JPS6353161B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention relates to improvements in dental eugene cement. Eugenol cement has been widely used and commercially available as a temporary sealing cement in dental treatment. Conventional Eugenol cement is a cement consisting of two components: a composition whose main ingredient is a zinc compound (hereinafter referred to as the base) and a composition whose main ingredient is Eugenol (hereinafter referred to as the Eugenol agent), and zinc oxide was used as the zinc compound. . For example, the product of Company A has a base of 60% zinc oxide, 25% rosin, and 15% calcium hydroxide, and contains Eugenol.
The composition consists of USP Eugenol (manufactured by Neo Kogyo Seiyaku Co., Ltd.), and the base of Company B's product is zinc oxide 70.
%, rosin 28% and zinc acetate 1 as a small additive
% and coloring agent 1%, and the eugenol agent is composed of 70% clove oil, 26% rosin, and 4% olive oil. There are various other products on the market, but the base is 60-75% zinc oxide, 20-30% rosin, etc.
%, and many also contain small amounts of zinc stearate and zinc acetate as additives. Eugenol agents are often mixtures of clove oil, olive oil, eugenol, viscosity modifiers, and the like. In these conventional products, the base is prepared as a powder or paste, and the eugenol agent is often prepared as a liquid when the base is a powder, and as a paste when the base is a paste. To use the dental eugenol cement prepared in this way, appropriate amounts of the base and eugenol agent are each weighed and kneaded together using a spatula on a glass plate. Generally speaking, temporary sealing cement must have contradictory properties such as sealability and removability, as well as weak bactericidal and analgesic effects, but conventional eugenol cement has insufficient sealing properties. As a result, infections often occur after temporary sealing, and in order to prevent this, it is necessary to add powerful disinfectants such as paraformaldehyde and parachlorophenol. In addition, the base of the above conventional product contains small amounts of additives such as zinc acetate and zinc stearate in addition to zinc oxide and rosin, and is made of a powder mixture of three or more components, so a homogeneous composition can be obtained. Therefore, during use, there were large variations in setting time during kneading, sealing properties and strength after curing, and stable performance could not be obtained. Furthermore, it has not been possible to obtain a mixing ratio of the eugenol agent and the base that satisfies both the workability of unhardened cement during mixing and the physical properties of cement after hardening. In other words, unless the mixing ratio of Eugenol agent/base is extremely small, the curing speed will be slow, which will reduce the sealing properties, and the product will become dry and almost powder-like, making it difficult to work with and difficult to fill into the affected area. Therefore, it must be pushed into the affected area with putty, and on the other hand, increasing the mixing ratio of Eugenol agent/base agent improves workability, but the setting time becomes longer and the strength after hardening is insufficient, making it difficult to use properly. The disadvantage was that it was difficult to obtain a suitable blending ratio. The present invention improves the above-mentioned drawbacks of conventional products and provides a dental eugenol cement that has good sealing properties and good workability. Therefore, the gist of the present invention is that in a dental eugenol cement consisting of two components, a composition containing a zinc compound as a main ingredient and a composition containing eugenol as a main ingredient, the zinc compound of the composition containing a zinc compound as a main ingredient is combined with calcium. Calcium Zinc Hydroxide Hydrate, a hydrate of zinc
(OH) ₃ ] ₂ ·2H ₂ O), and the composition containing the zinc compound as a main ingredient is a dental eugenol cement characterized in that it contains rosin. The present invention will be explained in detail below. In the present invention, calcium zinc hydroxide hydrate, which is used instead of zinc oxide in conventional products, is a hydrate of calcium and zinc, and X-ray diffraction reveals that the structural formula is Ca[Zn
(OH) ₃ ] ₂・2H ₂ O has been confirmed.
However, the base material in the present invention is the above-mentioned calcium.
It is manufactured by adding other ingredients to zinc hydroxide hydrate and pulverizing it, and is used either as a powder or by kneading it with 5-10% olive oil to form a paste. calcium
Other ingredients added to zinc hydroxide hydrate are not particularly limited;
It is preferable to use only rosin, and for example, a combination of 65 to 75% calcium zinc hydroxide hydrate and 25 to 35% rosin is suitable. In this way, the base powder consisting of only two components, calcium zinc hydroxide hydrate and rosin, has a small number of components, so it is mixed uniformly, and since there are no small amounts of additives, uniformity is ensured, making it easy to use. Variations in setting time during kneading with Eugenol agent, sealing properties after curing, strength, etc. are small, and stable performance can be obtained. In the above case, if the calcium zinc hydroxide hydrate content is less than 65%, there will be a large amount of unreacted parts of the eugenol agent during kneading, making it difficult to cure, and if it is more than 75%, workability during kneading will be poor. Become. Next, the eugenol agent used in the present invention is not particularly limited, and conventional eugenol agents can be used, but those containing clove oil, olive oil, and rosin as main ingredients and containing orthoethoxybenzoic acid. is preferred. For example, clove oil 65-75%, olive oil 3-5%, rosin 20%
A formulation of ~30% and 1-10% orthoethoxybenzoic acid is preferred. However, the above-mentioned eugenol agent is used as a liquid when the base is a powder. When the base is a paste, the amount of rosin is further increased, for example, 60 to 70% clove oil, 30 to 40% rosin, and 1 to 5% orthoethoxybenzoic acid are kneaded together and the eugenol agent is used as a paste. In the present invention, since calcium zinc hydroxide hydrate is used as the main ingredient of the base, workability and setting time can be adjusted by adjusting the composition of the eugenol agent. That is, if the amount of clove oil is too much than the above, the stickiness will only increase during kneading and there will be no special effect, while workability and filling properties will deteriorate, and if it is too little than the above, the stickiness will be insufficient and filling will not be possible. Moreover, if the amount of olive oil is too much than the above amount, the coagulation during kneading will be delayed so much that it becomes unusable, and if it is too less than the above amount, the workability and filling properties will be poor. If the rosin exceeds the above 30%, it exceeds the solubility in the Eugenol solution, causing a paste-like precipitate and cannot become liquid, and if the rosin exceeds 20%, coagulation will be delayed during kneading. Also, if the rosin exceeds the above 40%, the total amount of rosin will be too large when kneaded.
It promotes coagulation too much and impairs workability. Next, when orthoethoxybenzoic acid is added in the above-mentioned appropriate amount, it has the effect of improving workability for a certain period of time after kneading, shortening the time from the beginning of stiffness to hardening, and making the rise of the hardening curve steeper. When filling or adhering the Eugenol cement of the present invention to the affected area, it has particularly good workability and filling properties.
Moreover, in order to complete curing within 1 to 3 minutes after filling, the components of the Eugenol agent must be clove oil 68
~72%, olive oil 3-5%, rosin 25-27%,
Particularly preferred is 1 to 3% orthoethoxybenzoic acid. As mentioned above, the eugenol cement of the present invention has extremely good reactivity between the base and the eugenol agent, and is particularly easy to work with before filling or bonding the affected area. It is characterized by rapid hardening and good sealing properties and improved strength characteristics after hardening. This is because when the plate-shaped diamond-shaped crystals of calcium zinc hydroxide hydrate form a chelate with the eugenol agent, they form a chelate like a tempura roll, which has been observed using an electron microscope. This is thought to be because complete chelation occurs instantaneously after a certain period of time after kneading. Since complete chelation is performed in this way, the sealing properties are greatly improved. In addition, since the main ingredient of the base is calcium zinc hydroxide hydrate rather than zinc oxide, the specific gravity is significantly lower at 1.32 to 1.38 compared to 1.7 to 2.3 for conventional products, which reduces the feeling of foreign body when filling teeth. becomes less. Furthermore, the Eugenol cement of the present invention has superior strength properties compared to conventional products. That is, since the chelation occurs completely and instantaneously, the sustainability of compressive strength and adhesive strength from initial stage to long-term stage is excellent, and adhesive durability is particularly characteristic. Conventional products lose their adhesive strength after about 7 days and break down in the oral cavity.
For example, if the period of going to the dentist was extended even a little, or if some mechanical stimulation was applied, the porotu could peel off, but the product of the present invention prevents such accidents because it maintains the adhesive properties during filling for a long period of time. There isn't. In addition, the removability, which is another characteristic necessary for dental cement for temporary sealing, is good because the compressive strength is not so large, and it can be removed by scraping it off with a dental tool. Furthermore, in the present invention, since the base component can be made up of only two components, calcium zinc hydroxide hydrate and rosin, a uniform composition can be obtained upon mixing, which improves the workability of Eugenol cement before hardening. The properties of the cured product became uniform, and the setting time was 4.5 to 5.0 minutes, in one example, with very small variations. The effect of the eugenol cement of the present invention on sealing properties and other effects will be described in detail in Examples below. However, these Examples are merely illustrative of embodiments of the present invention and are not intended to limit the present invention. Example 1 Base: Calcium Zinc Hydroxide 67 g of hydrate and 33 g of rosin were mixed well, ground, and passed through a 200-mesh sieve to obtain a product. Eugenol agent: 69 g of clove oil, 25 g of rosin, 4 g of olive oil, and 2 g of orthoethoxybenzoic acid were mixed well to prepare a product. Example 2 Base: Calcium Zinc Hydroxide 70 g of hydrate and 30 g of rosin were mixed well, ground, and passed through a 200-mesh sieve to obtain a product. Eugenol agent: 65 g of clove oil, 30 g of rosin, 3 g of olive oil, and 2 g of orthoethoxybenzoic acid were mixed well to prepare a product. Example 3 Base: 10 g of olive oil was taken, 70 g of calcium zinc hydroxide hydrate and 30 g of rosin were added thereto, kneaded to form a paste, and the product was filled into a tube. Eugenol agent: Take 60 g of clove oil, 40 g of rosin, and 5 g of orthoethoxybenzoic acid,
The mixture was thoroughly kneaded and filled into a tube to produce a product. Experiment 1 The setting times of the Eugenol cements of the present invention obtained in Examples 1 to 3 above and the commercially available Eugenol cements of Companies A and B as comparative examples were each measured 12 times by the following experimental method, and the measured times were The range is shown in Table 1. 1 g of zinc agent and 0.4 ml of eugenol agent (Example 3)
In the case of a paste, take 0.5 g of Eugenol agent per 1 g of the base, knead for 30 seconds, and after 3 minutes have passed from the time you started kneading, mix it at a temperature of 37
Transfer to a thermostat at 100% relative humidity and weigh 300g.
Gently drop a Vicat needle (cross-sectional area of the needle: 1 mm ² ) onto the surface of the test piece (mixed Eugenol cement).
Check to see if any needle marks are left, and repeat the operation of gently dropping the Vicat needle onto the surface of the test piece until no needle marks are left.The time when no needle marks are left on the test piece is counted from the start of mixing. Let it be the setting time.

[Table] From Table 1, it can be seen that all of the Eugenol cements of the present invention have very small variations in setting time and are stable in quality. Experiment 2 The following measurements were carried out on the eugenol cements of the present invention obtained in Examples 1 to 3 above and the eugenol cements of companies A and B as comparative examples, and the measurement results are shown in Table 2. 1 g of base and 0.4 ml of eugenol (for the paste of Example 3, add 1 g of base to 0.4 ml of eugenol)
05g) was mixed for 30 seconds, and the adhesive strength, compressive strength, and specific gravity were measured.

[Table] From Table 2, all of the Eugenol cements of the present invention have lower specific gravity than conventional products, have higher adhesive strength and specific adhesive strength (adhesive strength/specific gravity) in long-term timber age, and are sustainable. I understand. However, the compressive strength is about 100Kg/ ^cm2 , which is not much different from the conventional product, and it can be seen that it has the same removability as the conventional product. Experiment 3 The results of the following experiment are shown in Table 3 for the eugenol cements of the present invention obtained in Examples 1 to 3 above and commercially available eugenol cements from companies A and B as well as company C as comparative examples. A glass tube with an inner diameter of 5 mm is cut into 5 cm lengths, and a 5 mm length area of the inner surface at the lower end of the tube is polished with a diamond point to make it rough. For paste 3, 0.5g of Eugenol agent per 1g of base)
It was filled with muddy eugenol cement mixed for 30 seconds and left for 10 minutes to completely harden. 7 of the total length of the glass tube that has been temporarily sealed and filled in this way.
The glass tube was filled with anhydrous copper sulfate powder up to the height of the fissure, and the upper end of the glass tube was closed with a dental temporary stopper and then fixed to a wooden frame. Prepare 10 such samples for each type of Eugenol cement, immerse the lower end of each tube in hot water at 37℃, observe for 10 days, and check the number of tubes whose copper sulfate turned blue due to water flow every day. Ta.

[Table] From Table 3, water was passed through all 10 bottles of Company A's product for 2 to 5 days, Company B's product for 4 to 7 days, and Company C's product for 6 to 9 days. Any product of the present invention
Even after 10 days, water did not pass through any of the tubes, which shows that the sealing properties are very good. Furthermore, there are 15 products of the present invention.
Although observation was continued until the third day, water did not pass through any of the samples.

Claims (1)

[Claims] 1. In a dental eugenol cement consisting of two components, a composition whose main ingredient is a zinc compound and a composition whose main ingredient is eugenol, the zinc compound of the composition whose main ingredient is a zinc compound is calcium, which is a hydrate of calcium and zinc. Calcium Zinc Hydroxide
Hydrate, Ca [Zn(OH) ₃ ] ₂・2H ₂ O),
A dental eugenol cement, wherein the composition containing a zinc compound as a main ingredient contains rosin.