JPH0617098A - Detergent composition and its production - Google Patents

Abstract

PURPOSE: To obtain particulate detergent compositions having a high active detergent content and a high bulk density of more than 650 g/l by completely mixing alkyl sulfate ester salts and alkoxylated nonionic surfactants with particulate starting materials in high speed mixing/densifying equipment.

CONSTITUTION: Particulate detergent compositions having a bulk density of more than 650 g/l are obtained by mixing particulate starting materials and a liquid surfactant composition comprising the following (a) to (c) in an amount of 0.1 to 50 wt.% of the objective particulate detergent compositions in high speed mixing/densifying equipment, (a) is 5 to 60 wt.% sodium or potassium salt of alkylsulfate ester, (b) is 40 to 95 wt.% alkoxylated nonion surfactant and (c) is (remaining) 0 to 20 wt.% water. The above production processes are continuously carried out and an average residence time in the highspeed mixing/densifying equipment is preferably 5 to 30 seconds. The chemical composition of the particulate starting materials is extremely free and include compounds normally seen in detergent compositions.

COPYRIGHT: (C)1994,JPO

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a method for producing a granular detergent composition having a high bulk density and good powder properties. In particular, the invention relates to a continuous process for the production of such detergent compositions, especially detergent compositions with high detergent activity. Furthermore,
The present invention relates to a granular detergent composition obtained by the production method of the present invention.

[0002]

2. Description of the Related Art Recently, in the detergent industry, for example, 600 g /
There is considerable interest in detergent powders, which have a relatively high bulk density of l or more.

Generally, there are two main types of methods for producing detergent powders. The first type consists of spray drying an aqueous detergent slurry in a spray drying tower. In the second type, the various ingredients are dry mixed and optionally agglomerated with a liquid such as a nonionic.

The most important factor controlling the bulk density of the detergent powder is the bulk density of the starting material in the dry mixing method.
In spray drying, it is the chemical composition of the slurry. Both factors can only fluctuate within a limited range. Therefore, a significant increase in bulk density causes densification of detergent powder.
It can only be achieved by additional manufacturing steps. There are several techniques known in the art that bring about such a high density. Of particular interest is the densification of the spray-dried powder by treatment after the spray-drying tower.

Due to the increasing concern for the environment, it is desirable to produce high density detergent powders containing alkyl sulfates as the active detersive ingredient. This type of active detersive material is easily biodegradable and therefore environmentally friendly.

European Patent Application Publication No. 337,330
No. Henkel relates to a continuous process for the production of high-density bulk detergent powders containing large amounts of anionic and nonionic surfactants, said process comprising spray-drying detersive substances to be nonionic. It consists of processing in a high-speed mixer so that the average residence time in the mixer is 10 to 60 seconds while adding substances. Alkyl sulphates are not mentioned here.

European Patent Application Publication No. 265,203
(Univerer) discloses a liquid surfactant composition containing anionic and nonionic surfactants. This patent also discloses the use of these compositions by spraying them onto a solid particulate absorbent material. In this specification, alkyl sulphates are specified as anionic surfactants that could be effectively used in surfactant compositions sprayed onto absorbent materials. The disadvantage of this method is that the amount of active detersive material that can be used in this method is limited and that the particulate solid material to which the liquid surfactant composition is added must be an absorbent material. Furthermore, when the amount of active detersive substance is increased, this method tends to produce sticky detergent powders with poor powder properties.

It has also been proposed to prepare granules containing highly active alkyl sulfates and to post-add these granules to a concentrated base powder essentially free of anionic substances. However, the method of making detergent particles containing this highly active alkyl sulfate ester is not attractive. This method requires a considerable amount of energy to separate and dry the alkyl sulfate paste containing water, or, as described in European Patent Application Publication No. 402,112 (P & G), the ethylene oxide group is removed. This is because additives having low cleaning activity and low biodegradability, such as ethoxylated nonionic surfactants containing 9 or more, must be mixed into the highly active detergent particles.

[0009]

An object of the present invention is to provide a granular detergent composition having a high active detergent content and a high bulk density of 650 g / l or more. Another object of the present invention is to provide a method for producing a high bulk density granular detergent composition having a high content of active detergent with low energy without adversely affecting the environment. A further object of the invention is
It is an object of the present invention to provide a method for producing a detergent composition containing an alkyl sulfate ester salt as one of the active detersive ingredients.

[0010]

The above and other objects have been achieved in a high speed mixing / densifying device (mixer / densif).
It can be achieved if a liquid surfactant system consisting of an alkylsulfate ester and an alkoxylated nonionic surfactant is thoroughly mixed with the starting material during the treatment of the particulate starting material in i. Knowledge was obtained.

First, the present invention comprises a bulk density of 65 comprising treating the particulate starting material in a high speed mixing / densifying device.
A method for producing a granular detergent composition of 0 g / l or more is provided.
The method is based on a granular detergent composition during the treatment of 0.1
˜50% by weight, (a) 5 to 60% by weight sodium or potassium salt of an alkyl sulfate (b) 40 to 95
% By weight of alkoxylated nonionic surfactant,
(C) A liquid surfactant composition, the balance of which consists of 0 to 20% by weight of water, is mixed with the starting material.

Secondly, the present invention provides a granular detergent composition obtained by the above method, having a particle porosity of less than 10%, preferably less than 5%.

The present invention relates to a method for producing a powder having a high active detergent content and a high bulk density. An important feature of the method is that the detersive material is maintained in particulate or granular form during the method. Cake formation, dough formation
Since an dough formation) is avoided, it is not necessary to add a step of reducing the particle size to the final product.

In the process of the present invention, the alkyl sulfate salt and the alkoxylated, preferably ethoxylated, nonionic surfactant are thoroughly mixed with the particulate starting material in a high speed mixing / densifying device. This is essentially an agglomeration process in which the particulate starting material is agglomerated by the liquid surfactant to produce detergent particles containing the particulate starting material and the surfactant phase. Usually, this surfactant phase acts as a binder for the particulate starting material.

The advantage of this agglomeration method over the method of absorbing a liquid surfactant composition into a particulate starting material is that the agglomeration results in a very large amount of the resulting detergent powder while maintaining good powder properties. That is, a liquid surface-active substance can be added.

This aggregation method can be carried out either continuously or batchwise. For economic reasons, it is preferred to carry out the process of the invention continuously in a high speed mixer / densifier with an average residence time of about 5 to 30 seconds.

Furthermore, this agglomeration method provides a well controlled and durable (robu) so that a detergent powder having a preferred particle size and powder characteristics comparable to those of currently available detergent powders is obtained.
st) method is important. In order to obtain a detergent powder having good powder characteristics, it is effective to add one or more components having a composition that significantly increases the viscosity of the total liquid composition obtained, to the liquid surfactant composition. When such a component is added, the viscosity is 5 times or more, preferably 10 times or more,
Most preferably, it increases 100-fold or more (measured with a Haake viscometer at shear rates of 0.1 and 20 S ^-1 ). As a result of the increased viscosity, the agglomeration method is easier to control and the powder properties of the detersive material produced by this method are improved.

Examples of such viscosity-increasing ingredients are water and especially fatty acids and a stoichiometric amount of an alkaline substance (eg caustic soda) sufficient to neutralize the fatty acids and form soaps.
It is a combination with.

In order to obtain a powder having a very high bulk density,
As described in EP-A-367,339, the detergent powder obtained by the method of the present invention is further subjected to a second step in a medium speed granulation / granulation device.
average residence time in an attor / densifier)
It may be treated in 10 minutes to be deformed or maintained in a deformable state, after which it is treated in a drying and / or cooling device in a third step.

Particulate Starting Material The method of the present invention is very flexible with respect to the chemical composition of the particulate starting material. This material includes compounds normally found in detergent compositions such as builders and cleaning actives. Compositions containing phosphates or zeolites and compositions with high or low active detergent contents can be used as particulate starting materials.

The detersive builders present in the starting material are:
Anything that can reduce the concentration of free calcium ions in the wash liquor, preferably other benefits such as making the pH alkaline, suspending dirt removed from the fibers, suspending the fabric softening clay material, etc. A composition having various properties is provided. Examples of suitable builders include alkali metal carbonates,
Precipitating builders such as bicarbonates, orthophosphates, alkali metal tripolyphosphates, sequestering builders such as nitrilotriacetates, amorphous alkali metal aluminosilicates, ion-exchange properties such as zeolites Builders are included.

The method is also suitable for making a calcite / sodium carbonate built detergent composition. The builder material used in the method of the present invention preferably consists of fine particles, desirably with a particle size of less than 10 microns. When obtaining a very bulky detergent powder, about 0.5-10% by weight of the total granular composition of a portion of the builder material is added.
As mentioned above, it is preferred to add the detergent powder during the second step of further processing in the medium speed granulator / densifier. This method is more fully disclosed in EP-A-390,251.

The amount of builder material present in the starting material is preferably 10 to 70% by weight of the total granular composition, most preferably 30 to 60% by weight.

The detersive active present in the starting material can be selected from anionic, zwitterionic, zwitterionic or nonionic detersive actives, or mixtures thereof. Examples of suitable synthetic anionic detergent compounds, (C ₉ ~C ₂₀₎ sodium benzene sulfonate and potassium salts, particularly linear secondary alkyl (C ₁₀ ~C ₁₅₎ sodium benzenesulfonate, alkyl glyceryl ether Included are sodium sulfates, especially ethers of higher alcohols derived from tallow or coconut oil and synthetic alcohols derived from petroleum. Suitable nonionics which can be used as components of the particulate starting materials include, in particular, compounds having hydrophobic groups and reactive hydrogen atoms, such as aliphatic alcohols, acids, amides or alkylphenols and alkylene oxides, especially ethylene oxide alone or Reaction products with ethylene oxide and propylene oxide are included. Special nonionic detersive compounds are generally 5 to 25 EO, ie alkyl (C _{6 to} C ₂₂ ) phenol ethylene oxide condensates with 5 to 25 units of ethylene oxide per molecule, and aliphatic (C _{8 to} C ₁₈ ). First or second straight or branched chain alcohols and ethylene oxide, generally 5 to
It is a condensation product with 40EO. The amount of washing active substance present in the starting material can be 0 to 30% by weight. This amount is preferably less than 10% by weight, more preferably less than 5% by weight.

Other examples of substances which may be present in the particulate starting material are fluorescent substances, polycarboxylate polymers, anti-redeposition agents such as carboxymethyl cellulose, fatty acids, fillers such as sodium sulphate, kaolin or Clays such as bentonite are included.

The particulate starting material used in the method of the present invention is
It can be prepared by any suitable method such as spray drying or dry mixing. It is also effective to add the components of the starting materials separately to the mixing / densification device. It is believed that one of the advantages of the process of the present invention is that high bulk density, high wash activity powders can be prepared from dry mixed or untreated starting materials without the need for expensive spray drying equipment. On the other hand, it is preferred that one or more of the components of the starting material is a liquid additive onto a solid component prepared by spray drying, granulation, or in situ neutralization in a high speed mixer.

The liquid surfactant composition which is mixed into the particulate starting material in the liquid surfactant-based mixing / densification apparatus is an anionic surfactant (sodium or potassium salt of an alkyl sulfate ester), an alkoxyl. A nonionic surfactant and water. The liquid surfactant composition is used in an amount of 0.1 to 50% by weight, preferably 20 to 50% by weight, based on the total amount of the obtained granular detergent.
It is more preferably 25 to 50% by weight. The surfactant composition of the present invention preferably has an alkyl sulfate salt content of 30% by weight or less and contains as little water as possible. Of particular interest are compositions in which the weight ratio of alkyl sulfate salt to alkoxylated nonionic surfactant is 0.125: 1 to 0.5: 1.

Preferred nonionic surfactants are ethoxylated or mixed ethoxy-propoxylated mixed primary or secondary aliphatic alcohols. Most preferred are ethoxylated primary alcohol, C ₈ -C ₁₅ primary alcohols that are particularly ethoxylated alcohol 1 2-25 moles per mole of ethylene oxide. The nonionic surfactant component of the liquid surfactant composition is the sodium or potassium salt of an alkyl sulfate. Suitable alkyl sulfates are C ₁₂ -C ₁₈ sodium alkyl sulfate esters, in particular a first sodium alkyl sulfate, alkyl potassium sulfate esters alkyl sulfates other than carbon chain length of this range can also be used.

As described above, the liquid surfactant composition contains
It is preferable to add one or more components having a composition that significantly increases the viscosity of the obtained total liquid composition. The total amount of these components is up to 20% by weight of the total liquid composition, preferably 2 to 10% by weight.

Densification Operation and Final Densification Powder For optimum densification, the particulate starting material is subjected to a three-step densification operation, as disclosed in detail in EP-A-367,339. There is a need.

The densified powder thus obtained preferably has a particle porosity of less than 10%, more preferably less than 5%. This powder can be used as a detergent powder by itself. However, in general, various additional ingredients may be added to obtain a more effective product. The amount of material post-added is generally about 10-200% by weight of the densified powder.

Examples of substances post-added to the densified powder include:
Enzymes, bleaches, bleach precursors, bleach stabilizers, foam inhibitors, fragrances, dyes are included. It is expedient to imbibe the liquid or pasty component in the solid, generally inorganic, porous particles and subsequently add this solid, porous particle to the densified powder obtained by the process of the invention.

[0033]

The method of the present invention is further illustrated by the following non-limiting examples. In the examples, percentages and percentages are by weight unless otherwise indicated. The following abbreviations are used in the examples.

PAS: First alkyl sulfate ester salt, sodium salt of C ₁₂ -C ₁₈ first alkyl sulfate ester.

NI: C ₁₂ -C ₁₄ nonionic surfactant (ethoxylated alcohol containing an average of 5 EO groups)
Made by Kolb.

Carbonate: sodium carbonate, AKZO
Made.

Silicate: Alkaline sodium silicate.

Zeolite: Zeolite A4 (Wess
alith [trademark]), manufactured by Degussa.

Soap: Sodium salt of C ₁₆ -C ₂₂ fatty acid, manufactured by Unichema.

Polymer: Sokalan CP5 / 7
Trademark type polymer, manufactured by BASF.

Sulfate: sodium sulfate.

Comparative Examples A and B The following zeolite-containing detergent granules were prepared by spray drying an aqueous slurry. The composition (% by weight) of the porous granules thus obtained is shown in Table 1.

[0043]

[Table 1] The granules were free flowing and had an average particle size of about 300 microns.

The granules were directly charged into a continuous low speed mixer. The rotation speed was about 30 rpm in each case. The average residence time of the granules in the mixer was about 2 minutes. In this device, the granules were sprayed with a mixture of 20% by weight of PAS and 80% by weight of nonionics until these granules were almost saturated. At this stage, the free-flowing properties of the granular detersive material began to decline. Table 2 shows the composition and physical properties of the obtained detergent granules.

[0045]

Table 2 Example A B Composition Zeolite 4A 57.6 - Sulfate 6.2 53.4 Carbonate - 19.0 Polymer - 1.3 water 11.2 1.3 PAS 5.0 5.0 Nonionic 3EO 20.0 20.0 100.0 100.0 Physical properties : Bulk density (g / l) 830 690 Dynamic flow rate (ml / s) 85 103 Particle diameter (micron) 320 270 In terms of powder characteristics obtained The maximum amount of cleaning active substance that can be spray dried is considered to be 25% by weight. Further, from the comparison of the particle size of the detergent granules before and after the treatment in the mixing device, it is considered that no aggregation has occurred.

Example 1 Several detergent ingredients whose solid material particle size was less than 200 microns were charged to a high speed batch mixing / densification device.
The average residence time of the granular detergent mixture in the batch mixer / densifier was about 3 minutes. The composition of the granular detergent powder leaving the batch mixing / densification device is shown in Table 3.

[0047]

[Table 3] The granular detergent composition thus obtained had good powder properties (DFR = 101 ml / s) and a bulk density of about 770 g / l. The amount of active detersive substance present in the detergent powder obtained (ie: 27.8% by weight) is higher than that obtained in the comparative example.

Examples 2 and 3 A continuous high speed mixer / densifier Loedi of several detergent ingredients whose solid material particle size is less than 200 microns.
The ge ™ Recycler CB30 was loaded.
The rotation speed was 1600 rpm. Lo of granular mixture
The average residence time in the edge recycler was about 10 seconds.

Table 4 shows the composition of the granular material discharged from the Loedige Recycler.

[0050]

[Table 4] The granular detergent composition thus obtained has good powder properties, a bulk density of about 700 g / l and a particle size of 500-60.
It had 0 micron. The amount of the active detersive substances present in the obtained detergent powder was 30.8% by weight and 3%, respectively.
It was 0.0% by weight. The amounts of these active detersive substances are much higher than those obtained in the comparative examples and also higher than the amounts of the active detersive substances obtained in Example 2. This is Re
It is a result of blending a combination of a fatty acid and a stoichiometric amount of caustic soda as a viscosity increasing substance into a liquid surfactant composition filled in a cycler. It is clear that soap was formed from this material during the mixing / densification operation.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Christoph Jio Ayu, Netherlands, 3063 Dese See Rotterdam, Oustmersland, 286 (72) Inventor Petrus Leonardos Ye Swinkels, Netherlands 6367・ S.B. Fürendaal, Her Juan Fuerde Kesutoart 8

Claims (10)

[Claims] 1. A method for producing a granular detergent composition having a bulk density of 650 g / l or more, which comprises treating the particulate starting material in a high-speed mixing / densifying device, wherein the granular detergent composition is included in the treatment. (A) 5 to 60% by weight of a sodium or potassium salt of an alkyl sulfate ester; (b) 40 to 95% by weight of an alkoxylated nonionic surfactant; c) A liquid surfactant composition comprising 0 to 20% by weight (the balance) water; 2. The method is carried out continuously, with high speed mixing /
The method according to claim 1, wherein the average residence time in the densification device is 5 to 30 seconds. 3. The amount of liquid surfactant system mixed with the starting material is 20 to 50% by weight, preferably 25 to 50% by weight.
The method according to claim 1 or 2, wherein 4. In addition to the liquid surfactant composition, one or more starting materials are mixed with one or more components having a composition that increases the viscosity of the total liquid composition obtained. The method described. 5. The method according to claim 4, wherein the additional component comprises a fatty acid and a stoichiometric amount of an alkaline substance sufficient to neutralize the fatty acid. 6. The method according to claim 4, wherein the total amount of the additional components is 20% by weight or less, preferably 2 to 10% by weight, of the total liquid composition obtained. 7. An average residence time of about 1 to 1 so that the particulate starting material is further (i) rendered deformable or maintained deformable in the second step.
The method according to any one of claims 1 to 6, wherein the treatment is performed in a medium-speed granulation / densification apparatus for 0 minutes, and (ii) in a drying and / or cooling apparatus in the third step. 8. The method according to claim 1, wherein the component (a) present in the liquid surfactant composition is a sodium salt of a C _{12 to} C ₁₈ primary alkyl sulfate ester. 9. components present in the liquid surfactant composition (b) has the formula _{R (OC 2 H 4) n} OH ( where R is C ₈ ~
9. The method according to claim 1, which is an ethoxylated nonionic surfactant represented by a C ₁₅ alkyl group and n is 2 to 25). 10. A granular detergent composition having a particle porosity of less than 10%, preferably less than 5%, obtained by the method according to any of claims 1-9.