JPH1135413A - Formed solid iodophor - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain the subject formed material easily sol-uble in water, having high storage stability and free from the formation of insoluble iodine at a low cost by compounding a iodoglycine complex, an alkali metal iodide and a foamable base and forming the mixture. SOLUTION: The objective formed material can be produced from a mixture of (A) 1 pt.wt. of an iodoglycine complex [e.g. tetraglycine hydroperiodide known as a general name globalin and expressed by the formula (NH2 CH2 COOH)4 HI.5/4I2 ], (B) 0.05-10 pts.wt. of an alkali metal iodide (potassium iodide, sodium iodide, lithium iodide, etc.) and (C) 0.01-0.5 pts.wt. of a foamable base (soditnn bicarbanate, potassium bicarbonate, ammonium bicarbonate, sodium carbonate, potassium carbonate, ammonium carbonate, etc.) by tableting or press molding the mixture under a pressure of 0.2-3 t/cm<2> , preferably 0.5-2 t/cm<2> .

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a solid iodine hole formed by granulating and molding a solid iodine hole composition. More specifically, a composition comprising an iodoglycine complex, an alkali iodide and a base having foaming properties,
Alternatively, the present invention relates to a solid iodine-hole molded product which is obtained by granulating and molding a composition further containing a solid acid and which is immediately soluble in water.

[0002]

2. Description of the Related Art As a germicidal disinfectant utilizing the bactericidal properties of iodine, iodine tincture obtained by dissolving iodine and potassium iodide in ethanol has been known. However, this is irritating and effective. In recent years, there has been a problem with the persistence of iodine-based fungicides such as polyvinylpyrrolidone, organic polymers such as polyvinyl alcohol, and surfactants such as alkylbenzenesulfonic acid, benzalkonium chloride, and nonylphenoxypolyethyleneoxyethanol. A hypoallergenic iodine hole was used. In particular, so-called povidone-iodine using polyvinylpyrrolidone as a carrier has been widely used as a bactericidal disinfectant in the field of medicine, and in recent years has been used in food processing other than medicine, and also in general environmental hygiene and the like.

[0003] Although this povidone-iodine dissolves in water,
At this time, it is not easily dissolved, and requires an extremely long time. Therefore, the user does not directly handle the solid substance of povidone-iodine, and usually obtains an aqueous solution of about 1% by weight of povidone-iodine,
It is generally used to dilute and use according to the purpose of use. Therefore, povidone-iodine is usually stored in the form of an aqueous solution. If storage conditions are poor, particularly at high temperatures, iodine vapor or the solution itself may leak, or the product itself may deteriorate and contain active ingredients. It is feared that a decrease in the amount is likely to occur. Further, there is a drawback in that the coated surface is foamed and sticky when used, and as the iodine hole, a solid iodine hole which is easy to handle and has more excellent storage stability is often required.

Hitherto, an iodoglycine complex has been known as a solid-state iodohole. The iodoglycine complex is a complex with glycine, iodine, and iodide, and does not have sublimability as iodine alone has and is a very stable compound. And the effective iodine which exists in the solution state in the aqueous solution of the iodoglycine complex is suppressed in volatilization by the presence of glycine and is present in the solution in a stable state, so that the irritation is reduced, and also compared to povidone-iodine, Since it is a relatively inexpensive solid iodine hole, it is considered to be a more effective substance as a disinfectant in food processing, general environmental hygiene and the like.

[0005]

The above-mentioned iodoglycine complex is soluble in water, is relatively quickly dissolved in water, and is a substance exhibiting bactericidal activity by releasing effective iodine. However, since insoluble iodine precipitates in the early stage of dissolution in water, an operation of stirring is indispensable for rapidly dissolving the entire amount in water.

[0006] Furthermore, when the amount of water to be introduced into water is large, insoluble iodine may remain as precipitated, and in such a case, a problem may occur in terms of safety. It is not preferable to use only an iodoglycine complex as a solid iodohole.

Therefore, when the iodoglycine complex is used as a component of the solid iodohole, it has been devised that the insoluble iodine as described above is not generated at all and that it is rapidly dissolved in water. Is strongly required.

The present invention provides an iodohole molded product using an iodoglycine complex having the above-mentioned excellent properties as an active ingredient. Accordingly, it is an object of the present invention to provide an inexpensive solid iodine-hole molded product which is free from any insoluble iodine in water when dissolved in water and used as a disinfectant, and which is safe even during storage. .

[0009]

Means for Solving the Problems The present inventors have intensively studied and studied to achieve the above object. As a result, a powdery composition in which a certain range of alkali iodide is blended with the iodoglycine complex is relatively insoluble in water, and is a composition that easily dissolves in water. However, it was also found that insoluble iodine may be generated in the early stage of the charging, although not as much as when the iodoglycine complex alone was charged into water. For this reason, it has been found that the above-described composition is not yet satisfactory in that an iodine composition which does not necessarily require a stirring operation, has easy water solubility, and does not generate insoluble iodine at all. Obtained.

The present inventors have further studied and found that, in addition to the above-mentioned components of the iodoglycine complex and the alkali iodide, a foaming component was blended, and a molded product obtained by granulation was obtained by the following method. An inexpensive, highly safe solid iodine-hole molded product that can have sufficient self-solubility in water, and can be dissolved very quickly without any insoluble iodine being generated from the initial stage of its introduction. It has been found that the present invention has been completed.

That is, the present invention relates to (1) a solid iodine-hole molded product which is formed by containing an iodoglycine complex, an alkali iodide and a base having foaming properties, and (2) an iodoglycine complex, Alkali iodide, a base having an effervescent property, and a solid acid are included, and a solid iodine-hole molded product is molded. (3) An iodoglycine complex is tetraglycine hydroperiodide,
The above (1) which is potassium tetraglycine triiodide or diglycine hydroperiodide or
A solid iodine hole molded product according to (2),
(4) The solid iodine-hole molded product according to the above (1) or (2), wherein the alkali iodide is at least one selected from the group consisting of potassium iodide, sodium iodide and lithium iodide, Further, (5) the base having an effervescent property is one or more selected from the group consisting of sodium hydrogencarbonate, potassium hydrogencarbonate, ammonium hydrogencarbonate, sodium carbonate, potassium carbonate and ammonium carbonate, wherein (1) or ( 2) The solid iodine molded product according to 2), and (6) the solid acid is at least one selected from the group consisting of oxalic acid, malonic acid, malic acid, tartaric acid, citric acid, fumaric acid and boric acid A solid iodine-hole molded product according to the above (2),

[0012]

BEST MODE FOR CARRYING OUT THE INVENTION The iodoglycine complex contained in the molded article of the present invention is, for example, a compound represented by the following formula (1) which is called by the general name globulin:

[0013]

Embedded image A tetraglycine hydroperiodide (hereinafter, referred to as globulin) represented by the general formula (2)

[0014]

Embedded image Potassium tetraglycine triiodide represented by the following formula (hereinafter referred to as potadine), and the following formula (3)

[0015]

Embedded image And diglycine hydroperiodide. These are known chemical substances that have been conventionally used as a disinfectant for drinking water in the field (INDUSTRIAL AND ENGINEERING CHEMISTRY Vo).
l.45 No.5 1013-1015), and as a production method, for example,
J. Am. Chem. 74, 1346 (1952).

The iodoglycine complex as exemplified above is generally a very stable compound and does not react with each other between different kinds thereof. Therefore, not only one kind but also two or more kinds may be used. It does not matter if it is used.

The alkali iodide contained in the molded article of the present invention includes potassium iodide, sodium iodide, lithium iodide and the like, and not only one kind but also two or more kinds are used. No problem.

The compounding ratio of the iodoglycine complex and the alkali iodide is preferably in the range of 0.05 to 10 parts by weight of alkali iodide per 1 part by weight of the iodoglycine complex, and more preferably in the range of 0.2 to 2 parts by weight. More preferably,

The base having effervescence contained in the molded article of the present invention specifically includes sodium hydrogencarbonate, potassium hydrogencarbonate, ammonium hydrogencarbonate, sodium carbonate, potassium carbonate and ammonium carbonate. These are not limited to one type, and two or more types may be used.

In the present invention, when the molded product contains globulin or diglycine hydroperiodide as an iodoglycine complex, it has foaming properties only by containing the base exemplified above. A molded product is obtained. In this case, the amount of the foaming base used is in the range of 0.01 to 0.5 part by weight per 1 part by weight of the iodoglycine complex. Further, when this molded product is dissolved in water, the pH of the solution is lowered. Is more preferably 8 or less. That is, when a base having a foaming property is contained in a mixing ratio such that the pH of the solution exceeds 8 when dissolved in water, a part of the effective iodine becomes inactivated during the dissolution. Therefore, it is not preferable.

When potadine is used as the iodoglycine complex, a foamed foam can be obtained by using a composition further containing a solid acid. Oxalic acid,
Examples thereof include malonic acid, malic acid, tartaric acid, citric acid, fumaric acid, boric acid, and the like. Not only one kind thereof but also two or more kinds may be used.

These solid acids may be contained only in an amount which can react with a base having a foaming property, and even if they are contained in a slightly excessive amount, the stability of the molded product itself and the loss of effective iodine during dissolution are considered. No activity takes place. The mixing ratio of the solid acid is desirably in the range of 1 to 2 parts by weight per 1 part by weight of the foaming base.

Also, in the case where globulin or diglycine hydroperiodide is contained in the molded article of the present invention, if the molded article contains a foaming base in an amount not less than the above-mentioned blending ratio, The solid acid described above is used as a neutralizing agent in 1 part by weight of the excess base.
It is desirable to mix within the range of 2 to 2 parts by weight.

The solid iodine-hole molded product of the present invention is a molded product having an arbitrary shape, and there is no limitation on the shape and size thereof. Various shapes of the molded product such as a hole-shaped disk shape and the like can be selected. Usually, there is no problem if the constituents are mixed at the above-mentioned ratio in the molded product, but the molded product has a diameter of 0.5 mm.
The above-mentioned size is more preferable since it does not float at all on the water surface and becomes a molded product having immediate solubility.

The method for producing the solid iodine-hole molded product of the present invention is not particularly limited as long as the components are well mixed, and may be obtained by mixing pulverized components. Alternatively, a method may be employed in which the raw material crystal components are put together in a pulverizer, mixed while pulverizing, and then produced. When performing these mixing operations, it is preferable to perform the mixing operation in a space that can be sealed as much as possible.

In molding, the above mixture can be molded by a known method such as tablet molding or press molding. The pressure during molding is usually 0.2 to 3 t / cm ²
And more preferably 0.5 to ² t / cm ² . Further, at the time of molding, if necessary, a lubricant such as calcium stearate, magnesium stearate, sodium stearate, sodium benzoate, orthoboric acid or the like may be added to the mixture by 0.1 to 2% by weight. , And can further facilitate molding.

Further, depending on the purpose, nitrite, silicate,
Inorganic corrosion inhibitors such as polyphosphates, organic corrosion inhibitors such as carboxylic acids, metal soaps, sulfonic acids, amines, esters, phosphates, etc., and corrosion inhibition of EDTA, gluconic acid, chelate compounds of nitrilotol acetate, etc. By mixing the necessary amount of the agent, a composition capable of suppressing the corrosiveness to metals can be obtained.

[0028]

EXAMPLES Hereinafter, the solid iodine-hole molded product of the present invention will be described in more detail with reference to Examples and Comparative Examples.
The present invention is not limited by these. In the following, all parts and percentages are by weight.
The iodoglycine complexes used below were produced as follows.

Production of Globulin 75.1 g (1.0 mol) of glycine and 114 g (0.5 mol) of a 56% aqueous solution of hydrogen iodide are added to 950 ml of pure water and dissolved. Then 225 g of glycine (3.0
Mol) and 80 g (0.32 mol) of iodine. After the temperature was raised to 70 ° C and aged at this temperature for 1 hour, gently 5 ° C
Cool down to The precipitated crystals were separated by filtration and dried under reduced pressure.
170.9 g of blackish brown needle-like crystals having a metallic luster were obtained. As a result of the elemental analysis, the obtained product was represented by the following formula (1)

[0030]

Embedded image Was confirmed.

Production of Potadine 75.1 g (1.0 mol) of glycine and 83.1 g (0.5 mol) of potassium iodide are added to 950 ml of pure water and dissolved. Then 225 g (3.0 mol) of glycine and 127 g (0.5 mol) of iodine are added at 60 ° C. with increasing temperature. Raise the temperature to 70 ° C and
After aging at this temperature for a period of time, gently cool to 5 ° C. The precipitated crystals were separated by filtration and dried under reduced pressure. 318.2 g of blackish brown needle-like crystals having a metallic luster were obtained. The product obtained as a result of the elemental analysis was represented by the following formula (2)

[0032]

Embedded image Was confirmed.

Example 1 45 parts by weight of globulin, 45 parts by weight of sodium iodide and 10 parts by weight of sodium hydrogen carbonate were put into a blender, mixed for 5 minutes, and 5.5 g of this powdery composition was subjected to 100 k with a tableting machine.
The mixture was molded under a press pressure of gf / cm ² to obtain a cylindrical tablet having a diameter of 25 mm and a height of 5 mm.

Example 2 45 parts by weight of globulin, 45 parts by weight of potassium iodide and 10 parts by weight of sodium bicarbonate were placed in a blender, mixed for 5 minutes, and 5.5 g of this powdery composition was placed in a tableting machine at 100 kgf.
/ Cm ² to obtain a cylindrical tablet having a diameter of 25 mm and a height of 5 mm.

Example 3 50 parts by weight of globulin, 35 parts by weight of sodium iodide and 15 parts by weight of sodium bicarbonate were put in a blender and mixed for 5 minutes, and 5 g of this powdery composition was put in a tableting machine at 100 kgf.
/ Cm ² to obtain a cylindrical tablet having a diameter of 25 mm and a height of 5 mm.

Example 4 40 parts by weight of potadine, 40 parts by weight of sodium iodide, 10 parts by weight of sodium carbonate and 10 parts by weight of citric acid were put into a blender and mixed for 5 minutes, and 7.1 g of this powdery composition was compressed into a tableting machine. At a press pressure of 100 kgf / cm ² at 25m diameter
Thus, a cylindrical tablet having a height of 5 mm and a height of 5 mm was obtained.

Example 5 45 parts by weight of globulin, 45 parts by weight of sodium iodide and 10 parts by weight of sodium bicarbonate were placed in a blender, mixed for 5 minutes, and 10 g of this powdery composition was placed in a tableting machine at 400 kgf.
A molded product obtained by molding at a press pressure of / cm ² was pulverized by a pulverizer to obtain 5.5 g of granules having a particle size of 0.5 to 2.0 mm.

Example 6 40 parts by weight of potadine, 40 parts by weight of sodium iodide, 10 parts by weight of sodium bicarbonate and 10 parts by weight of citric acid were put into a blender and mixed for 5 minutes, and 10 g of this powdery composition was compressed into a tableting machine. The molded product obtained by molding at a press pressure of 400 kgf / cm ² is pulverized by a pulverizer to obtain granules having a particle size of 0.5 to 2.0 mm.
7.1 g were obtained.

Comparative Example 1 2.5 g of globulin alone was molded with a tableting machine at a pressing pressure of 100 kgf / cm ² to obtain a cylindrical tablet having a diameter of 25 mm and a height of 2.5 mm.

Comparative Example 2 50 parts by weight of globulin and 50 parts by weight of sodium iodide were placed in a blender and mixed for 5 minutes.
g at a pressing pressure of 100 kgf / cm ^{2 using} a tableting machine.
A cylindrical tablet having a diameter of 25 mm and a height of 5 mm was obtained.

Comparative Example 3 10 g of povidone-iodine powder was applied to a tableting machine at 100 kgf / cm ^2.
To obtain a cylindrical tablet having a diameter of 25 mm and a height of 14 mm.

Test Example 1 (Solubility Test) Fifteen pieces of 1000 ml Erlenmeyer flasks each containing 1000 ml of ion-exchanged water were prepared, and the molded articles obtained in Examples 1 to 6 were placed therein. The solution was dissolved in a standing state or under a condition of slow stirring, and the time required for dissolution and the effective iodine concentration in the solution were measured. In addition, as a comparative test, a dissolution test by slow stirring was performed using the molded products of Comparative Examples 1 and 2 as test samples. Table 1 shows the results
Shown in

[0043]

[Table 1]

Test Example 2 (Storage Stability Test) The molded products obtained in Examples 1 to 6 and Comparative Examples 1 to 3 were respectively kept at a room temperature of 15 to 20 ° C. for 30 days or at a constant temperature of 40 ° C. After standing for 30 days, the effective iodine content contained in each of them was measured. Table 2 shows the results.

[0045]

[Table 2]

[0046]

As described in detail above, the solid iodine-hole molded product of the present invention comprising an iodoglycine complex, an alkali iodide and a foaming base can be easily formed by tableting or press molding a mixture of the components. When dissolved in water, it is very fast-soluble and does not generate insoluble iodine. That is, it can be said that the solid iodine hole can prepare an iodine solution having an arbitrary concentration in a very short time.

Further, the molded article of the present invention does not cause a decrease in effective iodine even when stored at a relatively high temperature for a long time, and is extremely stable. Therefore, the composition of the present invention is effective as a disinfectant for environmental hygiene in fields such as medical care, dairy farming, and food processing.

──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. ⁶ Identification code FI A01N 37/06 A01N 37/06 37/36 37/36 37/44 37/44 59/00 59/00 D 59/14 59 / 14 (72) Inventor Ryoichi Seki 1900 Togo, Mobara-shi, Chiba Mitsui Toatsu Chemicals Co., Ltd. (72) Inventor Hideyuki Yamaguchi 1579-206 Mobara, Mobara-shi, Chiba

Claims (6)

[Claims] 1. A solid iodine-hole molded article comprising an iodoglycine complex, an alkali iodide and an effervescent base. 2. An iodoglycine complex, an alkali iodide,
A solid iodine-hole molded article containing a foamable base and a solid acid, and molded. 3. The solid iodine hole molded product according to claim 1, wherein the iodoglycine complex is tetraglycine hydroperiodide, potassium tetraglycine triiodide or diglycine hydroperiodide. 4. The solid iodine-hole molded product according to claim 1, wherein the alkali iodide is at least one selected from the group consisting of potassium iodide, sodium iodide and lithium iodide. 5. The method according to claim 1, wherein the effervescent base is at least one selected from the group consisting of sodium bicarbonate, potassium bicarbonate, ammonium bicarbonate, sodium carbonate, potassium carbonate and ammonium carbonate. The solid iodine-hole molded product according to the above. 6. The solid iodine-hole molding according to claim 2, wherein the solid acid is at least one selected from the group consisting of oxalic acid, malonic acid, malic acid, tartaric acid, citric acid, fumaric acid and boric acid. Stuff.