JPH06116126A - Production of salt granule - Google Patents

Abstract

PURPOSE:To highly efficiently and simply produce the salt granules suitable for adding to tooth pastes. CONSTITUTION:The method for producing the salt granules is characterized by mixing salt particles with a water-insoluble substance having a melting point of >=30 deg.C and simultaneously heating the mixture to granulate and/or coat the salt particles with the water-insoluble substance.

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 salt granules, and more particularly to a method for producing salt granules which is excellent in treatment / prevention of periodontal diseases and which is suitable for dentifrice formulation.

[0002]

2. Description of the Related Art Conventionally, the problems to be solved by the invention
Dentifrice containing salt for the purpose of treatment / prevention of periodontal disease is commercially available.However, increasing the amount of salt in the dentifrice to improve the above-mentioned treatment / prevention results in increased saltiness. It will give a pleasant feeling.

Various attempts have been made to reduce the saltiness. For example, a method of mixing sodium malate with salt in a dentifrice (JP-A-56-83415) and a method of blending salt with a large particle size (Japanese Patent Publication No. 3-212).
No. 2) is known.

However, in the method described in Japanese Patent Laid-Open No. 56-83415, the optimum salt content is 9% by weight, and there is an upper limit to the content. On the other hand, in the method described in Japanese Patent Publication No. 3-2111, saltiness is high. Are not sufficiently reduced and the texture of the particles is not good. Further, a method of blending granulated and coated salt granules with a toothpaste is disclosed in JP-A-55-153709, but salt is not reduced here because salt is used as a coating agent. .

Therefore, it has been desired to develop a method for producing salt granules for blending dentifrice, which does not cause unpleasant saltiness by blending high-concentration salt and has a good feeling.

[0006]

Means for Solving the Problems As a result of intensive investigations in view of such circumstances, the present inventors have found that salt particles are uncomfortable when they are granulated and / or coated with a water-insoluble substance having a melting point of 30 ° C. or higher. It was found that salt granules for blending dentifrice with reduced saltiness and excellent treatment / prevention of periodontal disease can be obtained, and the present invention has been completed.

That is, according to the present invention, salt particles have a melting point of 3
The present invention provides a method for producing salt granules, which comprises heating the salt particles while mixing with a water-insoluble substance at 0 ° C or higher to granulate and / or coat the salt particles with the water-insoluble substance.

The present invention further comprises adding a heated melt of a water-insoluble substance having a melting point of 30 ° C. or higher or an organic solvent solution to the flowing salt particles, and granulating and / or coating the salt particles with the water-insoluble substance. The present invention provides a method for producing salt granules, which comprises:

As used herein, the term "granulation" refers to the production of granules in which two or more salt particles are aggregated by the action of a water-insoluble substance, and the term "coating" refers to single particles of salt or Covering all or part of the surface of two or more aggregates with a water-insoluble substance.

The method for producing salt granules of the present invention will be described below. The salt particles and the water-insoluble substance powder are mixed and heated in a granulating and / or coating device described later to granulate and / or coat the salt particles with the water-insoluble substance to obtain salt granules. The temperature for granulating and / or coating the salt particles is preferably at least the softening point of the water-insoluble substance. The heating method is not particularly limited, and examples thereof include a method of supplying hot water, steam and the like to the jacket of the granulating and / or coating apparatus, a method of supplying warm air to the apparatus, and the like.

Even if the heated and melted liquid of the substance is added and mixed instead of the powder of the water-insoluble substance and then cooled, the organic solvent solution of the substance is added and mixed, and then the organic solvent is dried.
May be removed.

The addition of the heated melt of the water-insoluble substance or the organic solvent solution is poured into the fluidized salt particles as it is,
It can be carried out by a method such as dropping or spraying with a spray nozzle.

Cooling can be carried out by blowing cold air into the granulating and / or coating apparatus, feeding cold water into the jacket of the apparatus, or the like.

The organic solvent can be dried and removed by a method of ventilating air, an inert gas or the like into the apparatus, or sending heated air, an inert gas or the like.

The granulating and / or coating apparatus used in the present invention may be any one capable of mixing salt particles and a water-insoluble substance, such as a stirring granulator, a fluidized bed granulator,
A stirred fluidized bed granulator or the like can be used. High speed mixer (Fukae Industry Co., Ltd.)
Vertical granulator (Pawrec Co., Ltd.)
Manufactured), CF granulator (Freund Industrial Co., Ltd.)
As a fluidized bed granulator, such as a flow coater (manufactured by Freund Industrial Co., Ltd.), a spray granulator (manufactured by Aeromatic Co., Ltd.), a powder coater (manufactured by Paulec Co., Ltd.), etc. Examples of the granulator include New Marmelizer (manufactured by Fuji Paudal Co., Ltd.), Spiraflow (manufactured by Freund Sangyo Co., Ltd.), and multiplex granulator (manufactured by Paulex Co., Ltd.).

The salt particles used in the present invention have a weight average particle diameter of 10 to 2000 μm, preferably 20 to 1000.
μm, more preferably 30 to 600 μm. If the weight average particle size is less than 10 μm, it is difficult to handle because salt is highly hygroscopic and easily aggregates, and its specific surface area is large, and a large amount of water-insoluble substance is required to reduce saltiness. Defects such as appear. On the other hand, 20
When salt granules obtained by granulating and / or coating salt particles having a diameter of more than 00 μm are blended in a dentifrice, a discomfort is felt during brushing, which is not preferable.

The shape of the salt particles is preferably a cube or a shape close to a cube because granulation and / or coating is easy.

The water-insoluble substance used in the present invention has a melting point of 30 ° C. or higher, preferably 30 to 130 ° C. If the melting point is less than 30 ° C, the salt granules are collapsed because the water-insoluble substance is softened or melted when the temperature exceeds 30 ° C in summer and the expected effect cannot be obtained. Also,
When the melting point is higher than 130 ° C., the water-insoluble substance is likely to solidify, and thus a coarse lump is likely to be formed, which may deteriorate the operability.

The content of the water-insoluble substance in the salt granules obtained by the method of the present invention is 5 to 95% by weight (hereinafter referred to simply as%).
), Preferably 5 to 70%. If it is less than 5%, the saltiness cannot be sufficiently reduced, while 95
Even if it is compounded in excess of%, the effect cannot be increased.

Specific examples of the water-insoluble substance having a melting point of 30 ° C. or higher include oils and fats such as hydrogenated castor oil and hydrogenated rapeseed oil, lauric acid, myristic acid, palmitic acid, stearic acid,
Fatty acids such as arachidic acid, carnauba wax, candelilla wax, spermaceti wax, beeswax, beeswax, polyoxyethylene beeswax, polyethylene wax, salasimon tan wax, ceresin, polyoxyethylene sorbit beeswax, microcrystalline wax, mokuro,
Rice bran wax, waxes such as synthetic hydrocarbon wax, higher alcohols such as myristyl alcohol, cetyl alcohol, stearyl alcohol, eicosyl alcohol, behenyl alcohol, sorbitan monopalmitate, sorbitan monostearate, sorbitan distearate, sorbitan tristearate, sorbitan Sorbitan fatty acid ester such as monobehenate, stearic acid monoglyceride, stearic acid diglyceride, stearic acid monodiglyceride, oleic acid monoglyceride, oleic acid monodiglyceride, oleic stearic acid monodiglyceride, etc. monodiglyceride, polyethylene glycol monostearate, polyethylene glycol Distearate, ethylene glycol distearate, propylene Include polyhydric alcohol fatty acid esters such as glycol monostearate, and the like, preferably a higher alcohol consisting of sorbitan fatty acid ester or an alkyl group having 16 or more carbon atoms consisting of 16 or more fatty acid group having a carbon. As the water-insoluble substance, one kind or a mixture of two or more kinds can be used.

For the purpose of improving the efficiency of granulation and coating by lowering the apparent viscosity of the water-insoluble substance, a solution of the water-insoluble substance in an organic solvent can be used.

The organic solvent used for the above purpose may be one which can dissolve a water-insoluble substance, and may be one kind or a mixture of two or more kinds. Specific examples include methanol, ethanol, propanol, xylene, hexane, methylene chloride, ethyl acetate and the like.

The content of the water-insoluble substance in the organic solvent is
It is preferably 1 to 98%. If it is less than 1%, the amount of solvent is so large that it is necessary to enhance the drying ability, which is uneconomical. On the other hand, when it is 98% or more, the apparent viscosity of the water-insoluble substance is not significantly decreased, which is not preferable.

The salt granules thus obtained have a weight average particle size of 50 to 5000 μm, preferably 80 to 2000 μm.
m, more preferably 100 to 700 μm. If the weight average particle size is less than 50 μm or more than 5000 μm,
When the salt granules are blended with a dentifrice, a good feel cannot be obtained during brushing.

[0025]

INDUSTRIAL APPLICABILITY According to the present invention, salt granules suitable for blending with dentifrice can be easily produced with high efficiency. A dentifrice prepared by incorporating such salt granules has a therapeutic / preventive effect on periodontal diseases, has a significantly reduced unpleasant saltiness, and has a good feel during brushing.

[0026]

EXAMPLES The present invention will be described in detail below with reference to examples, but the present invention is not limited thereto. In each example, the weight average particle size is JIS Z
It was measured using a standard sieve of 8801.

Example 1 425 g of salt particles (weight average particle size; 300 μm) and 75 g of sorbitan tristearate (melting point; 54 ° C.) powder
High speed mixer (Fukae Industry Co., Ltd .; LSS-
(GS-1J type), and hot water of 50 ° C. was passed through the jacket while stirring (650 rpm) to raise the temperature. Inner temperature is 4
After raising the temperature to 5 ℃, change the hot water to cooling water (tap water) at 35 ℃.
The salt particles were granulated and coated with sorbitan tristearate by cooling to. The composition of the obtained sodium chloride granules was 84.2% of sodium chloride and 15.8% of sorbitan tristearate, and the weight average particle diameter was 330 μm.
It was m. Most of the obtained salt granules were single salt particles coated with sorbitan stearate.

Example 2 1000 g of salt particles (weight average particle diameter; 400 μm) were added to a CF granulator (manufactured by Freund Sangyo Co., Ltd .; CF).
-360) and melted with stirring (170 rpm) at 90 ° C. hydrogenated castor oil (melting point 85-87 ° C.) 5
00g was sprayed using a spray nozzle (spray pressure 1.
0 kg / cm ² ) and salt particles were granulated and coated with hydrogenated castor oil. The composition of the obtained salt granules was 68.8 for salt.
%, Hydrogenated castor oil 31.2%, and the weight average particle diameter was 470 μm. The majority of the obtained salt granules were single salt particles coated with hydrogenated castor oil.

Example 3 800 g of salt particles (weight average particle diameter 55 μm) were added to Spiraflow (manufactured by Freund Industrial Co., Ltd .; SFC-LAB).
O), and air (40 ° C.) was supplied from the bottom of the granulator and stirred (350 rpm) to flow the salt particles. From a spray nozzle equipped on the bottom wall of the granulator, an organic solvent solution of a water-insoluble substance (sorbitan tristearate 15%, xylene 70%, ethanol 15%) 1400
g was sprayed at 6.5 g / min at an air pressure of 1.0 kg / cm ² , and salt particles were granulated and coated while being dried. The composition of the obtained sodium chloride granules was 81.6% sodium chloride and 18.4% sorbitan tristearate, and the weight average particle diameter was 24.
It was 0 μm. Most of the obtained salt granules are
It was composed of two or more salt particles and was coated with sorbitan tristearate.

Example 4 500 g of sodium chloride particles (weight average particle diameter 150 μm) were added to Numa-Marmelizer (Fuji Paudal Co., Ltd .; NQ-GM).
Mould), and warm air at 35 ° C from the bottom of the fluidized bed to 0.1 m ³
Blown salt particles were made to flow at a flow rate of / min. 2500 g of an organic solvent solution of a water-insoluble substance (stearyl alcohol (melting point 58 ° C.) 10%, ethanol 90%) is sprayed at 11.0 g / min and an air pressure of 2.0 kg / cm ² from a spray nozzle at the center of the bottom of the fluidized bed and dried. While salt particles were granulated and coated. The composition of the obtained salt granules was 66.
4%, stearyl alcohol 33.6%,
The weight average particle diameter was 270 μm. Most of the obtained salt granules consisted of two or more salt particles and were coated with stearyl alcohol.

Experimental Examples 1 to 4 and Comparative Experimental Example Dentifrice compositions 1 to 4 (Experimental Examples 1 to 4) containing the salt granules obtained in Experimental Examples 1 to 4 whose compositions are shown below and salt particles as they are. The blended toothpaste composition 5 (Comparative Experimental Example) was prepared according to a conventional method.

[0032]

[Table 1] Toothpaste composition 1 (Experimental example 1) (wt%) Granules prepared in Example 1 (salt; 25.0%) 29.7 Sorbitol 14.0 Glycerin 8.0 Sodium carboxymethylcellulose 1.5 Lauryl Sodium sulfate 2.0 Saccharin sodium 0.1 Dicalcium phosphate 28.0 Perfume 0.8 Water balance

[0033]

[Table 2] Toothpaste composition 2 (Experimental example 2) (wt%) Granules prepared in Example 2 (sodium salt; 25.0%) 29.8 Sorbitol 14.0 Glycerin 8.0 Sodium carboxymethylcellulose 1.5 Lauryl Sodium sulfate 2.0 Saccharin sodium 0.1 Dicalcium phosphate 30.0 Perfume 0.8 Water balance

[0034]

[Table 3] Toothpaste composition 3 (Experimental example 3) (wt%) Granules prepared in Example 3 (salt; 25.0%) 30.6 Sorbitol 14.0 Glycerin 8.0 Sodium carboxymethylcellulose 1.5 Lauryl Sodium sulfate 2.0 Saccharin sodium 0.1 Dicalcium phosphate 30.0 Perfume 0.8 Water balance

[0035]

[Table 4] Toothpaste composition 4 (Experimental example 4) (% by weight) Granules prepared in Example 4 (salt; 25.0%) 37.7 Sorbitol 14.0 Glycerin 8.0 Sodium carboxymethylcellulose 1.5 Lauryl Sodium sulfate 2.0 Saccharin sodium 0.1 Dicalcium phosphate 35.0 Perfume 0.8 Water balance

[0036]

[Table 5] Toothpaste composition 5 (comparative experimental example) (% by weight) Special grade purified salt (average particle size 300 µm) 25.0 Sorbitol 14.0 Glycerin 8.0 Sodium carboxymethyl cellulose 1.5 Sodium lauryl sulfate 2.0 Saccharin sodium 0.1 Dicalcium phosphate 40.0 Fragrance 0.8 Water balance

With respect to the dentifrice compositions 1 to 5 obtained in Experimental Examples 1 to 4 and Comparative Experimental Example, 10 panelists evaluated the tightness and saltiness of the gums according to the following criteria. The results are shown in Table 6.

Tightening of gums: Good; it feels tight. Normal; I feel a little tight. Bad; does not feel tight.

Saltiness: good; just right. Normal; Slightly salty. Poor; salty and uncomfortable.

[0040]

[Table 6]

As is clear from the results shown in Table 6, in the examples (Experimental Examples 1 to 4) in which the salt granules produced by the present invention were blended in the dentifrice composition, the feeling of tightening of the gums, which is the medicinal effect of salt, was observed. It can be seen that unpleasant saltiness is reduced while maintaining.

Claims (2)

[Claims] 1. A method for producing salt granules, which comprises heating salt particles and a water-insoluble substance having a melting point of 30 ° C. or higher while mixing to granulate and / or coat the salt particles with the water-insoluble substance. . 2. A salt solution that is melted by heating or melting a water-insoluble substance having a melting point of 30 ° C. or higher or an organic solvent solution to granulate and / or coat the salt particles with the water-insoluble substance. And a method for producing salt granules.