JPH10237498A - Production of powder soap - Google Patents

Abstract

PROBLEM TO BE SOLVED: To produce a powder soap having a high bulk density and good solubility in cold water by a simple and industrially efficient process reduced in energy consumption. SOLUTION: In producing a powder soap by mixing and neutralizing 1-10 equivalents of a solid water-soluble alkali inorganic compound with 1 equivalent of a fatty acid, the fatty acid in an amount 0.2-0.3 time as large as the total amount of the acid to be added is added to the solid water-soluble alkali inorganic compound kept it in a powdery state by agitation, the temperature of the mixture is kept at 40-90 deg.C, the mixture is agitated to keep it in a powdery state, and the remainder (0.7-0.8 time the total amount of the acid to be added) of the fatty acid is added over a period of time of 10min or longer.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a method for producing powdered soap. More specifically, the present invention has a high bulk density,
The present invention relates to a method for producing a powdered soap having good solubility in cold water.

[0002]

2. Description of the Related Art Powdered soaps used as detergents for clothing and the like are usually produced by spray-drying a soap aqueous solution containing a builder or the like. Powdered soap produced by spray drying has the advantage of good solubility in water, but the resulting product has a low bulk density,
It has disadvantages such as high energy cost due to evaporation of a large amount of water in the manufacturing process. Recently, compact detergents having a high bulk density have been preferred from the viewpoint of user-friendliness, and the necessity of energy saving has been highlighted. From such a background, a method for producing a detergent composition having a low energy cost at the time of production and a high bulk density of a product has been actively studied mainly for synthetic detergents such as salts of alkylbenzenesulfonic acid. For example, Japanese Unexamined Patent Publication (Kokai) No. 60-72999 discloses that an unneutralized sulfonate or sulfate is neutralized and mixed together with sodium carbonate and water in a strong shearing device, and then cooled and pulverized and granulated with zeolite. A method for producing a concentrated powder detergent is disclosed. This method has a disadvantage in that the neutralization reaction product is in the form of a dump, and a special machine having a large shearing force is required to complete the neutralization reaction. JP-A-3-33199 discloses that a solid alkaline inorganic compound such as sodium carbonate is fluidized in a mixer having a stirring function and a shearing function, and while maintaining the temperature at 55 ° C. or lower, alkylbenzene sulfonic acid or the like is used. A method is disclosed in which an acid precursor of an anionic surfactant is gradually added to cause neutralization while maintaining the granular form of the mixture, and then granulated by a mixer in the presence of a liquid binder. A similar method is disclosed in
No. 3,633,398 discloses that a solid water-soluble alkali-inorganic material is fluidized in a high-speed mixing / granulating machine, and a liquid acid precursor of an anionic surfactant is added to carry out a neutralization reaction while the mixture is particulate. A method of producing and granulating in the presence of a liquid binder is disclosed. Since these methods are a neutralization reaction by a solid-liquid reaction, there is a disadvantage that the neutralization reaction does not sufficiently proceed unless a highly reactive acid is used. For this reason, when a neutralization reaction is performed by a method similar to these using fatty acids having an extremely low acid strength as compared with phenylsulfonic acids such as alkylbenzenesulfonic acid, the neutralization reaction does not sufficiently proceed. However, there is a problem that the unneutralized fatty acid remains and the solubility in water is reduced. Therefore, such a method is not suitable for producing powdered soap. A similar attempt to improve the production method of powdered soap is disclosed in, for example, JP-A-49-82708. This method is a method in which a fatty acid is added to powdered sodium carbonate in the presence of moisture, or a fatty acid is added to powdered sodium carbonate to form a paste and neutralize. However, this method has a drawback that if the temperature is low, the neutralization reaction product becomes hard and pulverization becomes difficult. Therefore, it is necessary to heat the paste to 80 ° C. or higher to form a paste, dry the paste into a lump, and crush the lump. However, the paste easily adheres to the stirring blades and the reaction vessel wall, and the adhered paste solidifies, greatly impairing the efficiency of the machine.
Removal work is required after the end of production, which causes a problem in work.
In addition, a special machine having a large crushing power is required to crush a lump. In addition to the above-mentioned problems of the production method, powdered soap having a high bulk density has a problem that its solubility in water is essentially low because the surface area per unit weight is small. As one method for increasing the solubility of powdered soap in water, it is common practice to use potassium soap, which has higher solubility in water than sodium soap. However, potassium soap tends to become a sticky gel-like substance, and it is difficult to use potassium soap alone. Therefore, when increasing the solubility in water using potassium soap, a method of mixing sodium soap and potassium soap has been adopted. However, according to a method in which the neutralization step is carried out in a slurry state such as a spray drying method, such a soap can be easily obtained, but powdered soap is prepared from the above-described fatty acid and a solid water-soluble alkaline inorganic compound. In the production method, the reaction product gels during the neutralization step,
It is difficult to produce powdered soap.

[0003]

DISCLOSURE OF THE INVENTION The present invention aims to produce a powdered soap having a high bulk density and a good solubility in cold water with low energy consumption and a simple method in an industrially efficient manner. The purpose of the present invention is to provide a method for producing a powdered soap that can be used.

[0004]

Means for Solving the Problems The inventors of the present invention have conducted intensive studies to solve the above-mentioned problems, and as a result, the water-soluble alkaline inorganic compound has been stirred to maintain the powdery state while the total amount of the fatty acid added has been reduced. After about a quarter of the volume has been added, the reaction mixture is maintained at a temperature of 40 to 90 ° C., and the reaction mixture is stirred to maintain a powdery state, while the remaining fatty acids are gradually added to increase the bulk density. And found that powder soap having high solubility in cold water and good solubility in cold water could be produced efficiently, and based on this finding, the present invention was completed. That is, the present invention provides (1) solid water-soluble alkaline inorganic compounds 1 to 10
In preparing a powdered soap by mixing and neutralizing at a ratio of 1 equivalent to 1 equivalent of a fatty acid, a solid water-soluble alkaline inorganic compound is agitated and kept in a powdery state while maintaining 0.2 to 0.2 of the total amount of the fatty acid added. After adding 3 times by weight, the temperature of the reaction mixture is maintained at 40 to 90 ° C., and the reaction mixture is stirred to maintain a powder state, and 0.7 to 0.8 times the total amount of the remaining addition. (2) 2 to 30 parts by weight based on 100 parts by weight of the total amount of the solid water-soluble alkaline inorganic compound and the fatty acid, wherein the fatty acid is added over 10 minutes or more. (3) The method for producing a powdered soap according to item (1), wherein water is added, (3) a fatty acid emulsified with 2 to 30 parts by weight of water with respect to 100 parts by weight of the total of the solid water-soluble alkaline inorganic compound and the fatty acid. , To be added to the solid water-soluble alkaline inorganic compound ( 1) The method for producing a powdered soap according to the item,
(4) 70-99% by weight of sodium compound and 1-30 of potassium compound as solid water-soluble alkaline inorganic compound
(1) The method for producing a powdered soap according to the item (1), wherein (5) the solid water-soluble alkaline inorganic compound is
An amount corresponding to 0.01 to 2 equivalents to 1 equivalent of the fatty acid is added to the reaction mixture in the form of a solid or an aqueous solution after adding 0.5% by weight or more of the total amount of the added fatty acid to the reaction mixture. )).

[0005]

BEST MODE FOR CARRYING OUT THE INVENTION In the method for producing powdered soap of the present invention, 1 to 10 equivalents of a solid water-soluble alkaline inorganic compound and 1 equivalent of a fatty acid are mixed and neutralized. When the amount of the solid water-soluble alkaline inorganic compound is less than 1 equivalent relative to 1 equivalent of the fatty acid, the neutralization reaction is not completely performed, free fatty acids remain, and the solubility of the resulting soap powder in water decreases. There is a possibility that. When the amount of the solid water-soluble alkaline inorganic compound exceeds 10 equivalents relative to 1 equivalent of the fatty acid, the content of the fatty acid salt in the powdered soap decreases, and the detergency as the powdered soap may be reduced. The fatty acid used in the present invention is not particularly limited, but is preferably a fatty acid having 6 or more carbon atoms, and more preferably a fatty acid having 12 to 20 carbon atoms. Such fatty acids include, for example, tallow, lard,
Examples thereof include fatty acids obtained from vegetable oils such as animal oils such as sheep fat and fish oil, palm oil, palm kernel oil, coconut oil, soybean oil, rice bran oil, and sunflower oil, and synthetic fatty acids. Specific examples of such fatty acids include caproic acid,
Enanthic acid, caprylic acid, pelargonic acid, capric acid,
Undecanoic acid, lauric acid, myristic acid, palmitic acid, margaric acid, stearic acid, arachiic acid, linear saturated fatty acids such as behenic acid, 2-ethylhexanoic acid,
Examples include branched saturated fatty acids such as 3,5,5-trimethylhexanoic acid, and unsaturated fatty acids such as myristoleic acid, palmitoleic acid, oleic acid, elaidic acid, linoleic acid, linolenic acid, and erucic acid. One of these fatty acids can be used alone, or two or more can be used in combination. Among these, an unsaturated fatty acid having an iodine value of 70 or more can be particularly preferably used because a powdered soap having good solubility in low-temperature water is easily obtained.

The solid water-soluble alkaline inorganic compound used in the present invention includes salts of alkali metal inorganic acids, for example, alkali metal sulfites, bisulfites, carbonates, bicarbonates, silicates, and phosphoric acids. Salts, borates and the like, alkali metal hydroxides and the like can be mentioned. If the solid water-soluble alkaline inorganic compound exceeds the equivalent of the fatty acid, the resulting water-soluble soap contains the solid water-soluble alkaline inorganic compound in an unreacted state. In this case, it is preferable that the remaining unreacted water-soluble alkaline inorganic compound has low irritation. Examples of such a low-irritating solid water-soluble alkaline inorganic compound include sodium carbonate. When a strong alkali such as an alkali metal hydroxide such as sodium hydroxide or potassium hydroxide is used, the amount used is less than 1 equivalent, preferably less than 0.5 equivalent, relative to the fatty acid, It is preferable to use it in combination with another low-irritating solid water-soluble alkaline inorganic compound.

[0007] In the method of the present invention, as a first-stage reaction, an amount of 0.2 to 0.3 times by weight of the total amount of the fatty acid added while stirring the solid water-soluble alkaline inorganic compound in a powder state is maintained. Is added. The temperature of the reaction mixture in the first-stage reaction is not particularly limited, but is usually preferably 20 to 70 ° C. If the temperature of the reaction mixture in the first-stage reaction is lower than 20 ° C., the speed of the neutralization reaction may be reduced. If the temperature of the reaction mixture in the first-stage reaction exceeds 70 ° C., the hue of the resulting powdered soap may be deteriorated. If the temperature of the reaction mixture exceeds 70 ° C. at the end of the first-stage reaction, it may be difficult to maintain the temperature of the reaction mixture at 90 ° C. or lower in the second-stage reaction. In the method of the present invention, in the first-stage reaction, 0.2 to 0.3% by weight of the total amount of the added fatty acids is
It is preferable to add in 1 to 10 minutes. In the first-stage reaction, since the reaction rate between the solid water-soluble alkaline inorganic compound and the fatty acid is relatively fast, considering the productivity,
It is preferable that the addition rate of the fatty acid is high. In the method of the present invention, in the first-stage reaction, 0.2 to 0.3 times by weight of the total amount of the fatty acid to be added is added while the solid water-soluble alkaline inorganic compound is kept in a powdery state by stirring. . The solid water-soluble alkaline inorganic compound is added to the fatty acid in an amount of 0.2 to 0.3 times by weight of the total amount of the fatty acid while the solid water-soluble alkaline inorganic compound is being stirred and kept in a powdery state, so that the fatty acid is converted into the solid water-soluble alkaline inorganic compound. As in the case of the addition, it is possible to prevent the mixture of the neutralization reaction product, the solid water-soluble alkaline inorganic compound, the fatty acid, and the like from being gelled, caked, or agglomerated in the reaction vessel. In the present invention, the powder state refers to a state in which the powder has essentially fluidity and can be stirred by a known mixer or the like.

In the method of the present invention, in the first stage reaction, 0.2 to 0.3 times by weight of the total amount of the added fatty acids is added, and then the process proceeds to the second stage reaction. There is no particular limitation on the timing of the transition to the second-stage reaction. The first-stage reaction can be immediately followed by the second-stage reaction, or the first-stage reaction can be terminated after the first-stage reaction has been completed. And the process can shift to the second stage reaction. In the method of the present invention,
The temperature of the reaction mixture in the second stage reaction is 40-90.
C., more preferably 50-80.degree. When the temperature of the reaction mixture is lower than 40 ° C., the neutralization reaction does not sufficiently proceed, and the solubility of the resulting powdered soap in water may be reduced. When the temperature of the reaction mixture exceeds 90 ° C., the reaction mixture may be gelled, caked, agglomerated, or the like, and it may be difficult to maintain a powdery state. In the method of the present invention, the total amount of the remaining addition in the second stage reaction is 0.7 to 0.7.
Eight weight times the amount of fatty acid is added for more than 10 minutes, preferably for 20 to 120 minutes, more preferably 25 to 60 minutes.
Add in minutes. If 0.7 to 0.8 weight times the total amount of the remaining fatty acids is added in less than 10 minutes, the neutralization reaction does not sufficiently proceed, and the reaction mixture becomes gelled, rice caked, or agglomerated. However, it may be difficult to maintain the powder state.
There is no particular limitation on the method of adding the fatty acid in the second stage reaction. For example, the fatty acid can be added completely continuously, added dropwise, intermittently added, or added by spraying. can do.

In the method of the present invention, it is preferable to add 2 to 30 parts by weight of water based on 100 parts by weight of the total of the solid water-soluble alkaline inorganic compound and the fatty acid.
More preferably, 10 to 10 parts by weight of water are added. By adding water, the reactivity of the reaction mixture of the solid water-soluble alkaline inorganic compound and the fatty acid can be increased, and the solubility of the powdered soap in water can be increased. If the amount of water is less than 2 parts by weight based on 100 parts by weight of the total amount of the solid water-soluble alkaline inorganic compound and fatty acid, the effect of increasing the reactivity may not be sufficiently exhibited. The amount of water to be added is 10 in total of the solid water-soluble alkaline inorganic compound and fatty acid.
When the amount exceeds 30 parts by weight with respect to 0 parts by weight, the reaction mixture has tackiness, adheres to the reaction vessel, and deteriorates workability,
Yield may decrease. In the method of the present invention, there is no particular limitation on the method of adding water, and the water can be added all at once, dividedly or continuously. There is no particular limitation on the timing of water addition.
It can be added to the solid water-soluble alkaline inorganic compound before the start of the fatty acid addition in the stage reaction,
Can be added simultaneously with the fatty acid in the stage reaction,
It can be added before starting the addition of the fatty acid in the second-stage reaction, or can be added simultaneously with the fatty acid in the second-stage reaction. It is preferable to add water before the addition of 0.3 weight times the total amount of the fatty acid during the addition period of the water.

In the method of the present invention, when water is added at the same time as the fatty acid, it is preferably added as a fatty acid emulsified with water. By adding as a fatty acid emulsified with water, the neutralization reaction is performed more sufficiently, and as a result,
The solubility of the obtained powdered soap in cold water is improved. The emulsification of the fatty acid can be performed in the presence of an emulsifier, and as the emulsifier, a surfactant having a function of emulsifying the fatty acid, such as a normal anionic surfactant or a nonionic surfactant, may be used without any particular limitation. it can. These surfactants are used in an amount of 0.01 to 5 parts by weight per 100 parts by weight of the fatty acid.
It is preferably in parts by weight. In the method of the present invention, water can be added to the reaction mixture together with an additive such as a builder. In the method of the present invention, the solid water-soluble alkaline inorganic compound is a sodium compound 70
９９99% by weight and potassium compound 1-30% by weight. By using a potassium compound in combination as a solid water-soluble alkaline inorganic compound,
The solubility of the resulting powdered soap in cold water can be increased. If the amount of the potassium compound in the solid water-soluble alkaline inorganic compound is less than 1% by weight, the effect of increasing the solubility of the obtained powdered soap in cold water may not be sufficiently exhibited. When the amount of the potassium compound in the solid water-soluble alkaline inorganic compound exceeds 30% by weight, the reaction mixture becomes sticky and gels and adheres to the reaction vessel, so that the workability is deteriorated and the yield may be reduced. There is. Examples of the potassium compound to be used include potassium hydroxide, potassium carbonate and the like.

In the method of the present invention, when a potassium compound is used as the solid water-soluble alkaline inorganic compound, it is preferable to maintain the temperature of the reaction mixture at 50 to 80 ° C. When the temperature of the reaction mixture exceeds 80 ° C., the reaction mixture has tackiness and adheres to the reaction vessel, so that the workability may be deteriorated and the yield may be reduced. In the method of the present invention, as a solid water-soluble alkaline inorganic compound,
When a potassium compound is used in combination, it is preferable to maintain the temperature of the reaction mixture at 70 ° C. or lower in the first-stage reaction. In the first stage reaction, the temperature of the reaction mixture was 7
When the temperature exceeds 0 ° C., the reaction mixture has tackiness and adheres to the reaction vessel, so that the workability may be deteriorated and the yield may be reduced. In the method of the present invention, when a potassium compound is used in combination as the solid water-soluble alkaline inorganic compound, 2 to 10 parts by weight of water is added to 100 parts by weight of the total amount of the solid water-soluble alkaline inorganic compound and the fatty acid. It is preferred to add. If the amount of water is less than 2 parts by weight based on 100 parts by weight of the total amount of the solid water-soluble alkaline inorganic compound and the fatty acid, the neutralization reaction does not sufficiently proceed,
Solubility of the resulting powdered soap in cold water may be reduced. When the added amount of water exceeds 10 parts by weight based on 100 parts by weight of the total amount of the solid water-soluble alkaline inorganic compound and fatty acid, the reaction mixture has tackiness and adheres to the reaction vessel, so that workability is reduced. It may worsen and the yield may decrease.

In the method of the present invention, of the solid water-soluble alkaline inorganic compound, 0.0 to 1 equivalent of the fatty acid is used.
The amount equivalent to 1 to 2 equivalents is 0.5% of the total amount of the fatty acid added.
After adding the amount by weight or more, more preferably after adding the whole amount of the fatty acid, it can be added to the reaction mixture in the form of a solid or an aqueous solution. By adding the solid water-soluble alkaline inorganic compound after adding the fatty acid, the neutralization reaction proceeds more sufficiently, and the solubility of the resulting powdered soap in cold water is improved. If the amount of the solid water-soluble alkaline inorganic compound to be additionally added is less than 0.01 equivalent to 1 equivalent of the fatty acid, the effect of improving the solubility of the powdered soap in cold water may not be sufficiently exhibited. is there. If the amount of the solid water-soluble alkaline inorganic compound to be added additionally exceeds 2 equivalents to 1 equivalent of the fatty acid, the amount of the solid water-soluble alkaline inorganic compound is less than 0.5 weight times the total amount of the fatty acid added. There is a possibility that the charged amount of the basic alkaline inorganic compound becomes too small and the stirring becomes insufficient. In the method of the present invention, the neutralization reaction proceeds more sufficiently by adding a solid water-soluble alkaline inorganic compound to be added as an aqueous solution after adding an amount of 0.5 weight times or more of the total amount of the fatty acid added. In addition, the solubility of the obtained powdered soap in cold water is further improved. 0.1% of the total amount of fatty acids added
The solid water-soluble alkaline inorganic compound to be added after adding 5 times by weight or more can be the same compound as the solid water-soluble alkaline inorganic compound used in the first-stage reaction, or a different compound. It can be. When the solid water-soluble alkaline inorganic compound to be added after adding an amount of 0.5 weight times or more of the total amount of the fatty acid is different from the solid water-soluble alkaline inorganic compound used in the first-stage reaction, It is particularly preferable to use an aqueous solution of sodium silicate from the viewpoints of skin irritation of the product and industrial availability.

In the method of the present invention, it is preferable that pulverization and granulation are performed after the addition of the fatty acid is completed. By this operation, the neutralization reaction proceeds more sufficiently.
The time of pulverization and granulation is preferably 2 minutes or more,
More preferably, it is 5 minutes or more. In the method of the present invention, a so-called composite soap can be produced by adding an acid precursor of an anionic surfactant other than the fatty acid during or before or after the addition of the fatty acid. Acid precursors of anionic surfactants other than fatty acids include, for example, alkyl benzene sulfonic acid, α-olefin sulfonic acid and the like. The addition amount of the acid precursor of the anionic surfactant other than these fatty acids is preferably 1 to 15 parts by weight based on 100 parts by weight of the fatty acid. There is no particular limitation on the reactor used in the method of the present invention, for example,
Kneaders such as wheel type, ball type, blade type, roll type, and granulators such as extruder, crusher, stirring granulator, rubber cylinder type granulator, spiral pass granulator, etc. be able to. Among these, a mixer provided with both a stirrer and a shearing machine is particularly preferable. Examples of such a mixer include a high-speed mixer manufactured by Fukae Kogyo Co., Ltd. and a ready-mixed mixer manufactured by Matsuzaka Giken Co., Ltd. And a turbo sphere mixer manufactured by Sumitomo Heavy Industries, Ltd. In these mixers,
The amount of the solid water-soluble alkaline inorganic compound or fatty acid to be charged is preferably 1/4 to 2/3 of the volume.
The higher the rotation speed of the stirrer or shearing device of the mixer, the faster the fatty acid addition rate in the second-stage reaction can be increased, but in practice, the rotation speed of the stirrer is 10 to 1,000 rpm,
The rotational speed of the shearing machine is preferably in the range of 1,000 to 10,000 rpm. In the method of the present invention, a builder can be further added during, before or after the addition of the fatty acid. As such a builder,
For example, "Encyclopedia of Detergent and Cleaning" [Asakura Shoten, 199
0 years] on pages 56 to 75 can be used. Specifically, zeolite,
Edetate, oxalate, citrate, tartrate, gluconate, pyromellitic acid, benzotricarboxylate, polymer carboxylate and the like can be mentioned. The addition amount of these builders is preferably 1 to 50% by weight in the soap powder.

In the method of the present invention, an enzyme, a fluorescent whitening agent, a redeposition inhibitor, a bleaching agent, a foaming agent, a foam stabilizer, a foam inhibitor / foamer, a softener, a flow improver, Additives such as anti-caking agents, fragrances and dyes can be added during, before or after the addition of the fatty acid. As examples of these additives, for example, known additives described on pages 75 to 101 of the aforementioned “Detergent and Cleaning Dictionary” can be used. Specifically, an enzyme such as a protease, a fluorescent whitening agent such as a bis (triazinylamino) stilbene sulfonic acid derivative or a bisstyrylbiphenyl derivative, a re-contamination inhibitor such as carboxymethyl cellulose,
Bleaching agents such as sodium perborate, foaming agents such as alkyl benzene sulfonate, α-olefin sulfonate, alkane sulfonate, alkyl sulfate, alkyl polyoxyethylene sulfate, mono- or diethanolamide of fatty acid and higher Examples include foam stabilizers such as alcohols, foam inhibitors and foam breakers such as silicone and wax, softeners such as dialkyldimethylammonium salts, and flow improvers and anti-caking agents such as zeolite that is also used as a builder. be able to. The amount of these additives is preferably 0.01 to 10% by weight in the powdered soap. In the method of the present invention, a surfactant can be added as an additive during or before and after the addition of the fatty acid in order to improve the detergency and further enhance the solubility in cold water. As the surfactant to be added, for example, a known surfactant described on page 51 of the aforementioned “Detergent and Cleaning Dictionary” can be used. Specifically, anionic surfactants such as alkyl benzene sulfonate, α-olefin sulfonate, alkane sulfonate, alkyl sulfate, alkyl polyoxyethylene sulfate which can also be used as a foaming agent; Nonionic surfactants such as ethylene ether can be used. The addition amount of these surfactants is preferably 1 to 15% by weight in the powdered soap.

[0015]

EXAMPLES The present invention will be described in more detail with reference to the following Examples, which should not be construed as limiting the present invention. In Examples and Comparative Examples, the solubility test of the powdered soap was performed by the following method. [Solubility test] A 16 mesh (pore size: 1)
mm), and the powdered soap that has passed through the sieve is used as a sample. 0.33 g of calcium chloride in 6 liters of ion-exchanged water,
Hard water is prepared by dissolving 0.3 g of calcium carbonate.
0.5g of powdered soap sample in 500ml of hard water kept at 10 ° C
Is added and stirred at a constant speed for 5 minutes using a magnetic stirrer to dissolve. The solution was filtered through a sieve having a pore size of 0.3 mm, dried in a thermo-hygrostat at 25 ° C. and a relative humidity of 20% for 8 hours, and then the weight W of the undissolved matter attached to the sieve
(G) is measured, and the dissolution rate is determined by the following formula. Dissolution rate (%) = {(0.5-W) /0.5} × 100 Example 1 High-speed mixer [FS-GS-, manufactured by Fukae Kogyo Co., Ltd.]
10J type], 1,800 g of anhydrous sodium carbonate was charged. After rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, 200 g of water was added dropwise for 1 minute, and then 500 g of oleic acid [manufactured by NOF Corporation, NAA-34: neutralization value 202, iodine value 91] ( (0.053 equivalents to 1 equivalent of anhydrous sodium carbonate) was added dropwise at a rate of 100 g per minute over 5 minutes. During this time, the mixture in the mixer was in a powder state. When dropping 500 g of oleic acid,
The temperature of the mixture in the mixer was 41 ° C. Then
While rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, while gradually heating, 1500 g of oleic acid
(0.159 equivalents per equivalent of anhydrous sodium carbonate) was added dropwise at a rate of 70 g per minute over 21.4 minutes. During this time, the mixture in the mixer is kept in a powder state, and the temperature of the mixture in the mixer when the dropping of oleic acid is completed is 6%.
7 ° C. Finally, granulation was performed for 20 minutes while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm to obtain 3,500 g of powdered soap. The bulk density of the obtained powdered soap was 0.86 g / ml, and the dissolution rate in low-temperature hard water was 9%.
It was 1% by weight. Example 2 A Lodige mixer [M20, manufactured by Matsuzaka Giken Co., Ltd.]
3,800 g of anhydrous sodium carbonate was charged. The agitator was rotated at 600 rpm and the shears at 6,000 rpm,
After dropping 0 g in one minute, oleic acid [Nippon Yushi
Co., Ltd., NAA-34: neutralization value 202, iodine value 91]
800 g (0.040 per equivalent of anhydrous sodium carbonate)
Equivalent) was added dropwise over 1 minute. During this time, the mixture in the mixer was in a powder state. When the dropping of 800 g of oleic acid was completed, the temperature of the mixture in the mixer was 60 ° C. Then, the stirrer was set to 600 rpm and the shear was set to 6,000.
While rotating at rpm, 400 g of water was dropped at a rate of 60 g per minute over 6.7 minutes, and then, while gradually heating, 2,400 g of oleic acid (0.121 equivalent to 1 equivalent of anhydrous sodium carbonate) was added. Equivalent) at a rate of 200 g / min.
It was added dropwise over a period of minutes. During this time, the mixture in the mixer was kept in a powdery state, and the temperature of the mixture in the mixer when the dropping of oleic acid was completed was 86 ° C. Finally, granulation was performed for 10 minutes while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm to obtain 5,810 g of powdered soap. The bulk density of the obtained powdered soap is 0.82 g / ml,
The dissolution rate in low-temperature hard water was 92% by weight. Example 3 A Lodige mixer [M20, manufactured by Matsuzaka Giken Co., Ltd.]
Charge 3,800 g of anhydrous sodium carbonate, and stirrer 6
00 rpm, the shears were rotated at 6000 rpm and 300 g of water
Is dropped at a rate of 200 g per minute over 1.5 minutes, and then 850 g of oleic acid [manufactured by NOF CORPORATION, NAA-34: neutralization value 202, iodine value 91] (1 equivalent of anhydrous sodium carbonate) 0.043 eq) at a rate of 400 g per minute over 2.1 minutes. During this time, the mixture in the mixer was kept in a powder state, and when the dropping of 850 g of oleic acid was completed, the temperature of the mixture in the mixer was 38 ° C. Then, the stirrer was set to 600 rpm and the shear was set to 6,000 rp.
m, while gradually rotating, after the temperature of the mixture in the mixer reaches 40 ° C., oleic acid 2,
550 g (0.128 per equivalent of anhydrous sodium carbonate)
Equivalent) was dropped at a rate of 85 g / min over 30 minutes.
During this time, the mixture in the mixer was kept in a powder state, and the temperature of the mixture in the mixer when the dropping of oleic acid was completed was 68 ° C. Finally, while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, 500 g of a 40% by weight aqueous solution of sodium silicate (0.03 equivalent to 1 equivalent of oleic acid) is applied at a rate of 50 g per minute for 10 minutes. The mixture was dropped, and the stirrer was set at 500 rpm and the shear was set at 3,000
Granulation was performed for 10 minutes while rotating at rpm to obtain 6,760 g of powdered soap. The bulk density of the obtained powdered soap is 0.82.
g / ml, and the dissolution rate in low-temperature hard water was 100% by weight. Example 4 In a beaker having a capacity of 5,000 ml, anhydrous sodium carbonate 1,1 was added.
800 g and 200 g of water were charged and stirred with a glass rod.
The sodium carbonate containing water in the beaker was fluid and kept solid. Next, 2,000 g of this water-containing sodium carbonate was charged into a high-speed mixer [FS-GS-10J, manufactured by Fukae Kogyo Co., Ltd.], and the stirrer was rotated at 500 rpm and the shearing machine was rotated at 3,000 rpm. Oleic acid [manufactured by NOF Corporation, NAA-34: neutralization number 20]
2, Iodine value 91] 500 g (0.053 equivalent to 1 equivalent of anhydrous sodium carbonate) at a rate of 200 g / min.
It was added dropwise over a period of minutes. During this time, the mixture in the mixer was kept in a powder state, and when 500 g of oleic acid had been dropped, the temperature of the mixture in the mixer was 30 ° C. Next, the mixture was gradually heated while the stirrer was rotating at 500 rpm and the shearing machine was rotating at 3,000 rpm. After the temperature of the mixture in the mixer reached 40 ° C., 1500 g of oleic acid was further added.
(0.159 equivalents per equivalent of anhydrous sodium carbonate) was added dropwise at a rate of 80 g per minute over 18.8 minutes. During this time, the mixture in the mixer is kept in a powder state, and the temperature of the mixture in the mixer when the dropping of oleic acid is completed is 6%.
1 ° C. Finally, granulation was performed for 20 minutes while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm,
3,610 g of powdered soap was obtained. The bulk density of the obtained powdered soap was 0.85 g / ml, and the solubility in low-temperature hard water was 90% by weight. Example 5 High speed mixer [FS-GS-, manufactured by Fukae Kogyo Co., Ltd.]
10J type], 1,800 g of anhydrous sodium carbonate was charged. After rotating a stirrer at 500 rpm and a shearing machine at 3,000 rpm, and adding 50 g of water dropwise over 1 minute, 500 g of oleic acid [manufactured by NOF Corporation, NAA-34: neutralization value 202, iodine value 91] (500 g) (0.053 equivalents to 1 equivalent of anhydrous sodium carbonate) was added dropwise at a rate of 100 g per minute over 5 minutes. During this time, the mixture in the mixer was in a powder state. When the dropping of 500 g of oleic acid was completed, the temperature of the mixture in the mixer was 53 ° C. 1.65 g of sodium salt of oleic acid, 150 g of water and 1,500 g of oleic acid (0.15 g per equivalent of anhydrous sodium carbonate)
9 eq.) Were vigorously stirred and emulsified in a beaker. While gradually heating while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, this emulsion was added dropwise at a rate of 100 g per minute over 16.5 minutes. During this time, the mixture in the mixer maintained a powdery state, and the temperature of the mixture in the mixer when the dropping of oleic acid was completed was 84 ° C. As a result, 3,190 g of powdered soap was obtained, and the bulk density of the obtained powdered soap was 0.83 g / ml, and the dissolution rate in low-temperature hard water was 99% by weight. Example 6 A pressure kneader [manufactured by Moriyama Seisakusho Co., Ltd., DS1-5 type] was used.
40 g of anhydrous sodium carbonate and 86 g of sodium hydroxide were charged. The stirrer is rotated at 50 rpm, and 50 g of water is dropped at a rate of 25 g per minute over 2 minutes, and then 150 g of soybean oil fatty acid [neutralization value 199, iodine value 134] (total amount of anhydrous sodium carbonate and sodium hydroxide) 0 for
183 equivalents) was added dropwise at a rate of 20 g / min over 7.5 minutes. During this time, the mixture in the kneader maintained a powder state. When the dropping of 150 g of soybean oil fatty acid was completed, the temperature of the mixture in the kneader was 65 ° C. Next, while the stirrer was being rotated at 50 rpm, the temperature was maintained at 65 ° C., and 450 g of oleic acid (0.558 equivalent to the total amount of anhydrous sodium carbonate and sodium hydroxide) was added at 10 minutes per minute.
The solution was dropped at a speed of g over 45 minutes. During this time, the mixture in the kneader maintained a powder state. Finally, while rotating the stirrer at 50 rpm, polyoxyethylene monostearate [Nonion S-15, manufactured by NOF CORPORATION] 24
g and zeolite 4A (anhydrous) 30 g were added.
Granulation was performed for minutes to obtain 700 g of powdered soap. The bulk density of the obtained powdered soap was 0.85 g / ml, and the solubility in low-temperature hard water was 96% by weight. Example 7 High-speed mixer [FS-GS- manufactured by Fukae Kogyo Co., Ltd.]
10J type], 1,200 g of anhydrous sodium carbonate was charged. After rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, 200 g of water was dropped at a rate of 100 g per minute over 2 minutes, and then oleic acid [Nippon Oil & Fats Co., Ltd., NA
A-34: neutralization value 202, iodine value 91], 500 g (0.080 equivalent to 1 equivalent of anhydrous sodium carbonate) was dropped at a rate of 50 g per minute over 10 minutes. During this time, the mixture in the mixer was in a powder state. Oleic acid 5
When the addition of 00 g was completed, the temperature of the mixture in the mixer was 70 ° C. Stirrer at 500 rpm, shear at 3.0
While rotating at 00 rpm, while gradually heating, 1,300 g of oleic acid (0.207 equivalent to 1 equivalent of anhydrous sodium carbonate initially charged) was added dropwise at a rate of 130 g per minute over 10 minutes. Next, 600 g of sodium carbonate anhydride (1.57 equivalents per equivalent of oleic acid) was added, and then 200 g of oleic acid (1/10 of total oleic acid, 0.1 equivalent to 1 equivalent of anhydrous sodium carbonate initially charged). 032 equivalents) was added dropwise at a rate of 20 g / min over 10 minutes. During this time, the mixture in the mixer was kept in a powdery state, and the temperature of the mixture in the mixer when the dropping of oleic acid was completed was 88 ° C. Finally, granulation was performed for 20 minutes while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm to obtain 3,120 g of powdered soap. The bulk density of the obtained powdered soap is 0.85 g / ml,
The dissolution rate in low-temperature hard water was 98% by weight. Example 8 High speed mixer [FS-GS-, manufactured by Fukae Kogyo Co., Ltd.]
10J type], 1,800 g of anhydrous sodium carbonate was charged. A stirrer was rotated at 500 rpm and a shearing machine was rotated at 3,000 rpm, and 200 g of water was dropped at a rate of 100 g per minute over 2 minutes, and then oleic acid [NAA, manufactured by NOF Corporation]
-34: neutralization value 202, iodine value 91] 500 g (0.053 equivalent to 1 equivalent of anhydrous sodium carbonate) at 1 minute
It was dropped at a rate of 00 g over 5 minutes. During this time, the mixture in the mixer was in a powder state. Oleic acid 50
When the dropping of 0 g was completed, the temperature of the mixture in the mixer was 80 ° C. Then, with the stirrer rotating at 500 rpm and the shearing machine rotating at 3,000 rpm, 1,500 g of oleic acid (0.15 equivalent to 1 equivalent of anhydrous sodium carbonate) was added.
9 eq) at a rate of 60 g / min.
When 580 g of oleic acid was added dropwise over a period of minutes, the temperature of the mixture in the mixer became 90 ° C. due to the heat of the neutralization reaction. Thereafter, the addition rate of oleic acid was set to 10 g per minute, and the remaining 920 g of oleic acid was dropped over 92 minutes.
The average drop rate of 1500 g of oleic acid was 14.
7 g. During the dropping of oleic acid, the mixture in the mixer maintained a powdery state, and the temperature of the mixture in the mixer when all the dropping of oleic acid was completed was 89 ° C. As a result, 3,190 g of powdered soap was obtained, and the bulk density of the obtained powdered soap was 0.76 g / ml, and the dissolution rate in low-temperature hard water was 93% by weight. Example 9 High speed mixer [FS-GS-, manufactured by Fukae Kogyo Co., Ltd.]
10J type], 1,400 g of anhydrous sodium carbonate and 410 g of potassium hydroxide were charged. 500 rpm agitator,
A shearing machine was rotated at 3,000 rpm, and 110 g of water was dropped at a rate of 60 g / min over 1.8 minutes, and then oleic acid [manufactured by NOF Corporation, NAA-34: neutralization number 202,
Iodine value 91] of 520 g (0.056 equivalent times the total of anhydrous sodium carbonate and potassium hydroxide) at 26
g at a rate of 20 minutes. During this time, the mixture in the mixer was in a powder state. Oleic acid 520
g, the temperature of the mixture in the mixer is 5
5 ° C. Then, while gradually heating while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, 1,560 g of oleic acid (0.167 equivalent times the total of anhydrous sodium carbonate and potassium hydroxide). 78g per minute
Over 20 minutes. During this time, the mixture in the mixer maintained a powdery state, and the temperature of the mixture in the mixer when the dropping of oleic acid was completed was 76 ° C.
Finally, granulation was carried out for 20 minutes while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm to obtain a powder soap of 3,5.
40 g were obtained. The bulk density of the resulting powdered soap is 0.82 g / m
l, and the solubility in low-temperature hard water was 100% by weight. Example 10 High speed mixer [FS-GS- manufactured by Fukae Kogyo Co., Ltd.]
10J type], 1,960 g of anhydrous sodium carbonate was charged. After dropping 40 g of water in 1 minute while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, oleic acid [NAA-34, manufactured by NOF CORPORATION, neutralization number: 20]
2, iodine value 91] of 500 g (0.049 equivalent to 1 equivalent of anhydrous sodium carbonate) was added dropwise at a rate of 60 g per minute over 8.3 minutes. During this time, the mixture in the mixer was in a powder state. When the dropping of 500 g of oleic acid was completed, the temperature of the mixture in the mixer was 42 ° C. Next, while gradually heating the mixture while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm,
0 g (0.146 equivalents per equivalent of anhydrous sodium carbonate) was added dropwise at a rate of 60 g per minute over 25 minutes. During this time, the mixture in the mixer was kept in a powder state, and the temperature of the mixture in the mixer when the dropping of oleic acid was completed was 70 ° C. Finally, granulation was carried out for 20 minutes while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, to obtain 3,720 g of powdered soap. The bulk density of the obtained soap powder is 0.84 g / ml, and the dissolution rate in low-temperature hard water is 7%.
It was 2% by weight. Example 11 High-speed mixer [FS-GS-, manufactured by Fukae Kogyo Co., Ltd.]
10J type], 1,800 g of anhydrous sodium carbonate was charged. The stirrer was rotated at 500 rpm, and the shearing machine was rotated at 3,000 rpm, and oleic acid [NAA-34, manufactured by NOF Corporation:
Neutralization value 202, iodine value 91] (500 g (0.053 equivalent to 1 equivalent of anhydrous sodium carbonate)) was added dropwise at a rate of 60 g / min over 8.3 minutes. During this time, the mixture in the mixer was in a powder state. When 500 g of oleic acid has been dropped, the temperature of the mixture in the mixer is 71 ° C.
Met. Then, the stirrer was set to 500 rpm, and the shear was set to 3.0.
While rotating at 00 rpm, the temperature was maintained at 71 ° C., and 200 g of water was discharged at a rate of 8 g per minute at 1,500 g of oleic acid.
(0.159 equivalents per equivalent of anhydrous sodium carbonate) was added dropwise at a rate of 60 g per minute over 25 minutes.
During this time, the mixture in the mixer was in a powder state.
Finally, granulation was performed for 20 minutes while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, and the powdered soap 3,4
60 g were obtained. The bulk density of the resulting powdered soap is 0.81 g / m
l, and the solubility in low-temperature hard water was 78% by weight. Comparative Example 1 High-speed mixer [FS-GS-, manufactured by Fukae Kogyo Co., Ltd.]
10J type] and oleic acid [NAA-
34: neutralization value 202, iodine value 91] of 2,000 g (0.212 equivalents per equivalent of anhydrous sodium carbonate). When the stirrer was rotated at 500 rpm and the shearing machine at 3,000 rpm, 200 g of water was dropped in 1 minute, and then 1,800 g of anhydrous sodium carbonate was charged. The mixture in the mixer became a lump, and stirring was continued. It became difficult. At this time, the temperature of the mixture in the mixer was 50 ° C. Comparative Example 2 High-speed mixer [FS-GS-, manufactured by Fukae Kogyo Co., Ltd.]
10J type], 1,800 g of anhydrous sodium carbonate was charged. 200 g of water was dropped in 1 minute while the temperature of the mixture in the mixer was maintained at 25 ° C. through cold water through the jacket while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, and oleic acid [Nippon Oil & Fats Co., Ltd. NAA-34:
Neutralization value 202, iodine value 91], 500 g (0.053 equivalent to 1 equivalent of sodium carbonate) was added dropwise at a rate of 60 g per minute over 8.3 minutes. During this time, the mixture in the mixer was in a powder state. Then, the stirrer was turned on
m, while maintaining the temperature of the mixture in the mixer at 25 ° C. while rotating the shearing machine at 3,000 rpm, 1500 g of oleic acid (0.159 equivalents per equivalent of sodium carbonate) at 60 g / min. It was added dropwise at a speed over 25 minutes. During this time, the mixture in the mixer was in a powder state. Finally, granulation was performed for 20 minutes while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, and the powdered soap was 3,000 rpm.
0 g was obtained. The bulk density of the obtained powdered soap is 0.86 g / ml.
And the rate of dissolution in low-temperature hard water was 58% by weight. Comparative Example 3 High-speed mixer [FS-GS-, manufactured by Fukae Kogyo Co., Ltd.]
10J type], 1,800 g of anhydrous sodium carbonate was charged. After rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, 200 g of water was dropped at a rate of 100 g per minute over 2 minutes, and then oleic acid [Nippon Oil & Fats Co., Ltd., NA
A-34: neutralization value 202, iodine value 91], 500 g (0.053 equivalent to 1 equivalent of sodium carbonate) at 10 minutes per minute
It was dropped at a rate of 0 g over 5 minutes. During this time, the mixture in the mixer was in a powder state. Oleic acid 500
g, the temperature of the mixture in the mixer is 8
It was 0 ° C. Then, while gradually heating while rotating the stirrer at 500 rpm and the shearing machine at 3,000 rpm, 1,500 g of oleic acid (0.1 equivalent to sodium carbonate equivalent).
159 equivalents) at a rate of 60 g per minute.
When 580 g of oleic acid was added dropwise over 9.7 minutes, the temperature of the mixture in the mixer was raised to 90% by the heat of neutralization reaction.
° C. Without cooling, the dropping rate of the remaining 920 g of oleic acid was kept at 60 g / min, and the dropping was continued at 10.7 minutes, and when 640 g was added, the temperature of the mixture in the mixer became 91 ° C. Became rice cake-like. The dropping speed was kept at 60 g / min.
The addition of g of oleic acid was completed, but the mixture in the mixer remained cake-like until the addition was completed, and the temperature of the mixture at the end of the addition was 93 ° C. Comparative Example 4 High speed mixer [FS-GS-, manufactured by Fukae Kogyo Co., Ltd.]
10J type], 1,800 g of anhydrous sodium carbonate was charged. A stirrer was rotated at 500 rpm and a shearing machine was rotated at 3,000 rpm, and 200 g of water was added dropwise for 1 minute, and 500 g of oleic acid [manufactured by NOF CORPORATION, NAA-34: neutralization value 202, iodine value 91] (carbonic acid) 0.05 per equivalent of sodium
3 equivalents) was added dropwise at a rate of 60 g / min over 8.3 minutes. During this time, the mixture in the mixer was in a powder state. When the dropping of 500 g of oleic acid was completed, the temperature of the mixture in the mixer was 40 ° C. Then, with the stirrer rotating at 500 rpm and the shears rotating at 3,000 rpm,
While gradually heating, 1500 g of oleic acid (0.159 equivalent to 1 equivalent of sodium carbonate) was dropped at a rate of 200 g per minute. From the time when 900 g of oleic acid was dropped over 4.5 minutes The mixture in the mixer became a lump, and it was difficult to pulverize the lump as a lump until the end of the dropping. The temperature of the mixture in the mixer when the dropping of oleic acid was completed was 72 ° C. The production conditions of Examples 1 to 11 and Comparative Examples 1 to 4 are shown in Table 1, and the results are shown in Table 2.

[0016]

[Table 1]

[0017]

[Table 2]

While maintaining the powdery state by stirring anhydrous sodium carbonate and the like, 0.25 of the total amount of oleic acid and the like added is added.
After addition of a weight-fold amount, the temperature of the reaction mixture is increased to 40-9.
In Examples 1 to 11 in which the remaining oleic acid was added while maintaining the reaction mixture at 0 ° C and stirring the reaction mixture in a powder state, a powdered soap having a powdery state was obtained, and its bulk density was 0.76. It is as high as 0.86 g / ml and the solubility in hard water at 10 ° C. is 72 to 100% by weight, and the solubility is excellent. On the other hand, in Comparative Example 1 in which anhydrous sodium carbonate was added to oleic acid and in Comparative Example 4 in which oleic acid was added in a short time in the second-stage reaction, the reaction mixture became bulky, and In Comparative Example 3 in which the temperature exceeded 90 ° C.,
The reaction mixture became rice cake-like, and no powdery soap was obtained in any case. Further, in Comparative Example 2 in which the second-stage reaction was carried out at a temperature lower than 40 ° C., a powdery granular soap having a high bulk density was obtained, but the solubility in low-temperature hard water was low.

[0019]

According to the method of the present invention, a powdered soap having a high bulk density and a good solubility in cold water can be efficiently produced by a simple method.

Claims (5)

[Claims] 1. A solid water-soluble alkaline inorganic compound 1 to 1
When mixing and neutralizing at a ratio of 0 equivalent to 1 equivalent of a fatty acid to produce a powdered soap, the solid water-soluble alkaline inorganic compound is stirred and kept in a powdery state, while adding 0.2 to 0 of the total amount of the fatty acid added. After adding 0.3 times the amount, the temperature of the reaction mixture was maintained at 40 to 90 ° C., and the reaction mixture was stirred to maintain a powdery state, and the remaining addition amount was 0.7 to 0.8% by weight. A method for producing a powdered soap, wherein a double amount of a fatty acid is added over 10 minutes or more. 2. The method according to claim 1, wherein 2 to 30 parts by weight of water is added to 100 parts by weight of the total of the solid water-soluble alkaline inorganic compound and the fatty acid. 3. The solid water-soluble alkaline inorganic compound according to claim 1, wherein the fatty acid emulsified with 2 to 30 parts by weight of water is added to the solid water-soluble alkaline inorganic compound with respect to 100 parts by weight of the total amount of the solid water-soluble alkaline inorganic compound and the fatty acid. Method for producing powdered soap. 4. A solid water-soluble alkaline inorganic compound comprising 70 to 99% by weight of a sodium compound and potassium compound 1
The method for producing a powdered soap according to claim 1, comprising from 30 to 30% by weight. 5. An amount of 0.01 to 2 equivalents per 1 equivalent of a fatty acid of a solid water-soluble alkaline inorganic compound is added, after adding 0.5% by weight or more of the total amount of the added fatty acid. The method for producing a powdered soap according to claim 1, wherein the powdery soap is added to the reaction mixture in a solid or aqueous solution state.