JPS6072811A - Production of living pulp capping and root canal filler - Google Patents

Abstract

PURPOSE:To obtain an intermediate condensate for the titled filler without irritation nor discoloration for a long period, by reacting a phenol with formaldehyde in the presence of sulfuric acid or zinc sulfate as a catalyst at a specific temperature, washing thoroughly the reaction product with water, and adding glucose thereto. CONSTITUTION:A mixture of a phenol, e.g. guaiacol, creosote or eugenol, with an alcohol-soluble vegetable fat or oil, e.g. castor oil, or an ester interchange material of the above-mentioned fat or oil is reacted with formaldehyde or a polymer thereof in the presence of sulfuric acid or zinc sulfate as a catalyst in the atmosphere of an inert gas under heating at 100-130 deg.C to give a thick malt syrup. The resultant thick malt syruplike polymer is then washed with water to 7pH, and an adequate amount of glucose is added thereto to afford an intermediate condensate. Calcium hydroxice alone or a composition, obtained by roasting a powder prepared by mixing the calcium hydroxide as a main component with an X ray contrast medium, and consisting essentially of calcium oxide is added to the above-mentioned condensate to give the aimed filler used for cutting living pulp.

Description

DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for producing a vital dental pulp covering and root canal filling agent used when cutting vital dental pulp.

(Prior Art) This type of filler has been researched by the same applicant for many years in this field, and as a result, for example,
No. 8197 (Patent No. 212308), Special Publication No. 1973-3
No. 9834 (Patent No. 637507), Special Publication No. 46-4
No. 757 (% Permit No. 621124), Special Publication No. 1983-1985
No. 13 (Patent No. 793126) and patent application 1980-1980
There are issues such as No. 66. These inventions have undergone repeated improvements, and the invention disclosed in Japanese Patent Application No. 8066/1983 is particularly excellent in terms of irritating properties and inhibition of discoloration.

To summarize these inventions related to the same applicant, when reacting a phenol such as guaiacol with formaldehyde, the transesterification using an alcohol-soluble vegetable oil or the same vegetable oil and a polyhydric alcohol. When using a starch syrup-like intermediate condensate obtained by adding and reacting a starch syrup with water and purifying it (hereinafter simply referred to as an intermediate condensate), it is mainly composed of pure calcium hydroxide or calcium oxide, and an X-ray contrast agent is added to it. It is used by adding powder and kneading it.

The problem with the filler prepared in this way is that it becomes reddish brown after a long period of use, and that it has a slight irritating effect.

In order to solve this problem, the invention of the earlier application proposed that formaldehyde t When reacting with the polymer, an appropriate amount of ethanol is added to the reaction system, and the reaction compositions such as phenol, formaldehyde, vegetable oil, or their transesterified products are dissolved into each other using ethanol as a medium, resulting in a uniform reaction. The goal was to create a system.

However, in actual use, the irritation was significantly reduced and discoloration was suppressed for a long time;
After 0 years, discoloration started to be seen, albeit slightly locally.

This is probably because there is a small portion in the reaction system where phenol does not completely react, and this unreacted portion oxidizes and discolors over a long period of time.

(Purpose of the Invention) The present invention was made to solve the above-mentioned problems, and its purpose is to eliminate the unreacted portion of phenols, completely eliminate irritating properties, and produce living dental pulp that does not change color even over a long period of time. The present invention aims to provide a method for manufacturing a root canal filling agent that also serves as a root canal filling agent.

(Structure of the Invention) 3- The present invention, which has been made to achieve the above object, uses a divalent or trivalent organic acid alone or a mixture thereof as a catalyst, and an organic acid other than the above organic acid, an inorganic acid or Using one or a mixture of two or more of these salts as a cocatalyst, phenols such as guaiacol, creosote, and eugenol alone or a mixture of one or more of these salts are combined with an alcohol-soluble vegetable oil or the like. A starch syrup-like intermediate condensate obtained by adding a transesterified product of vegetable oil and fat with a polyhydric alcohol and reacting it with formaldehyde or its polymer is washed with water, purified, and subjected to X-rays using calcium hydroxide alone or mainly containing calcium hydroxide. In a method for producing a living dental pulp capping agent and root canal filling agent, which comprises roasting a powder mixed with a contrast agent to convert the calcium hydroxide into calcium oxide, and kneading the mixture into a paste form. Sulfuric acid or sulfuric acid 4-zinc is used as a catalyst when formaldehyde or its polymer is reacted with the above phenols and an alcohol-soluble vegetable oil or a transesterified product of the vegetable oil with a polyhydric alcohol. , set the heating temperature to 100°C to 130°C, heat in an inert gas atmosphere until it becomes starch syrup-like, wash the starch syrup-like polymer with water until the pH reaches 7, and add an appropriate amount of glucose. A method for producing a dental pulp covering and root canal filling agent characterized by the fact that polymerization progresses by using sulfuric acid or zinc sulfate as a catalyst and by setting the heating temperature in the range of 100°C to 130°C. Almost all unreacted parts are eliminated, and a colorless polymer is obtained. At the same time, discoloration during polymerization is prevented by creating an inert gas atmosphere, subsequent discoloration is suppressed by adding glucose, and by washing with water to pH 7. The stimulation is gone.

(Example) The phenols used in the present invention include guaiacol, creosote, cresol, eugenol, and resorcinol, and the use of guaiacol and eugenol is most effective. Formaldehyde may also be used as a polymer such as formaldehyde.

The alcohol-soluble vegetable oil used in the method of the present invention is castor oil, and the raw materials for the transesterified vegetable oil used in this condensation reaction include castor oil, soybean oil, peanut oil, Examples include olive oil, and polyhydric alcohols include glycerin, polyethylene glycol, and propylene glycol. In the transesterification reaction, the above fats and oils and polyhydric alcohols are blended in approximately equal amounts, and a catalyst such as saturated zinc sulfate is added to the mixture in an amount of about 10 to 10%.
Add 20CC.

The catalyst used in the condensation reaction between phenols and aldehydes used in the method of the present invention includes divalent or trivalent organic acids such as oxalic acid, tartaric acid, and citric acid, or monovalent sulfuric acid of about 18%
f is added. Furthermore, a certain amount of heat is applied during the reaction between the phenols and the aldehyde. This heating temperature is 100
°C or higher but not exceeding 130 °C, and is heated and stirred in an inert gas atmosphere to avoid discoloration during heating. The stirring time is about 50 minutes to 1 hour to make it into starch syrup.
It is washed several times with water and then the water is removed to maintain the starch syrup state.

The root canal filling agent of the present invention thus obtained, that is, the intermediate condensate, is actually used by kneading it with a composition powder mainly composed of calcium oxide. The pot life for this mixture to solidify is 8 to 10 minutes, which is sufficient and appropriate time for general treating physicians, and it does not cause discomfort due to irritation even when filled into the root canal. Not only was it observed that there was no discoloration at all, but it was also observed that even over a long period of time, the filled area often became even partially discolored to reddish brown.

Next, specific examples 1 to 8 of the present invention are summarized and listed in one table as follows.

The mixture of each of the above examples is heated at 100°C or above J-130°C.
Thereafter, the mixture is reacted for about 1 to 1.5 hours with stirring in an inert gas atmosphere such as nitrogen gas at around 120°C, and the reaction is stopped when the mixture becomes starch syrup-like.

In this case, if the heating temperature is below 100°C, the reaction will be slow to accelerate and unreacted portions will remain, resulting in discoloration and irritation.
If the temperature exceeds 130°C, the reaction will be rapid, but discoloration will occur due to heating, which is not preferable in either case.

The viscosity of the starch syrup-like mixture thus reacted is approximately 50,000 to 70,000 cps. The vegetable oil or transesterified vegetable oil may be added from the beginning of the reaction, or may be added during the reaction. The reaction product in the form of starch syrup is washed with purified water several times until the pH reaches 7 to completely remove the remaining catalyst, and then the moisture is sufficiently removed by means such as suction depressurization. Leave only. In order to further prevent discoloration at a later date, an appropriate amount (0.4~
After mixing the paste with about 5 g of glucose, it is stored tightly as a paste, avoiding air circulation, moisture, and light.

On the other hand, a composition powder mainly composed of calcium oxide contains an Elakis radiation contrast agent, and its composition is as follows.

Calcium hydroxide 20-907 (preferably around 507) Zinc oxide approximately 207 Barium sulfate approximately 307 Calcium hydroxide alone or the above composition is 540-7
Calcium hydroxide is converted into calcium oxide by roasting in air at 50°C, and the activated calcium agent is stored in a hermetically sealed manner in the same manner as above.

(Effect of the invention) The above-mentioned intermediate condensate paste and powder active calcium agent are used by kneading them, and after kneading, they are immediately filled or applied to the affected area. be. For example, it is effective in treating diseases of the pulp or plate end tissue when filling an infected root canal, for example, in an old socket of a pulped tooth, when covering the pulp wound surface (called pulp capping) when cutting a living tooth pulp, or when filling an infected root canal. , has sufficient disinfection effect to prevent reinfection, and
It is excellent for the treatment and disinfection of dental diseases, and as a covering material when cutting the living tooth pulp.Furthermore, its basic principle of bonding and solidifying with tooth calcareous material is that it is able to form inside the canaliculus in the tooth dentin through the ion exchange effect of calcium ions. [The intermediate condensate obtained by this method gradually penetrates deeply, and the intermediate condensate itself undergoes non-condensation and hardens itself to form a strong bond.This also kills the bacteria that have invaded the tubules in the tooth dentin. It goes without saying that it must be tightly sealed to prevent it from being infected or re-entering the outside world, thus completely preventing re-infection, but its manufacturing temperature is 100°C to 130°C.
Even if the polymerization reaction is carried out at a temperature of It has an excellent effect.

In addition, by washing the starch syrup-like intermediate condensate with water until the pH reaches 7, the remaining catalyst is removed, resulting in excellent effects such as a long life with almost no irritation to the affected area.

Claims (1)

[Claims] A divalent or trivalent organic acid alone or a mixture thereof is used as a catalyst, and an organic acid other than the above-mentioned organic acids, an inorganic acid, or a mixture of two or more of these salts is used as an auxiliary catalyst. Sort, phenols such as eugenol alone or a mixture of one or more of these are added with an alcohol-soluble vegetable oil or a transesterified product of the same vegetable oil with a polyhydric alcohol to produce formaldehyde or its heavy The starch syrup-like intermediate condensate resulting from the coalescence reaction is washed with water and purified, and before use, the calcium hydroxide alone or a powder containing mainly calcium hydroxide mixed with an X-ray contrast agent is roasted to convert the calcium hydroxide into calcium oxide. In the method for manufacturing a dental pulp capping agent and root canal filling agent, which consists of mixing in a state where the pulp is mixed and kneading it into a coating form, alcohol-soluble vegetable oil or the same vegetable oil is added to the above phenols. Formaldehyde LC is added to a transesterified product with a polyhydric alcohol, and when the polymer is reacted, sulfuric acid or zinc sulfate is used as a catalyst, and the heating temperature is 100°C to 130°C in an inert gas atmosphere. This method for producing a dental pulp capping agent and root canal filling agent is characterized by heating the polymer until it becomes like starch syrup, washing the starch syrup-like polymer with water until the pH becomes 7, and adding an appropriate amount of glucose.