JP2845953B2 - Process for producing concentrated surfactant granules - Google Patents

Description

Description: FIELD OF THE INVENTION The present invention relates to a process for preparing a quantity of concentrated surfactant active ingredients.

BACKGROUND OF THE INVENTION Granular surfactant compositions have been prepared primarily by spray drying or drum drying. In the spray drying method, the surfactant component, plus possibly the salt and builder,
A slurry is prepared by mixing with about 35 to 50% of water. The resulting slurry is heated and spray dried, which is expensive.

Such spray drying requires removing 30 to 40% by weight of water. The spray drying equipment used is expensive. The resulting granules have good solubility but low bulk density and therefore have a high filling capacity. Also, the particles may be sticky, especially when heated, and thus wall accumulation is an additional issue. There are other known disadvantages in preparing particulate matter by spray drying, for example, environmental concerns and heat sensitivity. On the other hand, the agglomeration method will be cleaner and less expensive both in terms of equipment and operating costs.

There are many prior art non-spray drying methods of preparing surfactant granules. However, most require that the surfactant be mixed with other materials, such as inorganic salts or aluminosilicate type materials. Some other methods are
It requires the use of a surfactant in acid form to operate. In most cases, the diluted surfactant particles
can get. A major challenge when using highly active surfactant pastes as starting materials in a one-step granulation process is stickiness.

U.S. Pat. No. 4,515,707, JP-A-58-183540 and JP-A-61-118500 disclose a high shear and / or cold mixing method. Typically, an excess of carbonate is needed to ensure reasonable conversion of the surfactant acid (2-10 molar excess). Excess carbonate raises the wash water pH to a very alkaline range that may be undesirable, especially for some phosphorus-free and peracid bleach-containing formulations. Such high shear cold mixing methods are known, but have drawbacks, for example, some require an extra milling step or some other utilization, and the addition of other components, primarily solids And Others use a dry neutralization technique in which a surfactant in acid form is mixed with sodium carbonate.

A practical problem with the use of the surfactant acid form is that it requires immediate use or cold storage. The reason is that highly reactive acids such as alkylsulfuric acid are apt to deteriorate unless cooled. Also, they are
It tends to undergo hydrolysis during storage to produce free sulfuric acid and alcohol. In fact, such prior art methods require a tight coupling between the granulation and the surfactant acid production, which requires an additional capital investment.

U.S. Pat. No. 4,162,994 discloses that formulations wherein the calcium salt is based on the sodium salt of an anionic surfactant and certain nonionic surfactants are non-spray dried (i.e.,
It is disclosed that it is necessary to solve the problem when processing by mechanical means. A disadvantage of that method is that insoluble calcium salts can reduce the solubility of the formulation, which has particular significance in stress situations, such as pouch-type formulations.

U.S. Pat.No. 4,427,417 discloses a method of preparing a granular detergent composition from a hydratable granular detergent salt or the like under conditions that guarantee complete hydration and coagulating to a storage-stable dry pourable aggregate. A method is disclosed.

SUMMARY OF THE INVENTION The present invention is directed to an economical method for preparing dense concentrated surfactant granules from highly active surfactant pastes using finely dispersed cold granulation.

OBJECTS OF THE INVENTION An important object of the present invention is to prepare a denser and denser surfactant particulate product by an agglomeration method without an expensive drying step. Another object is to provide thicker surfactant granules that can be stored and then mixed with other ingredients to give the final product. Another object of the method of the present invention is to provide formulated granules containing a total amount of surfactant greater than the amount of surfactant typically obtained by other means. It is still another object of the present invention to prepare very active surfactant granules that are essentially free of hydrated inorganic salts. Other objects of the present invention will be apparent in view of the following.

DETAILED DESCRIPTION OF THE INVENTION The method of the present invention consists of finely dispersing and mixing and cooling the highly active surfactant paste to give very dense surfactant granules. Most highly active surfactant pastes are too sticky at normal mixing temperatures and cannot be successfully granulated using finely dispersed mixing. Therefore, the highly active surfactant paste is cooled to the granulation temperature, if necessary, with mixing. Large, discrete particles (granules) are surprisingly prepared properly in a mixer. Thus, the "cold" of high surfactant paste
Granulation is achieved.

The granulation temperature according to the present invention is from about -65 ° C to 25 ° C using a critical fine dispersion mixing tip speed of about 5 m / sec to about 50 m / sec. Dry ice is a preferred cooling means.

An advantage of the present invention is that the preferred granules prepared according to the present invention are large, essentially pure surfactant granules. They preferably have a bulk density of about 0.4 to about 1.1 g /
cc, more preferably from about 0.5 to about 0.8 g / cc. Preferred particles of the present invention have a weight average particle size of about 200 to about 2,000 microns. More preferred granules have a particle size range of 300 to 1200μ. Yields between 25% and 85% within these ranges can be achieved. The second short mixing increases the yield of particulate particles within these preferred ranges. Also, oversized and undersized particles can be recycled.

More preferred granulation temperatures for the highly active surfactant paste are from about -40C to about 10C, most preferably from about -30C to about 0C. The evaluation of the present invention will be described later.

Surfactant granules prepared by the method of the present invention can consist of all or substantially all combinations of the components of the total composition, or can be used as intermediates. Thus, such granules greatly reduce or even eliminate the need to mix additional ingredients for the final detergent formulation. Also, the potential for segregation of components during transport, handling or storage is greatly reduced, especially if only small amounts of other substances of different particle size or density are incorporated.

Separately, the concentrate granules of the present invention can be mixed with detergent granules prepared by more conventional means to increase the total amount of surfactant in the final formulation.

Methods of Cooling the Highly Active Surfactant Paste Any suitable method of cooling the highly active surfactant paste to the granulation temperature can be used. The cooling jacket or coil can be integrated around or within the mixer. Chipped dry ice or liquid CO ₂ can be added or injected into the uniform paste. The idea is to lower the high active surfactant paste temperature to the granulation temperature so that the high active surfactant paste can be finely dispersed or "granulated" into individual particles.

Paste Viscosity and Processing Two important parameters of highly active surfactant pastes that can affect the parameters of the mixing / granulation process of the present invention are paste temperature and paste viscosity. Viscosity is a function of surfactant concentration and temperature.
The highly active surfactant of the present invention has a concentration of about 10,000 cps to 10,000,00,000.
It has a viscosity of 0 cps, preferably from about 70,000 to about 7,000,000 cps, more preferably from about 100,000 to about 1,000,000 cps. These viscosities are measured in the present invention at a temperature of about 50 ° C.

The highly active surfactant paste can be introduced into the mixer at an initial temperature in the range of about 5 to 70C, preferably about 20 to 30C. Higher temperatures reduce viscosity, but temperatures higher than about 70 ° C. may result in poor initial mixing due to increased product stickiness.

The method of the present invention surprisingly preferably comprises 200-1
Prepare large but usable granules in the range of 200μ. Such large granules are preferred, especially if the surfactant granules should be mixed with other substances that tend to be dusty. Similar sized particles are preferred to minimize segregation. No extra milling step is required or desirable. In general, the larger particles are less dusty, which is important in many consumer applications, especially those consisting of porous unitized dosage pouch-like products. Such porous products are:
It seeks to (1) avoid consumer contact with the product and (2) enhance the convenience and unity perception of unitized pouch form. If desired, insufficiently sized granules can be sieved after drying and recycled to a fine dispersion mixer.

Fine dispersion mixing and granulation Unless otherwise specified, "fine dispersion mixing" used here
And / or the term "granulation" is synonymous and mixing and granulating the highly active surfactant paste in a fine dispersion mixer using a blade tip speed of about 5 m / sec to about 50 m / sec. Means The total residence time of the mixing and granulation process is preferably on the order of 0.1 to 10 minutes, more preferably 0.5 to 8 minutes, most preferably 1 to 6 minutes. Longer preferred mixing tip speeds and granulation tip speeds are from about 10 to
40 m / s and about 15-35 m / s.

 Littleford with internal shredded blades
rd) Mixer, model # FM-130-D-12 and 7.75 a
Cuisinart Whoe with blades (19.7cm)
Processor (Cluisinart  Food Processor),
Model # DCX-Plus is two examples of suitable mixers
You. Have fine dispersion mixing and granulating ability and preferably
Any other mixer with a residence time on the order of 0.1 to 10 minutes
Can also be used. Has several blades on the rotation axis
"Turbine-type" impeller mixers are preferred. Departure
Lighting can be performed as a batch or continuous process.

The mixer must finely disperse the paste and, if desired, other ingredients. When cooling the contents of the mixer, mixing must be performed at the fine dispersion tip speed to granulate the surfactant into discrete particles. Care must be taken not to use too low or too high tip speed in the granulation process. Without being limited by theory, it is speculated that "too high shear" prevents granulation due to various stresses caused by higher tip speeds, such as a broader particle size distribution. Then, a larger amount of fine powder is generated.
Also, tip velocities that are too high increase the temperature of the material and require additional cooling.

Care must be taken not to overload the fine dispersion mixer with too much or too little surfactant paste material. If there is more than one material, the result is poor mixing and poor granulation. Thus, care must be taken to charge the mixer with a fixed amount of paste material so that satisfactory mixing and granulation is achieved. Overloading the mixer, as well as tip speeds that are too low, result in poor dispersion, reduced uniformity and large clumps. On the other hand, too high a tip speed increases the production of undesirable fines.

Work input The work input required for fine dispersion mixing in the practice of the present invention includes (1) the type of fine dispersion mixer used, (2) the mixer load level, (3) the viscosity of the paste material, and (4) If present, it will vary depending on the amount and type of dry solids used. For example, the total work required to mix and granulate several preferred paste materials using a laboratory Cuisinart food processor, Model # DCX-Plus, can range from about 7 BTU / lb.
Changed at 16 BTU. The corresponding incremental work varied from about 0.4 BTU to about 2.6 BTU per pound of paste material. The no-load work of the Cuisinart Food Processor is about 0.2 BTU /
Seconds. The Cuisinart food processor has a single 19.7 cm flat horizontal propeller and 1800 rpm
Operate with. It has a tip speed of about 18.55 m / sec.

The total work required to mix granulate the surfactant pastes of the present invention can vary from about 3 BTU to about 30 BTU per pound of material, depending on viscosity, loading, and the like. A preferred range is from about 5 BTU to about 20 BTU / lb. These BTU ranges for 1 kg of material are about 6.6-66 and about 11 respectively.
~ 14 BTU / kg.

Some of the benefits of finely dispersed mixing and granulation include granulated product glue prepared with a standard agglomerating mixer, such as a bread mixer, (1) small amounts of granulated fines; (2) uniform particle size distribution; (3) High-density granular material.

Highly active surfactant paste The activity of the aqueous surfactant paste is at least 50% and can go up to about 98%. Preferred activity is 60
~ 80% and 65% ~ 75%. The balance of the paste is primarily water, but can include processing aids such as mineral oil. The resulting concentrated surfactant granules can be added to the dry-detergent builder, or can usually be agglomerated with these builders or other substances with a binder to prepare the desired finished formulation composition.

In the method of the present invention, it is preferable to use a highly active surfactant paste during mixing and granulation to minimize the total amount of water in the system. The benefits of less water are: (1) greater amounts of other liquids in the formulation without sticking; (2) less cooling due to higher granulation temperatures;
And (3) to allow less granular drying to meet the final moisture limit.

It is important that the water or solvent (hereinafter "water") content of the highly active surfactant should not exceed 50%. Total moisture can be from about 2% to 50%, but is preferably from about 10 to about 40%, more preferably from about 15% to about 30%. Lower granulation temperatures are used for more water-containing pastes. Conversely, higher granulation temperatures can be used for lower moisture pastes.

Paste compositions having a lower water content of less than 5%, for example, about 1% to 4%, can contain an effective amount of an organic liquid solvent or processing aid. Examples of such auxiliaries are selected from suitable organic liquids, such as mineral oil, glycerin, short-chain alcohols and the like, and mixtures thereof. Processing aids can preferably be used in an amount of "0.5-20% by weight" of the paste, more preferably about 1-10%, most preferably about 2-5% by weight.

The desired water content of the surfactant granules of the present invention is determined by cooling,
It can be adjusted by adding other desired dry ingredients before granulation. Thus, no additional "drying" is needed in low moisture formulations. When desired, drying the individual granules can be accomplished with a standard fluid bed dryer. The idea is that the desired water content is 0.5-10%, preferably 1
To give a free flowing granulate having 5%.

Aqueous surfactant pastes include anionic surfactants, zwitterionic surfactants, amphoteric surfactants, nonionic surfactants,
It contains an organic surfactant selected from the group consisting of cationic surfactants and mixtures thereof. Anionic surfactants are preferred. Surfactants useful in the present invention are described in U.S. Pat. No. 3,664,961 and U.S. Pat. No. 3,919,678. Useful cationic surfactants also include those described in US Pat. No. 4,222,905 and US Pat. No. 4,239,659. The following are representative examples of surfactants useful in the present compositions.

Water soluble salts of higher fatty acids, or "soaps", are useful anionic surfactants in the present compositions. Examples of this type of surfactant include alkali metal soaps, for example, having about 8 to about 8 carbon atoms.
Sodium, potassium, ammonium and alkylol aluminum salts of higher fatty acids having about 24, preferably about 12 to about 18 carbon atoms. Soaps can be produced by direct saponification of fats or oils or by neutralization of free fatty acids. Particularly useful are the sodium and potassium salts of a mixture of fatty acids derived from coconut oil and tallow, i.e., sodium or potassium tallow and coconut soaps.

Useful anionic surfactants include water-soluble salts of organic sulfuric acid reaction products having an alkyl group having about 10 to about 20 carbon atoms and a sulfonic acid ester group or a sulfuric ester group in a molecular structure, preferably an alkali salt. Metal salts, ammonium salts and alkylol ammonium salts are included (the term "alkyl" embraces the alkyl portion of the acyl group). Examples of synthetic surfactants of this group are potassium sodium alkyl sulfate and alkyl sulfates, especially higher alcohols (C ₈ -C ₁₈ carbon atoms), for example, those produced by reducing the glycerides of tallow or coconut oil Obtained by sulfation; and sodium and potassium alkyl benzene sulfonates wherein the alkyl group has about 9 to about 15 carbon atoms in a linear or branched mirror configuration, for example,
It is of the type described in U.S. Pat. Nos. 2,220,099 and 2,477,383. Of particular value are linear linear alkyl benzene sulfonates having an average number of carbon atoms in the alkyl group of about 11 to ₁₃ (abbreviated C _{11 to} C ₁₃ LAS).

Other anionic surfactants of the present invention include sodium alkyl glyceryl ether sulfonates, especially ethers of higher alcohols derived from tallow and coconut oil; sodium coconut fatty acid monoglyceride sulfonate and sodium coconut fatty acid monoglyceride sulfate; About 1
A sodium or potassium salt of an alkylphenol ethylene oxide ether sulfate containing from about 8 to about 12 carbon atoms and the alkyl group containing from about 8 to about 12 carbon atoms; and from about 1 to about 10 units of ethylene oxide per molecule. And the sodium or potassium salts of alkyl ethylene oxide ether sulfate wherein the alkyl group has about 10 to about 20 carbon atoms.

Other anionic surfactants useful in the present invention include alpha-sulfonated fatty acids having about 6 to 20 carbon atoms in the fatty acid group and about 1 to 10 carbon atoms in the ester group. Water-soluble salts of esters; water-soluble salts of 2-acyloxyalkane-1-sulfonic acids having about 2 to 9 carbon atoms in the acyl group and about 9 to about 23 carbon atoms in the alkane moiety. Alkyl ether sulfates having about 10 to 20 carbon atoms in the alkyl group and having about 1 to about 30 moles of ethylene oxide; water-soluble salts of olefin sulfonic acids having about 12 to 24 carbon atoms; Β-alkyloxyalkanesulfonates having about 1 to 3 carbon atoms in the group and about 8 to about 20 carbon atoms in the alkane moiety are included.

Preferred anionic surfactant pastes have 10 to 10 carbon atoms.
A mixture of a linear or branched alkyl benzene sulfonate having 16 alkyls and an alkyl sulfate having an alkyl having 10 to 18 carbon atoms. These pastes are typically prepared by reacting a liquid organic substance with sulfur trioxide to produce a sulfonic acid or sulfur, and then neutralizing the acid to form a salt of the acid. Salt is a surfactant paste discussed throughout this specification.
Sodium salts are preferred because of the final performance benefits and costs of NaOH compared to other neutralizing agents, but are not required because other agents such as KOH may be used. Neutralization can be performed as part of the fine dispersion mixing step, but pre-neutralization of the acid in conjunction with acid generation is preferred.

Water-soluble nonionic surfactants are also useful as surfactants in the compositions of the present invention. Many final detergent compositions include a nonionic surfactant or a nonionic surfactant / anionic surfactant blend. Formulation of non-ionic surfactants in many applications is difficult due to potential degradation and environmental concerns, especially if using a spray drying method. in this way. The nonionic surfactant granules can be mixed with the spray-dried granules to prepare a preferred final formulation. Examples of such nonionic substances include compounds formed by condensation of an alkylene oxide group (having a hydrophilic property) with an organic hydrophobic compound that may have an aliphatic or alkylaromatic property. The length of the polyoxyalkylene group that is condensed with a particular hydrophobic group can be easily adjusted to produce a water-soluble compound having the desired degree of balance between the hydrophilic and hydrophobic elements.

Suitable nonionic surfactants include polyethylene oxide condensates of alkyl phenols, for example, alkyl phenols having alkyl groups having from about 6 to about 16 carbon atoms in either a linear or branched configuration and per mole of alkyl phenol. Condensates with about 4 to 25 moles of ethylene oxide are included.

Preferred nonionic surfactants are water-soluble condensates of aliphatic alcohols having 8 to 22 carbon atoms in either a linear or branched configuration with 4 to 25 moles of ethylene oxide per mole of alcohol. Particularly preferred are condensates of alcohols having an alkyl group of about 9 to 15 carbon atoms with about 4 to 25 moles of ethylene oxide per mole of alcohol, and condensates of propylene glycol with ethylene oxide.

As a semipolar nonionic detergent surfactant, a carbon number of about 10
A water-soluble amine oxide containing one alkyl moiety having from 18 to 18 carbon atoms and two moieties selected from the group consisting of alkyl and hydroxyalkyl groups having from 1 to about 3 carbon atoms;
A water-soluble phosphine oxide containing one alkyl moiety having 10 to 18 carbon atoms and two moieties selected from the group consisting of an alkyl group having about 1 to 3 carbon atoms and a hydroxyalkyl group: and an alkyl moiety having about 10 to about 18 carbon atoms. Water-soluble sulfoxides containing one and one moiety selected from the group consisting of alkyl and hydroxyalkyl moieties having about 1 to 3 carbon atoms are mentioned.

For amphoteric surfactants, the aliphatic moiety can be straight or branched, one of the aliphatic substituents has about 8 to 18 carbon atoms, and at least one aliphatic substituent is Derivatives of aliphatic secondary and tertiary amines or aliphatic derivatives of heterocyclic secondary and tertiary amines containing anionic water solubilizing groups are mentioned.

For amphoteric surfactants, one of the aliphatic substituents has about 8
Aliphatic quaternary ammonium having -18 carbon atoms,
Derivatives of phosphonium and sulfonium compounds are mentioned.

Highly active surfactant paste formulations must be solid at about room temperature unless the granules are kept cold until mixed with other detergent solids.

The terms “LAS” and “AS” as used herein mean “sodium laurylbenzenesulfonate” and “alkyl sulfate”, respectively. Terms such as "C _45", unless otherwise specified, refers to a C ₁₄ and C ₁₅ alkyl. Some of these AS and LAS surfactants do not require cooling if used at about 20-25 ° C.

All examples are Cuisinart food processors with 19.7 cm metal blades operating at 1800 rpm,
Model # DCX-Plus was used. The tip speed is 18.55m / sec.

Detergent builders The surfactant granules of the present invention can be prepared using some detersive builders and / or inorganic water-soluble salts. Thus, the surfactant paste can contain such materials in a salt / builder to surfactant active ingredient ratio of about 0: 1 to about 1: 1 (on a dry weight basis). A compatible detergency builder or combination of builders or water-soluble salts can be used in the present process to produce the desired end product or intermediate.
However, in most cases, the incorporation of such solid materials is unnecessary and undesirable. The present invention aims to prepare purer, denser surfactant granules.

The granular detergent of the present invention can contain a neutral salt or an alkaline salt having a pH of 7 or more in a solution, and can be either organic or inorganic in nature. The builder salt helps provide the desired density and bulk to the detergent granules of the present invention. Some of the salts are inert, but many of them
It also functions as a detergency builder substance in the washing liquid.

Examples of neutral water-soluble salts include the chlorides, fluorides and sulfates of alkali metals, ammonium or substituted ammonium. Alkali metal salts, especially the sodium salts, of the above are preferred. Sodium sulphate is typically used in detergent granules and is a particularly preferred salt.

Other useful water-soluble salts include compounds commonly known as detersive builder substances. Builders generally include various water soluble alkali metal, ammonium or substituted ammonium phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, silicates, borates, and polyhydroxysulfonic acids. Selected from salt.
Alkali metal salts, especially the sodium salts, of the above are preferred.

Particular examples of inorganic phosphate builders are sodium and potassium tripolyphosphates, pyrophosphates, polymeric metaphosphates having a degree of polymerization of about 6 to about 21, and orthophosphates. Examples of polyphosphonate builders are
Sodium and potassium salts of ethylene diphosphonic acid, sodium and potassium salts of ethane-1-hydroxy-1,1-disphosphonic acid, and ethane-1,1,2
-The sodium and potassium salts of triphosphonic acid. Other phosphorus builder compounds are described in U.S. Pat.
No. 3,213,030, 3,422,021, 3,422,137, 3,400,176, and 3,400,148.

Examples of phosphorus-free inorganic builders include sodium and potassium carbonates, bicarbonates, sesquicarbonates, tetraborate decahydrate, and a molar ratio of SiO ₂ to alkali metal oxide of about 0.5.
A silicate having a pH of from about 4.0 to about 4.0, preferably from about 1.0 to about 2.4. The compositions prepared by the method of the present invention do not require excess carbonate for processing and are preferably disclosed in U.S. Pat.
It does not contain more than 2% of finely ground calcium carbonate as disclosed in the specification of 196,093, and preferably does not contain the latter.

In the method of the present invention, it is preferable that the hydratable builder salt is not hydrated in the fine dispersion mixer.

Other Optional Ingredients Other ingredients commonly used in detergent compositions can, but need not, be incorporated into the compositions of the present invention to prepare the desired end-product laundry product, to demonstrate the breadth of the present invention. Will be included here. These include flow aids, color speckles, bleach and bleach activators, lather enhancers or defoamers, anti-fogging and anti-corrosion agents, soil settling inhibitors, soil release agents, dyes, Filler, optical brightener,
Examples include germicides, pH adjusters, non-builder alkaline sources, hydrotropes, enzymes, enzyme stabilizers, chelating agents and fragrances.

Examples The present invention will be better understood in view of the following non-limiting examples. Percentages are by weight in the mixture before subsequent drying, unless otherwise specified. Additional processing disclosure is shown in the numbered examples following the table.

The terms “LAS” and “AS” as used herein mean “sodium laurylbenzenesulfonate” and “alkyl sulfate”, respectively. Terms such as "C _45", unless otherwise specified, refers to a C ₁₄ and C ₁₅ alkyl. Some of these AS and LAS surfactants do not require cooling if used at about 20-25 ° C.

In all cases, a Cuisinart food processor with a 19.7 cm metal blade operating at 1800 rpm, model # DCX-Plus, is used. Tip speed is 18.
55m / sec. The mixer residence time is as for the best mode of Example 6.

Measure the viscosity of LAS and AS using Brookfield HAT pass No. 74002 as follows: for 60% and 70% at 0.5 rpm with spindle TA at 50 ° C .; for 74% AS At 50 ° C with spindle TE
At 0.5 rpm; with 50% AS, spindle TA at 50 ° C
At 2.5 rpm.

The granulation temperature for each high activity surfactant paste is determined on a case-by-case basis.

Example 1 Detergent activity 70% (balance water) mixed with dry ice plus small amounts of unreacted reactants and aqueous anionic C ₁₃ LAS surfactant paste having sodium sulfate as a reaction by-product in the Cuisinart Food Processor I do. The viscosity of the paste is about 800,000 cps. (See note below on viscosity measurement techniques). The paste temperature was initially about 25 ° C. The paste temperature drops from about 25 ° C to -50 ° C,
Surfactant granules are prepared.

 The following table summarizes some examples of the present invention.

(A) sodium sulfate (b) 35% for sodium carbonate monohydrate in Examples 4 and 10
And used at 37%. (C) Lauryl (12, 14, 16 blend) dimethylamine oxide. Barlox 12 is a trade name of Lonza Incorporated.

(B) Coconut based imidazoline amphoteric surfactants (monocarboxylic acids). Amphoterg
e) K is the trade name of Lonza Incorporated.

(E) Example 8 was prepared using 7.7% mineral oil as a processing aid.

Example 2 60% active (vs70%) except for using C ₁₃ LAS is Example 2
Is the same as in Example 1. Paste viscosity is about 350,000cps
It is. The granulation temperature is about -20C.

Example 3 except Ruru added to 70% active C ₁₃ LAS 10% Sodium sulfate, Example 3 is similar to Example 1. The ratio of builder salt to surfactant active ingredient is 0.16. Granulation temperature is about -35
° C.

Example 4 Using 93% active C ₁₃ LAS, sodium carbonate monohydrate 35
% Was added to the surfactant paste,
Is the same as Paste viscosity is> 1,000,000 cps. Builder has a salt to surfactant active ingredient ratio of 0.54
It is. The granulation temperature is about 4 ° C.

Example 5 C ₁₃ LAS and C ₄₅ of the AS 1: 1 except using a blend, Example 5 is similar to Example 1. Both pastes have an activity level of 70%. The viscosity of C ₄₅ AS is> 7,000,000 cps. The granulation temperature is about -5C.

Example 6 Best Mode: Example 6 is similar to Example 1 except that 74% active C ₄₅ AS (vs. 70% active C ₁₃ LAS) is used. The viscosity of the paste is> 7,000,000 cps. The granulation temperature is about 23 ° C.

The yield of these particulates within the particle size range of 200-2,000μ is about 42%. Set the granules under ambient conditions, return to the mixer and mix for about 15 seconds. Final yield is about 85%
It is. Moisture is about 14%.

Example 7 Example 7 except that 50% activity (vs 74%) C ₄₅ AS is used
Is the same as in Example 6. The viscosity of the paste is about 25,000cp
s. The granulation temperature is about -5C.

Example 8 Except that 7.7% mineral oil was added as a processing aid, Example 8
Same as Example 6. The granulation temperature is about -2C.

Example 9 except 87% active Bal Rocks 12 a (C _{12 to 16} dimethyl amine oxide) is used instead of the 70% C ₁₃ LAS, Example 9
Is the same as in Example 1. Paste viscosity> 1,000,00
It is 0cps. The granulation temperature is about -60C.

Example 10 87% active Vallox with 37% sodium carbonate monohydrate
Example 10 is the same as Example 9 except for addition to 12. The ratio of builder salt to surfactant active ingredient is 0.65. The granulation temperature is about -40C.

But using Example 11 70% Anhotage K instead of 70% active C ₁₃ LAS is Example 11 is similar to Example 1. The viscosity of the paste is about 500,000 cps. The granulation temperature is about -52C.

In the above example, dense, dense, highly active surfactant granules are successfully prepared utilizing the method of the present invention.

────────────────────────────────────────────────── ─── Continuation of front page (72) Inventor Thomas, Eugene, Lobo, Ohio, USA, Fremont, Melody, Court, 1910 David, Young (56) References JP-A-60-72998 (JP, A (58) Field surveyed (Int. Cl. ⁶ , DB name) C11D 17/06 C11D 11/00

Claims (9)

(57) [Claims] (A) a surfactant active ingredient content of at least 50
% Of the surfactant paste is cooled to a granulation temperature of −65 ° C. to 25 ° C .; (B) granulating the cooled paste using fine dispersion mixing at a tip speed of 5 to 50 m / sec. The surfactant is a group consisting of an anionic surfactant, a zwitterionic surfactant, an amphoteric surfactant, a nonionic surfactant, a cationic surfactant and a mixture thereof. Selected from
A method for producing condensed surfactant granules, wherein the mixing and granulation are carried out with a mixer residence time of 0.1 to 10 minutes. 2. The surfactant paste has a surfactant active ingredient content of up to 98%; the paste has a viscosity at 50 ° C. of 1%.
The method of claim 1, wherein the surfactant paste of step A has a temperature of 5C to 70C. 3. The method of claim 2, wherein the condensed surfactant granules have a surfactant active ingredient content of at least 50%. 4. The method of claim 1, wherein said granulation temperature of said paste is from -40 ° C to 10 ° C. 5. The method of claim 1 wherein said tip speed is 10-40 m / sec and said dwell time is 0.5-8 minutes. 6. The paste according to claim 1, wherein the amount of the surfactant is 60 to 60%.
Has a viscosity of 70,000-7,000,000 cps
Surfactant paste comprising said individual particles prepared from said paste, wherein said paste is used at an initial temperature of 20-30C, said granulation temperature is -30C to 0C. Has a mean particle size of from 200 to 2,000 and the dry granules have a bulk density of from 0.4 to 1.1 g / cc. 7. The paste has an amount of the surfactant active ingredient of 65 to 75%; and the bulk density of the particulate matter is 0.5 to 0.7%.
2. The method of claim 1, wherein the method is g / cc. 8. The surfactant paste as claimed in claim 1, wherein the surfactant paste contains a substance selected from inorganic salts or builders and mixtures thereof (the weight ratio of the substance to the surfactant active ingredient is from 0: 1 to 1: 1). The method described in. 9. The method according to claim 9, wherein the water content in the granular material comprising the individual particles is reduced by drying in a fluidized-bed dryer.
2. The method of claim 1, wherein said method is reduced to 8%.