JPS61176519A - Production of tablet - Google Patents

Abstract

PURPOSE:To obtain a tablet of a foamable composition storable stably until it is used by a consumer, by mixing an organic acid with polyethylene glycol in molten state, cooling and pulverizing the mixture, adding sodium (bi)carbonate thereto, and tableting the composition. CONSTITUTION:The objective tablet can be produced by mixing (A) 100pts.wt. of an organic acid essentially devoid of water of free from isolation of the water of crystallization at <=50 deg.C (e.g. citric acid, malic acid, succinic acid, etc.) with (B) preferably 2-10pts. of a plyethylene glycol (preferably having an average molecular weight of 4,000-20,000) under melting, cooling and pulverizing the mixture, adding sodium carbonate, sodium bicarbonate or other component thereto and tableting the obtained composition. When the above mixture is brought into contact with carbon dioxide gas, 1mol of sodium carbonate is converted to 2mol of sodium bicarbonate by the reaction with 1mol of water and 1mol of carbon dioxide gas. Accordingly, the water-content in the system is lowered and the stability of the product is further improved.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing tablets of an effervescent composition that has good storage stability and rapidly dissolves while effervescent carbon dioxide gas in water.

[Conventional technology]

Forming a compound containing a carbonate, bicarbonate and an organic acid into an effervescent/foaming composition by tabletting or granulation
It is applied to products such as cleaning agents, bath additives, bath water purifiers, and pool disinfectants. When Tora's products are added to water,
At the same time, its components have the advantage of quickly dissolving while generating carbon dioxide gas when they react, and they also have the effect of increasing the product value by giving consumers a comfortable feeling of use, especially in bath additives. The blood circulation promoting effect of carbon dioxide gas is actively utilized.

However, when a carbonate or bicarbonate and an organic acid coexist, a reaction occurs even with a small amount of water, and the internal pressure of the packaging container increases due to the generation of carbon dioxide gas, causing the container to swell.
In some cases, it may cause damage. When such a situation occurs, there is a strong possibility that not only the value of the product will be significantly damaged, but also the trust of consumers will be lost.

In order to obtain a stable product by completely mixing carbonate or bicarbonate with an organic acid, it is most important to thoroughly prevent the contamination of water. Therefore, during manufacturing, raw materials and processes are strictly controlled, and attention is paid to preventing moisture from entering. Furthermore, in order to keep the product stable until it is manufactured and used by consumers, the product is sealed and packaged to prevent moisture absorption. Despite this, it is difficult to say that the problem has been resolved.

In order to solve this problem, Japanese Patent Application Laid-open No. 58-213714 proposes a method in which a double salt of carbonate and mirabilite salt is prepared in advance into 111#, and an organic acid is mixed therein.

Furthermore, in JP-A-58-105910, 30 to 70% by weight of polyethylene glycol/LC (hereinafter abbreviated as PICG) with an average molecular weight of 950 to 3,700 is blended with 70 to 30% by weight of other foaming components. A method is disclosed in which the foaming component is then heated to melt the PEG and embed the foamable component in the PEG.

[Problems to be solved by the invention] However, mixing a large amount of ingredients in order to stabilize the product results in a corresponding decrease in the amount of carbon dioxide gas generated, which impairs the consumer's comfortable feeling of use. Not only that, but the amount of active ingredients that fulfill the purpose of the product will be reduced.
- The amount used per use also increases, resulting in higher costs. Bath additives that actively use the carbon dioxide gas generated,
In cleaning agents that utilize the generated foam, a reduction in the amount of carbon dioxide gas generated is a fatal drawback.

On the other hand, from the viewpoint of productivity, especially in tabletting products, obtaining mechanical strength of the tablets and adhesion to the tablets and punches are problems, and the use of binders and mold release agents is essential. Ingredients also contribute to the decrease in carbon dioxide emissions.Furthermore, the commonly used mold release agents, such as metal soap and fine powder such as talc, are insoluble in water, so consumers may not be aware of the inconvenience when using them. It may give you a feeling of pleasure.

In order to overcome the above drawbacks, the technology required for foamable compositions is to reduce the amount of stabilizers, binders, mold release agents, etc.
Moreover, it is necessary to develop a composition and a devitrification method with good productivity.

[Means for solving problems]

Therefore, the present inventors conducted intensive research to develop such a technology and found that by pre-treating the organic acid with a small amount of PEG, the acid and carbonate or bicarbonate can be mixed even after tableting. We discovered a manufacturing method that cuts off contact with the plant and stabilizes the product, and completed the BA.

However, the present invention does not contain substantially water or S.
An organic acid that does not release water of crystallization below aC and PIG are combined at 60%
- Provides a method for creating tablets, which is characterized by heating and melting and mixing in IQDC, cooling and powdering, adding sodium bicarbonate and sodium carbonate to the powder, and compressing into tablets.

The organic acid and PEG can be heated and melted in a jacketed mixer, fluidized bed granulation dryer, etc., while heating with hot water or hot air, or vigorously mixed with a vertical stirring mixer. The temperature may be increased by the heat generated. After melting and mixing at a temperature equal to or higher than the melting point of PEG, the mixture is cooled with moderate stirring to obtain a powdery treated product.

The organic acid used here is selected from one or more of oxalic acid, citric acid, malic acid, succinic acid, and tartaric acid, which are solid at room temperature. However, from the viewpoint of action on metals and safety, succinic acid is preferable. Moreover, the average molecular weight of PEG is preferably 4,000 to 20,000. organic acids 10
The ratio of PEG to 0 parts by weight is preferably 1 to 20 parts by weight, preferably 2 to 10 parts by weight. If the ratio of PEG is small, the stabilizing effect will be poor and the tableting properties will be poor. On the other hand, when the ratio of PIG is high, VcFi not only deviates from the stabilization of VcFi with a small amount of components, which is the objective of the present invention, but also wastes a large amount of energy in heating and cooling processes, and moreover, aggregates are likely to form. It becomes difficult to obtain a powdered processed product.

It was found that when 17cum carbonate and sodium bicarbonate were pretreated with PEG instead of organic acids, the stability was not sufficient. The reason for this is thought to be that sodium bicarbonate gradually decomposes during pretreatment at high temperatures, producing carbon dioxide gas and water, and this water reduces the stability of the final product.

Sodium monocarbonate, sodium bicarbonate, and other ingredients are mixed with the organic acid pretreated with PEG. Other ingredients include fragrances, pigments, surfactants, mirabilite, sodium sesquicarbonate, various condensed phosphates, inorganic clay such as salt,
Hydrogen peroxide adducts such as sodium octate and sodium percarbonate, as well as optional additives such as disinfectants, anti-inflammatory agents, crude drug extracts, etc., can also be used. It is desirable that these substances be essentially anhydrous, but any substance that does not liberate water of crystallization at 50C or lower can be used.

When these mixtures are brought into contact with carbon dioxide gas,
The charcoal #f) easily changes from water molecules and carbon dioxide molecules to two molecules of bicarbonate (IJ), reducing the water content in the system, making the product even more stable. Become.

The tablets obtained according to the present invention are stable and have an excellent appearance.

〔Example〕

Examples of the present invention are shown below, but the present invention is not limited to these Examples. In addition, all blending ratios indicate parts by weight.

Example 1 Succinic acid 10 kp and PEG (average molecular weight 6000) 0.
20 and Nauta mixer (Hosokawa Micron (*) H
wx-sll, volume 30J) to 7QC, 10
After stirring for a minute to melt and mix, the mixture was cooled to obtain a powdery pretreated product.

40.4% of this pre-treated material, 30% sodium bicarbonate, 20% sodium carbonate, 9.4% Glauber's salt, and 0.2% fragrance.
a mixture 10k)i of the same Nauta mixer as above;
After mixing with
The tablets were compressed to give a total weight of 0.09. This was placed in nine bags made of polypropylene with aluminum foil laminated with a film laminated with polyethylene terephthalate, and sealed and packaged using a heat sealer.

Example '2 13 kg of succinic acid and PKG (average molecular weight 2 D, Q
Q Q) 0.5kIP and 0.5kIP were heated to 75C in a super mixer (Kakuda Seisakusho C Co., g S M V-20 type), stirred and melt-mixed, and then cooled to form a powdery pretreated product. I got it.

A mixture of 42.5% of this pretreated product, 30% of sodium bicarbonate, 20% of sodium carbonate, 7.2% of mirabilite, 0.2% of fragrance, and 0.1% of colorant was compressed into tablets in the same manner as in Example 1. , packaged.

Example 3 In Example 2, during mixing before tabletting, stirring was carried out for 10 minutes while blowing carbon dioxide gas at a flow rate of 1 ONJ/Win from the gas blowing nozzle attached to the lower part of the Nauta mixer. Thereafter, the tablets were compressed and packaged in the same manner as in Example 1.

Example 4 Succinic acid 237.5 kp and PICG (average molecular weight 60
00) 12.5kp￥j! -, Henschel mixer (Mitsui Miike Kakoki C Co., Ltd. FM500R type, capacity 5oon)
The mixture was stirred and heated to 700℃ to obtain a pretreated product.

A mixture of 40% of this pretreated product, 32% of sodium bicarbonate, 16% of sodium carbonate, 11.7% of Glauber's salt, 0.2% of fragrance, and 0.1% of pigment is called ITon? Mix with a Nauta mixer C (manufactured by Honkawa Micron Co., Ltd., volume 2.5 m),
The same tablet press as in Example 1 was operated continuously for 4 hours. All tablets were sealed and packaged. Even after continuous tableting, no significant adhesion to the punches of the tableting machine was observed, and there was no occurrence of capping or chipping.

Comparative Example 1 Sodium bicarbonate 4.5kp, sodium carbonate 3kg and PEG (average molecular weight 20,000 α375k)
was pretreated in the same manner as in Example 2.

Next, 10 kg of a mixture of 52.5% of this pretreated product, 40% of succinic acid, 7.2% of Glauber's salt, 0.2% of fragrance, and 0.1% of coloring matter was added to a Nauta mixer in the same manner as in Example 1. After mixing, tablet and package.

Comparative Example 2 In Example 4, without pretreatment of PEG and uccinic acid,
When all the raw materials were mixed and compressed into tablets, within 2 hours, the amount of adhesion to the punches of the tablet machine increased significantly, and the tablet surface became extremely uneven, so tablet compression was stopped.

Test Example The tablets prepared in Examples 1 to 4 and Comparative Example 1.2 were tested for stability.

The test method for evaluating the stability of tablets is to test 10 packaged products by
The sample was left in a constant temperature bath at 50C for 24 hours, and the volume change of each sample was measured before and after that, the average value was taken, and the smaller the volume change, the higher the stability was determined. At this time, in order to accurately measure the volume change, a water tank (volume 3J) was placed on an electronic balance, and the packaged tablets were submerged in the water tank to measure the weight change of the increased volume of water. used.

The results are shown in Table 1.

Table 1 Ax n=10 [Effects of the Invention] As is clear from the stability test results in Table 1, the tablets obtained by pretreating an organic acid with pge according to the present invention are different from the tablets obtained by other methods. It is extremely stable, with less volume increase during storage.

Claims (1)

[Claims] 1. An organic acid that does not substantially contain water or does not release water of crystallization at 50°C or below, and polyethylene glycol.
A method for producing tablets, which comprises heating, melting and mixing at 0 to 100°C, cooling and powdering, adding sodium bicarbonate and sodium carbonate to the powder, and compressing into tablets. 2. The method according to claim 1, wherein the organic acid is succinic acid. 3. The method according to claim 1, characterized in that the mixture to be compressed into tablets is brought into contact with carbon dioxide gas and then compressed into tablets.