression material composition comprising a is provided.
일 실시예에 있어서, 상기 말단이 비닐기로 치환된 V폴리다이메틸실록산의 함량이 30~60중량부이고, 상기 오르가노하이드로겐폴리실록산의 함량이 5~10중량부일 수 있다.In one embodiment, the content of the V polydimethylsiloxane having the terminal substituted with a vinyl group may be 30 to 60 parts by weight, and the content of the organohydrogenpolysiloxane may be 5 to 10 parts by weight.
일 실시예에 있어서, 상기 말단이 비닐기로 치환된 V폴리다이메틸실록산은, 25℃ 점도가 100~500cP인 제1 V폴리다이메틸실록산, 25℃ 점도가 750~1500cP인 제2 V폴리다이메틸실록산 및 25℃ 점도가 5000~25000cP인 제3 V폴리다이메틸실록산을 포함할 수 있다.In one embodiment, the V polydimethylsiloxane whose terminal is substituted with a vinyl group, the first V polydimethylsiloxane having a 25 ° C viscosity of 100 to 500 cP, and the second V polydimethylsiloxane having a 25 ° C viscosity of 750 to 1500 cP Siloxane and 25 ℃ viscosity may include a third V polydimethylsiloxane of 5000 ~ 25000cP.
일 실시예에 있어서, 상기 제1 V폴리다이메틸실록산의 함량은 10~15중량부이고, 상기 제2 V폴리다이메틸실록산의 함량은 20~25중량부이며, 상기 제3 V폴리다이메틸실록산의 함량은 10~15중량부일 수 있다.In one embodiment, the content of the first V polydimethylsiloxane is 10 to 15 parts by weight, the content of the second V polydimethylsiloxane is 20 to 25 parts by weight, the third V polydimethylsiloxane The content of may be 10 to 15 parts by weight.
일 실시예에 있어서, 상기 말단이 비닐기로 치환된 폴리다이메틸실록산의 비닐 함량 및 상기 오르가노하이드로겐폴리실록산의 Si-H 함량의 비(Si-H/비닐)가 1.5~3일 수 있다.In one embodiment, the ratio (Si-H/vinyl) of the vinyl content of the polydimethylsiloxane whose terminal is substituted with a vinyl group and the Si-H content of the organohydrogenpolysiloxane may be 1.5 to 3.
일 실시예에 있어서, 상기 치과용 인상재 조성물에 경화시킨 석고 모형의 기포면적이 20% 이하일 수 있다.In one embodiment, the bubble area of the gypsum model cured in the dental impression material composition may be 20% or less.
일 실시예에 있어서, 폴리다이메틸실록산, 필러, 촉매제 및 경화지연제로 이루어진 군에서 선택된 하나 이상을 더 포함할 수 있다.In one embodiment, it may further include at least one selected from the group consisting of polydimethylsiloxane, a filler, a catalyst, and a curing retardant.
일 실시예에 있어서, 상기 폴리다이메틸실록산 0~1중량부, 상기 필러40~70중량부, 촉매제 0~2중량부 및 경화지연제 0~1중량부를 포함할 수 있다.In one embodiment, 0 to 1 part by weight of the polydimethylsiloxane, 40 to 70 parts by weight of the filler, 0 to 2 parts by weight of the catalyst, and 0 to 1 part by weight of the curing retardant may be included.
일 실시예에 있어서, 상기 촉매제는 백금계 또는 팔라듐계일 수 있다.In one embodiment, the catalyst may be platinum-based or palladium-based.
일 실시예에 있어서, 상기 필러는 무기 필러 및 비정질 합성 필러로 이루어진 군에서 선택된 하나 이상일 수 있다.In one embodiment, the filler may be at least one selected from the group consisting of an inorganic filler and an amorphous synthetic filler.
일 실시예에 있어서, 상기 인상재 조성물은 37℃ 경화 시간이 2~3분일 수 있다.In one embodiment, the impression material composition may have a curing time of 2 to 3 minutes at 37 ° C.
본 명세서의 일 측면에 따르면, 부가중합형 실리콘 인상재 제조 시 발생하는 수소가스의 발생을 최소화하여 인상체의 모델의 정확성을 확보하고, 적절한 경화시간을 확보할 수 있다.According to one aspect of the present specification, it is possible to secure the accuracy of the impression body model and secure an appropriate curing time by minimizing the generation of hydrogen gas generated during the manufacture of an addition polymerization type silicone impression material.
본 명세서의 일 측면의 효과는 상기한 효과로 한정되는 것은 아니며, 본 명세서의 상세한 설명 또는 청구범위에 기재된 구성으로부터 추론 가능한 모든 효과를 포함하는 것으로 이해되어야 한다.Effects of one aspect of the present specification are not limited to the above effects, and should be understood to include all effects that can be inferred from the configuration described in the detailed description or claims of this specification.
도 1은 본 명세서의 일 실시예 및 비교예에 따른 인상재 조성물로부터 형성된 기포를 촬영한 사진이다.1 is a photograph of bubbles formed from an impression material composition according to an embodiment and a comparative example of the present specification.
도 2는 본 명세서의 일 실시예 및 비교예에 따른 인상재 조성물의 경화 시간을 나타낸 그래프이다.2 is a graph showing the curing time of impression material compositions according to one embodiment and a comparative example of the present specification.
도 3은 본 명세서의 일 실시예 및 비교예에 따른 인상재 조성물의 가속노화에 따른 경화시간을 나타낸 그래프이다.3 is a graph showing the curing time according to accelerated aging of impression material compositions according to one embodiment and a comparative example of the present specification.
이하에서는 첨부한 도면을 참조하여 본 명세서의 일 측면을 설명하기로 한다. 그러나 본 명세서의 기재사항은 여러 가지 상이한 형태로 구현될 수 있으며, 따라서 여기에서 설명하는 실시예로 한정되는 것은 아니다. 그리고 도면에서 본 명세서의 일 측면을 명확하게 설명하기 위해서 설명과 관계없는 부분은 생략하였으며, 명세서 전체를 통하여 유사한 부분에 대해서는 유사한 도면 부호를 붙였다.Hereinafter, one aspect of the present specification will be described with reference to the accompanying drawings. However, the descriptions in this specification may be implemented in many different forms, and thus are not limited to the embodiments described herein. And in order to clearly explain one aspect of the present specification in the drawings, parts irrelevant to the description are omitted, and similar reference numerals are attached to similar parts throughout the specification.
본 명세서에서 수치적 값의 범위가 기재되었을 때, 이의 구체적인 범위가 달리 기술되지 않는 한 그 값은 유효 숫자에 대한 화학에서의 표준규칙에 따라 제공된 유효 숫자의 정밀도를 갖는다. 예를 들어, 10은 5.0 내지 14.9의 범위를 포함하며, 숫자 10.0은 9.50 내지 10.49의 범위를 포함한다.When ranges of numerical values are set forth herein, unless the specific range is stated otherwise, the values have the precision of significant digits provided in accordance with the standard rules in chemistry for significant digits. For example, 10 includes the range 5.0 to 14.9, and the number 10.0 includes the range 9.50 to 10.49.
치과용 인상재 조성물Dental impression material composition
본 명세서의 일 측면에 따른 치과용 인상재 조성물은, 말단이 비닐기로 치환된 V폴리다이메틸실록산; 및 Si-H 함량이 3~4.5mmol/g인 오르가노하이드로겐폴리실록산;을 포함할 수 있다.A dental impression material composition according to one aspect of the present specification includes V polydimethylsiloxane substituted with a vinyl group at the terminal; and an organohydrogenpolysiloxane having a Si-H content of 3 to 4.5 mmol/g.
상기 말단이 비닐기로 치환된 V폴리다이메틸실록산의 일 예시는 아래 화학식 1과 같이 표현될 수 있다.An example of the V polydimethylsiloxane in which the terminal is substituted with a vinyl group may be represented by Formula 1 below.
[화학식 1][Formula 1]
상기 식에서 n은 1~1000일 수 있으나 이에 제한되는 것은 아니다. 다만 상기 범위를 벗어나면 점도가 과도하게 상승하여 목적하는 특성 구현이 어려울 수 있다.In the above formula, n may be 1 to 1000, but is not limited thereto. However, outside the above range, the viscosity increases excessively, and it may be difficult to implement desired characteristics.
상기 말단이 비닐기로 치환된 V폴리다이메틸실록산은 말단에 반응성 비닐기가 부여되어 광경화 내지 열경화가 가능하므로, 이를 포함하는 인상재 조성물의 가교 특성이 우수하여 석고 경화를 통한 인상체를 채득에 유리할 수 있다.Since the V polydimethylsiloxane whose terminal is substituted with a vinyl group is endowed with a reactive vinyl group and can be photocured or thermally cured, the impression material composition containing the V polydimethylsiloxane has excellent crosslinking properties and is advantageous in obtaining an impression through gypsum curing. can
상기 오르가노하이드로겐폴리실록산은 Si-H 구조를 포함하여 상기 V폴리다이메틸실록산의 비닐기와 반응할 수 있다. 상기 Si-H 구조의 수소가 비닐기의 이중결합과 부가중합되어 3차원 망상구조를 형성함으로써 중합체 사슬 간의 상대적인 운동을 억제하고, 인상재의 장기 보관성을 개선할 수 있다. 다만 이러한 반응에서 발생한 수소가스로 인하여 인상체 표면에 기포가 발생할 수 있으므로, 상기 Si-H 구조의 함량은 3~4.5mmol/g으로 제어될 수 있다. 예를 들어, 상기 오르가노하이드로겐폴리실록산으로는 Si-H 구조를 3mmol/g, 3.1mmol/g, 3.2mmol/g, 3.3mmol/g, 3.4mmol/g, 3.5mmol/g, 3.6mmol/g, 3.7mmol/g, 3.8mmol/g, 3.9mmol/g, 4mmol/g, 4.1mmol/g, 4.2mmol/g, 4.3mmol/g, 4.4mmol/g, 4.5mmol/g 또는 이들 중 두 값의 사이 범위의 함량을 갖는 것을 사용할 수 있다. 이러한 오르가노하이드로겐폴리실록산으로는 시판되는 제품을 사용할 수 있으며, 시판 제품의 Si-H 값에 따라 Si-H 구조의 함량을 특정할 수 있다.The organohydrogenpolysiloxane may have a Si-H structure and react with the vinyl group of the V-polydimethylsiloxane. Hydrogen of the Si-H structure is added-polymerized with the double bond of the vinyl group to form a three-dimensional network structure, thereby suppressing relative movement between polymer chains and improving the long-term storage property of the impression material. However, since bubbles may be generated on the surface of the impression body due to hydrogen gas generated in this reaction, the content of the Si-H structure may be controlled to 3 to 4.5 mmol/g. For example, as the organohydrogenpolysiloxane, the Si-H structure is 3mmol/g, 3.1mmol/g, 3.2mmol/g, 3.3mmol/g, 3.4mmol/g, 3.5mmol/g, 3.6mmol/g , 3.7mmol/g, 3.8mmol/g, 3.9mmol/g, 4mmol/g, 4.1mmol/g, 4.2mmol/g, 4.3mmol/g, 4.4mmol/g, 4.5mmol/g or two of these values Those having a content in the range between can be used. A commercially available product can be used as the organohydrogenpolysiloxane, and the content of the Si-H structure can be specified according to the Si-H value of the commercially available product.
상기 Si-H 구조의 함량이 3mmol/g 미만이면 경화시간이 과도하게 증가할 수 있고, 4.5mmol/g 초과이면 수소가스가 과도하게 많이 발생하여 전술한 방법으로도 기포면적을 개선하기 어려울 수 있다.If the content of the Si-H structure is less than 3 mmol / g, the curing time may excessively increase, and if it exceeds 4.5 mmol / g, hydrogen gas is generated excessively, making it difficult to improve the bubble area even by the above method. .
상기 오르가노하이드로겐폴리실록산의 일 예시는 아래 화학식 2와 같이 표현될 수 있다.An example of the organohydrogenpolysiloxane may be represented by Formula 2 below.
[화학식 2][Formula 2]
목적하는 기술 효과의 달성을 위해서 상기 말단이 비닐기로 치환된 V폴리다이메틸실록산의 함량이 30~60중량부이고 상기 오르가노하이드로겐폴리실록산의 함량이 5~10중량부인 치과용 인상재 조성물을 사용할 수 있다.In order to achieve the desired technical effect, a dental impression material composition containing 30 to 60 parts by weight of the V polydimethylsiloxane whose terminal is substituted with a vinyl group and 5 to 10 parts by weight of the organohydrogenpolysiloxane can be used. there is.
상기 말단이 비닐기로 치환된 V폴리다이메틸실록산의 함량은, 예를 들어, 30중량부, 32중량부, 34중량부, 36중량부, 38중량부, 40중량부, 42중량부, 44중량부, 46중량부, 48중량부, 50중량부, 52중량부, 54중량부, 56중량부, 58중량부, 60중량부 또는 이들 중 두 값 사이 범위일 수 있다. 상기 V폴리다이메틸실록산의 함량이 30중량부 미만이면 가교시간이 과도하게 길어지거나 필러 등의 첨가제가 쉽게 응집하여 인상재에 필요한 수준의 탄성 구현이 어려울 수 있다. 상기 V폴리다이메틸실록산의 함량이 60중량부 초과이면 가교가 불충분하게 이루어져 기포 생성으로 인한 보관안정성이 저하되고, 인상체의 채득 시 형상이 무너질 수 있다.The content of the V polydimethylsiloxane whose terminal is substituted with a vinyl group is, for example, 30 parts by weight, 32 parts by weight, 34 parts by weight, 36 parts by weight, 38 parts by weight, 40 parts by weight, 42 parts by weight, 44 parts by weight parts, 46 parts, 48 parts, 50 parts, 52 parts, 54 parts, 56 parts, 58 parts, 60 parts, or a range between two of these values. If the content of the V-polydimethylsiloxane is less than 30 parts by weight, the crosslinking time may be excessively long or additives such as fillers may easily aggregate, making it difficult to realize the level of elasticity required for the impression material. If the content of the V-polydimethylsiloxane exceeds 60 parts by weight, crosslinking is insufficient, resulting in deterioration in storage stability due to generation of air bubbles, and the shape may collapse when the impression body is taken.
상기 오르가노하이드로겐폴리실록산의 함량은, 예를 들어, 5중량부, 5.5중량부, 6.0중량부, 6.5중량부, 7.0중량부, 7.5중량부, 8중량부, 8.5중량부, 9.0중량부, 9.5중량부, 10중량부 또는 이들 중 두 값 사이 범위일 수 있다. 오르가노하이드로겐폴리실록산의 함량이 상기 범위를 벗어나면 가교가 불충분하게 수행되어 인상체의 채득 시 형상 유지가 어렵거나, 가교밀도가 과도하게 상승하여 인상재의 탄성이 부족해질 수 있다.The content of the organohydrogenpolysiloxane is, for example, 5 parts by weight, 5.5 parts by weight, 6.0 parts by weight, 6.5 parts by weight, 7.0 parts by weight, 7.5 parts by weight, 8 parts by weight, 8.5 parts by weight, 9.0 parts by weight, 9.5 parts by weight, 10 parts by weight or a range between any two of these values. If the content of the organohydrogenpolysiloxane is out of the above range, crosslinking may be insufficiently performed, making it difficult to maintain the shape upon taking an impression body, or the crosslinking density may excessively increase, resulting in insufficient elasticity of the impression material.
본 명세서에서의 “점도”는 점도측정계로 25℃에서에서 측정한 값을 의미한다. 예를 들어, TA instruments 社의 AR 2000ex rotational rheometer를 이용하여 25℃에서 cup&bob attachment에 약 20g의 시료를 넣어 전단율(Shear rate) 0.1~50 1/s로 측정한 값일 수 있다."Viscosity" in the present specification means a value measured at 25 ℃ with a viscometer. For example, it may be a value measured at a shear rate of 0.1 to 50 1/s by putting a sample of about 20 g in a cup & bob attachment at 25 ° C using an AR 2000ex rotational rheometer from TA Instruments.
V폴리다이메틸실록산의 특성을 확인하기 위한 물성 중 하나로 25℃에서의 점도가 있다. 상기 말단이 비닐기로 치환된 V폴리다이메틸실록산으로는 25℃에서의 점도가 100~25000 cP인 것을 사용할 수 있다. 예를 들어, 상기 말단이 비닐기로 치환된 폴리다이메틸실록산의 25℃에서의 점도가 100cP, 150cP, 200cP, 250cP, 300cP, 350cP, 400cP, 450cP, 500cP, 550cP, 600cP, 650cP, 700cP, 750cP, 800cP, 850cP, 900cP, 950cP, 1000cP, 1050cP, 1100cP, 1150cP, 1200cP, 1250cP, 1300cP, 1350cP, 1400cP, 1450cP, 1500cP, 1600cP, 1800cP, 2000cP, 3000cP, 4000cP, 5000cP, 6000cP, 7000cP, 8000cP, 9000cP, 10000cP, 11000cP, 12000cP, 13000cP, 14000cP, 15000cP, 16000cP, 17000cP, 18000cP, 19000cP, 20000cP, 21000cP, 22000cP, 23000cP, 24000cP, 25000cP 또는 이들 중 두 값 사이 범위일 수 있으나, 이에 제한되는 것은 아니다. One of the physical properties for confirming the characteristics of V polydimethylsiloxane is viscosity at 25°C. As the V polydimethylsiloxane in which the terminal is substituted with a vinyl group, one having a viscosity of 100 to 25000 cP at 25° C. may be used. For example, the viscosity at 25 ° C. of the polydimethylsiloxane substituted with a vinyl group at the terminal is 100 cP, 150 cP, 200 cP, 250 cP, 300 cP, 350 cP, 400 cP, 450 cP, 500 cP, 550 cP, 600 cP, 650 cP, 700 cP, and 750 cP. P, 800cP, 850cP, 900cP, 950cP, 1000cP, 1050cP, 1100cP, 1150cP, 1200cP, 1250cP, 1300cP, 1350cP, 1400cP, 1450cP, 1500cP, 1600c P, 1800cP, 2000cP, 3000cP, 4000cP, 5000cP, 6000cP, 7000cP, 8000cP, 9000cP, 10000cP, 11000cP, 12000cP, 13000cP, 14000cP, 15000cP, 16000cP, 17000cP, 18000cP, 19000cP, 20000cP, 21000cP, 22000cP, 2300 It may be 0cP, 24000cP, 25000cP or a range between two values thereof, but is not limited thereto.
일 예시로, 다양한 점도를 가지는 폴리다이메틸실록산을 혼용하여 인상재의 물성을 보다 세밀하게 조절할 수 있다.As an example, the physical properties of the impression material can be more precisely controlled by using polydimethylsiloxanes having various viscosities together.
일 예로, 상기 말단이 비닐기로 치환된 V폴리다이메틸실록산은, 25℃ 점도가 100~500cP인 제1 V폴리다이메틸실록산 10~15중량부, 25℃ 점도가 750~1500cP인 제2 V폴리다이메틸실록산 20~25중량부 및 25℃ 점도가 5000~25000cP인 제3 V폴리다이메틸실록산 10~15중량부를 포함할 수 있다.For example, the V polydimethylsiloxane whose terminal is substituted with a vinyl group includes 10 to 15 parts by weight of the first V polydimethylsiloxane having a viscosity of 100 to 500 cP at 25 ° C. and a second poly polydimethylsiloxane having a viscosity of 750 to 1500 cP at 25 ° C. 20 to 25 parts by weight of dimethylsiloxane and 10 to 15 parts by weight of 3 V polydimethylsiloxane having a viscosity of 5000 to 25000 cP at 25°C.
상기 제1 V폴리다이메틸실록산은, 예를 들어, 10중량부, 10.5중량부, 11중량부, 11.5중량부, 12중량부, 12.5중량부, 13중량부, 13.5중량부, 14중량부, 14.5중량부, 15중량부, 이들 중 두 값 사이 범위의 함량으로 포함될 수 있다. 상기 제1 V폴리다이메틸실록산은 상대적으로 낮은 점도를 가지는 저분자량 성분으로, 인상재에 유동성을 부여하며 가교밀도를 상승시킬 수 있다.The first V polydimethylsiloxane is, for example, 10 parts by weight, 10.5 parts by weight, 11 parts by weight, 11.5 parts by weight, 12 parts by weight, 12.5 parts by weight, 13 parts by weight, 13.5 parts by weight, 14 parts by weight, 14.5 parts by weight, 15 parts by weight, it may be included in the content of the range between the two values. The first V-polydimethylsiloxane is a low molecular weight component having a relatively low viscosity, and may impart fluidity to the impression material and increase crosslinking density.
상기 제2 V폴리다이메틸실록산은, 예를 들어, 20중량부, 20.5중량부, 21중량부, 21.5중량부, 22중량부, 22.5중량부, 23중량부, 23.5중량부, 24중량부, 24.5중량부, 25중량부 또는 이들 중 두 값 사이 범위의 함량으로 포함될 수 있다. 상기 제2 V폴리다이메틸실록산은 중간 정도의 점도를 가지는 성분으로, 상기 치과용 인상재 조성물의 전체적인 특성을 부여할 수 있다.The second V polydimethylsiloxane is, for example, 20 parts by weight, 20.5 parts by weight, 21 parts by weight, 21.5 parts by weight, 22 parts by weight, 22.5 parts by weight, 23 parts by weight, 23.5 parts by weight, 24 parts by weight, It may be included in an amount of 24.5 parts by weight, 25 parts by weight or a range between these two values. The second V-polydimethylsiloxane is a component having a moderate viscosity, and may impart overall characteristics of the dental impression material composition.
상기 제3 V폴리다이메틸실록산은, 예를 들어, 10중량부, 10.5중량부, 11중량부, 11.5중량부, 12중량부, 12.5중량부, 13중량부, 13.5중량부, 14중량부, 14.5중량부, 15중량부 또는 이들 중 두 값 사이 범위의 함량으로 포함될 수 있다. 상기 제3 V폴리다이메틸실록산은 높은 점도를 가지는 고분자량 성분으로, 인상재의 가교밀도를 감소시킬 수 있다.The 3-V polydimethylsiloxane is, for example, 10 parts by weight, 10.5 parts by weight, 11 parts by weight, 11.5 parts by weight, 12 parts by weight, 12.5 parts by weight, 13 parts by weight, 13.5 parts by weight, 14 parts by weight, It may be included in an amount of 14.5 parts by weight, 15 parts by weight or a range between these two values. The third V polydimethylsiloxane is a high molecular weight component having high viscosity, and can reduce the crosslinking density of the impression material.
상기 오르가노하이드로겐폴리실록산의 Si-H 함량 및 상기 말단이 비닐기로 치환된 V폴리다이메틸실록산의 비닐 함량의 비(Si-H/비닐)는 1.5~3일 수 있다. 예를 들어, Si-H/비닐은 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3.0 또는 이들 중 두 값의 사이 범위일 수 있다. 상기 범위를 벗어나면 가교에 과도하게 긴 시간이 소요되거나, 인상체 채득 시 표면에 기포가 과도하게 생성될 수 있다.The ratio (Si-H/vinyl) of the Si-H content of the organohydrogenpolysiloxane and the vinyl content of the V-polydimethylsiloxane having the terminal substituted with a vinyl group may be 1.5 to 3. For example, Si-H/vinyl can be 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3.0 or a range between two of these values. can If it is out of the above range, crosslinking may take an excessively long time, or air bubbles may be excessively generated on the surface when taking an impression.
본 명세서의 일 측면에 따르면 상기 제1 내지 제3 V 폴리다이메틸실록산과 상기 오르가노하이드로겐폴리실록산의 비율을 조절하여 치과용 인상재 조성물의 경화 특성, 보관안정성을 유지하면서 수소가스로 인한 문제점을 개선할 수 있다.According to one aspect of the present specification, problems caused by hydrogen gas are improved while maintaining curing characteristics and storage stability of the dental impression material composition by adjusting the ratio of the first to third V polydimethylsiloxanes and the organohydrogenpolysiloxane. can do.
상기 오르가노하이드로겐폴리실록산의 Si-H 구조는 상기 V폴리다이메틸실록산 말단의 비닐기와 반응할 수 있으므로, Si-H 구조의 함량과 V폴리다이메틸실록산의 비닐 함량의 비율을 조절하여 인상재 조성물의 가교밀도를 조절할 수 있다. 인상재 조성물의 가교밀도가 과하게 낮으면 인장강도가 저하되거나 인상재가 찢어지기 쉽고, 가교밀도가 과도하게 높으면 탄성이 부족해질 수 있다.Since the Si-H structure of the organohydrogenpolysiloxane can react with the vinyl group at the end of the V-polydimethylsiloxane, the ratio of the content of the Si-H structure and the vinyl content of the V-polydimethylsiloxane is adjusted to obtain the impression material composition. The crosslinking density can be adjusted. If the crosslinking density of the impression material composition is excessively low, the tensile strength may be lowered or the impression material may be easily torn, and if the crosslinking density is excessively high, elasticity may be insufficient.
또한 Si-H 구조와 비닐기 간의 반응에 의해 발생한 수소가스가 인상체의 채득 시 기포를 형성하는 요인이 되므로, 가교밀도, 가교속도, 보관안정성, 수소가스 발생량 등의 특성은 종래 트레이드오프 관계에 있었다.In addition, since the hydrogen gas generated by the reaction between the Si-H structure and the vinyl group is a factor in forming bubbles when the impression body is taken, the characteristics such as crosslinking density, crosslinking rate, storage stability, and amount of hydrogen gas generated are in a conventional trade-off relationship. there was.
이러한 트레이드오프 관계를 긍정적으로 개선하기 위해, 치과용 인상재 조성물로 말단이 비닐기로 치환된 V폴리다이메틸실록산을 주 성분으로 포함하되, 오르가노하이드로겐폴리실록산의 Si-H 함량을 조절하고, 점도가 다른 V폴리다이메틸실록산 간의 비율을 제어하여 보관안정성, 가교밀도 및 수소가스 형성 억제를 양립시킬 수 있다.In order to positively improve this trade-off relationship, the dental impression material composition includes V polydimethylsiloxane whose terminal is substituted with a vinyl group as a main component, but the Si-H content of the organohydrogenpolysiloxane is adjusted, and the viscosity is By controlling the ratio between different V polydimethylsiloxanes, storage stability, crosslinking density, and suppression of hydrogen gas formation can be achieved.
예를 들어, 상기 제1 V폴리다이메틸실록산의 비율이 상대적으로 높으면 인상재 조성물의 가교밀도가 상승하고, 수소가스 발생량이 증가할 수 있다. 상기 제2 V폴리다이메틸실록산의 비율이 상대적으로 높으면 인상재 조성물의 가교밀도가 감소하고, 수소가스 발생량이 감소할 수 있다. 동시에 상기 제1 V폴리다이메틸실록산은 인상재 조성물의 유동성을 증가시킬 수 있고, 상기 제3 V폴리다이메틸실록산은 인상재 조성물의 보관안정성을 개선할 수 있다.For example, when the ratio of the first V polydimethylsiloxane is relatively high, the crosslinking density of the impression material composition may increase and the amount of hydrogen gas generated may increase. When the ratio of the second V polydimethylsiloxane is relatively high, the crosslinking density of the impression material composition may decrease and the amount of hydrogen gas generated may decrease. At the same time, the first V polydimethylsiloxane can increase the fluidity of the impression material composition, and the third V polydimethylsiloxane can improve storage stability of the impression material composition.
본 명세서에서 사용된 “기포면적”은 상기 인상재 조성물에 석고를 붓고 경화시킴으로써 가로30㎜×세로30㎜의 시편을5개 제조한 후 인상재와의 계면에서 전체 면적 대비 기포가 발생한 면적(%)의 평균을 의미할 수 있다.As used herein, “bubble area” is the area (%) of the area (%) in which bubbles are generated at the interface with the impression material after preparing five specimens of 30 mm wide × 30 mm long by pouring gypsum into the impression material composition and curing it. can mean average.
본 명세서에서 사용된 “보관안정성”은 보관기간이 길어짐에 따른 인상재 조성물의 특성 내지 형상의 변화율이 작은 것을 의미할 수 있다.As used herein, "storage stability" may mean that the rate of change in the characteristics or shape of the impression material composition is small as the storage period is prolonged.
상기 치과용 인상재 조성물은 가교반응에서 발생한 수소기체가 인상체 표면에 기포를 형성하는 것을 억제할 수 있다. 상기 인상재 조성물에 경화시킨 석고 모형의 기포면적은 20% 이하일 수 있으며, 예를 들어, 상기 기포면적은 20% 이하, 19% 이하, 18% 이하, 17% 이하, 16% 이하, 15% 이하, 14% 이하, 13% 이하, 12% 이하, 11% 이하, 10% 이하, 9% 이하, 8% 이하, 7% 이하, 6% 이하, 5% 이하, 4% 이하, 3% 이하, 2% 이하, 1% 이하, 0%(1% 미만의 경우 기포가 발생하지 않은 것으로 간주) 또는 이들 중 두 값 사이 범위일 수 있으나, 이에 제한되는 것은 아니다. 상기 치과용 조성물에 의한 기포면적이 상기 범위 초과이면 인상재 조성물을 사용하여 인상 채득 시 기포가 많이 발생하여 인상체 모델의 정확성이 저하될 수 있다.The dental impression material composition can suppress the formation of air bubbles on the surface of the impression body by hydrogen gas generated in the crosslinking reaction. The bubble area of the gypsum model cured in the impression material composition may be 20% or less, for example, the bubble area is 20% or less, 19% or less, 18% or less, 17% or less, 16% or less, 15% or less, 14% or less, 13% or less, 12% or less, 11% or less, 10% or less, 9% or less, 8% or less, 7% or less, 6% or less, 5% or less, 4% or less, 3% or less, 2% Or less, 1% or less, 0% (if less than 1%, it is considered that no bubbles are generated), or a range between two values thereof, but is not limited thereto. If the bubble area of the dental composition exceeds the above range, a lot of bubbles are generated during impression taking using the impression material composition, and the accuracy of the impression body model may deteriorate.
상기 치과용 인상재 조성물은 폴리다이메틸실록산, 사슬연장제, 실리콘계 필러, 촉매제 및 경화지연제로 이루어진 군에서 선택된 하나 이상을 더 포함할 수 있다. 예를 들어, 상기 폴리다이메틸실록산 0~1중량부, 상기 사슬연장제 0~1중량부, 상기 실리콘계 필러 40~70중량부, 촉매제 0~2중량부 및 경화지연제 0~1중량부를 포함할 수 있다. 각 성분의 첨가는 선택사항이므로, 0중량부인 경우 포함하지 않는 경우를 의미할 수 있다.The dental impression material composition may further include at least one selected from the group consisting of polydimethylsiloxane, a chain extender, a silicone-based filler, a catalyst, and a curing retardant. For example, 0 to 1 part by weight of the polydimethylsiloxane, 0 to 1 part by weight of the chain extender, 40 to 70 parts by weight of the silicone-based filler, 0 to 2 parts by weight of the catalyst, and 0 to 1 part by weight of the curing retardant. can do. Since the addition of each component is optional, it may mean that it is not included in the case of 0 parts by weight.
상기 폴리다이메틸실록산은 말단이 비닐로 치환되지 않은 것으로 소포제의 역할을 수행할 수 있다. 상기 폴리다이메틸실록산은 25℃ 점도가 100~1000cP인 것을 사용할 수 있으나, 이에 한정되는 것은 아니다. 상기 폴리다이메틸실록산의 함량은 예를 들어, 0중량부, 0.001중량부, 0.003중량부, 0.005중량부, 0.007중량부, 0.01중량부, 0.02중량부, 0.03중량부, 0.04중량부, 0.05중량부, 0.06중량부, 0.07중량부, 0.08중량부, 0.09중량부, 0.1중량부, 0.2중량부, 0.3중량부, 0.4중량부, 0.5중량부, 0.6중량부, 0.7중량부, 0.8중량부, 0.9중량부, 1.0중량부 또는 이들 중 두 값 사이 범위일 수 있다. 상기 폴리다이메틸실록산의 함량이 1중량부를 초과하면 전술한 가교특성의 균형이 파괴될 수 있다.The polydimethylsiloxane, which is not substituted with a vinyl end, may serve as an antifoaming agent. The polydimethylsiloxane may have a viscosity of 100 to 1000 cP at 25° C., but is not limited thereto. The content of the polydimethylsiloxane is, for example, 0 parts by weight, 0.001 parts by weight, 0.003 parts by weight, 0.005 parts by weight, 0.007 parts by weight, 0.01 parts by weight, 0.02 parts by weight, 0.03 parts by weight, 0.04 parts by weight, 0.05 parts by weight. 0.06 parts by weight, 0.07 parts by weight, 0.08 parts by weight, 0.09 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight, 1.0 parts by weight or a range between any two of these values. If the content of the polydimethylsiloxane exceeds 1 part by weight, the above-described balance of crosslinking properties may be destroyed.
상기 필러는 무기 필러 및 비정질 합성 필러로 이루어진 군에서 선택된 하나 이상일 수 있다. 상기 무기 필러와 비정질 합성 필러를 조합하여 사용하는 경우, 이들의 중량비는 각각 40~60 : 3~10일 수 있다. 상기 범위를 만족하면 탄성이 저하되지 않는 수준에서 장기간 보관이 가능하고, 최적의 경화속도를 만족시키는 범위에서 인상재에 필요한 보관안정성을 부여할 수 있다.The filler may be at least one selected from the group consisting of inorganic fillers and amorphous synthetic fillers. When the inorganic filler and the amorphous synthetic filler are used in combination, their weight ratio may be 40 to 60:3 to 10, respectively. When the above range is satisfied, long-term storage is possible at a level where elasticity is not lowered, and necessary storage stability can be imparted to the impression material within a range satisfying an optimal curing speed.
예를 들어, 상기 무기 필러는 인상재에 필요한 강도와 우수한 보관안정성 구현을 위해 첨가되는 것으로, 크리스토발라이트, 결정성 천연 실리카, 바륨 알루미늄 실리케이트, 스트론튬 알루미늄 실리케이트, 규산바륨 유리, 규산스트론튬 유리, 보레이트 알루미늄 실리케이트 유리, 포스페이트 알루미늄 실리케이트 유리, 플루오르알루미노실리케이트 유리, 글라스비드, 규산칼슘, 규산지르코늄 및 규산나트륨알루미늄으로 이루어진 군에서 선택된 하나 이상을 포함할 수 있다. 상기 비정질 합성 필러는 보강제의 역할을 수행할 수 있다. 예를 들어, 상기 비정질 합성 필러는 퓸드 실리카, 실리카 겔, 침전 실리카, 실리카 졸 및 규소산으로 이루어진 군에서 선택된 하나 이상일 수 있다.For example, the inorganic filler is added to realize the strength and excellent storage stability required for impression materials, and cristobalite, crystalline natural silica, barium aluminum silicate, strontium aluminum silicate, barium silicate glass, strontium silicate glass, borate aluminum silicate glass , Phosphate aluminum silicate glass, fluoroaluminosilicate glass, glass beads, calcium silicate, zirconium silicate and sodium aluminum silicate may include at least one selected from the group consisting of. The amorphous synthetic filler may serve as a reinforcing agent. For example, the amorphous synthetic filler may be at least one selected from the group consisting of fumed silica, silica gel, precipitated silica, silica sol, and silicic acid.
상기 필러의 함량은 40~70중량부일 수 있다. 예를 들어, 상기 필러의 함량은 40중량부, 42중량부, 44중량부, 46중량부, 48중량부, 50중량부, 52중량부, 54중량부, 56중량부, 58중량부, 60중량부, 62중량부, 64중량부, 66중량부, 68중량부, 70중량부 또는 이들 중 두 값 사이 범위일 수 있다. 상기 필러의 함량이 40중량부 미만이면 인상재 조성물에 충분히 분산되지 못하여 장기 보관이 어려울 수 있고, 70중량부 초과이면 장기 보관 시 변형률이 높아질 수 있다. The content of the filler may be 40 to 70 parts by weight. For example, the content of the filler is 40 parts by weight, 42 parts by weight, 44 parts by weight, 46 parts by weight, 48 parts by weight, 50 parts by weight, 52 parts by weight, 54 parts by weight, 56 parts by weight, 58 parts by weight, 60 parts by weight parts by weight, 62 parts by weight, 64 parts by weight, 66 parts by weight, 68 parts by weight, 70 parts by weight or a range between two of these values. If the content of the filler is less than 40 parts by weight, long-term storage may be difficult because it is not sufficiently dispersed in the impression material composition, and if it exceeds 70 parts by weight, strain may increase during long-term storage.
일 예시로, 상기 인상재 조성물은 크리스토발라이트 실리카와 퓸드 실리카를 포함할 수 있다. 크리스토발라이트 실리카는 규산염광물의 하나이며, 268℃ 부근을 경계로 그것보다 높은 온도에서는 등축정계, 낮은 온도에서는 정방정계에 속한다. 등축정계의 것을 α-크리스토발라이트, 정방정계의 것을 β-크리스토발라이트라 부르며, 필러로는 β-크리스토발라이트를 사용하는 것이 일반적일 수 있다.As an example, the impression material composition may include cristobalite silica and fumed silica. Cristobalite silica is one of the silicate minerals, and it belongs to the tetragonal system at higher temperatures and the tetragonal system at lower temperatures around 268 ° C. The tetragonal one is called α-cristobalite and the tetragonal one is called β-cristobalite, and it may be common to use β-cristobalite as a filler.
퓸드 실리카는 3차원적 구조 결합을 형성하고 있어 전단력이 작용하면 실리카 분자의 상호간 결합이 쉽게 끊어지며, 액체 상태의 졸과 같은 형태로 변하는 틱소트로피(thixotropy)한 성질을 가지고 있다. 따라서, 퓸드 실리카를 포함하는 조성물은 흐름성이 향상될 수 있다. 필러로 사용되는 퓸드 실리카의 입자는 일반적으로 나노 사이즈이며 구형일 수 있다. 예를 들어, 평균 입자 크기가 1~600nm이고, 표면적은 5~600m2/g인 퓸드 실리카를 사용할 수 있다.Fumed silica forms a three-dimensional structural bond, so when shear force acts on it, the mutual bond between silica molecules is easily broken, and it has a thixotropy property that changes into a sol-like form in a liquid state. Therefore, the flowability of the composition containing the fumed silica can be improved. Particles of fumed silica used as a filler are generally nano-sized and may be spherical. For example, fumed silica having an average particle size of 1 to 600 nm and a surface area of 5 to 600 m 2 /g may be used.
상기 촉매제는 백금계 또는 팔라듐계일 수 있다. 예를 들어, 상기 촉매제는 백금, 백금화합물, 팔라듐, 팔라듐화합물일 수 있다. 상기 촉매제는 반응의 시간을 단축할 뿐 아니라, 수소흡착제로서도 역할을 할 수 있다. 수소흡착제로서의 역할이란 상기 인상재 조성물에 석고를 부어 인상체의 제조 시 발생하는 수소가스를 흡착하는 것을 의미하며, 그 결과 기포발생을 억제하여 정확한 인상체의 모델을 채득하는데 도움을 줄 수 있다.The catalyst may be platinum-based or palladium-based. For example, the catalyst may be platinum, a platinum compound, palladium, or a palladium compound. The catalyst not only shortens the reaction time, but also serves as a hydrogen adsorbent. The role as a hydrogen absorbent means to adsorb hydrogen gas generated during the manufacture of an impression body by pouring gypsum into the impression material composition, and as a result, it can help to obtain an accurate impression body model by suppressing the generation of air bubbles.
상기 촉매제는, 예를 들어, 0중량부, 0.001중량부, 0.1중량부, 0.2중량부, 0.3중량부, 0.4중량부, 0.5중량부, 0.6중량부, 0.7중량부, 0.8중량부, 0.9중량부, 1.0중량부, 1.1중량부, 1.2중량부, 1.3중량부, 1.4중량부, 1.5중량부, 1.6중량부, 1.7중량부, 1.8중량부, 1.9중량부, 2.0중량부 또는 이들 중 두 값 사이 범위의 함량으로 포함될 수 있다. 상기 촉매제의 함량이 2중량부 초과이면 경화가 과도하게 빠르게 수행되어 인상물을 채득하는데 어려움이 생기거나, 기포형성 억제가 어려울 수 있다. The catalyst, for example, 0 parts by weight, 0.001 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight Part, 1.0 part, 1.1 part, 1.2 part, 1.3 part, 1.4 part, 1.5 part, 1.6 part, 1.7 part, 1.8 part, 1.9 part, 2.0 part, or two of these It may be included in an amount in the range between. If the content of the catalyst exceeds 2 parts by weight, curing is performed excessively quickly, resulting in difficulty in obtaining an impression or suppression of bubble formation.
상기 경화지연제는 작업시간을 조절하기 위해 사용될 수 있다. 상기 경화지연제는, 예를 들어, 0중량부, 0.001중량부, 0.003중량부, 0.005중량부, 0.007중량부, 0.01중량부, 0.02중량부, 0.03중량부, 0.04중량부, 0.05중량부, 0.06중량부, 0.07중량부, 0.08중량부, 0.09중량부, 0.1중량부, 0.2중량부, 0.3중량부, 0.4중량부, 0.5중량부, 0.6중량부, 0.7중량부, 0.8중량부, 0.9중량부, 1.0중량부 또는 이들 중 두 값 사이 범위로 포함될 수 있다. 상기 경화지연제의 함량이 1중량부 초과이면 불순물로 작용할 수 있다.The curing retardant may be used to control the working time. The curing retardant, for example, 0 parts by weight, 0.001 parts by weight, 0.003 parts by weight, 0.005 parts by weight, 0.007 parts by weight, 0.01 parts by weight, 0.02 parts by weight, 0.03 parts by weight, 0.04 parts by weight, 0.05 parts by weight, 0.06 parts by weight, 0.07 parts by weight, 0.08 parts by weight, 0.09 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight part, 1.0 parts by weight or a range between two values thereof. If the content of the curing retardant exceeds 1 part by weight, it may act as an impurity.
상기 인상재 조성물은 트레이에 채워진 후 치열 및 지대를 압접하고, 경화 시까지 유지시킴으로써 치열의 형상, 즉 인상 부조를 얻을 수 있다. 이러한 인상 부조에 석고 모형을 부은 후 경화시킴으로써 인상체가 제조될 수 있다. 따라서 인상재의 사용성을 개선하려면 경화 시간을 조절할 필요가 있다.After the impression material composition is filled in a tray, the shape of the dentition, that is, the impression relief, can be obtained by press-contacting the dentition and the base and maintaining the dentition until hardening. An impression body can be manufactured by pouring a plaster model into the impression relief and then curing it. Therefore, it is necessary to adjust the curing time to improve the usability of the impression material.
상기 인상재 조성물 37℃ 경화 시간이 2~3분일 수 있고, 예를 들어, 2분, 2분 10초, 2분 20초, 2분 30초, 2분 40초, 2분 50초, 3분 또는 이들 중 두 값의 사이 범위일 수 있다. 경화시간이 상기 범위를 벗어나면 구강에 적용하기 전에 인상재가 경화되거나, 경화 중에 밀림 현상이 발생하여 정확한 인상의 채득이 어려울 수 있다.The impression material composition 37 ℃ curing time may be 2 to 3 minutes, for example, 2 minutes, 2 minutes 10 seconds, 2 minutes 20 seconds, 2 minutes 30 seconds, 2 minutes 40 seconds, 2 minutes 50 seconds, 3 minutes or It may be a range between two of these values. If the curing time is out of the above range, the impression material is hardened before application to the oral cavity, or a push phenomenon occurs during curing, making it difficult to obtain an accurate impression.
상기 인상재 조성물은 필요에 따라 계면활성제, 산화방지제, 기포제거제 및 색소로 이루어진 군에서 선택된 하나 이상을 더 포함할 수 있다. 예를 들어, 상기 계면활성제 0~2중량부, 상기 산화방지제 0~1중량부, 상기 기포제거제 0~1중량부, 상기 색소 0~1중량부를 포함할 수 있다.The impression material composition may further include at least one selected from the group consisting of a surfactant, an antioxidant, an anti-foaming agent, and a pigment, if necessary. For example, 0 to 2 parts by weight of the surfactant, 0 to 1 part by weight of the antioxidant, 0 to 1 part by weight of the defoaming agent, and 0 to 1 part by weight of the pigment may be included.
상기 계면활성제는 치아와의 젖음성(맞닿는 각각의 표면이 접촉을 유지하는 능력)을 향상시키고, 수소가스 발생량을 낮출 수 있다. 상기 계면활성제는, 예를 들어, 0중량부, 0.001중량부, 0.1중량부, 0.2중량부, 0.3중량부, 0.4중량부, 0.5중량부, 0.6중량부, 0.7중량부, 0.8중량부, 0.9중량부, 1.0중량부, 1.1중량부, 1.2중량부, 1.3중량부, 1.4중량부, 1.5중량부, 1.6중량부, 1.7중량부, 1.8중량부, 1.9중량부, 2.0중량부 또는 이들 중 두 값 사이 범위의 함량으로 포함될 수 있다. 상기 범위를 벗어나면 수소 발생을 통한 기포를 제어하는데 어려움이 있을 수 있으며, 제품 사용 시 치아와의 젖음성이 낮아 정확한 인상체의 모델을 채득하기 어려울 수 있다.The surfactant can improve wettability with teeth (the ability of each contacting surface to maintain contact) and reduce the amount of hydrogen gas generated. The surfactant is, for example, 0 parts by weight, 0.001 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight 1.0 parts by weight, 1.1 parts by weight, 1.2 parts by weight, 1.3 parts by weight, 1.4 parts by weight, 1.5 parts by weight, 1.6 parts by weight, 1.7 parts by weight, 1.8 parts by weight, 1.9 parts by weight, 2.0 parts by weight or two of these It can be included in the content of the range between the values. Outside of the above range, it may be difficult to control air bubbles through hydrogen generation, and it may be difficult to obtain an accurate impression body model due to low wettability with teeth when using the product.
상기 계면활성제는 비이온성 계면활성제, 라우릴황산나트륨, 모노글리세라이드황산염, 라우로릴살코신 나트륨, 자당 지방산 에스테르, 라우린산 디에탄올 아미드, 폴리옥시에틸렌, 트리실록산 에톡실레이트, 불소계 계면활성제로 이루어진 군에서 선택된 하나 이상을 포함할 수 있으나, 이에 한정되는 것은 아니다.The surfactant is composed of a nonionic surfactant, sodium lauryl sulfate, monoglyceride sulfate, lauroyl sarcosine sodium, sucrose fatty acid ester, lauric acid diethanol amide, polyoxyethylene, trisiloxane ethoxylate, and fluorine-based surfactant. It may include one or more selected from the group, but is not limited thereto.
상기 산화방지제는 장기간 물성 유지를 위하여 통상의 것을 사용할 수 있다. 상기 산화방지제는, 예를 들어, 0중량부, 0.001중량부, 0.003중량부, 0.005중량부, 0.007중량부, 0.01중량부, 0.02중량부, 0.03중량부, 0.04중량부, 0.05중량부, 0.06중량부, 0.07중량부, 0.08중량부, 0.09중량부, 0.1중량부, 0.2중량부, 0.3중량부, 0.4중량부, 0.5중량부, 0.6중량부, 0.7중량부, 0.8중량부, 0.9중량부, 1.0중량부 또는 이들 중 두 값 사이 범위로 포함될 수 있다. 상기 범위를 벗어나면 불순물로서 작용하여 기포 발생 제어 및 경화시간 조절이 어려울 수 있다.As the antioxidant, a conventional antioxidant may be used to maintain physical properties for a long period of time. The antioxidant is, for example, 0 parts by weight, 0.001 parts by weight, 0.003 parts by weight, 0.005 parts by weight, 0.007 parts by weight, 0.01 parts by weight, 0.02 parts by weight, 0.03 parts by weight, 0.04 parts by weight, 0.05 parts by weight, 0.06 parts by weight parts by weight, 0.07 parts by weight, 0.08 parts by weight, 0.09 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight , 1.0 parts by weight or a range between these two values. If it is out of the above range, it may act as an impurity and it may be difficult to control the generation of bubbles and adjust the curing time.
상기 기포제거제는, 예를 들어, 0중량부, 0.001중량부, 0.003중량부, 0.005중량부, 0.007중량부, 0.01중량부, 0.02중량부, 0.03중량부, 0.04중량부, 0.05중량부, 0.06중량부, 0.07중량부, 0.08중량부, 0.09중량부, 0.1중량부, 0.2중량부, 0.3중량부, 0.4중량부, 0.5중량부, 0.6중량부, 0.7중량부, 0.8중량부, 0.9중량부, 1.0중량부 또는 이들 중 두 값 사이 범위의 함량으로 포함될 수 있다. 상기 범위를 벗어나면 불순물로 작용하여 장기 보관이 어렵거나, 기포제거 효과를 나타내지 못할 수 있다.The defoaming agent, for example, 0 parts by weight, 0.001 parts by weight, 0.003 parts by weight, 0.005 parts by weight, 0.007 parts by weight, 0.01 parts by weight, 0.02 parts by weight, 0.03 parts by weight, 0.04 parts by weight, 0.05 parts by weight, 0.06 parts by weight parts by weight, 0.07 parts by weight, 0.08 parts by weight, 0.09 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight , 1.0 parts by weight or may be included in the content of the range between the two values. If it is out of the above range, it may act as an impurity, making it difficult to store for a long time, or may not exhibit the effect of removing air bubbles.
상기 색소는 인상재 조성물을 구강 내 도포 시, 구강 색과 구분이 용이하도록 첨가될 수 있다. 상기 색소는, 예를 들어, 0중량부, 0.001중량부, 0.003중량부, 0.005중량부, 0.007중량부, 0.01중량부, 0.02중량부, 0.03중량부, 0.04중량부, 0.05중량부, 0.06중량부, 0.07중량부, 0.08중량부, 0.09중량부, 0.1중량부, 0.2중량부, 0.3중량부, 0.4중량부, 0.5중량부, 0.6중량부, 0.7중량부, 0.8중량부, 0.9중량부, 1.0중량부 또는 이들 중 두 값 사이 범위의 함량으로 포함될 수 있다. 상기 범위를 벗어나면 불순물로 작용할 수 있다.The pigment may be added to easily distinguish the color of the oral cavity when the impression material composition is applied in the oral cavity. The pigment is, for example, 0 parts by weight, 0.001 parts by weight, 0.003 parts by weight, 0.005 parts by weight, 0.007 parts by weight, 0.01 parts by weight, 0.02 parts by weight, 0.03 parts by weight, 0.04 parts by weight, 0.05 parts by weight, 0.06 parts by weight 0.07 parts by weight, 0.08 parts by weight, 0.09 parts by weight, 0.1 parts by weight, 0.2 parts by weight, 0.3 parts by weight, 0.4 parts by weight, 0.5 parts by weight, 0.6 parts by weight, 0.7 parts by weight, 0.8 parts by weight, 0.9 parts by weight, It may be included in an amount of 1.0 parts by weight or a range between these two values. If it is out of the above range, it may act as an impurity.
이하, 본 명세서의 실시예에 관하여 더욱 상세히 설명하기로 한다. 다만, 이하의 실험 결과는 상기 실시예 중 대표적인 실험 결과만을 기재한 것이며, 실시예 등에 의해 본 명세서의 범위와 내용이 축소되거나 제한되어 해석될 수 없다. 아래에서 명시적으로 제시하지 않은 본 명세서의 여러 구현예의 각각의 효과는 해당 부분에서 구체적으로 기재하도록 한다.Hereinafter, the embodiments of the present specification will be described in more detail. However, the following experimental results are only representative experimental results among the above examples, and cannot be interpreted as the scope and contents of the present specification are reduced or limited by the examples. Each effect of the various embodiments of the present specification that is not explicitly presented below is to be described in detail in the corresponding section.
실시예 및 비교예Examples and Comparative Examples
제1 폴리다이메틸실록산, 제2 폴리다이메틸실록산 및 제3폴리다이메틸실록산을 하기 표 1의 Si-H/Vinyl 값에 맞게 각각 혼합하고, 하기 표 1의 Si-H함량(제조사, Evonik)을 포함하는 오르가노하이드로겐폴리실록산 7중량부, 폴리다이메틸실록산 0.05중량부, 크리스토발라이트 실리카 50중량부, 퓸드실리카 6.5중량부, 백금촉매 1중량부, 경화 지연제 0.5중량부, 계면활성제 1중량부, 산화방지제 0.5중량부, 기포제거제 0.5중량부, 색소 0.5중량부를 진공교반기를 사용하여 혼합하고, 자동혼합용 카트리지(automixing cartridge)에 담아 원심분리기를 사용하여 100rpm의 회전속도로 5분동안 돌린 후 인상재 조성물을 제조하였다.The first polydimethylsiloxane, the second polydimethylsiloxane, and the third polydimethylsiloxane were mixed according to the Si-H/Vinyl values in Table 1 below, and the Si-H content in Table 1 below (manufacturer, Evonik) Organohydrogenpolysiloxane 7 parts by weight, polydimethylsiloxane 0.05 parts by weight, cristobalite silica 50 parts by weight, fumed silica 6.5 parts by weight, platinum catalyst 1 parts by weight, curing retardant 0.5 parts by weight, surfactant 1 weight part 0.5 part by weight of antioxidant, 0.5 part by weight of anti-foaming agent, and 0.5 part by weight of pigment were mixed using a vacuum stirrer, placed in an automixing cartridge, and rotated for 5 minutes at a rotational speed of 100 rpm using a centrifuge. A post impression material composition was prepared.
구분division | 비교예 1Comparative Example 1 | 실시예 1Example 1 | 실시예 2Example 2 | 실시예 3Example 3 |
Si-H/VinylSi-H/Vinyl | 2.42.4 | 2.42.4 | 2.02.0 | 2.02.0 |
Si-H 함량Si-H content | 4.24.2 | 3.23.2 | 4.24.2 | 3.23.2 |
실험예 1Experimental Example 1
비교예 및 실시예의 인상재 조성물로 가로30㎜×세로30㎜의 정사각형 시편을5개 제조하여 각각 경화되기까지 걸리는 시간을 측정하여 평균을 나타내었고, 경화 후 발생된 기포를 확인하여, 전체 면적 대비 기포발생 면적(%)의 평균을 나타내었다.Five square specimens of 30 mm in width × 30 mm in length were prepared with the impression material compositions of Comparative Examples and Examples, and the time taken to cure each was measured and averaged. The average of the occurrence area (%) was shown.
구분division | 비교예 1Comparative Example 1 | 실시예 1Example 1 | 실시예 2Example 2 | 실시예 3Example 3 |
기포면적(% Area)Bubble area (% Area) | 32.532.5 | 1.21.2 | 14.414.4 | -- |
37℃ 경화 시간37° |
1분 33초1 minute 33 |
2분 2초2 |
1분 57초1 minute 57 |
2분 22초2 minutes 22 seconds |
표 2및 도면(도 1, 도 2)을 참고하면, 실시예의 인상재 조성물을 이용하여 제조한 시편은 기표면적이 15미만으로 나타내어 인상체 모델의 정확성을 확보할 수 있었고, 경화 시간은 1분 50초 이상으로 단시간에 굳지 않아 정확한 인상을 채득하기에 우수하였다. 특히 오르가노하이드로겐폴리실록산의 Si-H함량이 3.2mmol/g인 실시예 3의 시편은 기포가 발생하지 않았고, 경화 시간 또한 2분 22초로 너무 단시간 또는 장시간이 아닌, 적절한 경화시간을 나타내었다. 이는 Si-H함량 및 Si-H/비닐의 조절을 통해 최적의 가교 사슬 길이 및 가교 비로 인해 수소가스의 역할을 최소화했기 때문으로 판단된다.Referring to Table 2 and drawings (FIGS. 1 and 2), the specimens manufactured using the impression material compositions of Examples showed a surface area of less than 15, ensuring the accuracy of the impression body model, and the curing time was 1 minute 50 It did not harden in a short time of more than a second, so it was excellent for taking accurate impressions. In particular, the specimen of Example 3, in which the Si-H content of the organohydrogenpolysiloxane was 3.2 mmol/g, did not generate bubbles, and the curing time was also 2 minutes and 22 seconds, indicating an appropriate curing time, not too short or long. This is considered to be due to the minimization of the role of hydrogen gas due to the optimum crosslinking chain length and crosslinking ratio through the control of Si—H content and Si—H/vinyl.
실험예 2Experimental Example 2
비교예 및 실시예의 인상재 조성물로 가로30㎜×세로30㎜의 정사각형 시편을 85℃ 오븐에서 가속 노화한 후 레오미터를 이용하여 구강 내 경화 시간을 측정하여 나타내었다. 가속 노화 결과는 인상재의 보관안정성 결과를 의미하며, 변화율이 적을수록 안정적이고, 장기 보관이 가능함을 의미한다.After accelerated aging of square specimens of 30 mm in width x 30 mm in length with the impression material compositions of Comparative Examples and Examples in an oven at 85 ° C., the curing time in the oral cavity was measured using a rheometer. The accelerated aging result means the result of the storage stability of the impression material, and the smaller the change rate, the more stable and long-term storage is possible.
구분division | 비교예 1Comparative Example 1 | 실시예 1Example 1 | 실시예 2Example 2 | 실시예 3Example 3 |
가속 0년 후 경화 시간Curing time after 0 years of |
1분 33초1 minute 33 |
2분 2초2 |
1분 57초1 minute 57 |
2분 22초2 minutes 22 seconds |
가속 1년 후 경화 시간Curing time after 1 year of |
2분 41초2 minutes 41 |
2분 18초2 minutes 18 |
2분 27초2 minutes 27 |
2분 37초2 minutes 37 seconds |
가속 2년 후 경화 시간Curing time after 2 years of |
3분 25초3 |
2분 30초2 |
3분 50초3 minutes 50 |
2분 43초2 minutes 43 seconds |
변화 시간(가속2년-가속0년)Time of change ( |
1분 52초1 minute 52 seconds |
28초28 |
1분 53초1 minute 53 seconds | 21초21 seconds |
변화율rate of change | 120%120% | 23%23% | 97%97% | 15%15% |
표 3 및 도 3을 참고하면, 실시예의 인상재 조성물은 변화율 100%미만을 타나내었고, 특히 도 2의 기표면적이 가장 적게 나타났던 실시예 3의 변화율이 15%로 가장 우수하게 나타났고, 장기 보관함에도 불구하고 큰 변화가 없어 보관안정성이 우수함을 나타내었다.Referring to Table 3 and FIG. 3, the impression material composition of Example showed a change rate of less than 100%, and in particular, the change rate of Example 3, which had the smallest surface area in FIG. 2, was 15%, which was the most excellent. There was no significant change despite storage, indicating excellent storage stability.
전술한 본 명세서의 설명은 예시를 위한 것이며, 본 명세서의 일 측면이 속하는 기술분야의 통상의 지식을 가진 자는 본 명세서에 기재된 기술적 사상이나 필수적인 특징을 변경하지 않고서 다른 구체적인 형태로 쉽게 변형이 가능하다는 것을 이해할 수 있을 것이다. 그러므로 이상에서 기술한 실시예들은 모든 면에서 예시적인 것이며 한정적이 아닌 것으로 이해해야만 한다. 예를 들어, 단일형으로 설명되어 있는 각 구성 요소는 분산되어 실시될 수도 있으며, 마찬가지로 분산된 것으로 설명되어 있는 구성 요소들도 결합된 형태로 실시될 수 있다.The above description of the present specification is for illustrative purposes, and those skilled in the art to which one aspect of the present specification pertains can easily be modified into other specific forms without changing the technical spirit or essential features described in the present specification. you will be able to understand Therefore, the embodiments described above should be understood as illustrative in all respects and not limiting. For example, each component described as a single type may be implemented in a distributed manner, and similarly, components described as distributed may be implemented in a combined form.
본 명세서의 범위는 후술하는 청구범위에 의하여 나타내어지며, 청구범위의 의미 및 범위 그리고 그 균등 개념으로부터 도출되는 모든 변경 또는 변형된 형태가 본 명세서의 범위에 포함되는 것으로 해석되어야 한다.The scope of the present specification is indicated by the following claims, and all changes or modifications derived from the meaning and scope of the claims and equivalent concepts should be interpreted as being included in the scope of the present specification.
Claims (11)
- 말단이 비닐기로 치환된 V폴리다이메틸실록산; 및V polydimethylsiloxane having a vinyl group substituted at the terminal; andSi-H 함량이 3~4.5mmol/g인 오르가노하이드로겐폴리실록산을 포함하는, 치과용 인상재 조성물.A dental impression material composition comprising an organohydrogenpolysiloxane having a Si-H content of 3 to 4.5 mmol/g.
- 제1항에 있어서,According to claim 1,상기 V폴리다이메틸실록산의 함량이 30~60중량부이고, The content of the V polydimethylsiloxane is 30 to 60 parts by weight,상기 오르가노하이드로겐폴리실록산의 함량이 5~10중량부인, 치과용 인상재 조성물.The content of the organohydrogenpolysiloxane is 5 to 10 parts by weight, dental impression material composition.
- 제1항에 있어서,According to claim 1,상기 말단이 비닐기로 치환된 V폴리다이메틸실록산은,V polydimethylsiloxane in which the terminal is substituted with a vinyl group,25℃ 점도가 100~500cP인 제1 V폴리다이메틸실록산;1st V polydimethylsiloxane having a 25° C. viscosity of 100 to 500 cP;25℃ 점도가 750~1500cP인 제2 V폴리다이메틸실록산; 및 a second V polydimethylsiloxane having a 25° C. viscosity of 750 to 1500 cP; and25℃ 점도가 5000~25000cP인 제3 V폴리다이메틸실록산을 포함하는, 치과용 인상재 조성물.A dental impression material composition comprising a 3-V polydimethylsiloxane having a viscosity at 25° C. of 5000 to 25000 cP.
- 제3항에 있어서,According to claim 3,상기 제1 V폴리다이메틸실록산의 함량은 10~15중량부이고,The content of the first V polydimethylsiloxane is 10 to 15 parts by weight,상기 제2 V폴리다이메틸실록산의 함량은 20~25중량부이며,The content of the second V polydimethylsiloxane is 20 to 25 parts by weight,상기 제3 V폴리다이메틸실록산의 함량은 10~15중량부인, 치과용 인상재 조성물.The content of the third V polydimethylsiloxane is 10 to 15 parts by weight, dental impression material composition.
- 제1항에 있어서,According to claim 1,상기 오르가노하이드로겐폴리실록산의 Si-H 함량 및 상기 말단이 비닐기로 치환된 V폴리다이메틸실록산의 비닐 함량의 비(Si-H/비닐)가 1.5~3인, 치과용 인상재 조성물.The ratio (Si-H / vinyl) of the Si-H content of the organohydrogenpolysiloxane and the vinyl content of the V polydimethylsiloxane whose terminal is substituted with a vinyl group (Si-H / vinyl) is 1.5 to 3, dental impression material composition.
- 제5항에 있어서,According to claim 5,상기 치과용 인상재 조성물에 경화시킨 석고 모형의 기포면적이 20% 이하인, 치과용 인상재 조성물.The dental impression material composition, wherein the bubble area of the gypsum model cured in the dental impression material composition is 20% or less.
- 제1항에 있어서,According to claim 1,폴리다이메틸실록산, 필러, 촉매제 및 경화지연제로 이루어진 군에서 선택된 하나 이상을 더 포함하는, 치과용 인상재 조성물.A dental impression material composition further comprising at least one selected from the group consisting of polydimethylsiloxane, a filler, a catalyst and a curing retardant.
- 제7항에 있어서,According to claim 7,상기 폴리다이메틸실록산 0~1중량부, 상기 필러40~70중량부, 촉매제 0~2중량부 및 경화지연제 0~1중량부를 포함하는, 치과용 인상재 조성물.A dental impression material composition comprising 0 to 1 part by weight of the polydimethylsiloxane, 40 to 70 parts by weight of the filler, 0 to 2 parts by weight of the catalyst and 0 to 1 part by weight of the curing retardant.
- 제7항에 있어서,According to claim 7,상기 촉매제는 백금계 또는 팔라듐계인, 치과용 인상재 조성물.The catalyst is a platinum-based or palladium-based, dental impression material composition.
- 제7항에 있어서,According to claim 7,상기 필러는 무기 필러 및 비정질 합성 필러로 이루어진 군에서 선택된 하나 이상인, 치과용 인상재 조성물.The filler is at least one selected from the group consisting of inorganic fillers and amorphous synthetic fillers, dental impression material composition.
- 제1항에 있어서,According to claim 1,상기 인상재 조성물은 37℃ 경화 시간이 2~3분인, 치과용 인상재 조성물.The impression material composition has a 37 ° C. curing time of 2 to 3 minutes, a dental impression material composition.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002537023A (en) * | 1999-02-18 | 2002-11-05 | カー コーポレイション | Curable silicone impression material modified to hydrophilic |
JP2002541167A (en) * | 1999-04-08 | 2002-12-03 | デンツプライ インターナショナル インコーポレーテッド | Improved polyvinylsiloxane impression material |
KR101543335B1 (en) * | 2014-04-29 | 2015-08-12 | (주) 베리콤 | Composition for Dental Impression Materials of Improved Mechanical Properties |
WO2015167038A1 (en) * | 2014-04-29 | 2015-11-05 | (주) 베리콤 | Dental impression material composition with improved mechanical property |
KR101674067B1 (en) * | 2015-04-23 | 2016-11-08 | (주) 베리콤 | Composition for dental impression material having improved scanning performance and mechanical property, and dental impression material comprising the same |
-
2021
- 2021-12-08 KR KR1020210174649A patent/KR20230086219A/en not_active Application Discontinuation
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- 2022-05-27 WO PCT/KR2022/007580 patent/WO2023106519A1/en unknown
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002537023A (en) * | 1999-02-18 | 2002-11-05 | カー コーポレイション | Curable silicone impression material modified to hydrophilic |
JP2002541167A (en) * | 1999-04-08 | 2002-12-03 | デンツプライ インターナショナル インコーポレーテッド | Improved polyvinylsiloxane impression material |
KR101543335B1 (en) * | 2014-04-29 | 2015-08-12 | (주) 베리콤 | Composition for Dental Impression Materials of Improved Mechanical Properties |
WO2015167038A1 (en) * | 2014-04-29 | 2015-11-05 | (주) 베리콤 | Dental impression material composition with improved mechanical property |
KR101674067B1 (en) * | 2015-04-23 | 2016-11-08 | (주) 베리콤 | Composition for dental impression material having improved scanning performance and mechanical property, and dental impression material comprising the same |
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