JPH0210126B2 - - Google Patents

Description

[Detailed description of the invention]

[Industrial Application Field] 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. [Prior Art] Forming a composition containing a carbonate, a bicarbonate, and an organic compound into a foaming composition by tabletting or granulation is useful for cleaning agents, bath additives, and bath water cleaners. , applied to products such as pool disinfectants. These products have the advantage that when added to water, the components react and dissolve quickly while generating carbon dioxide gas. At the same time, they provide consumers with a comfortable feeling of use, which has the effect of increasing the product value. Particularly in bath additives, the blood circulation promoting effect of the carbon dioxide gas generated is actively utilized. However, when carbonate or bicarbonate coexists with an organic acid, 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 or even break. It may cause When such a situation occurs, not only the product value is significantly damaged, but also
There was a strong fear that consumer trust would be lost. In order to obtain a stable product by 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 from the time it is manufactured until the time it is used by the consumer, the product is sealed and packaged to prevent moisture absorption. Despite this, it was difficult to say that the problem had been resolved. In order to solve this problem, JP-A-58-213714 proposes a method in which a double salt of carbonate and Glauber's salt is prepared in advance and an organic acid is mixed therein. Furthermore, in JP-A-58-105910, 30-70% by weight of polyethylene glycol (hereinafter abbreviated as PEG) with an average molecular weight of 950-3700 and 70-30% by weight of other foaming components are blended and then heated. tePEG
A method of melting and embedding an effervescent component into PEG is disclosed. [Problem to be solved by the invention] However, mixing a large amount of ingredients in order to stabilize the product will only reduce the amount of carbon dioxide gas generated and impair the comfortable feeling of use for consumers. First, the amount of effective ingredients that achieve the intended purpose of the product will be reduced, and the amount used per time will also increase, resulting in higher costs. In particular, a decrease in the amount of carbon dioxide gas generated is a fatal drawback in bath additives that actively utilize the carbon dioxide gas generated, and cleaning agents that utilize the foam generated. On the other hand, from the viewpoint of productivity, especially in tabletting products, obtaining mechanical strength of tablets and adhesion to dies and punches are problems, and the use of binders and mold release agents is essential. These ingredients also contribute to the reduction in the amount of carbon dioxide gas generated.Moreover, the fine powders such as metal soap and talc, which are commonly used mold release agents,
Because it is insoluble in water, it may cause discomfort to consumers when used. 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., and to develop compositions and manufacturing methods with good productivity. be. [Means for Solving the Problems] Therefore, the present inventors conducted intensive research to develop such a technology, and as a result, they found that by pre-treating an organic acid with a small amount of PEG, it is possible to compress the organic acid into tablets. After that, the contact between the acid and the carbonate or bicarbonate is cut off,
We have discovered a manufacturing method that achieves product stability and completed the present invention. That is, the present invention uses an organic acid that does not substantially contain water or does not release water of crystallization at temperatures below 50°C.
The present invention provides a method for producing tablets, which comprises heating and melt-mixing PEG and PEG at 6 to 100°C, cooling and powdering, adding sodium bicarbonate and sodium carbonate to the mixture, and compressing into a tablet. The heating and melting of organic acids and PEG can be done using a mixer with a jacket, a fluidized bed granulation dryer, etc., while raising the temperature with hot water or hot air, or by vigorously mixing with a vertical stirring mixer. The temperature may be raised using heat. After melt mixing at a temperature above the melting point of PEG,
Cool with moderate stirring to obtain a powdered product. The organic acids used here include oxalic acid, citric acid, malic acid, succinic acid, and tartaric acid, which are solid at room temperature.
A species or two or more species are selected. 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. The ratio of PEG to 100 parts by weight of the organic acid is preferably 1 to 20 parts by weight, preferably 2 to 10 parts by weight. If the ratio of PEG is low, the stabilizing effect will be poor;
Moreover, tableting properties are poor. On the other hand, if the ratio of PEG is high, not only will it fail to achieve the stabilization with a small amount of components that is the objective of the present invention, but also a large amount of energy will be wasted in heating and cooling, and moreover, aggregates will easily form. Therefore, it becomes difficult to obtain a powdery processed product. It was found that when sodium 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 carbonate, sodium bicarbonate, and other ingredients are mixed with the PEG-pretreated organic acid. Other ingredients include fragrances, pigments, surfactants, mirabilite, sodium sesquicarbonate, various condensed phosphates, inorganic substances such as salt, sodium perborate,
Hydrogen peroxide adducts such as sodium percarbonate, and if necessary, bactericides, 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 temperatures below 50°C can be used. When these mixtures are brought into contact with carbon dioxide gas, the sodium carbonate easily changes from one molecule of water and one molecule of carbon dioxide to two molecules of sodium bicarbonate, reducing the moisture content in the system. Product stability is further improved. The tablets obtained according to the present invention are stable and have an excellent appearance. [Examples] 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 10 kg of succinic acid and 0.2 kg of PEG (average molecular weight 6000) were mixed in a Nauta mixer (Nx manufactured by Hosokawa Micron Co., Ltd.).
-S type, volume 30), the temperature was raised to 70°C, stirred for 10 minutes to melt and mix, and then cooled to obtain a powdery pretreated product. This pre-treated product 40.4%, sodium bicarbonate 30%,
Sodium carbonate 20%, Glauber's salt 9.4%, and fragrance 0.2%
Mix 10 kg of the mixture in the same Nauta mixer as above, remove coarse particles with a 16-mesh sieve, and then make one tablet with a tablet machine (DC-WD model manufactured by Masina Co., Ltd.).
It was compressed into tablets weighing 50g. This was placed in a bag made of polypropylene layered with aluminum foil and further laminated with polyethylene terephthalate, and sealed and packaged using a heat sealer. Example 2 Succinic acid 8Kg and PEG (average molecular weight 20000) 0.5Kg
Super mixer (SMV manufactured by Kawada Seisakusho Co., Ltd.)
20 type), the mixture was heated to 75°C, stirred, melted and mixed, and then cooled to obtain a powdery pretreated product. This pre-treated material 42.5%, sodium bicarbonate 30%,
10 kg of a mixture of 20% sodium carbonate, 7.2% Glauber's salt, 0.2% fragrance, and 0.1% 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 10/min 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 237.5Kg and PEG (average molecular weight 6000) 12.5
Kg, Hensiel mixer (manufactured by Mitsui Miike Kakoki Co., Ltd.)
The mixture was stirred using an FM500E model (volume 500) and heated to 70°C to obtain a pretreated product. 1 ton of a mixture of 40% of this pretreated product, 32% sodium bicarbonate, 16% sodium carbonate, 11.7% mirabilite, 0.2% fragrance, and 0.1% pigment was mixed in a Nauta mixer (manufactured by Hosokawa Micron Co., Ltd., volume 2.5 m ³ ). The same tablet press as in Example 1 was operated continuously for 4 hours. All tablets were packaged in sealed packaging. Even after continuous tableting, no significant adhesion to the punches of the tableting machine was observed, and no capping or chipping occurred. Comparative example 1 Sodium bicarbonate 4.5Kg, sodium carbonate 3Kg
and 0.375 kg of PEG (average molecular weight 20000) were pretreated in the same manner as in Example 2. Next, this pretreatment 52.5%, succinic acid 40%, Glauber's salt
10Kg of a mixture of 7.2%, fragrance 0.2%, and color 0.1%
were mixed in a Nauta mixer in the same manner as in Example 1, then tableted and packaged. Comparative Example 2 In Example 4, all blended raw materials were mixed and compressed into tablets without pre-treatment with PEG and succinic acid.
After 2 hours, the adhesion to the punch of the tablet machine increased significantly and the tablet surface became extremely uneven, so tableting was discontinued. Test Example The stability of the tablets prepared in Examples 1 to 4 and Comparative Examples 1 and 2 was tested. The test method for evaluating the stability of tablets is
The sample was left in a constant temperature bath at 50°C for 24 hours, the volume change of each sample before and after was measured, the average value was taken, and the smaller the volume change, the higher the stability. At this time, in order to accurately measure the volume change, a method was used in which a water tank (volume 3) 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. . The results are shown in Table 1.

〔Effect of the invention〕

As is clear from the stability test results in Table 1,
Tablets obtained by pretreating an organic acid with PEG according to the present invention show less volume increase during storage and are extremely stable compared to tablets obtained by other methods.

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 are heated and melted and mixed at 60 to 100°C, then cooled and powdered, and then A method for manufacturing tablets, which comprises adding sodium carbonate and sodium carbonate and compressing into tablets. 2 Claim 1 in which the organic acid is succinic acid
The method described in section. 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.