JPS5835105A - Two liquid composition for dental impression material preparation, manufacture of impression material and impression material thereby - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a two-component composition for preparing a dental impression agent, a method for manufacturing an impression agent using the same, and an impression agent obtained thereby.

An impression agent for making an impression of the part where a partial denture (p & rial d@ntur axis) is to be made, an impression agent for manufacturing a prototype model in orthodontic treatment, or an impression agent for making an impression of the part where a partial denture (p & rial d@ntur axis) is to be made, an impression agent for manufacturing a prototype model in orthodontic treatment, or an oral cavity where a complete denture is required (@
Alginic acid compositions have been used in the field of dentistry for a long time as impression agents for making primary impressions (nl@ntulous mouth) and as orthodontic materials for secondary impressions of all types. There is.

Thermoreversible hydrocolloid, which is mainly composed of agar, can be made into a gel by heating and fluidizing the material and then lowering the temperature, but unlike that, alginate compositions are made into gel through a chemical reaction. be able to. Once an alginate gel is formed, it cannot be changed back into a fluid state or sol state by physical means, and therefore alginate is known as a thermoirreversible hydrocolloid. The use of alginate in the field of dental treatment A/y -y a') 7
'y, (Ralph Ph1llips) (7
) Author (Elsmenta of l1listental)
(see Chapter 9).

Alginate compositions made for use in dental treatments are typically formulated as a powder suitable for mixing with water to prepare a viscous sol. This sol is placed in an impression tray (1xpr*5m1ont) inside the oral cavity.
ray), where it undergoes a series of chemical reactions to form an elastic gel.

After gel formation is complete, the gel impression is removed from the mouth and used to create a denture.

Examples of powdered alginate impression agents that have been used in the past include those containing the following composition.

The important ingredients in this composition are 12% potassium alginate (wt%, same hereinafter), 74% diatomaceous earth, 12% calcium sulfate dihydrate and 2% sodium phosphate. It is a water-soluble potassium alginate. When this powdered alginate composition is mixed with water, the water-soluble alginate reacts with calcium sulfate to form a gel-like substance consisting of insoluble calcium alginate. Since this reaction must occur and be completed within the oral cavity, the reaction must be delayed until the water-added composition is delivered into the oral cavity and added to the impression tray. In order to efficiently delay this reaction and save a reasonable amount of time,
Reaction retarders such as sodium phosphate are included in the composition. It is believed that the effect of this reaction retarder is produced by the following mechanism. That is, before calcium sulfate reacts with water-soluble alginate, it first reacts with sodium phosphate, and as long as sodium phosphate is present, the gelation reaction caused by water-soluble alginate and calcium sulfate is prevented.

Fillers such as diatomaceous earth (nu@r) have also been added to the composition, which can increase the strength and firmness of the gel, allowing it to roll over non-stick hard surfaces.

The final structure of the resulting gel is a network of brush deposits of calcium alginate fibers, retaining excess water and filler internally.

Conventional powdered alginate compositions have several inherent properties. One problem is that the water used to prepare the gel usually contains minerals such as calcium and iron salts, which alter the concentration of the desired divalent metal ions during use. That's true. The presence of this additional metal ion can cause particle agglomeration during mixing, non-uniform gel formation, and even have an adverse effect on curing time control. This type of openness is particularly large in areas where the supplied water has a high mineral concentration or where the mineral concentration of the supplied water varies throughout the day.

The second component found in conventional powdered alginate compositions is
The interval is related to the temperature of the water used in preparing the gel. This is because this temperature is one of the major factors in determining the gelling or curing time.

Generally, the gel time of an alginate composition is inversely proportional to the temperature of the water added. As the temperature of the water increases, the gelation time decreases. Similarly, if the fluidity or flowability of the material is such as to be measured, the same relationship arises for the temperature of the mixing water. That is, the duration of fluidity is inversely proportional to the temperature of the water. Flowability is one of the important properties of materials. This is because the impression material must have sufficient fluidity to move into the tissue and provide intimate contact and an accurate impression. The alginate composition is designed to cure typically in 2 to 6 minutes when mixed with water at a temperature of 72 degrees Fahrenheit. However, in most regions the temperature of the supplied water varies from day to day or within the day, making it difficult to control flow properties and curing times.

Also, to minimize inaccuracies due to impression shrinkage as a result of water volatilization, stone dye must be quickly applied to conventional alginate impression materials. Must be.

Furthermore, the shelf life of powdered alginate compositions has been limited.

That is, under high temperatures, in the presence of moisture, or both, powdered alginate compositions deteriorate such that when water is added, they do not cure at all or cure occurs too quickly. . This problem is particularly exacerbated by the presence of small amounts of water in each of the ingredients used in making the composition.

Thus, until the alginate is ready for use, it is separated from the divalent metal ions and the water is self-retained in the composition, thereby avoiding the aforementioned impediments regarding changes in water temperature and dissolved mineral ions. It would be desirable to provide an alginate system in which the system is formed of a humectant (--oimt) and a plasticizer, with improved stability and impression accuracy.

That is, the present invention provides: (1) an aqueous paste composition containing an alkali metal alginate selected from the group consisting of sodium alginate, potassium alginate, and mixtures thereof; and an alkali metal alginate in the composition. About 0.5 to 1.2 parts of a slightly water-soluble divalent metal salt per 1 part of the salt (parts by weight, same hereinafter) and about 0.02 to 0.16 parts per 1 part of the divalent metal salt. A two-component composition for preparing a dental impression agent, comprising Composition 1, which contains a reaction retardant and is made into a paste by using about 0.75 to 2 parts of a fluid plasticizer to 11 parts of the divalent metal #1. Regarding.

Examples of the alginate alkali metal salts used in the present invention include sodium alginate, potassium alginate, and mixtures thereof.

Whereas conventional powdered alginate compositions require the use of a small amount of calcium salt and a relatively low molecular weight alkali metal alginate to facilitate dissolution of the calcium salt and alkali metal alginate during use. According to the present invention, relatively large amounts of calcium salts and high molecular weight alkali metal alginate salts can be used, since these salts are predissolved as described below, thereby providing stronger gel strength. What can be done with alginate impression materials? Alginate alkali metal salts can be obtained from seaweed ash and they generally have a molecular weight of about 32,000 to 250,000. Alginic acid is a type of polysaccharide in which the carboxylic acid groups of each molecule of β-D+Yunneuron remain free and the aldehyde groups are glycosidic bonded between molecules, and it has a pyranose ring! A linear form of neuronic acid is a remer.

The divalent metal salt that can react with the alginate alkali metal salt to provide a curable dental composition is preferably a slightly water-bathable and non-toxic salt, such as calcium sulfate,
Iron sulfate, zinc sulfate, calcium oleate, furin m
ferrous stearate or mixtures thereof. A particularly effective divalent metal salt is calcium sulfate.

The divalent metal salt is generally about 0.6 to 1.2 parts, preferably about 0.75 to 1.0 parts per part of the alkali metal alginate.
Use the amount of parts.

The reaction retarder used in the present invention is contained in the two-component composition containing the divalent metal salt, but may also be contained in the composition containing the alginate alkali metal salt.

This reaction retarder regulates the rate of reaction between the divalent metal salt and the alkali metal alginate, giving the impression material appropriate working and curing times. Examples of the reaction rate retarder include sodium phosphate, potassium phosphate, sodium birophosphate, potassium birophosphate, sodium citrate, potassium citrate, trisodium silicate, tripotassium silicate, or mixtures thereof. .

When the reaction retarder is added to a composition containing a divalent metal ring, it is usually added in an amount of about 0.02 to 0.0% per part of the divalent metal salt.
．． 1! It is included in an amount of i part, preferably 0.04 to 0.08 part. When the reaction retarder is added to the composition containing the alkali metal alginate, it may be contained in an amount of about 0.02 to 0.08 parts per part of the alkali metal alginate.

The plasticizer contained in the composition containing the divalent metal salt and used as a fluid medium may be a monohydric alcohol, a polyhydric alcohol, a vegetable oil, a light oil, a light silicone oil, or a mixture thereof. Specific examples of monohydric alcohols or polyhydric alcohols include oleyl alcohol, propylene glycol, polyether glycol, and glycerol. The fluid plasticizer is usually used in an amount of about 0.75 to 2 parts, preferably 0.9 to 1.5 parts, per part of the divalent metal salt. Preferred mixtures of fluid plasticizers include, for example, mixtures of glycerol and light silicone oil or mixtures of glycerol and light silicone oil.

The gel strength of alginate impressions can be increased by including metal oxides in the composition on the divalent metal salt side. Metal oxides that can be used include zinc oxide and oxide! Gnesium or a mixture thereof, generally used in an amount of about 0.02 to 1 part, preferably about 0.08 to 0.6 part, per part of divalent gold II4#1. Attempts to include metal oxides in alginate compositions tend to be unsuccessful because when water is added to the powder, the metal oxides affect the solubility of the sodium alginate and the aqueous medium This is because it becomes difficult to mix the powder smoothly in the mixture, and furthermore, there is a tendency for the aqueous composition to become granular.

The filler is preferably contained in the alkali metal alginate composition. Specific examples of fillers that can be used include:
Examples include diatomaceous earth, silica, talc or mixtures thereof.

A particularly preferred filler is diatomaceous earth.

The filler is usually used in an amount of about a to 10 parts, preferably about 5 to 8 parts per part of the alkali metal alginate.

Water is added to the alginate alkali metal salt composition, thereby providing aqueous fluidity to the alginate alkali metal salt component and aqueous conditions to produce an insoluble alginate by interaction of the alginate alkali metal salt and the divalent metal salt. will be granted. Water is usually about 13 to 25 parts, preferably about 15 to 21 parts, per part of alginate alkali metal salt.
Use the amount of parts.

A reaction retarder selected from the group consisting of phosphoric acid, vinyl phosphoric acid, citric acid, and silicic acid sodium salts, potassium salts, and mixtures thereof can be included in the alginate alkali metal salt composition, but is not limited thereto. An amount of about 0.02 to 0.08 parts, preferably about 0.03 to 0.06 M, is used per part of the alginate alkali metal salt.

Moisture is removed from the alginate alkali metal salt composition.
It is preferred to add a humectant (hum·0-t) to improve the accuracy of the impression. Specific examples of humectants that can be used include glycols such as propylene glycol, polyether glycol and diethylene glycol, sugar alcohols such as sorbitol, sugars such as dextrose, or mixtures thereof. Humectan F is usually used in an amount of about 0.1 to 1 part, preferably about 0.15 to 0.5 part, per part of the alkali metal alginate.

Hereinafter, the composition containing the alginate alkali metal salt will be referred to as 1 composition M1, and the composition containing the divalent metal salt will be referred to as 1 composition B1. Compositions M and 1 consist of dry and liquid components and thus form a thin paste. These pastes can be removed from a suitable container and easily and smoothly mixed into a curable composition in the oral cavity. When used, compositions M and B contain about 0.0 parts of divalent metal salt per 1 part of alginate alkali metal salt.
5 to 1 part is mixed. Specifically, by mixing 4 parts by volume of Composition A with 1 part by volume of Composition B, the alkali metal salt of alginate and 2 parts by volume are mixed in the above weight ratio.
Valance metal salts can be mixed.

Next, the present invention will be explained in more detail with reference to Examples and Comparative Examples, but the present invention is not limited only to these Examples.

In Examples 1 to 4 that follow, compositions A and B
was prepared by stirring the dry and liquid ingredients into a thin paste with a high speed stainless steel stirrer. These compositions contain 4 parts of component B and 4 parts of component B1.
By mixing parts by volume, it was possible to determine the weight ratio of alginate alkali metal salt and divalent metal salt convenient for the reaction. Also, the properties of compositions A and B are such that their (1
) The shell 7 rye before mixing (selfllf・) and (b) the difficulty of mixing were evaluated, and the composition after mixing compositions M and B was evaluated by its (4) curing time and (g) 72° y.
It was evaluated based on the dehydration rate. Compositions M and 1 were mixed by hand in a plastic bowl. Cure time was measured as the time for the flowable composition to convert into a tack-free gel. In addition, the dehydration rate was calculated from the weight change of the composition within a specific period of time.

Example 1 (Composition M) Sodium alginate 11 parts, diatomaceous earth 84 parts, Bita potassium phosphate 1 part, dextrose 2 parts, diethylene glycol 2NS, water 150 parts, trace amount of preservative, trace amount of fragrance (composition B) Oxidation! 5 parts of silica, 45 parts of calcium sulfate, 4 parts of potassium pyruphosphate, 55 m of glycanol, 5 parts of silicone oil, 16 parts of diatomaceous (1) Shell 7 Lie 7; Good (B) Difficulty in mixing; Very (7) Curing time: 3 minutes (B) Dehydration rate (60 minutes): 0.4% by weight Example 2 (Composition M) 11 parts of sodium alginate, 84 parts of diatomaceous earth, biw
1 part potassium nonaphosphate, 4 parts diethylene glycol, 1 part water
50 parts, trace amount of preservative, trace amount of fragrance (composition B) 5 parts of magnesium oxide, 45s of calcium sulfate, 4 parts of pyrophosphate, 65 parts of glyceryl, 5 parts of silicone oil, 6 parts of diatomaceous earth (1) Shell 7 Lie 7; Good (difficulty in homogeneous mixing; very easy (4) Curing time: 16 minutes (b) Dehydration rate (60 minutes): 0.5% by weight Example 6 (Composition A) 12 parts of sodium alginate, 86 parts of diatomaceous , 2 parts of potassium pyrophosphate, 1501S water, trace amount of tlj preservative,
Trace amount of fragrance (composition B) 5 parts of magnesium oxide, 45 parts of calcium sulfate, 4 parts of potassium pyrophosphate, 55 parts of glycerol, 5 parts of silicone oil, 6 parts of diatomaceous earth (υ Shell 7 Lie 7; Good (B) mixing) #l Easy; Very easy (b) Curing time! &, 5 minutes (b) Dehydration rate (60 minutes > 1.9*ji) Example 4 (Composition) Potassium alginate 11 parts, diatomaceous earth 50 parts, 0.5 parts of Biken sodium phosphate, 5 parts of sorbitol, 2 parts of Butan pyrene glycol, 150 m of water, 0.4 parts of fragrance, 0.2 parts of preservative (composition 1) 50 parts of calcium sulfate, 4 parts of sodium phosphate part, glyceryl 60 parts, silica 11 parts (1) Shell 7 Lie 7: Good (B) Difficulty of mixing: Very easy (does not form lumps) (2)
Curing time: 6 minutes (B) Dehydration rate (60 minutes'): 0.2 weight ≦ Example 5 (Composition M) Potassium alginate 20 parts, talc 50 parts, polyphosphorus fluorium 6 parts, sorbitol 10 parts, Composition A, which consisted of 120 parts of water, a trace amount of fragrance, a trace amount of coloring agent, and a trace amount of preservative, was a putty-like and extremely viscous composition.

The following Examples 6 to 11 show each component of the vine composition used as component 1 and the amount added thereof.

Example 6 50 parts of calcium sulfate, 2 parts of potassium pyrophosphate, 68 parts of pyrene glycol, 10 parts of zinc oxide Example 7 50 parts of calcium sulfate, 2 parts of sodium pyrophosphate, 55 parts of diethylene glycol, 8 parts of zinc oxide Example 8 60 parts of sulfur mM, 4 parts of Bita sodium phosphate, 50 parts of glyceryl, oxidation! 5 parts of gnesium, 9 parts of diatomaceous earth,
2 parts of sodium heptadide Example 9 50 parts of calcium sulfate, 6 parts of sodium phosphate, 2 parts of glycerol, 40 parts of mineral oil, 5 parts of magnesium oxide Example 10 60 parts of calcium sulfate, 4 parts of birulin, 34 parts of silicone oil , zinc oxide 1.5 parts, zinc heptadide 0.
5 parts Example 11 Calcium sulfate 10 parts, sodium birophosphate 0.5 parts
s, oleyl alcohol 55 parts, magnesium II chloride 1
Comparative Example 1 A composition having the following components was blended and prepared according to a conventional method.

(Powdered composition) 11 parts of sodium alginate, 60 parts of diatomaceous earth, 1 part of potassium pyrophosphate, 5 parts of dextosheath, 2 parts of diethylene glycol, 1411s of calcium sulfate, 2 parts of potassium titanium fluoride, 5 parts of magsium oxide, preservative A small amount of agent, a small amount of fragrance Immediately after preparation, a portion of this composition was taken out and mixed with an appropriate amount of water, and the curing time was determined to be 6 minutes. The remaining composition was left for 6 months at 55% humidity.
Thereafter, the shelf life before mixing with water, the difficulty of mixing with water, and the curing time were investigated. As a result, the composition that had been left agglomerated in the container, and when water was added and mixed, it became grainy and difficult to mix. The curing time of the composition was 1.5 minutes. This deterioration of Shell 7 Lie 7 is believed to be due to calcium sulfate reacting with a considerable amount of sodium pyrophosphate due to absorption of moisture.

Comparative Example 2 This comparative example shows that when the alkali metal alginate composition (composition M) contains a metal oxide and a bimetallic salt (a salt having two metal ions), the shelf life is relatively short. It shows that it gets worse over time.

(Composition A) 10 parts of sodium alginate, 60 parts of diatomaceous earth, 0.6 parts of sodium phosphate, oxidized! 10 parts of gnesium,
Potassium titanium heptadide 0.5 parts, fructose 6 parts, glycerol 7 parts, water 140 parts, trace amount of fragrance, trace amount of coloring agent,
Composition A4 volume immediately after preparing a small amount of preservative and after being left for 30 days □
The resulting system was mixed with 1 part by volume of Composition B of Example 1 and the resulting system was examined for ease of mixing, curing time and compressive strength. The results are shown in Table 1.

Chapter 1 Table

Claims (1)

[Scope of Claims] 1. (1) An aqueous paced composition containing an alkali metal alginate mass derived from the group consisting of sodium alginate, potassium alginate and mixtures thereof, and alginic acid of the composition. About 0.5 to 1.2 parts by weight of a slightly water-bathable divalent metal base per 1 part by weight of the alkali metal salt and about 0.02 parts by weight per 1 part by weight of the divalent metal salt.
Composition B contains ~0.13 parts by weight of a reaction retardant and is made into a paste with 0.75 to 2 parts by weight of a fluidity plasticizer per 1 part by weight of the divalent metal salt. A two-liquid composition for preparing dental impression agents. 2 Composition 1 is an alginate alkali metal salt 1
A two-part composition according to claim 1 containing about 0.5 to 0.75 parts by weight of a slightly water-soluble divalent metal salt. 6 Composition 1 is about 0.0% per 1 part by weight of the divalent metal salt.
The two-part composition according to claim 1, containing 0.04 to 0.08 parts by weight of a reaction retarder. 4 Composition 1 is about 0.9 parts by weight of the divalent metal salt
2. The two-part composition of claim 1, wherein the two-component composition is pasted with ~1.5 parts of a flowable plasticizer. 5. The method according to claim 1, wherein the divalent metal salt is one from the group consisting of calcium sulfate, ferrous sulfate, zinc sulfate, divalent metal salts of ferrous sulfate, and mixtures thereof. Two-part composition. 6. The two-part composition according to claim 5, wherein the divalent metal salt is calcium sulfate. 7 The reaction retarder is phosphoric acid) 13um, potassium phosphate, sodium birophosphate, potassium birophosphate,
2, which is a package selected from the group consisting of sodium citrate, potassium citrate, sodium silicate, potassium silicate, and mixtures thereof;
liquid composition. 8 ii from the group where the fluidity plasticizer is a mixture of monohydric alcohol, polyhydric alcohol, II compound M, light oil, light silicone oil, and soft straw! The two-liquid composition according to claim 1, which is one of the known two-component compositions. 9. The two-liquid composition according to claim 8, wherein the fluid 1M agent is glycerol. 10 Composition B contains about 0.02 to 1 part of the metal oxide selected from the group consisting of zinc oxide, multilayered magnesium, and mixtures thereof, per part of the divalent metal salt. Claim 1: The two-part composition according to claim 1. 11 Composition: Approximately 1 part by weight of alginate alkaline earth metal salt! 1 to 10 parts by weight of filler and about 16
2. A two-part composition according to claim 1, containing ~25 parts by weight of water. 12. The two-part composition according to claim 11, wherein the composition contains about 0.02 to 0.08 parts by weight of a reaction retarder per 1 part by weight of the alkali metal alginate. 16. The two-pot composition of claim 12, wherein the composition contains about 0.1 to 1 part by weight of hiemectant per 1 part by weight of the alginate alkali metal salt. i4 (i) Sodium alginate, an aqueous paste composition A containing an alginate alkali metal ring selected from the group consisting of potassium alginate and mixtures thereof, and (b) 1 weight of the alginate alkali metal salt of the composition A. about 0.5 to 1.2 parts by weight of a slightly water-soluble divalent metal salt per part and about 0.5 to 1.2 parts by weight of i1! divalent metal salt.
Composition 1 contains 02 to 0.13 parts by weight of a reaction retardant, and is made into a paste with about 0.75 to 2 parts by weight of a fluid plasticizer per 1 part by weight of the divalent metal salt. A method for producing a dental impression agent, comprising allowing two-component compositions to interact with each other. 15 The divalent metal salt is calcium sulfate, sulfur g! 1I
15. The method for manufacturing Ill according to claim 14, wherein the 1111m is selected from the group consisting of jl11-iron, zinc sulfate, divalent metal salts of Ababa Kama, and mixtures thereof. 16. The manufacturing method according to claim 15, wherein the divalent metal salt is calcium sulfate. 17 11 fl Reaction retardant is from the group consisting of sodium phosphate, potassium phosphate, sodium pyrophosphate, potassium pyrophosphate, sodium citrate, potassium citrate, sodium silicate, potassium silicate and mixtures thereof. 15. The production method according to claim 14, which is a seed. 18. The manufacturing method according to claim 14, wherein the fluid plasticizer is one type excluded from the group consisting of monohydric alcohol, polyhydric alcohol, l111[1, light oil, light silicone oil, and mixtures thereof. . 19. The manufacturing method according to claim 18, wherein the fluid plasticizer is Guriryu-pol. 20 Composition 1 contains 1 part by weight of the divalent metal salt, zinc oxide, oxide! 15. The method of claim 14, comprising about 0.02 to 1 part by weight of a metal oxide selected from the group consisting of basesium and mixtures thereof. 21 The composition contains about 3 to 10 parts by weight of filler and about 16 to 25 parts by weight of alginate alkali metal salt.
Claim 114. Contains parts by weight of water. Manufacturing method described in section. 22. The method according to claim 21, wherein the composition contains about 0.02 to 0.08 parts by weight of a reaction retarder per 1 part by weight of the alkali metal alginate. 26. The method of claim 22, wherein Composition A contains about 0.1 to 1 part by weight of hyomectant per 1 part by weight of the alginate alkali metal salt. 24 (i) an aqueous paste composition containing an alkali metal salt of alginate selected from the group consisting of sodium alginate, calylum alginate, and mixtures thereof; and (b) algin #alkali metal salt 1 of the composition. about 0.5 to 1.2 parts by weight of a slightly water-bathable divalent metal salt and about 0.02 parts by weight of the divalent metal salt.
Composition 1 containing ~0.16 parts by weight of a reaction retarder and made into a paste with about 0.75 to 2 parts by weight of a fluid plasticizer per 1 part by weight of the divalent metal salt. A dental impression agent obtained by making liquid compositions interact with each other.