JPH0959697A - Production of high-bulk-density detergent composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain granules which are energy- and space-saving, have a degree of freedom of balancing the water content in a single apparatus, and are excellent in flowability by heaving from the outside when an acidic precursor of an anionic surfactant is neutralized with an excess of a solid alkali. SOLUTION: In the neutralization of an acidic precursor of an anionic surfactant with an inorg. alkali powder, granules having an adjusted water content and an excellent flowability can be obtd. since the resulting product can be dried to a suitable water content simultaneously with the neutralization conducted with heat given from the outside. Thus, three steps of neutralization, drying, and granulation (density increase) can be carried out with a single apparatus; the heat of neutralization can be used as a part of energy necessary for evaporating water, contributing to energy saving; the dwell time is short; and the temp. of the product itself does not become high because of the latent heat of evaporation, causing no discoloration. Granules with a bulk density of 0.6g/cc or higher are continuously obtd.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to detergent ingredients and methods of making detergent compositions. In particular, it relates to a method of making a high bulk density detergent composition comprising neutralizing an acidic precursor of an anionic surfactant.

[0002]

2. Description of the Related Art In recent years, a detergent manufacturing method which does not use a spray drying method, which requires a lot of energy and space, has been attracting attention in the detergent industry. The production method involving neutralizing an acidic precursor of an anionic surfactant with a solid alkali inorganic material is one of the most important ones. That is, a method for producing a high-bulk density detergent using an acidic precursor of an anionic surfactant (water content of 1% or less) as a starting material requires a neutralization step, but the surfactant which is the mainstream of the current detergent production method Unlike the manufacturing method using the aqueous slurry (water content of 30 to 70%) as a starting material, a large-scale spray-drying device is not required, so that the facility cost is low and there is an advantage of energy saving. However, in the method using this acidic precursor as a starting material, it is necessary to add water in order to allow the neutralization reaction to proceed sufficiently, and if sufficient water is used, the neutralization product solidifies (the post-process becomes complicated). However, there is a problem that the water content is restricted because the physical properties of the detergent powder (fluidity, storage solidification, etc.) are deteriorated.

A method for producing a granular detergent using an acidic precursor of an anionic surfactant as a starting material is disclosed in JP-A-60-7.
2998, JP-A-60-72999, JP-A-61-166798, and the like, after neutralizing and mixing an unneutralized sulfonate with sodium carbonate and water in a strong shearing device, cooling aging is performed. Further, a method of pulverizing and granulating has been proposed. However, these methods have the drawbacks that a large amount of power is required due to the use of a strong shearing device and that the neutralized product is in the form of lumps, so that a cooling / aging and crushing step must be installed in the next step.

Further, in JP-A-3-146599, an acidic precursor of an anionic surfactant and a solid alkali inorganic material are neutralized with a high speed mixer, treated with a medium speed mixer, and then dried or cooled. Further, in JP-A-3-33199, a solid inorganic alkaline substance fluidized in a high speed mixer / granulator while keeping the temperature at 55 ° C. or lower is added with an anionic surfactant acidic precursor. A method of neutralizing and granulating has been proposed. However, the former method has a drawback in that it requires a plurality of steps and requires a drying or cooling step after granulation, and the latter method requires that the temperature be maintained at 55 ° C or lower. However, it has a drawback that it requires a long neutralization time.

Further, JP-A-4-363398 discloses a batch system in which an anionic acidic precursor is gradually added to a solid alkali inorganic material in a batch mixer, and then granulated in the presence of a liquid binder. JP-A-5-86400
In the single publication, the water content of the product is adjusted to 5 to 15%, and the neutralization of the anionic surfactant acidic precursor and the solid alkali inorganic material is achieved by a high speed mixer / granulator in a single step of 80% or more. Has been proposed. But,
The former method is not suitable for mass production because it is a batch process, and it has the disadvantage of requiring a relatively long neutralization reaction time.The latter method also has a short residence time in the device. For this reason (5 to 30 seconds), the water content of the treated material for promoting the neutralization reaction is strictly limited to 5 to 15%, and liquid components that exceed the range are directly blended too much. I can't do it,
The water content of the neutralized product is determined by the water content brought in from the raw material to be processed, so if the water content of the neutralized product is high, the water content of the product will naturally rise, that is, there is not much freedom in terms of water balance. In addition, depending on the conditions, a complete neutralization reaction may not be achieved.

Further, Japanese Patent Publication No. 7-503750 proposes a method in which an acidic precursor of an anionic surfactant is used in a high shear mixer with an excess of finely divided granular neutralizing agent having an average particle size of less than 5 μm. However, according to the method,
Since the average particle size of the granular neutralizing agent (alkali builder) is set to 5 μm or less, it must be finely pulverized by a pulverizer in advance, which complicates the process and causes dust generation.

[0007]

SUMMARY OF THE INVENTION Accordingly, the present invention provides a flowable, free-flowing water balance in a single device that includes neutralizing anionic surfactants in an energy and space efficient manner. An object of the present invention is to provide a method for producing an excellent detergent composition powder or granule.

Conventionally, in the neutralization reaction between an anionic surfactant acidic precursor and a solid alkali inorganic substance, the reaction rate is largely dependent on the water content of the raw material to be neutralized, and the above reaction is carried out continuously. In this case, the neutralization reaction had to be completed in a short time, and it was necessary to increase the water content of the treated material in order to accelerate the reaction. If the water content of the neutralized product to be treated is high, there is concern about adhesion to equipment, aggregation of the neutralized product, and formation of dough. Further, since the water content of the neutralized product is reflected in the water content of the final product, if the water content of the neutralized product is high, the water content of the final product will naturally be high. Further, from the above, when neutralizing the anionic surfactant acidic precursor and the solid alkali inorganic material, a liquid material that is another detergent component (anionic surfactant aqueous solution or nonionic surfactant aqueous solution, soap,
It was not possible to add a very large amount of the fluorescent agent dispersion, etc.). Furthermore, in order to improve the handling property of the neutralized product and adjust the water content of the neutralized product, it is necessary to perform drying and cooling with another device after the neutralization, that is, a plurality of devices are required. I was there.

[0009]

Means for Solving the Problems For example, when continuously performing a neutralization reaction between an anionic surfactant acidic precursor and a solid alkali inorganic material with a stirring granulator equipped with a high-speed rotating blade, The reaction was carried out without cooling or actively heating. As a result of intensive studies by the present inventors,
The present inventors have found that it is possible to complete the reaction in a short time by applying heat from the outside to accelerate the neutralization reaction, and arrived at the present invention.

That is, according to the present invention, in a method of neutralizing an anionic surfactant acidic precursor by mixing with a solid alkali inorganic material in excess of at least an amount necessary to neutralize the acidic precursor. In addition, it is possible to continuously obtain a powdery material having a bulk density of 0.6 g / cc or more and excellent in fluidity while drying the neutralized product while promoting the reaction by externally applying heat during the neutralization reaction. A method of making a featured high bulk density detergent composition is provided.

In the neutralization reaction between the acidic precursor of the anionic surfactant and the powdered alkaline inorganic material, in the conventional method, even if the neutralized product to be treated has a high water content, it adheres to the equipment or the neutralized product is neutralized. Although there was a concern about the influence on agglomeration and dough formation and moisture of the final product, in the method of the present invention, it is possible to simultaneously dry the moisture of the treated product to an appropriate moisture while performing the neutralization reaction by the heat applied from the outside. Since it becomes possible, a granulated product with controlled water content and excellent fluidity can be obtained.
As a result, in the neutralization of the anionic surfactant acidic precursor and the solid alkali-inorganic material, a liquid material that could not be added in a large amount until now (dispersion of anionic surfactant, nonionic surfactant, soap, and fluorescent agent) (Liquid etc.) can be blended. Further, according to this method, three steps of neutralization, drying and granulation (densification) can be carried out by a single device. Further, the method of the present invention has the following advantages. B) In the drying process of the neutralized product, the heat of neutralization generated by the neutralization reaction is used as it is as a part of the heat required for evaporation of water, which is very rational in terms of energy. B) Since the residence time is relatively short and the product temperature itself does not become too high due to the latent heat of vaporization during drying, there is no fear of deterioration in color tone due to heating. C) The fluidity of the obtained neutralized product is the temperature of the neutralized granulated product discharged by dividing the jacket of the equipment and using the first half for heating and drying and the latter half for cooling the neutralized product. It is further improved by lowering.

[0012]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in more detail. The method for producing a high bulk density detergent composition of the present invention comprises a neutralization reaction and a treated product while externally applying heat in an operation of mixing an anionic surfactant acidic precursor with a solid alkali inorganic material for neutralization treatment. The steps of drying and granulating are carried out by a single device. According to this method, the neutralization reaction is completed in a short time, and the water content of the neutralized treated product can be adjusted as desired, so that powdery granules having excellent fluidity can be continuously obtained. To be

Any solid alkaline inorganic material can be used in the method of the present invention, but preferably
It is an alkali builder that combines sodium carbonate and potassium carbonate, or a combination thereof. Further, as the anionic surfactant acidic precursor, linear alkylbenzene sulfonic acid, α-olefin sulfonic acid, alkyl sulfate, polyoxyethylene alkyl ether sulfuric acid, etc. alone known acidic precursor of the surfactant as a detergent component, or those It is arbitrarily selected from the combination of.

In carrying out the present invention, the amount of water brought in from the raw material introduced is preferably 25% or less and 2% or more, and more preferably 20% or less and 3% or more. If the water content exceeds 25%, the amount of water to be evaporated increases, and the scale of the equipment for the amount of treatment increases, which is not efficient in terms of cost. It becomes difficult to proceed. If the water content of the material to be treated is within the above range, in addition to the anionic surfactant acidic precursor and solid alkali inorganic material, other components generally found in detergents are supplied in arbitrary amounts and in combination. be able to. In this case, examples of other components that can be supplied include an aqueous solution of an anionic surfactant metal salt such as an α-olefin sulfonate metal salt and an α-sulfo fatty acid ester metal salt, a nonionic surfactant, soap, zeolite, and tripolyphosphoric acid. Soda, anti-redeposition agent (carboxymethyl cellulose, etc.), fluorescent agent, extender (sodium sulfate, etc.)
Generally, known materials are used as the detergent component. Any one of these materials or a combination of two or more of them may be directly supplied to the apparatus.

As an apparatus for carrying out the present invention, a horizontal cylindrical type apparatus equipped with a rotating blade for stirring and mixing inside, and having a jacket for a heat medium and an inlet / outlet port for hot air or carrier gas is used. Preference is given to using. For example, solid air (manufactured by Hosokawa Micron), flash reactor (manufactured by Okawara Seisakusho), DT dryer (manufactured by Tsukishima Kikai), CB recycler, reedige mixer (manufactured by Reedige), proshare mixer (manufactured by Pacific Kiko), etc. To be

In carrying out the present invention, preferable conditions in the above apparatus are as follows. The clearance between the rotary blade and the inner wall surface of the apparatus is 8 mm or less, preferably 5 mm or less, and the peripheral speed of the blade tip is 5 m / s.
ec or more, preferably 7 m / sec or more. The heating for promoting the neutralization and drying the neutralized product may be a method by indirect heating in which a heating medium is passed through the jacket, a method by direct heating in which hot air is introduced into the apparatus, or both methods. The temperature of the heated neutralized product is 60 ° C or higher and 150
C. or lower, preferably 70 to 120.degree. C. In the method using indirect heating, the jacket is divided into a heating and drying zone and a cooling zone, and the dried processed material is cooled in a cooling zone near the discharge port. The temperature of the cooled neutralized product is 5
It is 0 ° C or lower, preferably 40 ° C or lower. By this operation, the fluidity of the processed product is further improved. The proportion of the divided heating zones is appropriately 2/3 to 3/4 of the entire heat transfer area. The water vapor generated during drying is entrained outside by the carrier gas (hot air when hot air is used) introduced into the apparatus. The discharged carrier gas is discharged to the atmosphere after collecting some of the entrained fine powder with a dust collector such as a bag filter or a scrubber.

In such a structure, the anionic surfactant acidic precursor and the solid alkali inorganic material supplied to the cylindrical stirring evaporator are forcibly finely dispersed and mixed by a stirring blade in the apparatus and neutralized. It At this time, the temperature is raised by contact with the inner wall surface heated by the heat medium passed through the jacket or by the heat when hot air is introduced, and the neutralization reaction is promoted. Further, when the water content of the neutralized product is high and needs to be dried, the neutralized product is dried by the heat from the heated inner wall surface or the heat from the hot air and the heat of neutralization generated by the neutralization reaction. The water content of the dried neutralized product is 10% or less, preferably 8% or less. When the water content is 10% or more, the neutralized product becomes soft, which may cause adhesion in the device or deteriorate fluidity. The neutralized product is discharged while being densified and granulated to a BD of 0.6 or more by a stirring blade.

The embodiments of the present invention can be summarized as follows. (1) In the method of neutralizing an acidic precursor of an anionic surfactant by mixing an alkaline precursor and inorganic powder material in excess of the amount required to neutralize the acidic precursor, a horizontal cylindrical shape with a jacket is used. In the center of the vessel, equipped with a shaft equipped with a blade for stirring and mixing, using a continuous stirring device having a hot air or carrier gas inlet and outlet,
Moreover, while externally applying heat during the neutralization reaction to accelerate the reaction and dry the neutralized product, it is possible to continuously obtain a granular material having a bulk density of 0.6 g / cc or more and excellent fluidity. A method for producing a high bulk density detergent composition, which is characterized. (2) The method for producing the high bulk density detergent composition, wherein the continuous stirring device has a heating part and a cooling part.

[0019]

The present invention will be described in more detail with reference to the following Examples, which should not be construed as limiting the technical scope of the present invention. In the following examples and comparative examples,
The device used was solid air manufactured by Hosokawa Micron. This device had a horizontal cylindrical container and a jacket, and the center of the container consisted of a variable rotary shaft equipped with a number of paddles whose shape and angle could be varied. The residence time of the processed material in the container can be changed by changing the paddle angle and the rotation speed. The liquid raw material of the example was continuously charged into each apparatus by a metering pump, and the powder raw material was continuously charged into each apparatus by a metering feeder (circle feeder).

Examples 1- (1) to 1- (2) and Comparative Examples 1 to 2 LAS-H (pure content: 96.3%, water content: 0.34%) as an anionic surfactant acidic precursor. OIL minutes: 1.7
%, Sulfuric acid content: 1.6%) and, if necessary, AS-H (pure content:
About 92% was used immediately (within 1 hour) after sulfation by known methods. Since the acid decomposition of this compound starts immediately after sulfation, a number such as OIL content could not be given. The}, as a solid alkaline inorganic material Na ₂ CO
₃ (pure content: 99.9%) as other components, zeolite (pure content: 80%, water content: 10%, other solid content: 10)
%) To produce a high bulk density detergent composition in the above apparatus. Table 1 shows the composition ratio of the raw material mixture, the operating conditions, and the quality of the obtained product. The degree of neutralization was measured as follows. After treating a known amount of the neutralized product, one of the neutralized products is immediately added to an 80% IPA solution in a container connected to a carbon dioxide gas electrode (Toa Denpa Kogyo KK). The container was closed, and the amount of carbon dioxide gas generated by the reaction of the unneutralized acid was measured with a carbon dioxide gas electrode. A calibration curve was taken in advance, and the degree of neutralization was calculated using the calibration curve.

[0021]

[Table 1]

In Comparative Example 1, without heating with the jacket,
LAS-H and AS-H were neutralized with sodium carbonate, but the neutralization reaction was not completed and the angle of repose and the color tone were poor. On the other hand, Example 1 shows the promotion of the neutralization reaction under heating. In Comparative Example 2, cold water was passed through the jacket to lower the temperature of the neutralized product for neutralization, but the angle of repose was not significantly improved, and the neutralization reaction was not completed.

Examples 2 to 4 In the same manner as in Example 1- (1), AOS-K aqueous solution (pure content: 69.1%, water content: 27.9%, free) was used as the other component in the starting material. Alkaline: 2.1%, OIL content 0.93%) and soap (pure content 68.8%, free alkali content: 0.2%, water content: 31%) are added to produce a high bulk density detergent composition. did. Table 2 shows the composition ratio of the raw material mixture, the operating conditions, and the quality of the obtained product.

[0024]

[Table 2]

In Example 2, since the water content of the neutralized product was 8.6%, the angle of repose (flowability) was improved. Further, in the third embodiment, the latter half ⅓ of the jacket is used as the cooling zone and the temperature of the neutralized product is lowered, so that the angle of repose is further improved.

[0026]

INDUSTRIAL APPLICABILITY According to the present invention, in the neutralization of the anionic acidic precursor and the solid alkaline inorganic substance, the neutralization treatment can be completed continuously in a short time, and it is possible to add until now. Simultaneous processing of liquid raw materials is possible. Furthermore, the obtained product has good fluidity and high bulk density, so energy saving without using a drying tower,
It enables space-saving and very simple production of high bulk density granular detergent.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Hitoshi Tanaka 1-3-7, Sumida-ku, Tokyo Inside Lion Corporation (72) Inventor Tomoki Kubo 1-3-7, Sumida-ku, Tokyo Within Lion Corporation

Claims (1)

[Claims] 1. A method for neutralizing an anionic surfactant acidic precursor by mixing with a solid alkali inorganic material in excess of an amount necessary to neutralize the acidic precursor, at the time of the neutralization reaction. A high bulk density characterized by continuously obtaining powdery material having a bulk density of 0.6 g / cc or more and excellent in fluidity while drying the neutralized product while accelerating the reaction by externally applying heat. A method for producing a detergent composition.