JPH04146999A - Production of detergent composition - Google Patents

Abstract

PURPOSE:To improve flowability and preservation stability by spray drying a slurry containing a sulfonate of a fatty acid low alkyl ester, a specific inorganic builder, polyacrylic acid or a salt thereof, and water. CONSTITUTION:A detergent composition is obtained by spray drying 5 to 35 wt.% sulfonate of a fatty acid low alkyl ester represented by the formula (wherein R<1> represents 8 to 22C alkyl or alkenyl; R<2> represents 1 to 3C alkyl; and M represents a counter ion), 10 to 50wt.% at least one inorganic builder selected from the group consisting of zeolite, Na2SO4, and Na2SO3, 0.5 to 10wt.% polyacrylic acid or a salt thereof having a weight average molecular weight of 8,000 or less, and 35 to 40wt.% water. 1 to 15wt.% of this composition is mixed with 99 to 85wt.% of the other detergent components and the resulting mixture is granulated to obtain high bulk density detergent particles having a bulk density of 0.5 to 1.2g/cc.

Description

DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for producing an industrially superior detergent composition.

Conventional laundry detergents include a bulking agent (usually glauber's salt is used) that hardly contributes to cleaning performance, and this is spray-dried to a bulk density of 0.3 g/ml. It was produced as bead-like hollow particles of about cc.

However, such detergents have a low specific gravity and a low active agent concentration, which increases transportation costs and requires a considerable amount of space for storage and display.Furthermore, even in ordinary households, it is difficult to find a place to store them and it is difficult to measure them. Ta. So recently,
A method for manufacturing a high bulk density granular detergent that can be cleaned with a small amount of detergent has been proposed (Japanese Patent Application Laid-Open No. 60-96698), and has also been made into a top cloth.

On the other hand, sulfonates of fatty acid lower alkyl esters are
It is a surfactant with excellent detergency, especially hard water resistance, and high bulk density detergent compositions containing it have been reported (Japanese Patent Laid-Open Publication Nos. 62-597).

Sulfonic acid salts of fatty acid lower alkyl esters are generally obtained as an aqueous solution neutralized with an aqueous solution of an alkaline substance such as sodium hydroxide, so they can be prepared by spray-drying them alone or together with other components to remove moisture, and making them into high-bulk density detergents. It is desirable to use it for manufacturing.

However, sulfonate salts of fatty acid lower alkyl esters have the drawbacks of poor powder properties of the resulting spray-dried product, poor subsequent handling, and poor productivity for high bulk density detergents. The bulk density of the high bulk density detergent composition can be easily controlled by powder-mixing separately prepared spray-dried detergent particles to the high bulk density detergent particles to obtain the final high bulk density detergent composition. Moreover, the present applicant had previously proposed a method for improving solubility (Japanese Patent Application Laid-open No. 1-222388).
Publication No.).

If the powder physical properties (particle strength, angle of repose, etc.) of spray-dried detergent particles used for post-addition are poor, the storage stability of the detergent composition may deteriorate, causing caking or worsening fluidity. let

The same situation applies when spray-dried detergent particles containing a sulfonate of a fatty acid lower alkyl ester are used as they are or mixed with other ingredients as a detergent composition. desired.

Problems to be Solved by the Invention The present invention provides a method for producing spray-dried detergent particles (composition) containing a sulfonate of fatty acid lower alkyl ester as a cleaning active ingredient and having excellent powder physical properties.

The present invention also provides a method for producing a high bulk density detergent composition that is easy to produce and has excellent productivity, using the above-mentioned spray-dried detergent particles as a raw material dry product base.

Retrospective structure The method for producing the spray-dried detergent composition of the present invention includes the following (a)
) to (d) A slurry containing the components is spray-dried.

Further, the method for producing a high bulk density detergent composition of the present invention includes spray-drying a slurry containing the following components (a) to (d), and granulating the obtained spray-dried particles and other detergent components. to form high bulk density detergent particles.

(a) Sulfate of fatty acid lower alkyl ester = 5
~35% by weight.

(b) At least one or more inorganic builder selected from zeolite, sodium sulfate, and sodium sulfite:
] D ~ 30 heavy view%.

(c) Polyacrylic acid or its salt: 0.5 to 10% by weight.

(d) Moisture: 30-45% by weight.

The present invention will be explained in more detail below.

In the present invention, a detergent slurry containing the above-mentioned components (a) to (d) is spray-dried according to a conventional method.

The sulfonate of fatty acid lower alkyl ester as component (a) is typically represented by the following general formula (1), which is α
- Also called sulfo fatty acid ester salt.

R1-CHC○○R2 803M...(1)(R":
C, ~2. alkyl group or alkyl group R2: C, -3 alkyl group M: counter ion) As the counter ion, water-soluble salts are used, but alkali metal salts, particularly sodium salts, are preferred.

Sulfonic acid salts of saturated fatty acid lower alkyl esters are produced by transesterification or esterification of fatty acids to produce fatty acid lower alkyl esters with a predetermined number of carbon atoms, and then reacted with a sulfonating agent such as sulfuric anhydride using an ordinary sulfonating apparatus. It can be obtained by fermenting, aging and bleaching if necessary, and then neutralizing. It can also be obtained by converting a sulfonated fatty acid into a lower alkyl ester.

Sulfonic acid salts of lower alkyl esters of unsaturated fatty acids are also used, and are produced in the same manner as above using unsaturated fatty acids having a predetermined number of carbon atoms as starting materials.

As raw fatty acids, fatty acids with a predetermined number of carbon atoms derived from animals and plants derived from beef tallow, coconut oil, palm oil, etc., and synthetic fatty acids are used.

The number of carbon atoms in the fatty acid residue of the fatty acid lower alkyl ester sulfonate is preferably 8 to 22, preferably 10 to 1.
It is 8.

Component (a), fatty acid lower alkyl ester sulfonate, is present in the slurry in an amount of 5 to 35% by weight, preferably 10 to 3% by weight.
0% by weight is added. If the blending amount is less than 5% by weight, the detergency will be poor, while if it exceeds 35% by weight, the powder physical properties of the spray-dried particles obtained will deteriorate.

In addition, among the sulfonates of fatty acid lower alkyl esters, there are generally di-salt compounds whose ester bonds have been cleaved (α-sulfolipid fat resin salts R1-CHC○0M 5O,M...(U)(R1 ,M
is the same as the above-mentioned general formula (1)). in general,
This di-salt compound is contained in the fatty acid lower alkyl ester sulfonate in an amount of 3 to 20% by weight, but in the present invention, the di-salt compound is also calculated as a part of the fatty acid lower alkyl ester sulfonate.

As the inorganic builder of component (b), one or more of zeolite, sodium sulfate, and sodium sulfite is used. (b) Component inorganic builder contains 10 to 3
It is blended in an amount of 0% by weight, preferably 20 to 30% by weight. If the amount is less than 10% by weight, the powder physical properties of the resulting spray-dried particles will deteriorate, while if it exceeds 30% by weight, the detergency will decrease.

The polyacrylic acid of the component (c) may be in the acid form or the salt form (including partially neutralized products), but the pH of the detergent slurry is 5 to 1.
It is desirable to select a value in the range of 0, preferably in the range of 6 to 9. By setting the pH of the detergent slurry within this range, decomposition of the sulfonic acid salt of fatty acid lower alkyl ester of component (a) can be effectively prevented.

The weight average molecular weight of polyacrylic acid or its salt is 80
00 or less, particularly preferably 6000 or less. Molecular weight is 5o
If it exceeds oo, the effect of improving the powder properties of the resulting granulated particles will be poor.

In addition, the polyacrylic acid or its salt as component (c) is contained in the slurry in an amount of 0.5 to 10% by weight, preferably halo 65 to 5%.
% by weight is added. If the amount added is less than 0.5% by weight, the effect of improving the powder properties will be poor, while if it is added in excess of 10% by weight, the effect will be saturated, which will rather restrict the combination of other cleaning ingredients. .

An anionic surfactant, an alkali builder, a fluorescent agent, and the like can be further added as optional components to the aqueous slurry containing the components (a), (b), and (c). Alkali builders such as carbonates, bicarbonates, and silicates have the effect of improving the thermal stability of the slurry and preventing scorching during spray drying. Promotes hydrolysis of sulfonates. Therefore, when adding an alkali builder, it is desirable to add it in an amount of 5% by weight or less, preferably 3% by weight or less, in the detergent slurry.

The spray-dried detergent particles (composition) obtained by spray-drying the detergent slurry containing the above components (a), (b), and (c) have strong particle strength and good fluidity (angle of repose). , itself is easy to handle and has good storage stability.

On the other hand, spray-dried detergent particles obtained from a detergent slurry containing only peripheral components (a) and (b) and no component (c) have inferior particle strength, and are not suitable as raw materials for high bulk density detergent particles. When used, handling during manufacturing is poor and productivity is poor. In addition, high bulk density detergent compositions obtained by powder-mixing these spray-dried detergent particles break down during mixing due to the inferior particle strength of the spray-dried particles added afterward, making it difficult to control the bulk density. The particles deteriorate fluidity and storage stability.

When producing a high bulk density detergent composition, spray-dried detergent particles containing components (a), (b), and (c) obtained in the above spraying step are mixed with other necessary detergent components, and then granulated. The detergent particles have a high bulk density of 0.5 to 1.2 g/cc. In this case, since the spray-dried particles of the present invention have good particle strength and are excellent in handling, a series of granulation steps can be performed with high productivity, and an industrially excellent manufacturing method can be realized.

This granulation is carried out by mixing spray-dried particles containing fatty acid lower alkyl ester sulfonate and other detergent components in a kneader or the like, as described in JP-A No. 62-597.
This can be done by kneading, crushing with a crusher such as a cutter mill, granulating, and further coating with water-insoluble powder such as zeolite. A high bulk density detergent composition can be obtained by powder mixing a bleach activator and the like. It can also be obtained by stirring and granulating spray-dried particles and other detergent components, and the granulation method is not particularly limited.

A high bulk density detergent composition can also be prepared by powder-mixing spray-dried detergent particles with the high bulk density detergent particles obtained as described above, thereby increasing the bulk of the final high bulk density detergent composition. Density can be easily controlled and solubility is improved.

In this case, the spray-dried detergent particles are preferably added in an amount of 1 to 15% by weight based on the high bulk density detergent particles. The spray-dried detergent particles have the above-mentioned (a), (b),
The spray-dried particles may include component (c) or may be spray-dried particles of other compositions such as conventional spray-dried detergents. Since the former spray-dried particles contain polyacrylic acid or its salt as component (c), the particles are less likely to be destroyed during or after mixing, making it easier to control the bulk density, and also making it easier to control the bulk density of the detergent composition. Good fluidity (angle of repose) and storage stability (caking resistance).

Next, other detergent components that are granulated together with the spray-dried detergent particles of the present invention to form a high bulk density detergent composition will be described.

Other detergent components include anionic surfactants, nonionic surfactants, and other additives.

Examples of anionic surfactants include the following.

1) Linear alkylbenzene sulfonate having an alkyl group having an average of 8 to 16 carbon atoms, 2) α-olefin sulfonate having an average of 10 to 20 carbon atoms, 3) Alkyl sulfate having an average of 10 to 20 carbon atoms, 4 )
Alkyl ether sulfate or alkenyl ether sulfate having a linear or branched alkyl group or alkenyl group with an average carbon number of 10 to 20 and an average of 0.5 to 8 moles of ethylene oxide added, 5) Average carbon number 10-22 saturated or unsaturated fatty acid salts.

As the counter ion in these anionic surfactants, alkali metal salts such as sodium and potassium are usually suitable.

As the nonionic surfactant, the following are suitable.

(1) An E○ addition type nonionic surfactant in which an average of 4 to 25 moles of ethylene oxide (EO) is added to a JR or 2R alcohol having 8 to 18 carbon atoms.

(2) EO-P○ addition type nonionic interface in which an average of 4 to 25 moles of ethylene oxide (EO) and an average of 3 to 15 moles of propylene oxide (PO) are added to a primary or secondary alcohol having 8 to 18 carbon atoms. Activator.

Other additives include zeolite, sodium sulfate,
Inorganic builders such as sodium sulfite, sodium tripolyphosphate and sodium pyrophosphate; calcium ion scavengers such as sodium citrate, sodium ethylenediaminetetraacetate, nitrilotriacetate, sodium acrylate-sodium maleate anhydride copolymer, polyacetal carboxylate Builders; Alkali builders such as carbonates, bicarbonates, and silicates; Anti-recontamination agents such as carboxymethyl cellulose and polyethylene glycol; Rinse improvers for soaps, etc.; para-toluenesulfonates, toluenesulfonates, and xylene sulfonates , viscosity modifiers such as urea; proteases, lipases, cellulases.

Enzymes such as amylase; softening agents such as quaternary ammonium salts and bentonite; bleaching agents, fluorescent agents, fragrances, pigments, etc. can be used.

The alkali builder is present in the high bulk density detergent composition in an amount of 10 to 4
It is preferable to add it so that it is contained in an amount of 0% by weight.

Effect of the invention - According to the present invention, by spray-drying a slurry containing (a) a sulfonate of a lower alkyl ester of a fatty acid, (b) an inorganic builder, and (c) polyacrylic acid or a salt thereof, lower alkyl fatty acids can be obtained. Spray-dried detergent particles containing ester sulfonate and having strong particle strength and excellent handling characteristics during production are obtained.

In addition, by granulating these spray-dried detergent particles and other detergent components to form high bulk density detergent particles, a high bulk density detergent composition containing a sulfonate of fatty acid lower alkyl ester can be produced with high productivity. can be manufactured, and a totally superior manufacturing system can be realized.

Example (1) Preparation of spray-dried detergent particles A detergent slurry having the composition shown in Clothing-1 below was prepared and spray-dried in a countercurrent spray drying tower to prepare spray-dried detergent particles. The properties of the obtained detergent particles are also shown in Table 1.

Here, the crushing value is calculated by placing a sample in a cell with a diameter of 5 cm and a height of 5.30 mm, applying a load of 3 kg for 3 minutes to create a test piece, and measuring the load required to break this test piece. value. The measurement temperature is 45°C.

From Table 1, it can be seen that the spray-dried detergent particles of the present invention have a small crush value and excellent particle strength.

(The following is a blank space) (2) Preparation of high bulk density detergent composition Other detergent components were added to the spray-dried detergent particles in Table 1 and granulated to prepare a high bulk density detergent composition.

Here, in each example, spray-dried detergent particles obtained in each example were used.

The spray-dried detergent particles and other detergent components shown in Table 2 were mixed and kneaded using a kneader.

Then, the obtained intimate mixture pellets (]Om+nφX 20+nm) and type A zeolite or finely powdered sodium carbonate were quantitatively fed into a pulverizer (manufactured by Kaida Seiko, Speed Mill ND-30 type). The pulverizer rotated 4 stages of pulverizing blades with a diameter of 15 cm at 3000 rpm, and the screen used was a punching metal with a diameter of 21I and 111φ and an aperture ratio of 20%.

In the above manufacturing process of high bulk density detergent particles, since the spray-dried detergent particles (example product), which is the raw material base powder, have excellent powder physical properties such as particle strength and fluidity, storage and
It was easy to handle, such as transport and loading, and could be manufactured with high productivity.

2 parts by weight of finely powdered zeolite were mixed into the high bulk density detergent particles obtained by pulverization, and 10 parts by weight of the above spray-dried detergent particles were added.
A high bulk density detergent composition was prepared by mixing parts by weight, spraying perfume and adding enzyme.

The composition and properties of the obtained detergent composition are shown in Table-2.

Here, storage stability was evaluated as follows.

Evaluation of preservability' - Detergent composition was tested at 660rnQ (11X 4 X 15
After filling 90% of the neo-sand carton (cm) and gluing it, it was stored in an atmosphere of 35° C. and 85% RH for 7 days.

After that, the package is opened, the amount passing through the 6-mesh screen is measured, and the amount is judged according to the following criteria.

O: Unpassed amount 10% or less @: Amount of untransparent passage 10-20 %: Untraveled amount 20-30 %: Unpassed amount 30% or more (Margin below)

Claims (1)

[Scope of Claims] 1. A method for producing a spray-dried detergent composition, which comprises spray-drying a slurry containing the following components (a) to (d). (a) Sulfonate of fatty acid lower alkyl ester: 5
~35% by weight (b) At least one inorganic builder selected from zeolite, sodium sulfate, and sodium sulfite: 10 to 30% by weight (c) Polyacrylic acid or its salt: 0.5 to 10% by weight (d) Moisture: 30-45% by weight 2. Spray-dry a slurry containing the following components (a) to (d), and granulate the obtained spray-dried particles and other detergent components to obtain high bulk density detergent particles. A method for producing a high bulk density detergent composition. (a) Sulfonate of fatty acid lower alkyl ester: 5
~35% by weight (b) At least one inorganic builder selected from zeolite, sodium sulfate, and sodium sulfite: 10 to 30% by weight (c) Polyacrylic acid or its salt: 0.5 to 10% by weight (d) Moisture: 30-45% by weight