JP3296474B2 - Manufacturing method of curing agent for impression material - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a curing agent for curing an impression material used for molding teeth and other molds.

[0002]

2. Description of the Related Art Alginate impression materials are generally used for molding teeth for restoring teeth. The alginate impression material utilizes the fact that an alginate as a base and calcium sulfate as a curing agent are kneaded with water to obtain a gel-like cured product.

[0003] Alginate impression materials are classified into two types, a powder type and a paste type, according to their packaging. The powder type is a type in which a base material and a curing agent are mixed in a powder state and kneaded with water at the time of use. On the other hand, the paste type is a type in which a base and a curing agent are separately kneaded with water in advance to form a paste, and the base paste and the curing agent paste are kneaded when used.

As a curing agent for such a paste-type alginate impression material, a curing agent comprising calcium sulfate as a main component and a poorly water-soluble liquid admixture and a surfactant has been proposed (Japanese Patent Laid-Open Publication (Kokai) No. 2002-284,837). 62-62020
JP-A-4-235109). It is also known to add magnesium oxide, phosphate and potassium fluorotitanate for the purpose of adjusting the curing time (Japanese Patent Laid-Open No. 4-235109).

[0005]

However, when a curing agent containing magnesium oxide is used as a curing agent for an alginate impression material, a certain curing time is exhibited if the curing agent is mixed with a base immediately after adjusting the curing agent. The present inventors have found that mixing with the base after storage for a long period of time causes a problem that the curing time is delayed. When the curing time changes depending on the storage time of the curing agent, the waiting time until curing in the impression material molding must be changed,
There is an inconvenience that the operation cannot always be performed under certain conditions. Therefore, there is a demand for a curing agent that does not delay the curing time even after long-term storage and keeps the curing time constant.

[0006]

Means for Solving the Problems The inventors of the present invention have conducted intensive studies in order to solve such problems, and as a result, a mixture of magnesium oxide, which is a component of a curing agent, and a surfactant was heated at 50 ° C.
It has been found that by heating to ~ 80 ° C , a good curing agent that overcomes the above problems can be obtained, and the present invention has been completed.

That is, the present invention provides a method for producing a curing agent for an impression material comprising calcium sulfate and / or lead silicate, a surfactant, magnesium oxide, and a poorly water-soluble liquid compound as main components. A method for producing a curing agent for an impression material, comprising heating a mixture of a surfactant and a surfactant to 50 to 80 ° C.

[0008]

DESCRIPTION OF THE PREFERRED EMBODIMENTS As calcium sulfate and / or lead silicate used in the present invention, known ones used for conventional impression materials are used without any limitation. Specific examples of particularly preferably used ones include calcium sulfate dihydrate, calcium sulfate hemihydrate, calcium sulfate anhydrous, and the like, alone or in combination. Further, lead silicate can be used alone or in combination with calcium sulfate.

As the surfactant used in the present invention, known surfactants can be used without any limitation, and anionic surfactants, cationic surfactants, amphoteric surfactants and nonionic surfactants can be used. Any of the activators can be used. Specific examples of the surfactant include anionic surfactants such as alkyl sulfonates, alkylbenzene sulfonates, and alkyl ether carboxylates. As cationic surfactants, alkylamine salts,
Quaternary ammonium salts and the like, and amphoteric surfactants include aminocarboxylates. Examples of the nonionic surfactant include polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene-polyoxypropylene block polymer, polyoxyethylene glycerin aliphatic ester, sucrose ester, and polyoxydiethylene amine. ,
Examples include block polymers of polysiloxanes and polyoxyethylenes.

In the present invention, nonionic surfactants such as polyoxyethylene alkyl ether, polyoxyethylene alkylphenyl ether and polyoxyethylene are particularly preferred as surfactants because of their great effect of keeping the curing time constant. -Use of a nonionic surfactant having a polyoxyalkylene chain such as a polyoxypropylene block polymer, a polyoxyethylene glycerin aliphatic ester, a polyoxydiethyleneamine, or a block polymer of a polysiloxane and a polyoxyethylene is preferably used. can do.

The amount of the surfactant used is not particularly limited, but it is necessary to uniformly mix the powder component constituting the curing agent and the poorly water-soluble liquid compound, and to knead the curing agent and the base material. In order to speed up the mixing of the curing agent and the base material, the amount is preferably 0.1 to 10 parts by weight, more preferably 0.5 to 5 parts by weight, per 100 parts by weight of calcium sulfate and / or lead silicate. It is preferably in parts by weight.

The magnesium oxide used in the present invention is:
This has the effect of shortening the curing time and reducing the difference between the curing start time and the curing end time. The amount of magnesium oxide to be used is not particularly limited. However, in order to adjust the curing allowance time from kneading to curing to an appropriate value to improve the operability of molding, calcium sulfate and / or lead silicate 100 are preferred.
It is preferably 5 to 50 parts by weight based on parts by weight.

Magnesium oxide includes light magnesia,
There are types such as heavy magnesia and magnesia clinker, and any magnesium oxide can be used.
Particularly, as the magnesium oxide effective for adjusting the curing time, light magnesia having a specific surface area of 100 to 200 m ² / g and an average particle diameter of 1 to 10 μm and having high reactivity is preferably used. Can be

In the present invention, the poorly water-soluble liquid compound is
An organic solvent having poor compatibility with water is used as a solvent for forming the curing agent into a paste. Especially water at 20 ° C 100
An organic solvent having a solubility in g of 5 g or less can be suitably used. Examples of the poorly water-soluble liquid compound include hydrocarbons, aliphatic alcohols, aromatic alcohols, fatty acids, salts or esters thereof, and hydrophobic polymers, and hydrocarbons are particularly preferably used. The hardly water-soluble liquid compound preferably has 6 or more carbon atoms for suppressing volatilization.

As the hydrocarbon, any of a chain type and a cyclic type can be used. Specific examples of hydrocarbons that can be suitably used in the present invention are as follows. For example, aliphatic chain hydrocarbons such as hexane, heptane, octane, nonane, decane, undecane, dodecane, tridecane, tetradecane, pentadecane, kerosene, 2,7-dimethyloctane, 1-octene, cycloheptane, cyclononane, liquid paraffin And other aliphatic cyclic hydrocarbons.

Examples of the aliphatic alcohol include saturated aliphatic alcohols such as 1-hexanol and 1-octanol, and unsaturated aliphatic alcohols such as citroneol and oleyl alcohol.

Examples of the aromatic alcohol include benzyl alcohol and meta-cresol.

Examples of the fatty acid include saturated fatty acids such as hexanoic acid and octanoic acid, and unsaturated fatty acids such as oleic acid and linoleic acid. Examples of fatty acid esters include ethyl octanoate, dibutyl phthalate, glyceride oleate, vegetable oils such as olive oil and sesame oil, and animal oils such as liver oil and whale oil.

Examples of the hydrophobic polymer include polysiloxane. Specific examples include polydimethylsiloxane, polymethylphenylsiloxane, polymethylhydrogensiloxane, and polyphenylhydrogensiloxane.

The amount of the above-mentioned poorly water-soluble liquid compound used is such that calcium sulfate and / or lead silicate are used in order to obtain a uniform paste, to have good fluidity, and to maintain good kneadability with the base. It is preferably from 10 to 200 parts by weight, more preferably from 30 to 150 parts by weight, per 100 parts by weight.

The most characteristic feature of the present invention is that at least a mixture of magnesium oxide and a surfactant among the components of the curing agent for an impression material is heated at a temperature of 50 ° C. to 80 ° C.

The heating time depends on the heating temperature, but the higher the heating temperature, the shorter the heating time. The heating time is generally 1
It is preferable to select in the range of hours to several days.

As a specific method for preparing the curing agent for an impression material of the present invention, the following method can be exemplified.
(1) After mixing the two components of magnesium oxide and surfactant with a kneader at room temperature, heating at a temperature of 50 ° C to 80 ° C ,
Other components calcium sulfate and / or lead silicate,
A method for producing a curing agent for an impression material by mixing with a poorly water-soluble liquid compound. (2) magnesium oxide which is the main constituent of impression materials for curing agents, surfactants, mixed calcium sulphate and / or lead silicate, a poorly water-soluble liquid compound at room temperature, followed by 5
A method of heating to 0 ° C to 80 ° C. (3) In the above (1) and (2), a method of mixing two components of magnesium oxide and a surfactant, or a main component of a curing agent for an impression material at 50 ° C to 80 ° C in addition to these two components. .

Since the curing agent for an impression material produced in the present invention easily absorbs moisture, it is preferable to store it in a glass container, a metal container, or an aluminum pack formed by laminating aluminum with a resin film, which does not easily transmit moisture.

As components other than the above, potassium fluoride titanate, phosphate, zinc oxide and the like may be added for adjusting the curing time. Further, an inert inorganic powder such as silica, titania, and alumina may be added as a filler. Furthermore, after mixing powders such as the above calcium sulfate, lead silicate, magnesium oxide, potassium fluoride titanate, and inert inorganic powder with a poorly water-soluble liquid admixture, the particles of these powders settle. In order to prevent this, ultrafine silica, titania, and zirconia having a primary particle diameter of 0.1 μm may be added. These ultrafine particles may be either those whose surface has been subjected to a hydrophobic treatment or those which have not been subjected to a hydrophobic treatment, or may be used as a mixture of both. In particular,
In order to enhance the dispersing effect, it is preferable to use ultrafine particles that have been hydrophobized. These ultrafine particles may be mixed with a surfactant and a poorly water-soluble liquid admixture simultaneously with each of the above powders. Particularly, in order to enhance the sedimentation prevention effect of the powder particles in the curing agent for the impression material, after mixing the powder particles, the surfactant, and the poorly water-soluble liquid admixture, these ultrafine particles are added,
Mixing is preferred.

As the mixing and kneading machine for producing the above-mentioned curing agent for an impression material, any known kneading machine can be used without any limitation. Specifically, it has a horizontal axis or a vertical axis such as a rotary container type mixing and kneading machine such as a ball mill, a ribbon mixer, a co-kneader, an internal mixer, a screw kneader, a Henschel mixer, a universal mixer, a Ledige mixer, a butterfly mixer and the like. A fixed container type mixing and kneading machine is exemplified. These mixing and kneading machines may be used alone or in combination. In particular, a method in which only the above powder is mixed in advance with a Loedige mixer and then mixed with a poorly water-soluble liquid admixture using a butterfly mixer is preferable because a uniform hardener can be produced in a short time.

[0027]

According to the method of the present invention, a curing agent for an impression material having a long curing time stable can be obtained. Further, the change in viscosity of the curing agent is also stabilized for a long period of time. Therefore, since the curing time is constant at the time of taking an impression, it can be safely removed after being placed in the oral cavity after a fixed time. Further, since the viscosity of the curing material is constant, it can be mixed and kneaded with the base with the same kneading property at all times, and an impression agent having uniform and stable properties can be obtained. Therefore, a precise impression surface can be obtained.

[0028]

The present invention will be described more specifically with reference to examples and comparative examples below, but the present invention is not limited to these examples. The curing time and storage stability shown in the following Examples and Comparative Examples were measured according to the following methods.

(1) Curing time The paste-like curing agent and the paste-like base were sufficiently mixed on a mixing paper. Then, the curing time was JIST-6505.
It was measured according to.

(2) Storage stability After the curing agent was stored at 40 ° C. for a predetermined time, it was kneaded with the base and the curing time was measured. The curing time before storage is taken as the initial curing time, and the difference from the curing time after storage is compared.
It is determined that the smaller the fluctuation, the higher the storage stability.

(3) Viscosity An appropriate amount of a curing agent was sampled, and the viscosity was measured at 23 ° C. using a high shear rheometer manufactured by Ishida Giken Co., Ltd.

Example 1 18 parts by weight of magnesium oxide (light magnesium oxide, average particle size 3.5 μm, specific surface area 146 m ² / g) and 9 parts by weight of a surfactant (polyoxyethylene oleyl ether) were stirred in a container. Mix well. The mixture was stored in a thermostat at 70 ° C. for 5 hours, and then 100 parts by weight of calcium sulfate (25 parts by weight of calcium sulfate dihydrate, 75 parts by weight of anhydrous calcium sulfate) and 17 parts by weight of granular silica were added to the mixture. , 50 parts by weight of liquid paraffin, 10 parts by weight of zinc oxide, 2 parts by weight of trisodium phosphate, 9 parts by weight of potassium fluorotitanate, and 5 parts by weight of ultrafine silica, and sufficiently mixed with a planetary mixer to form a paste. Was prepared.

On the other hand, 3.6 parts by weight of potassium alginate,
A paste base (pH 7.4) consisting of 9 parts by weight of silica powder, 0.3 parts by weight of potassium hydroxide, 1.8 parts by weight of polyacrylic acid, and 100 parts by weight of water was prepared.

Next, when the initial curing time was measured using the above-mentioned curing agent and base, it was 2 minutes and 38 seconds. Further, after the curing agent was stored at 40 ° C. for 90 days, the curing time was measured and found to be 2 minutes and 42 seconds. The curing time hardly fluctuated, indicating that the storage stability was high. The viscosity was 710 poise at the initial stage and 730 poise after storage, and hardly changed. The curing agent was sealed and stored in an aluminum pack.

Example 2 Same as Example 1, 18 parts by weight of magnesium oxide, 9 parts by weight of a surfactant (polyoxyethylene phenyl ether),
50 parts by weight of liquid paraffin, 100 parts by weight of calcium sulfate, and 17 parts by weight of granular silica were mixed at 80 ° C. for 3 hours to prepare a paste-like curing agent. The curing time and viscosity were 2 minutes 15 seconds and 660 poise at the initial stage, and 2 minutes 25 seconds and 670 poise after storage at 40 ° C. for 90 days, and hardly changed. The curing agent was sealed and stored in a glass container.

Example 3 Each component used in Example 2 was mixed at room temperature for 20 hours at 20 ° C., and this paste-form curing agent was placed in a 55 ° C. constant temperature bath.
The heat treatment was performed over a period of days. The curing time and viscosity were initially 2 minutes 1 second and 780 poise, and after storage at 40 ° C. for 90 days, 2 minutes 15 seconds and 790 poise, and hardly changed. The curing agent was sealed and stored in an aluminum pack.

Comparative Example 1 18 parts by weight of magnesium oxide of Example 1, 9 parts by weight of a surfactant (polyoxyethylene oleyl ether), 50 parts by weight of liquid paraffin, 100 parts by weight of calcium sulfate, 17 parts by weight of granular silica, zinc oxide 10 parts by weight, 2 parts by weight of trisodium phosphate, 9 parts by weight of potassium fluorotitanate, and 5 parts by weight of ultrafine silica were mixed well with a planetary mixer to prepare a paste-like curing agent.

Next, when the initial curing time was measured using the base of Example 1, it was 1 minute and 0 seconds. Further, after storing the curing agent at 40 ° C. for 21 days, the curing time was measured to be 2 minutes and 10 seconds. The cure time was significantly delayed. The viscosity was initially 650 poise, but was 9 after storage.
It had changed to 20 poise.

Example 4 18 parts by weight of magnesium oxide (light magnesium oxide, average particle size 4.1 μm, specific surface area 110 m ² / g), 9 parts by weight of a surfactant (polyoxyethylene oleyl ether), 100 parts by weight of calcium sulfate (Calcium sulfate 2
Water salt 25 parts by weight, calcium sulfate anhydrous salt 75 parts by weight),
17 parts by weight of granular silica, 50 parts by weight of liquid paraffin, 10 parts by weight of zinc oxide, 2 parts by weight of trisodium phosphate, 9 parts by weight of potassium fluorotitanate, and 5 parts by weight of ultrafine silica are put into a butterfly mixer at 75 ° C. Mix for 8 hours,
A paste-like curing agent was prepared.

Next, when the initial curing time was measured using the base material of Example 1, it was 2 minutes and 55 seconds. further,
When the curing time was measured after storing the curing agent at 40 ° C. for 90 days, the curing time was 3 minutes 03 seconds, and there was almost no change. The viscosity was 760 poise at the beginning and 780 poise after storage.

────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-6-56620 (JP, A) JP-A-6-32709 (JP, A) JP-A-62-265210 (JP, A) (58) Investigation Field (Int.Cl. ⁷ , DB name) A61K 6/10

Claims (1)

(57) [Claims] A method for producing a curing agent for an impression material comprising calcium sulfate and / or lead silicate, a surfactant, magnesium oxide, and a poorly water-soluble liquid compound as main components.
At least a mixture of magnesium oxide and surfactant
A method for producing a curing agent for an impression material, wherein the curing agent is heated to 50 to 80C .