KR970004983B1 - Compact detergent manufacturing method having improved fluidity and productivity - Google Patents

Abstract

High density detergent is produced by (1) grinding powder detergent of beads shape which is made by spraying detergent slurry containing surfactant of at least one species and a builder of at least one species downward from top of drying tower by counter-current spray dryer with a grinder. (2) In the mixture stirring assembler that multiple stirring wings of central axis is installed in opposing direction to each other and it is in a cylinder structure with central axis that rotates in high speed, the first stirring assembling under the existence of binder of at least one species, (3) after producing high density granular detergent of specific gravity of 0.7-1g/cm3 by processing the second stirring assembly process under the existence of surface modifier, add dense ash.

Description

Manufacturing method of highly concentrated detergent with improved fluidity and productivity

The present invention relates to a method for producing a high density powder detergent.

More specifically, the present invention has a cylindrical cylinder structure having a central axis rotating at high speed after grinding a powder of beads on a bead prepared by a counter-current spray drying apparatus in a grinder. After the first stirring granulation in the presence of a binder in a mixed stirring granulator in a different stirring direction in a different direction in the shaft, and having a horizontal stirring shaft inside the horizontal mixing tank, and put into the mixing mixer in which the stirring blade is installed on the shaft After the second stirring granulation treatment in the presence of a surface modifier to prepare a high-density concentrated detergent having good fluidity, neutralization (sodium carbonate apparent specific gravity 0.8 to 1.2 g / cm ³ ) was added to prevent caking and improve fluidity. It relates to a method for producing a high density powder detergent by post-addition.

In order to increase the density of the detergent, a high-density powder detergent is put into a high speed mixer (High Speed Mixer), and after grinding, the liquid material is sprayed to form contact points on the pulverized dry particles, and then into a water-insoluble substance such as zeolite. Applying a high-density detergent with good fluidity by spraying, or pulverizing the spray-dried detergent into a mixing mixer having a horizontal stirring shaft inside a horizontal mixing tank and having a stirring blade installed on the shaft, the binder and the surface modifier are present. Although a method of carrying out the stirring granulation process has been proposed, these methods have a problem in that a poor mass is generated due to poor productivity, and the detergent becomes sticky after concentration.

Methods for densifying powder detergents prepared by countercurrent spray drying apparatuses are described in Japanese Patent Nos. 61-69900, 61-69898, 78-43710, and Japanese Patent Publication No. 4-5080. It is.

However, in the method described in the patent, dry powder is put into a high-speed rotary granulator and pulverized, followed by stirring granulation in the presence of a binder and a surface modifier, or after grinding the dry powder, a horizontal stirring shaft is placed inside the horizontal mixing tank. It is put into a mixer (Rodige Mixer) having a stirring blade on the shaft, and then subjected to agitation granulation treatment in the presence of a binder and a surface modifier to densify. In the process, the binder and the surface modifier work together to produce agglomerates at the concentration of the powder detergent and the dense detergent becomes sticky, resulting in poor fluidity and agglomeration.

In general, in order to increase the density of powder detergents containing 10 to 60% by weight of surfactants, a process of pulverizing these detergents is required first. When this process occurs in a mixer, the particles are not uniform and the crushed particles are separated from the binder. In the presence of the surface modifier, agglomerates are generated by the addition of a binder in the process of stirring granulation, and even when the surface modifier is added, the formation of particles is uneven, resulting in a decrease in productivity and yield and agglomeration of the particles.

Accordingly, the present inventors have diligently studied to solve the above-mentioned conventional problems, and as a result, a detergent slurry containing at least one surfactant and one builder is sprayed from the top of the drying tower by a countercurrent spray dryer. The powder detergent (apparent density 0.2 to 0.5 g / cm ³ ) on the beads made by downward injection was pulverized in a pulverizer, and then formed into a cylindrical cylinder structure having a central axis rotating at a high speed. After the first stirring granulation in the presence of the binder in the mixing stirring granulator installed in the direction, the mixture is placed in the mixing stirring granulator having a horizontal stirring shaft inside the horizontal mixing tank, and the stirring blade is installed on the shaft, and the secondary in the presence of the surface modifier. After carrying out the stirring granulation process to make a high-density granular detergent, and after adding the heavy ash (specific gravity 0.8 to 1.2 g / cm ³ ) to this, it is excellent in fluidity and lump It has been found that a high density powder detergent is obtained which is free of particles and which is even in particles and which has good productivity.

In the present invention, as the surface modifier, aluminosilicate having an average particle diameter of 10 μm or less, which acts as a ions removal agent of Ca ions, is preferable. Inorganic fine powders such as bentonite, clay, and talc may also be used.

The surface modifier is used 1 to 40 parts by weight per 100 parts by weight of the spray dried detergent particles. At this time, when the surface modifier is less than 1 part by weight, it is difficult to obtain a good fluidity powder, when the surface modifier is more than 40 parts by weight, the fluidity is lowered, the amount of the binder is unnecessarily increased, and fine powder may be generated to reduce the feeling of use.

It is preferable to use 1-10 weight part of binders.

If the amount of the binder is less than 1 part by weight, the contact is not formed and the density is not increased. If the amount of the binder is 10 parts by weight or more, large particles are formed and have a fatal adverse effect on the fluidity.

In addition, the heavy ash used after densification is most preferably 1 to 30 parts by weight. If the amount is 1 part by weight or less, the fluidity is not sufficient, and when the amount exceeds 30 parts by weight, performance may be degraded.

The apparent specific gravity of the preferred high density detergent is 0.7 to 1.0 g / cm ³ , if the apparent specific gravity exceeds this range may adversely affect the solubility of the powder.

Preferred average particle diameters are 150 to 900 m. If the average particle diameter is less than 150 µm, fine powder generation increases, and if it exceeds 900 µm, solubility deteriorates.

Surfactants that can be used in the present invention include straight or branched chain alkylbenzenesulfonates having an alkyl group having an average carbon number of C10-C16; Alkyl or alkenyl ether sulfates containing linear or branched alkyl or alkenyl groups having an average carbon number of C8-C20 and having an average of 3 to 9 moles of ethylene oxide, propylene oxide or butylene oxide in one molecule; Alpha olefin sulfonic acid lead having a carbon atom having an average carbon number of C8-C20; Alkyl or alkenyl sulfate which has an alkyl group or alkenyl group of average C8-C20; Alkanesulfonates having a carbon atom having an average carbon number of C10-C20; Saturated or unsaturated fatty acids having carbon atoms of average carbon number C8-C20; Alkyl sulfates having a carbon atom having an average carbon number of C8-C20; General formula

Α-sulfofatty acid salts or esters, wherein A is a C1-C3 alkyl group, B is a Na or Ca ion, and R is a C8-C20 alkyl or alkenyl group; Polyoxyethylene alkyl or alkenyl ethers having an alkyl group or alkenyl group having an average carbon number of C8-C20 and to which 1 to 25 mol of ethylene oxide is added or an alkyl group or alkenyl group having an average carbon number of C8-C20 and having 1 to 30 moles of ethylene in total Nonionic surfactants with added oxides or propylene oxides are included.

As the builder in the present invention, an alkaline salt such as sodium carbonate, seskey sodium carbonate, sodium silicate, alumina silicate, bentonite, or the like may be used.

Preferred of these alumina silicates are of the general formula X '(D' ₂ O or DO) .Al ₂ O ₃ .y '(SiO ₂ ) .WH ₂ O where D' is an alkyl metal atom and D is Ca and Crystalline alumina silicate of X ', y', W being an exchangeable alkaline earth metal atom, X ', 0.5' to 2.0, y 'is 0.5 to 8, and W is any integer in moles of each component; or General formula X (D ₂ O) Al ₂ O ₃ y (SiO ₂ ) WH ₂ O (where D is Na, X, y, W are moles of each component, X is 0.5 to 1.5, y Is 1.2 to 3.5, and W is any integer).

Particularly preferred as a detergent builder is a compound of the general formula:

_{Na 2 O · Al 2 O 3} · nSiO 2 · WH 2 O

Wherein n is 1.5 to 3.5 and W is 1 to 8.

Metal ion encapsulants such as sodium diphosphate, sodium triphosphate, 1-hydroxyethane-1,1-diphosphonic acid amino trismethylene, phosphonic acid nitrilotriacetic acid, ethylene diamine hetaacetic acid citric acid or poly One or two or more anti-contamination agents selected from acrylic acid (maleic acrylate copolymer), polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone and CMC, bleaching agents such as sodium percarbonate or sodium perborate, enzymes, eg For example, alkalase, protease or cellulase, fluorescent dyes such as biphenyl or stilbene, photobleaches or perfumes can be further used.

The anti-contamination agent may contain 0.05 to 7%.

The dry powder used in the present invention is obtained by spray-drying a mixed slurry of a surfactant and a builder except for raw materials unnecessary for heat.

In the present invention, the specific gravity and the particle size of the detergent are not important, and the water content is preferably 10% or less. When the amount of water exceeds 10%, the particle fluidity is poor after assembly, and the amount of the surface modifier is unnecessarily increased.

The assembly method of the present invention basically includes three steps as follows:

1.crushing process

The spray-dried detergent particles are pulverized by introducing detergent particles while rotating the shaft of a grinder having a horizontal axis inside a horizontal grinder and a grinding arm mounted on the shaft. Grind so that the apparent specific gravity is 0.03 to 0.4 g / cm ³ larger than the initial particles. In the present invention, any kind of grinder can be used.

2. Primary assembly process

Following the above process, it has a cylindrical cylinder structure having a central axis which rotates at a high speed continuously, and in the mixed axis granulator, in which a plurality of agitator blades are installed in different directions, the detergent particles pulverized in the presence of a binder are first mixed and stirred. Assemble The granulator used in the present invention is a mixer in the form of a Schugi Mixer.

3. Secondary Assembly Process

Subsequently, in the primary assembly process, a detergent was assembled in the primary assembly process in a mixing mixer having a horizontal stirring shaft in a horizontal mixing tank continuously and a stirring blade was installed on the shaft, followed by secondary stirring assembly in the presence of a surface modifier. Is done. The secondary granulator used in the present invention is Lodige Mixer (Lodige). The heavy ash (specific gravity 0.8 to 1.2 g / cm ³ ) granulated with the fluidity improving aid is added here.

Detergent particles produced according to the present invention is performed in a different process, such as the above-mentioned grinding → primary granulation → secondary granulation, so that the particles of the densified densities are uniform, the whole process can be continuously operated per unit time Productivity is excellent, and the flowability of the powder is excellent, the lump prevention is superior to other detergents.

Hereinafter, the present invention will be described in detail with reference to Examples, but these Examples do not limit the technical scope of the present invention.

Example 1

Spray dry the detergent of the following composition:

LAS 30%

AS 5%

Sodium Silicate 7%

Na ₂ SO ₄ 14.7%

Fluorescent Dye 0.3%

AOS 10%

PEG 2%

Na ₂ CO ₃ 25%

Moisture 6%

The average particle size of the obtained detergent is 500-600 μm, and the apparent specific gravity is 0.35 g / cm ³ . 100 parts by weight of the dried detergent particles are continuously ground in a CB mixer (Lodige). The apparent specific gravity is 0.45 g / cm ³ and the average particle size is 100 to 200 μm. After the pulverized particles were passed through a Schugi mixer (Schugi, Netherlands) as a binder using 3 parts by weight of non-ion (AE-7, Korean polyol) as a binder, 20 weight of 3 μm zeolite was used as a surface modifier in a Lodige mixer. After the addition, secondary stirring granulation was carried out to remove 12 mesh or more, and 10 parts by weight of heavy ash (specific gravity 0.8 to 1.2 g / cm ³ ) was added to make a detergent. The apparent specific gravity, average particle diameter, mass, flowability and yield of the obtained detergent were measured and the values are shown in Table 1. The fluidity of the detergent is determined by the time required when 100 ml of powder is dropped from the apparent specific gravity hopper configured in KS-2709. At this time, when the time is small, it is determined that the fluidity is good. Yields are recorded after 12 grams, with 100 g taken and 12 mesh passes. If there are many 12 mesh passages, it is determined that the yield is good. The mass is measured by breaking the pressure bar when the detergent bar having a diameter of 2.5 cm and a length of 12 cm is produced at a constant pressure, and it is determined that the mass is small when the breaking pressure is small.

Example 2

Spray dry the detergent of the following composition:

LAS 30%

AS 5%

Sodium Silicate 7%

Fluorescent dye 0.3%

AOS 10%

PEG 2%

Na ₂ SO ₄ 14.7%

Moisture 6%

The average particle size of the obtained detergent was 400 to 600 μm, and 100 parts by weight of detergent particles having an apparent specific gravity of 0.35 g / cm ³ were continuously crushed in a CB mixer (Lodige) to produce particles having a specific gravity of 0.45 g / cm ³ and an average particle diameter of 130 μm. After the pulverized particles were passed through a Schugi mixer (Schugi, The Netherlands), 3 parts by weight of water was used as a binder for primary mixing and granulation, and then charged into a Lodige mixer and 20 parts by weight of a zeolite having an average particle diameter of 3 μm was added as a surface modifier. After the stirring granulation, the yield is measured, and then particles of 12 mesh or more are removed, and 20 parts by weight of heavy ash is added thereto to form a detergent. The apparent specific gravity, average particle diameter, mass, and fluidity of the obtained detergent were measured and the values are shown in Table 1.

3 to implementation

The dry powder used in Example 1 was stirred and granulated in the same manner as in Example 1, except that 20 parts by weight of clay having an average particle diameter of 15 μm was used instead of the zeolite as the surface modifier.

Example 4

The dry powder used in Example 1 was stirred and granulated in the same manner as in Example 1, except that 3 parts by weight of maleic acid-acrylic acid copolymer (45%) was used as the binder.

Example 5

The dry powder used in Example 1 was stirred and granulated in the same manner as in Example 1, except that 20 parts by weight of talc was used instead of zeolite as the surface modifier.

Comparative Example 1

100 parts by weight of the dry powder of Example 1 was added to a high speed mixer (Fukae powtac), pulverized for 10 minutes, and then 3 parts by weight of non-ion (AE-7, Korean polyol) and 20 parts by weight of zeolite having an average particle diameter of 3 μm were added. Next, stirring granulation is performed and the yield is measured. After removal of particles larger than 12 mesh, the apparent specific gravity, fluidity, mass and average particle diameter are measured. The results are shown in Table 1.

Comparative Example 2

100 parts by weight of the dry powder of Example 1 was added to a high speed mixer (Fukae powtac), pulverized for 10 minutes, and then 3 parts by weight of water and 20 parts by weight of zeolite having an average particle diameter of 3 μm were added, followed by stirring granulation to measure the yield. do. After removal of particles larger than 12 mesh, the apparent specific gravity, fluidity, mass and average particle diameter are measured. The results are shown in Table 1.

Claims (5)

Bead-based powder detergent (from an apparent density of 0.2 to 1) made by spraying a detergent slurry containing at least one surfactant and one builder down from the top of the drying tower by a counter-corrunt spray dryer. 0.5g / cm ³ ) is pulverized in a pulverizer, and has a cylindrical cylinder structure having a central axis which rotates at high speed, and at least one binder is present in a mixed stirrer granulator having a plurality of stirring blades installed in different directions on the central axis. After primary stirring granulation under the mixing, it was put into a mixing mixer having a horizontal stirring shaft inside a horizontal mixing tank and provided with stirring blades on the shaft, and then subjected to a secondary stirring granulation treatment in the presence of a surface modifier to give a specific gravity of 0.7 to 1 g. / cm ^{3 After} the high density granular detergent is prepared, it is added to the middle ashes to improve the fluidity, the yield is good, and the agglomerated powder detergent does not clump. method. The method of claim 1 wherein the surface modifier is aluminosilicate, bentonite, clay or talc having an average particle diameter of 10 μm or less. The process according to claim 1 or 2, wherein the surface modifier is used in an amount of 1 to 40 parts by weight based on 1 part by weight of the spray dried product. The method of claim 1 wherein the amount of binder is 1 to 10 parts by weight. The method of claim 1, wherein the heavy ash has an apparent specific gravity of 0.8 to 1.2 g / cm ³ and is used at 1 to 30 parts by weight.