JPH0374500A - Production of detergent composition of high bulk density - Google Patents

Abstract

PURPOSE:To obtain the subject composition readily producible and having excellent productivity by subjecting slurry containing a sulfonate of an aliphatic acid lower alkyl ester, an inorganic builder, a benzoic acid salt and water to spray drying and treating of granulation together with other detergent component. CONSTITUTION:(A) 5-35wt.% sulfonate of an aliphatic acid lower alkyl ester is mixed with (B) 10-50wt.% inorganic builder composed of zeolite and/or sodium sulfate (or sulfite), (C) 1-10wt.% alkali metallic salt of benzoic acid and (D) 30-50wt.% water and contained in a slurry. Then, the slurry is subjected to spray drying and the resultant dried material is subjected to granulating treatment together with other detergent component to afford the aimed composition. Besides, said composition is able to suppress decomposition of the component A.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing an industrially superior high bulk density detergent composition.

Conventional laundry detergents include a bulking agent (usually mirabilite is used) that hardly contributes to cleaning performance, and are spray-dried to a bulk density of 0°3 g/ml. It was produced as bead-shaped hollow particles of about 1.

However, such detergents have a low specific gravity and a low concentration of active agent, which increases transportation costs and requires a considerable amount of space for storage and display.Furthermore, even in ordinary households, they are difficult to take up space and are difficult to measure. Ta. So recently,
A method for producing a high bulk density granular detergent that can be cleaned with a small amount of detergent has been proposed (Japanese Patent Laid-Open No. 60-96698).

It is also upholstered.

On the other hand, sulfonates of fatty acid lower alkyl esters are
It is a surfactant with excellent detergency, especially hard water resistance, and a high bulk density detergent composition containing it has been reported (Japanese Patent Application Laid-Open No. 62-597).

Sulfonate 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 alone or together with other components to remove water, and then forming a high-bulk density detergent. It is desirable to use it for manufacturing.

However, sulfonic acid salts of fatty acid lower alkyl esters tend to increase the viscosity of the slurry, making it difficult to handle and making it difficult to use a pressure nozzle during spray drying. Another drawback was that the physical properties of the dried powder easily deteriorated. moreover.

There is also the problem that when sulfonate salts of fatty acid lower alkyl esters are in contact with alkaline substances for a long time in detergent slurry or during heating during spray drying, the ester bonds are easily broken and decomposed into di-salt compounds.

The present invention, which is being developed, contains a sulfonate of a fatty acid lower alkyl ester as a cleaning active ingredient, is easy to manufacture, has excellent productivity, and has a high bulk that can suppress the decomposition of the fatty acid lower alkyl ester sulfonate. The present invention provides an industrially superior method for producing a density detergent composition.

In the method for producing a high bulk density detergent composition of the present invention (first invention), a slurry containing the following components (a) to (d) is spray-dried, and the resulting spray-dried product and It is characterized by granulating other detergent components into high bulk density detergent particles.

In addition, in addition to the components (a) to (d), the same operation as above was performed except that a slurry containing the component (e) was used.
Thermal stability during spray drying can also be improved (second invention).

(a) Sulfonate 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:
10-50% by weight.

(c) Benzoic acid alkali metal salt = 1 to 10% by weight.

(d) Moisture: 30-50% by weight.

(8) At least one alkali builder selected from carbonates, bicarbonates, and silicates (where the salt is sodium or potassium): O, S to 5% by weight.

The present invention will be explained in more detail below.

1) Spray dry the slurry containing the above-mentioned components (a) to (d) according to a conventional method. The slurry may contain methyl sulfate (alkyl sulfate), a fluorescent agent, and a small amount of anionic surfactant, which are by-products during the production of (a) In order to prevent decomposition into salts, it is desirable that alkaline substances are essentially not included. Alkaline substances such as alkali builders, which are necessary for detergent compositions, are introduced in the granulation process into high bulk density detergent particles in the first process. can do.

The slurry consisting of components (a) to (d) has a low viscosity and is easy to handle, and can be easily atomized using a pressure nozzle during spraying. Moreover, since the powder properties of the obtained spray-dried product are excellent, a manufacturing system with excellent productivity as a whole can be realized.6 Next, each component of the slurry will be explained in sequence.

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

R″-CHCoOR” [So, M...(1)
(R": Alkyl group or alkenyl group of C, . . . R": Alkyl group of C, . M: Counter ion) As the counter ion, a water-soluble salt is used, and an alkali metal salt, particularly a sodium salt, is preferable.

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. Let me.

It can be obtained by aging and bleaching if necessary and then neutralizing it. 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.

Fatty acid lower alkyl ester sulfonate.

5-35% by weight in the spray-dried product, preferably 10-30%
% 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 properties of the spray-dried product obtained will deteriorate.

In addition, among the sulfonates of fatty acid lower alkyl esters, there are generally di-salt compounds in which the ester bond has been cleaved (α-sulfolipid fat Fujisalt R''-CHCooM "So, M ... (II) (R ″、
M is the same as in the above-mentioned general formula (1). Generally, the di-salt compound is contained in the fatty acid lower alkyl ester sulfonate in an amount of 3 to 20% by weight;
In the present invention, di-salt compounds are also calculated as part of fatty acid lower alkyl ester sulfonates.

(b) As an inorganic builder component, one or more of zeolite, sodium sulfate, and sodium sulfite is used in an amount of 10 to 5
0% by weight, preferably 20-50% by weight. If the blending amount is less than 10% by weight, the powder physical properties of the obtained powder mist-dried product will deteriorate, while if it exceeds 50% by weight, the detergency will decrease.

Component (c), the alkali metal benzoate salt, is blended into the slurry in an amount of 1 to 10% by weight, preferably 1.5 to 5% by weight. If the amount is less than 1% by weight, the viscosity-lowering effect will be poor, while if it exceeds 10% by weight, the concentration of the cleaning component will decrease accordingly.

This is not preferable because the cost of raw materials also increases.

2B) The same as the first invention described above except that a small amount of alkali builder is added as component (6) to the slurry. By adding a small amount of alkali builder, in addition to the effects obtained in the first invention, the thermal stability of the slurry is improved, scorching during heating is prevented, and high-temperature hot air is used during spray drying. Productivity improves because it can be done.

As the alkali builder of component (a), one or more of carbonates, bicarbonates, and silicates are used, and as the salt, sodium salts or potassium salts are used.

(6) Ingredient Flukali Builder is 0.5% in the slurry.
~5% by weight, preferably 1-3% by weight. If the amount is less than 0.5% by weight, the thermal stability will not be sufficiently improved, while if it exceeds 5% by weight, it will promote the decomposition of the fatty acid lower alkyl ester sulfonate into di-salt, which is undesirable. .

° The spray-dried product obtained in the above step and other necessary detergent components are mixed and granulated to give a bulk density of 0.5 to 1.2 g/cc.
of high bulk density detergent particles. This granulation is carried out by JP-A-62-
As described in No. 597, a spray-dried product containing a fatty acid lower alkyl ester sulfonate and other detergent components are mixed and kneaded using a kneader or the like, and then crushed and manufactured using a crusher such as a cutter mill. It is obtained by granulating it and then coating it with a water-insoluble powder such as zeolite.

It can also be obtained by stirring and granulating the spray dried product and other detergent components, and the granulation method is not particularly limited.

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

Examples of anionic surfactants include the following.

1) Straight-chain alkylbenzene sulfonate having an alkyl group having an average carbon number of 8 to 16; 2) α-olefin sulfonate having an average carbon number of 10 to 20.

3) Alkyl sulfate having an average of 10 to 20 carbon atoms, 4) Having a linear or branched alkyl group or alkenyl group having an average of 10 to 20 carbon atoms, and having an average of 0.5 to 8 moles of ethylene oxide added. Alkyl ether sulfate or alkenyl ether sulfate, 5) Saturated or unsaturated fatty acid salt having an average carbon number of 10 to 22.

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 EO-added nonionic surfactant prepared by adding an average of 4 to 25 moles of ethylene oxide (EO) to a primary or secondary alcohol having 8 to 18 carbon atoms.

(2) EO-PO addition type nonionic interface in which an average of 4 to 25 moles of ethylene oxide (E O) 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; sodium citrate, sodium ethylenediaminetetraacetate, nitrilotriacetate, sodium polyacrylate, sodium acrylate-sodium maleate anhydride copolymer, polyacetal carboxylate Calcium ion scavenging builders such as; alkaline builders such as carbonates, bicarbonates, silicates;
Anti-recontamination agents such as carboxymethyl cellulose and polyethylene glycol; Rinse improvers for soaps, etc.; Viscosity modifiers such as para-toluene sulfonate, toluene sulfonate, xylene sulfonate, and urea; Protease, lipase, cellulase, amylase, etc. Enzymes; softening agents such as quaternary ammonium salts and bentonite; bleaching agents, fluorescent agents, perfumes, pigments, etc. can be used.

According to the present invention, when producing a high bulk density detergent composition, (a) a sulfonate of a fatty acid lower alkyl ester;
(b) A slurry containing a specific inorganic builder, (C) sodium benzoate, and (d) water in a specific amount is spray-dried, and the spray-dried product and other detergent components are granulated to form high bulk density detergent particles. By doing so, it is possible to prevent the decomposition of the fatty acid lower alkyl ester sulfonate during production, and in addition, it is possible to reduce the viscosity of the slurry, resulting in excellent productivity. It has excellent powder properties and is easy to handle, making it possible to realize an overall excellent manufacturing system.

Furthermore, by adding 0.5 to 5% by weight of a specific alkali builder to the above slurry, it is possible to suppress the hydrolysis of fatty acid lower alkyl ester sulfonate and improve the thermal stability of the slurry. Since this does not occur, high-temperature hot air can be used and productivity is improved.

Example 1 A slurry having the composition shown below (after Example 2) was prepared, and the viscosity was measured.
) had a low viscosity and were easy to handle, and they were also easy to micronize using a pressure nozzle during spray drying. In addition, the obtained dried fine powder has a bulk density of 0.25 to 0.3 g/
The particles had a smooth powder of cc and had good physical properties. On the other hand, in the comparative example (Sample &l, 2), the slurry viscosity was high, and it was impossible to refine the slurry using a pressure nozzle during spring drying.

Example 2 A slurry having the composition shown in Table 2 below was prepared.

Examples of the present invention where viscosity was measured (Sample & 13 to 17)
Both had low viscosity and were easy to handle, and they were also easy to micronize using a pressure nozzle during spray drying. Also,
It has high thermal stability and can use high temperature hot air during spray drying. Furthermore, the obtained dried fine powder has a bulk density of 0.25 to 0.
The particles were free flowing and had good physical properties of 3 g/cc. On the other hand, in the comparative example (sample Mail, 12), the slurry viscosity was high, making it impossible to refine the slurry using a pressure nozzle during spray drying, and the thermal stability was also poor.

(Space below) Example 3 Using the spray-dried product obtained in Sample &4 or 14, a high bulk density detergent composition (bulk density:
0.801/cc) respectively.

First, the spray-dried product and other detergent components are kneaded in a kneader, and the resulting intimate mixture pellets (2 ci + square) are crushed using a crusher (Speed Mill N, manufactured by Okada Seiko) and A-type zeolite.
D-30 type). At this time, 15° C. cold air was introduced together with the crushed material at a ratio of 15Q/kg of crushed material. The crusher has 300 crushing blades with a diameter of 15 cm and 4 cross stages.
Rotates with 0rp ceramic, screen is 2■φ, opening rate is 20%
punched metal was used.

Next, the obtained crushed product and A-type zeolite with an average particle diameter of 3μ were transferred to a transfer drum (D = 30cm, L = 60ci).
z) at a ratio of 97=3, 30rp seaweed,
The coated product was discharged after a residence time of 5 minutes. The resulting high bulk density detergent composition was prevented from hydrolyzing the α-sulfo fatty acid ester salt, and fully exerted the excellent detergency that is inherent in detergents containing the α-sulfo fatty acid ester salt.

Fatty acid (C□I-1@) Sodium zeolite Potassium carbonate Sodium carbonate Sodium silicate (Na, O/SiO, = 1/3) Sodium sulfate Sodium sulfite Sodium benzoate Others (fluorescent agent, enzyme, etc.) 1wt% 25wt% 7wt % 12vt% 0wt% 16wt% 3wt% 4wt% 3wt% 7vt% lvt% 25vt% 7wt% 12vt% lvt% 15wt% 3vt% 4wt% 3vt% 7wt%

Claims (1)

[Claims] 1. A slurry containing the following components (a) to (d) is spray-dried, and the resulting spray-dried product and other detergent components are granulated to form 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 50% by weight (c) Alkali metal benzoate: 1 to 10% by weight (d) Water: 30 to 50% by weight 2. High bulk density according to claim 1, wherein the slurry further contains the following component (e): A method for producing a detergent composition. (e) At least one kind of alkali builder selected from carbonates, bicarbonates, and silicates (salt is sodium or potassium): 0.5 to 5% by weight