KR20010076515A - Method for preparing laundry powder detergent - Google Patents

Abstract

PURPOSE: A powdery detergent for washing clothes is provided to maximize neutralization of fatty acid and amount of liquid components; to improve stability of product and color and to reduce odor by neutralizing liquid fatty acid containing material at high temperature. CONSTITUTION: The detergent is produced by a process comprising dry-neutralizing fatty acid or liquid ingredient containing fatty acid with alkali builder. The process includes a first step of introducing and mixing powdery raw material containing alkali builder in a mixer; a second step of providing un-neutralized surfactant for the fatty acid or the liquid ingredient into the mixture at 40-70 deg.C, and mixing it at 90-150 deg.C to neutralize the surfactant; and a third step of modifying surface of the neutralized product by adding a surface modifier. The liquid ingredient is at least one selected from polyoxyethylene alkylether, polyoxyethylene/oxypropylene alkylether; polyoxypropylene alkylether, polyoxyethyleneglycol, 30-60wt.% of alpha-olefine sulfonate solution and 30-60wt.% of alkylsulfonate solution.

Description

Manufacturing method of washing powder detergent {METHOD FOR PREPARING LAUNDRY POWDER DETERGENT}

[Industrial use]

The present invention relates to a method for producing a laundry powder detergent, and in particular, to a method for preparing a laundry powder detergent produced by dry neutralizing a fatty acid or a fatty acid-containing liquid component, wherein the neutralization more efficiently The present invention relates to a method for preparing a laundry powder detergent, which may contain components and which may solve the problem of aroma and color of a product, which are not completely neutralized.

[Prior art]

The conventional method for preparing a laundry powder detergent by neutralizing fatty acids follows the following two methods.

First, as described in Japanese Patent Laid-Open Publication Nos. S61-69900, S61-69898, and 5-5080, countercurrent spraying of slurry prepared by neutralizing acidic surfactants in a neutralization tank and then transferring them to a blending tank. After preparing low-density dry particles having a dry density of 0.5 g / cc by a spray dryer, the dry particles are separately mixed / pulverized such as a high speed mixer and a Loedige mixer. It is a method of manufacturing a high-density detergent by injecting into a device, pulverizing, spraying a liquid substance to form a contact point between the pulverized dry particles, and then modifying the surface with a water-insoluble material such as zeolite and talc. This method is poorly soluble due to the drying process, poorly soluble due to the complex process of neutralization-blending-drying and condensing, and is denatured by heat of detergent raw materials, equipment investment cost and manufacturing cost for production are high. The disadvantage is low energy efficiency.

On the other hand, it is well known that when nonionic surfactant is used as the main cleaning component of detergent, it exhibits much better cleaning power than the anionic surfactant and excellent physical properties such as bubble characteristics (Detergent washing detergent: Surfactants and interfacial) phenomena, Milton Rosen, Willey). However, polyoxyethylene alkyl ether, which is most widely used among these nonionic surfactants, is poor in thermal stability, and when the countercurrent drying apparatus is used, the polyoxyethylene alkyl ether is denatured in the drying process to form a non-aqueous substance, which is not absorbed by the dry particles and spills onto the surface. It is obtained in such a state that problems such as poor fluidity and caking have arisen, and there is a problem in that manufacturing by drying, which is a normal detergent manufacturing process, is impossible.

The second attempt was made to solve the above problem, using dry neutralization rather than liquid neutralization as described in Japanese Patent Application Laid-Open Nos. Hei 5-125400, Hei 6-9997, Hei 6-9999, and Hei 62-263299. It is a method for preparing a powder detergent. When manufacturing by this manufacturing method, the most careful thing is a neutralization process. If the neutralization is not made completely, a higher content of the liquid component is required, or due to unneutralization, a odor occurs in the detergent and has a problem of darkening the color of the product powder.

Looking at the dry neutralization method in detail, an unneutralized surfactant is introduced into a high speed rotary granulator equipped with stirring blades on a vertical and horizontal rotating shaft rotating at a high speed, and an alkali builder and other powder raw materials causing a neutralization reaction with a neutralized surfactant. After the addition of the non-ionic surfactant is added, or the unneutralized surfactant and the non-ionic surfactant at the same time to be directly neutralized and granulated. In this case, the neutralizing reactivity of the unneutralized surfactant, particularly fatty acid, is significantly lower than that of other anionic surfactants. In addition, the temperature of the fatty acid or the liquid component containing fatty acids at the time of addition has a great influence on the neutralization reaction.

When these fatty acids are added alone without mixing with other liquid components, they are usually added at a temperature of about 5 to 15 ° C. above the melting point of the fatty acids. This temperature is approximately 40 to 70 ℃. At this temperature, when fatty acid is applied to powders containing soda ash and dry direct neutralization, a large amount of fatty acids are condensed before contacting with soda ash to react, which significantly reduces the contact area. The neutralization of is not good. Therefore, a mass containing a lot of fatty acids (lump) is generated, and the neutralization is not good, resulting in a fatty acid odor. In order to neutralize, an effort to increase the contact area with the powder, such as increasing the stirring time in the mixer, increase the number of revolutions, or increase the number of blades is required.

In addition, when the fatty acid is mixed with other liquid components, it is possible to improve a lot of problems that occur in the case of directly injecting fatty acids alone, but it is also difficult to completely neutralize and take a long time to neutralize. Thus, because the unneutralized fatty acids act in the liquid phase, they require a larger amount of powder to form particles. Therefore, it limits the content of the liquid component.

In the present invention, in consideration of the problems of the prior art, in the method of manufacturing a laundry powder detergent prepared by dry neutralizing a fatty acid or a fatty acid-containing liquid, maximizing the amount of the liquid component by activating the neutralization of fatty acids as much as possible To improve the stability of the product, the object of the present invention is to provide a method for producing a laundry powder detergent that can improve the odor of the product caused by the neutralization, the color of the product.

[Means for solving the invention]

In the present invention, in order to achieve the above object, in the manufacturing method of a laundry powder detergent prepared by dry neutralizing a fatty acid or a liquid component containing a fatty acid with an alkali builder,

a) injecting and mixing the powder raw materials including alkali builders in the mixer

step;

b) a fatty acid at a temperature of 40 to 70 ° C. in the powder raw material mixture of step a) or

An unneutralized surfactant of the fatty acid-containing liquid component was added thereto, and then 90 to 150 ° C.

Neutralizing the unneutralized surfactant while mixing at a temperature of;

c) modifying the surface by mixing the surface modifier with the neutralization of step b);

It provides a method for manufacturing a laundry powder detergent comprising a.

Hereinafter, the present invention will be described in detail.

[Action]

In the present invention, when a direct neutralization reaction between an acidic unneutralized anionic surfactant and an alkali builder used in a conventional detergent is used in a mixer having a vertical or horizontal rotating shaft, the neutralized anionic surfactant is bonded and absorbed to generate a liquid non-ion. It is possible to use a large amount of surfactant and find that the rate and degree of neutralization reaction is very sensitive to temperature. In other words, by neutralizing the fatty acid or the liquid component containing fatty acids in the high temperature state by heating in the mixer, the neutralization of fatty acids is maximized to maximize the amount of the liquid component, improve the stability of the product, and generate by neutralization Odor generated in the product, the color of the product has been improved.

In the present invention, depending on the type of fatty acids, the phenomenon of fatty acid condensation by supplying steam or hot air into the mixer so that the fatty acid or fatty acid-containing liquid component introduced into the mixer at 40 to 70 ℃ is neutralized at a high temperature of about 90 to 150 ℃. Significantly diminish and allow the neutralization reaction to occur quickly. Therefore, it is possible to solve the problem occurred when manufacturing the powder detergent by the conventional dry neutralization method.

If the neutralization is not complete and not neutralized in a short time, it also adversely affects the long-term stability of the liquid component. Because carbon dioxide generated during dry direct neutralization of fatty acids and soda ash, etc. acts to form voids in the particles to maintain a stable liquid component. In the conventional method, since the neutralization reaction is late, the formation of voids is also slow, which causes a problem of keeping the liquid component stable. However, in the present invention, since the neutralization occurs in a high temperature state by the internal heating of the mixer within a short time, the generation of voids is also fast, and since the neutralization reaction is performed at a high temperature, water generated together with carbon dioxide is generated in the form of water vapor so The amount increases. As a result, it is effective to keep the liquid component stable for a long time.

Fatty acid applied in the present invention is represented by the following formula (1).

R ₁ COOM

Where

R ₁ is an alkyl group having 6 to 23 carbon atoms, and M is an alkali metal.

The liquid components used in the present invention include polyoxyethylene alkyl ether, polyoxyethylene / oxypropylene alkyl ether, polyoxypropylene alkyl ether, polyoxyethylene glycol, aqueous solution of alpha olefin sulfonate having a content of 30 to 60 weight, Alkyl sulfonate aqueous solution of 30 to 60 weight, and the like.

R ₂ -CH ₂ -O- (CH ₂ -CH ₂ -O) n ₁ -R ₇

R ₃ -CH ₂ -O- (CH ₂ -CH ₂ -O) n _2- (CH ₂ -CH ₂ -CH ₂ -O) n ₃ -R ₇

R ₄ -CH ₂ -O- (CH ₂ -CH ₂ -CH ₂ -O) n ₄ -R ₇

HO- (CH ₂ -CH ₂ -O) n ₅ -H

R ₅ -O-SO ₃ M

R _6- (CH ₂ -CH ₂ -O) n ₆ -SO ₃ M

Where

R ₂ to R ₆ is an alkyl group having 6 to 20 carbon atoms,

R ₇ is a hydrogen atom or an alkyl group having 1 to 3 carbon atoms,

M represents an alkali metal,

n ₁ to n ₆ represent the average added moles of ethylene oxide and propylene oxide.

N ₁ represents 3 to 20 mol, n ₂ to n ₄ , n ₆ is 1 to 7 mol,

Formula 5 has an average molecular weight of 1000 to 6000.

And the dry direct neutralization reaction applied in the present invention consists of the form of the following schemes 1-3.

2RCOOH + M ₂ CO _3- > RCOOM + RCOOH + MHCO _3- > 2RCOOM + H ₂ O + CO ₂ ↑

2RSO ₃ H + M ₂ CO _3- > RSO ₃ M + RSO ₃ H + MHCO _3- > 2RSO ₃ M + H ₂ O + CO ₂ ↑

2ROSO ₃ H + M ₂ CO _3- > RSO ₃ M + RSO ₃ H + MHCO _3- > 2RSO ₃ M + H ₂ O + CO ₂ ↑

Where

R is an alkyl group and M represents an alkali metal.

As the powder component to be applied in the present invention, an alkali builder, a neutralized anionic surfactant, clay, bentonite, zeolite and the like are applied. As the alkali builder, one selected from the group consisting of M ₂ CO ₃ , MHCO ₃ , M ₂ SO ₄ , and MHSO ₄ may be used. M here means an alkali metal. Neutralized anionic surfactants are alkylbenzene sulfonates, alkyl sulfonates, alphaolefin sulfonate powders and the like.

More specifically, the manufacturing method of the present invention, first, the powder raw material is mixed in a horizontal or vertical mixer, and then the fatty acid alone or a liquid component containing fatty acid is injected into the mixer by a method such as spraying at a temperature of 40 to 70 ℃. Put it in. In particular, it is preferable to add a fatty acid and a liquid component together. At the same time as the liquid component is added, steam of 100 ° C. or more, or hot air of 150 to 300 ° C. is added to the inside of the mixer to raise the temperature inside the mixer so that the liquid component is neutralized at a high temperature. Similar to the detergent process.

When the liquid phase components are neutralized at a high temperature due to the internal heating of the mixer, it is easier to control the stirring time. In general, when neutralized at low temperature, after a certain point of time, the product does not become a particle and the product becomes sticky or a lot of lumps are generated. However, neutralizing at high temperature makes the proper stirring time long, making the adjustment easier.

The final powder detergent is prepared by adding a surface modifier to the sticky particles neutralized at a high temperature to modify the surface and add an additive. The surface modifier applied in the present invention employs one or more selected from the group consisting of zeolites, clays, talc, and silicas used in common detergent processes.

The present invention will be described in more detail with reference to the following examples and comparative examples. However, the examples are only for illustrating the present invention and are not limited thereto.

EXAMPLE

Example 1

As the composition shown in Table 1, the powder consisting of soda ash, forget-me-not and white clay was added and mixed in a vertical mixer, and then the liquid components composed of fatty acids alone were injected by mixing at a temperature of 40 to 70 ° C. At the same time as adding the liquid component of polyoxyethylene alkyl ether and polyoxyethylene glycol, the inside of the mixer was heated with hot air so that the inside temperature of the mixer became a high temperature of 90 to 150 ° C. so that the liquid component was neutralized at a high temperature. . In addition, the mill speed is 50 to 3000 rpm so that the unneutralized fatty acid and soda ash and dry neutralization in the process of grinding and granulation. In this process, powder particles having a concentrated surface were formed, and zeolite was added as a surface modifier to the particles having a concentrated surface to modify the surface of the particles to form detergent particles. Powder detergent for washing was prepared by mixing fluorescent dyes, fragrances, enzymes and antifoaming agents.

The powder detergent prepared was shown in Table 1 by measuring yield, apparent density, solubility, odor measurement, and whiteness.

Yield was calculated as the ratio of the weight of the final detergent to the weight of the feedstock, the apparent density was used with a powder tester (Howgawa Micron, Japan), the fluidity is 100 ml of laundry powder detergent 10 mm in the lower diameter The time passed through the funnel was measured, and the solubility was added to 10 g of the laundry powder detergent in 1 L of ion-exchanged water, and stirred for about 5 minutes to allow the detergent solution to pass through a standard mesh of 200 mesh. The dry weight of the residue was measured to determine the weight of the detergent dissolved in the initial 10 g, and the odor measurement was carried out by sensory evaluation to 10 evaluators using the scent of each prepared detergent sample on the scale of sensory fatty acid odor on a 5-point scale. Averaged (e.g. no fatty acid odor occurs at 5 points), and the whiteness was determined by using a colorimeter (SPECTRO COLOR METER SE 2000 from NIPPON DENSHOKU). It was measured by the WB value representing the whiteness value.

Example 2

Powdered laundry detergent was prepared in the same manner as in Example 1, except that fatty acid, polyoxyethylene alkyl ether, and polyoxyethylene glycol were added together as a liquid component as shown in Table 1.

Example 3

Powdered detergent for laundry as in Example 1, except that fatty acid and polyoxyethylene alkyl ether were added together as a liquid component and alkyl sulfonate (30 weight), which is a risk of corrosion, was separately added as shown in Table 1. Was prepared.

Example 4

Powdered laundry detergent was prepared in the same manner as in Example 1, except that fatty acid, polyoxyethylene alkyl ether, and polyoxyethylene glycol were added together as a liquid component as shown in Table 1.

Comparative Example 1

As in the composition shown in Table 1, first, the fatty acid was added alone as a liquid component, and then washed in the same manner as in Example 1 except that the liquid components of polyoxyethylene alkyl ether and polyoxyethylene glycol were mixed without adding hot air. Powder detergent was prepared.

Comparative Example 2

Powdered detergent for laundry as in Example 1 except that fatty acid, polyoxyethylene alkyl ether and polyoxyethylene glycol were added together as liquid components and mixed without adding hot air when the liquid components were added as shown in Table 1. Was prepared.

division Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 Composition (part by weight) fatty acid 5.0 5.0 5.0 5.0 5.0 5.0 Polyoxyethylene alkyl ether 16.0 16.0 16.0 18.0 16.0 16.0 Polyoxyethylene glycol 1.0 1.0 - - 1.0 1.0 Alkyl sulfonate - - 2.0 - - - Soda ash (sodium carbonate) 30.0 30.0 30.0 30.0 30.0 30.0 Forget-me-not (sodium sulfate) 12.0 12.0 12.0 10.0 12.0 12.0 Clay 5.0 5.0 5.0 5.0 5.0 5.0 Zeolite 30.0 30.0 30.0 30.0 30.0 30.0 Fluorescent dyes 0.3 0.3 0.3 0.3 0.3 0.3 enzyme 0.3 0.3 0.3 0.3 0.3 0.3 Antifoam 0.4 0.4 0.4 0.4 0.4 0.4 Detergent Properties Yield () 91.4 97.2 94.5 93.7 82.2 83.5 Apparent specific gravity (g / cc) 0.84 0.85 0.87 0.87 0.84 0.85 Fluidity (sec) 24 23 24 26 31 30 Solubility (weight) 98.3 99.4 99.1 99.0 95.2 96.5 Odor measurement 3.52 4.92 4.76 4.84 1.42 2.25 Whiteness (WB) 92.1 97.8 95.7 96.8 80.1 87.5

In the above table, the fluorescent dye is Tinopal CBS-X manufactured by Ciba Specialty Chemical, Switzerland, the enzyme is Savinase 12.0T, manufactured by Novo Nordisk, Denmark, and the antifoaming agent is manufactured by DC Silicon, Korea. LDC1215.

As can be seen in the above table, the laundry powder detergent of the present invention was found to be excellent in terms of fluidity, solubility, yield, smell measurement and color.

The manufacturing method of the present invention maximizes the amount of the liquid component by activating the neutralization of the fatty acid to the maximum by neutralizing the liquid component containing the fatty acid or fatty acid in a high temperature state by heating inside the mixer without using a countercurrent spray drying device In addition, it can improve the stability of the product, improve the smell of the product caused by the neutralization, and improve the color of the product. In addition, since heat is supplied to the liquid raw materials by the internal heating method of the mixer, it is possible to eliminate the cooling effect generated when the liquid components are transferred compared to the method of heating and neutralizing the liquid components before adding the mixer. The efficiency can be maximized, and the variation of liquid components by heating can be minimized. Therefore, the laundry powder detergent prepared by the method of the present invention is excellent in fluidity, solubility, yield, smell measurement, and color.

Claims (3)

In the manufacturing method of the laundry powder detergent prepared by dry neutralizing a fatty acid or a liquid component containing fatty acids with an alkali builder, a) injecting and mixing the powder raw materials including alkali builders in the mixer step; b) a fatty acid at a temperature of 40 to 70 ° C. in the powder raw material mixture of step a) or An unneutralized surfactant of the fatty acid-containing liquid component was added thereto, and then 90 to 150 ° C. Neutralizing the unneutralized surfactant while mixing at a temperature of; c) modifying the surface by mixing the surface modifier with the neutralization of step b); Method of manufacturing a powder detergent for washing comprising a. The method of claim 1, The temperature of step b) is to increase the temperature to 90 to 150 ℃ by adding steam or 100 or 150 to 300 ℃ hot air inside the mixer. The method of claim 1, The liquid component of step b) is polyoxyethylene alkyl ether, polyoxyethylene / oxypropylene alkyl ether, polyoxypropylene alkyl ether, polyoxyethylene glycol, 30 to 60 weight of alpha olefin sulfonate aqueous solution, and 30 to 60 weight The manufacturing method of the laundry powder detergent chosen from 1 or more types from the alkylsulfonate aqueous solution of this.