JP2022164451A - Method for producing detergent composition - Google Patents

Abstract

To provide a method for producing a detergent composition having excellent handleability even if a sodium alkylbenzenesulfonate produced using a solid acid catalyst is used.SOLUTION: A method for producing a detergent composition comprises following Step 1. Step 1; a step of preparing a slurry containing following components (a) to (c). The component (a): a linear or branched-chain sodium alkylbenzenesulfonate (LAS) having an average carbon chain length of 10 or more and 15 or less (provided that the component (a) contains 2-LAS and the amount of 2-LAS in the component (a) is 20 mass% or more); the component (b): an inorganic salt (provided that the component (b) contains a potassium salt); and the component (c): water (provided that a molar ratio of [potassium]/[sodium] in the detergent composition is 0.01 or more and 5 or less.SELECTED DRAWING: None

Description

The present invention relates to a method for producing a detergent composition containing sodium alkylbenzenesulfonate.

From the viewpoint of economic efficiency and foamability, many detergent compositions containing detergent particles mainly composed of an anionic surfactant such as sodium alkylbenzenesulfonate are produced.

The current mainstream method for producing sodium alkylbenzenesulfonate is a method using olefin as a raw material and hydrogen fluoride as a catalyst (Patent Document 1). A manufacturing method using a solid acid catalyst (DETAL method) is also known.

JP-A-5-271115

The present inventors investigated preparation of detergent particles using sodium alkylbenzenesulfonate produced using a solid acid catalyst. However, it has been found that when sodium alkylbenzenesulfonate produced using a solid acid catalyst is used, the slurry becomes viscous, causing problems such as clogging in pipes.

Accordingly, the present invention relates to providing a method for producing a detergent composition which is excellent in handling even when sodium alkylbenzenesulfonate produced using a solid acid catalyst is used.

The present invention relates to the following [1] to [6].
[1] A method for producing a cleaning composition comprising the following step 1.
Step 1: A step of preparing a slurry containing the following components (a) to (c).
Component (a): Linear or branched sodium alkylbenzenesulfonate (LAS) having an average carbon chain length of 10 or more and 15 or less (where component (a) contains 2-LAS and 2- The amount of LAS is 20% by mass or more.)
Component (b): Inorganic salt (However, Component (b) contains potassium salt.)
Component (c): water (provided that the [potassium]/[sodium] molar ratio in the detergent composition is 0.01 or more and 5 or less.)
[2] The production method according to [1] above, further comprising step 2 below.
Step 2: A step of spray-drying the slurry obtained in Step 1 to prepare detergent particles.
[3] the above [1] or [2], wherein the component (b) further contains a sodium salt, and the molar ratio of [potassium]/[sodium] in the component (b) is 0.01 or more and 10 or less; Method of manufacture as described.
[4] The production method according to any one of [1] to [3] above, wherein the slurry in step 1 further contains 0.1% by mass or more and 10% by mass or less of the following component (d).
Component (d): Cationic surfactant [5] Any one of the above [1] to [4], wherein the slurry in step 1 further contains 0.1% by mass or more and 10% by mass or less of the following component (e): 1. The manufacturing method according to item 1.
Component (e): Water-soluble polymer [6] Use of the cleaning composition obtained by the production method according to any one of [1] to [5] as a laundry detergent.

According to the present invention, it is possible to provide a method for producing a detergent composition that is excellent in handling even when sodium alkylbenzenesulfonate produced using a solid acid catalyst is used.

When the inventors of the present invention investigated this thickening phenomenon, it was found that sodium alkylbenzenesulfonate produced by a method using hydrogen fluoride as a catalyst and sodium alkylbenzenesulfonate produced by the DETAL method produced isomers of alkylbenzenesulfonic acid. We found that there is a difference in the distribution. Since the sodium alkylbenzenesulfonate produced by the DETAL method contains a large amount of highly crystalline 2-LAS, it is speculated that the proportion of 2-LAS affects the viscosity of the slurry containing sodium alkylbenzenesulfonate. did.
The present inventors have further studied, even if sodium alkylbenzene sulfonate with a large amount of 2-LAS is blended as a constituent component of the slurry, if the molar ratio of [potassium] / [sodium] in the slurry is within a certain range , unexpectedly found that the increase in viscosity of the slurry can be suppressed, and completed the present invention.

The production method of the present invention is characterized by including Step 1 shown below.

1. Step 1: Step of preparing a slurry Step 1 is a step of preparing a slurry containing components (a) to (c).

Component (a)
Component (a) is linear or branched sodium alkylbenzenesulfonate (LAS) having an average carbon chain length of 10 or more and 15 or less. However, component (a) contains 2-LAS, and the amount of 2-LAS in component (a) is 20% by mass or more. In the present specification, for the sake of convenience, not only straight-chain alkyl groups but also branched-chain alkyl groups are abbreviated as LAS.

Component (a) is composed of various isomers of LAS. 2-LAS is one of the isomers of LAS, and has a structure in which a benzenesulfonic acid group is bonded to the second carbon atom of the alkyl chain of LAS. The structural formula below is an example of 2-LAS.

The present inventors have found that the ratio of isomers differs depending on the production method of LAS, and that the higher the ratio of 2-LAS, the higher the viscosity of the prepared slurry.

In the production method of the present invention, even when the proportion of 2-LAS in component (a) is high, specifically when the amount of 2-LAS in component (a) is 20% by mass or more, This method can suppress the increase in viscosity.
Therefore, in the production method of the present invention, the amount of 2-LAS in component (a) is preferably 25% by mass or more, more preferably 30% by mass, from the viewpoint of using the LAS produced using the DETAL method as it is. On the other hand, from the same viewpoint, it is preferably 50% by mass or less, more preferably 40% by mass or less.

The alkyl chains in LAS of component (a) are linear or branched and have an average carbon chain length of 10 or more and 15 or less. The average carbon chain length is preferably 12 or more from the viewpoint of detergency, and preferably 14 or less from the viewpoint of detergency.

The amount of component (a) in the slurry in step 1 is preferably 8% by mass or more, more preferably 10% by mass or more, still more preferably 12% by mass or more, still more preferably 14% by mass, from the viewpoint of detergency. That's it. On the other hand, from the viewpoint of drying properties during spray drying, the amount of component (a) in the slurry is preferably 50% by mass or less, more preferably 40% by mass or less, even more preferably 30% by mass or less, and even more preferably It is 25% by mass or less, more preferably 23% by mass or less.

component (b)
Component (b) is an inorganic salt and includes at least a potassium salt. Further containing the component (b) in the slurry in step 1 of the production method of the present invention is preferable because the effect of ensuring the particle strength of the spray-dried particles can be expected. By using a monovalent cation having a larger ionic radius than sodium ion, such as potassium ion, as the cation in the inorganic salt, the slurry viscosity can be unexpectedly reduced. Potassium salts include potassium carbonate, potassium sulfate, potassium silicate and the like. The ratio of the potassium salt in the component (b) is preferably 3% by mass or more, more preferably 4.5% by mass or more, still more preferably 30% by mass or more, and 100% by mass, from the viewpoint of suppressing an increase in viscosity of the slurry. is more preferred.

As the inorganic salt other than the potassium salt, which constitutes the component (b), any one known in the field of detergent compositions can be used without limitation. silicates; alkali metal salts having sulfate radicals and sulfite radicals;
More specific examples include sodium carbonate, sodium hydrogencarbonate, sodium silicate, sodium sulfate, sodium chloride, sodium sulfite and the like. These may be blended singly or in combination of two or more.

The amount of component (b) blended in the slurry is preferably 10% by mass or more, more preferably 15% by mass or more, and still more preferably 20% by mass or more of the entire slurry from the viewpoint of cleaning effect. From the viewpoint of suppressing separation and sedimentation of the slurry, it is preferably 50% by mass or less, more preferably 45% by mass or less, and still more preferably 40% by mass or less of the entire slurry.

When a sodium salt is further added as component (b), the molar ratio of [potassium]/[sodium] in component (b) is preferably 0.01 or more, more preferably 0.01 or more, from the viewpoint of reducing the viscosity of the slurry. It is 0.03 or more, more preferably 0.1 or more, and on the other hand, from the viewpoint of suppressing separation and sedimentation of the slurry during production, it is preferably 10 or less, more preferably 8 or less, still more preferably 6.5 or less, and still more preferably 6.5 or less. It is preferably less than 0.3, more preferably 0.25 or less, still more preferably 0.2 or less.

Component (c)
Component (c) is water. Water plays the role of a medium during slurry preparation.
The amount of water in the slurry in step 1 is preferably 20% by mass or more, more preferably 30% by mass or more, and still more preferably 40% by mass or more from the viewpoint of slurry handling. On the other hand, from the viewpoint of fuel cost during spray drying, the amount of water in the slurry is preferably 43% by mass or less, more preferably 42% by mass or less, and even more preferably 40% by mass or less.

Component (d)
Component (d) is a cationic surfactant. It is preferable that the slurry in step 1 of the production method of the present invention further contains the component (d), since effects such as sterilization and antibacterial properties during washing can be expected.
As the cationic surfactant, any one known in the field of detergent compositions can be used without limitation. Cationic surfactants that can be preferably used in the production method of the present invention include, for example, dodecyltrimethylammonium chloride, tetradecyltrimethylammonium chloride, hexadecyltrimethylammonium chloride, dodecylbenzyldimethylammonium chloride, tetradecylbenzyldimethylammonium chloride, didecyldimethylammonium ethylsulfate, and dioctyldimethylammonium ethylsulfate. Among these, hexadecyltrimethylammonium chloride is preferred.

The content of the cationic surfactant in the slurry in step 1 is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, and still more preferably 1.5% by mass or more, from the viewpoint of exhibiting the desired effect. It is 0% by mass or more. On the other hand, from the viewpoint of detergency, the amount of cationic surfactant in the slurry is preferably 10% by mass or less, more preferably 5% by mass or less, and even more preferably 3% by mass or less.

component (e)
Component (e) is a water-soluble polymer. Further containing the component (e) in the slurry in step 1 of the production method of the present invention is preferable because the effect of improving the particle strength of the detergent particles prepared in step 2 can be expected.
As the water-soluble polymer, any one known in the field of detergent compositions can be used without limitation. silicates, carboxymethylcellulose, polyethylene glycol. These may be blended singly or in combination of two or more. Preferably, it is one or more components selected from the group consisting of carboxymethylcellulose, polyethylene glycol and polyacrylic acid.

The amount of component (e) in the slurry in step 1 is preferably 0.1% by mass or more, more preferably 0.2% by mass or more, and still more preferably 0.2% by mass or more, from the viewpoint of exhibiting the desired effect. It is 3% by mass or more. On the other hand, the amount of component (e) in the slurry is preferably 10% by mass or less, more preferably 7% by mass or less, and even more preferably 5% by mass or less, from the viewpoint of suppressing separation and sedimentation of the slurry during production.

Other ingredients that may be blended into the slurry The slurry may contain other ingredients that may be blended in the laundry detergent, such as sodium polyoxyethylene alkyl ether sulfate, alpha sulfo fatty acid ester salt, fatty acid methyl ester ethoxylate, polyoxyethylene Alkyl ether; chelating agent may be further blended. Only one type of such component may be blended, or two or more types may be blended. The total amount of these components to be added to the slurry is preferably 0.1 parts by mass or more, more preferably 0.5 parts by mass or more, and preferably 5 parts by mass with respect to the total slurry amount of 100 parts by mass. Below, more preferably 3 parts by mass or less.

Slurry Preparation Method A slurry can be prepared by mixing the above components.
Although the mixing conditions are not particularly limited, for example, the temperature of the slurry is preferably 30° C. or higher from the viewpoint of uniformly stirring each component, and the temperature of the slurry is preferably 80° C. from the viewpoint of suppressing thermal decomposition of each component. Below.

Viscosity of Slurry The production method of the present invention can reduce the viscosity of the prepared slurry.
The specific viscosity of the slurry is not particularly limited, but from the viewpoint of handling, the viscosity at 60° C. is preferably 2700 mPa·s or less, more preferably 2000 mPa·s or less, and still more preferably 1500 mPa·s or less. On the other hand, from the viewpoint of suppressing separation and sedimentation of the slurry during production, the viscosity of the slurry at 60° C. is preferably 500 mPa·s or more, more preferably 800 mPa·s or more, and still more preferably 1000 mPa·s or more.
The viscosity of the slurry is obtained by measuring by the method described in Examples below.

2. Step 2: Step of preparing detergent particles There are various methods for producing a detergent composition using the slurry prepared in Step 1, and the slurry is spray-dried to prepare detergent particles. A method with steps is preferred. Therefore, the production method of the present invention preferably further includes step 2 below.
Step 2: A step of spray-drying the slurry obtained in Step 1 to prepare detergent particles.

Spray-drying conditions The conditions for spray-drying are not particularly limited as long as they do not substantially affect each component blended in the slurry, and the conditions for commonly used spray-drying can be adopted. can.

The spray-drying temperature is preferably 150° C. or higher, more preferably 160° C. or higher from the viewpoint of improving drying efficiency, and preferably 300° C. or lower from the viewpoint of suppressing decomposition.

A commonly known spray-drying tower can be used as a device for spray-drying, and the exhaust air temperature of the spray-drying tower is preferably adjusted to 80 to 130°C.

Physical Properties of Detergent Particles Physical properties of the detergent particles prepared in step 2 are described below.
The fluidity of the detergent particles is evaluated as the fluidity time measured by the method described in Examples below. The shorter the fluidization time, the higher the fluidity of the cleaning agent particles.

The bulk density of the detergent particles is preferably 200 g/L or more, more preferably 350 g/L or more, and preferably 1,200 g/L or less, more preferably 1,000 g/L or less. Bulk density is measured by the method specified by JIS K 3362.

The average particle size of the detergent particles is preferably 150 µm or more, more preferably 200 µm or more, and preferably 600 µm or less, more preferably 500 µm or less, from the viewpoint of handling and appearance. For the average particle size, a JIS K 8801 standard sieve (opening 2000 to 125 μm) is vibrated for 5 minutes, and then the median size is calculated from the weight fraction according to the sieve mesh size.

Surface Modification A step of adding a surface modifier to the detergent particles to modify the surface of the detergent particles (surface reforming step) may be performed.
Examples of surface modifiers include one or more selected from the group consisting of zeolites, tripolyphosphates and clay minerals.

Clay minerals include talc, pyrophyllite, smectite (saponite, hectorite, sauconite, stevensite, montmorillonite, beidellite, nontronite, etc.), vermiculite, mica (phlogopite, biotite, cinwald mica, muscovite, paragonite). , celadonite, glauconite, etc.), chlorite (clinochlore, chamosite, nimite, pennantite, pseudoite, donbasite, etc.), brittle mica (clintonite, margarite, etc.), thulite, serpentine minerals (antigorite, lizardite, etc.) , chrysotile, amesite, cronstedite, vercellin, greenalite, garnierite, etc.), kaolin minerals (kaolinite, dickite, nacrite, halloysite, etc.). These can be used singly or in combination of two or more.

The average particle size of the surface modifier is desirably 1/10 or less of the average particle size of the detergent particles from the viewpoint of coverage. If the average particle size is within this range, a sufficient effect of improving caking resistance can be expected while avoiding a decrease in solubility. The average particle size of the surface modifier can be measured using, for example, a laser diffraction/scattering particle size distribution analyzer with a dry measurement unit. Specifically, it can be measured by connecting a dry measurement unit "G0310630" to "Partica LA-950" manufactured by Horiba, Ltd. using the Mie scattering method.

The amount of the surface modifier is preferably 2 parts by mass or more, more preferably 2.5 parts by mass or more with respect to 100 parts by mass of the detergent particles, from the viewpoint of fluidity. The preferred upper limit is 20 parts by mass or less, more preferably 15 parts by mass or less, relative to 100 parts by mass of the detergent particles.

There are no particular restrictions on the conditions of the surface modification method, and conditions that allow the surface modifier to be distributed as evenly as possible on the surfaces of the detergent particles are preferred. As the surface-modifying device, a Loedige mixer or a high-speed mixer, which can give a strong stirring force and a cutting force at the same time and uniformly modify the surface, is preferably used.

3. Cleaning composition In the production method of the present invention, the cleaning agent particles themselves obtained by drying the slurry prepared in step 1 by a known method (preferably the cleaning agent particles themselves prepared in step 2, or more Preferably, the detergent particles themselves which have undergone a surface-modifying treatment can be used as the detergent composition. Alternatively, a composition obtained by mixing such detergent particles with known components for laundry detergent (e.g., crystalline aluminosilicate, enzyme, sodium percarbonate, alkaline agent) is used as the detergent composition in the production method of the present invention. It can be used as an object.
Such detergent compositions can be used, for example, as laundry detergents.

The molar ratio of potassium/sodium in the detergent composition is 0.01 or more, preferably 0.03 or more, more preferably 0.1 or more from the viewpoint of reducing the viscosity of the slurry. From the viewpoint of suppressing separation and sedimentation of the slurry, it is 5 or less, more preferably 2.5 or less, still more preferably 0.25 or less, and still more preferably 0.2 or less.
Potassium and sodium in the detergent composition include not only those derived from component (b) but also those derived from components other than component (b). For example, sodium derived from component (a) is also treated as sodium in the detergent composition.

The production method of the present invention will be specifically described below with reference to examples. It should be noted that this example is merely an illustration of the present invention and does not imply any limitation. Parts in the examples are parts by weight unless otherwise specified. In addition, "ordinary pressure" indicates 101.3 kPa, and "ordinary temperature" indicates 25°C.

Example 1
Step 1: Preparation of slurry 35.785 L of water was put into a mixing tank and heated. 12 kg, sodium silicate 3.28 kg, sodium sulfate 29.54 kg, potassium sulfate 1.48 kg, carboxymethyl cellulose (CMC) 0.34 kg, polyethylene glycol 0.47 kg, 40% sodium polyacrylate aqueous solution 7.025 kg, Stirred for 20 minutes. The slurry thus prepared had a viscosity of 2520 mPa·s at 60°C.

Step 2: Spray-drying of slurry The slurry prepared above was spray-dried as follows to prepare detergent particles.
That is, the slurry was supplied to a spray-drying tower (countercurrent type) by a pump, and sprayed at a spray pressure of 2.5 MPa from a pressure spray nozzle installed near the top of the tower. A hot gas supplied to the spray drying tower was supplied at a temperature of 230°C from the bottom of the tower and discharged from the top of the tower at a temperature of 120°C to obtain cleaning agent particles.

Examples 2-5, Comparative Examples 1-3 and Reference Example 1
In the same manner as in Example 1, each component was blended so as to have the mass ratio shown in Table 1 to prepare each slurry. The viscosity of each slurry was also measured in the same manner as in Example 1.
In Reference Example 1, LAS containing 16% by mass of 2-LAS in component (a) was used. This LAS corresponds to LAS produced by a hydrogen fluoride-catalyzed process.
The resulting slurry was spray-dried in the same manner as in step 2 of Example 1 to obtain detergent particles.

The details of the main components in Examples etc. are as follows.
Carboxymethyl cellulose (CMC): manufactured by Nippon Paper Industries; trade name: B2B
Polyethylene glycol (PEG): manufactured by Kao Corporation (mass average molecular weight of 1300)
Sodium polyacrylate: manufactured by Kao Corporation; having a mass average molecular weight of 10,000 Quaternary ammonium chloride: hexadecyltrimethylammonium chloride

With regard to LAS, sodium dodecylbenzenesulfonate manufactured by Kao Corporation, by appropriately changing the production conditions, 2-LAS of 30% by mass, 26.5% by mass, 23% by mass, and 16% by mass was prepared. The amount of 2-LAS in LAS was obtained by separating dodecylbenzene (LAB), which is the raw material of each LAS before sulfonation, by gas chromatography and calculating the ratio from the peak area.

Viscosity of Slurry Viscosity of Slurry 3, It was obtained by measuring under the conditions of 60 r/min and 60°C.

Fluidity of Detergent Particles Fluidity of detergent particles was evaluated as fluidization time.
The flow time was the time required for 100 mL of powder to flow out from the hopper for bulk density measurement defined by JIS K 3362.
Fluidity was evaluated according to the following criteria.
Good: The time required for outflow was 6 seconds or less.
Δ: The time required for outflow exceeded 6 seconds and was 10 seconds or less.
x: The time required for outflow exceeded 10 seconds.

*: Proportion of 2-LAS in LAS.
**: Values are molar ratios.
Table 1 shows the blending amount of each component and the evaluation results. The amount of each component in Table 1 is mass %. In addition, since the compounding amount of each component was rounded off, the total of each component may not be 100% by mass.

From Table 1, it was found that in Examples, the viscosity of the slurry was suppressed and the flowability of the obtained detergent particles was good.
On the other hand, it was found that in the comparative examples in which the detergent composition did not contain a predetermined amount of potassium, the viscosity of the slurry was high and the fluidity of the resulting detergent particles was poor.
From Reference Example 1, it was confirmed that the viscosity of the slurry containing the alkylbenzenesulfonate produced by the conventional method using hydrogen fluoride as a catalyst was low. This means that even those skilled in the art will not be able to perceive an increase in slurry viscosity when using conventionally produced alkylbenzene sulfonates.

The detergent composition obtained by the production method of the present invention can be suitably used as a laundry detergent.

Claims (10)

A method for producing a cleaning composition comprising the following step 1.
Step 1: A step of preparing a slurry containing the following components (a) to (c).
Component (a): Linear or branched sodium alkylbenzenesulfonate (LAS) having an average carbon chain length of 10 or more and 15 or less (where component (a) contains 2-LAS and 2- The amount of LAS is 20% by mass or more.)
Component (b): Inorganic salt (However, Component (b) contains potassium salt.)
Component (c): water (provided that the [potassium]/[sodium] molar ratio in the detergent composition is 0.01 or more and 5 or less.) The manufacturing method according to claim 1, further comprising step 2 below.
Step 2: A step of spray-drying the slurry obtained in Step 1 to prepare detergent particles. 3. The production method according to claim 1 or 2, wherein component (b) further contains a sodium salt, and the [potassium]/[sodium] molar ratio in said component (b) is 0.01 or more and 10 or less. 4. The production method according to any one of claims 1 to 3, wherein the slurry in step 1 contains 8% by mass or more and 50% by mass or less of component (a). 5. The production method according to any one of claims 1 to 4, wherein the slurry in step 1 contains 10% by mass or more and 50% by mass or less of component (b). The production method according to any one of claims 1 to 5, wherein the slurry in step 1 contains 20% by mass or more and 43% by mass or less of component (c). The production method according to any one of claims 1 to 6, wherein the slurry in step 1 further contains 0.1% by mass or more and 10% by mass or less of the following component (d).
Component (d): cationic surfactant The production method according to any one of claims 1 to 7, wherein the slurry in step 1 further contains 0.1% by mass or more and 10% by mass or less of the following component (e).
Component (e): water-soluble polymer The production method according to any one of claims 1 to 8, wherein the slurry obtained in step 1 has a viscosity at 60°C of 2700 mPa·s or less. Use of the detergent composition obtained by the production method according to any one of claims 1 to 9 as a laundry detergent.