JPS63150392A - Production of bulky detergent composition - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for industrially mass-producing a high bulk density detergent composition with excellent solubility at a high yield.

Currently, spray-dried products are the mainstream of laundry detergents on the market. This detergent is made into bead-like hollow particles with an average particle diameter of about 200 to 800 μm by a spray drying method, and has a low bulk density of about 0.3 g/cc. However, spray-dried detergents are expensive to transport, require a considerable amount of space for storage and display, and are difficult to store and weigh even in general households.

In response, a composition and manufacturing method of a high bulk density granular detergent that eliminates the drawbacks of conventional spray-dried detergents and can be concentrated to enable cleaning with a smaller amount of detergent has been proposed (Japanese Patent Application Laid-Open No. 1983-1989-1). No. 72998, No. 60-72999, No. 60-96698, No. 61-69899, No. 61-76597)a JP-A-61-698
No. 99 proposes that a spray shaft product is compacted and then crushed and granulated in the presence of a surface modifier to produce a high bulk density granular detergent.

However, the granular detergent obtained by this method has problems in that it has poor solubility in cold water, and that the product generates dust during production and is extremely poor in commercial value.

Further, Japanese Patent Application Laid-Open No. 51-67302 proposes post-treating the spray-dried product with a marumerizer to increase the bulk density. However, this detergent composition has poor solubility and low surfactant content (25% or less).
There are few benefits for consumers. On the other hand, when the content of surfactant is increased, fluidity is poor and adhesion to equipment occurs, which is not preferable as an industrial manufacturing method.

INDUSTRIAL APPLICABILITY The present invention provides a method for industrially producing a high bulk density detergent with improved solubility and excellent appearance and powder properties at a high yield.

Example 1 The method for producing a high bulk density detergent composition of the present invention comprises a detergent raw material composition containing 30 to 45% by weight of an anionic surfactant and 45 to 65% by weight of a detergent pilder consisting of zeolite and carbonate. The dried product obtained by spray drying the slurry and a nonionic surfactant were mixed under strong shearing force in an anionic surfactant/nonionic surfactant ratio of 20/1 to 3/1 (weight ratio). Mix and knead uniformly, then use a cutter mill type crusher with a screen classification function to crush the mixture in multiple stages by sequentially feeding it from a crusher with a large screen hole diameter to a crusher with a small screen hole diameter. It is characterized by

The present invention will be explained in more detail below.

In the present invention, first, 30 to 45% by weight of an anionic surfactant is used.
, preferably 35 to 40% by weight, and 45 to 65% by weight, preferably 50 to 60% by weight of a detergent pilder consisting of zeolite and carbonate.

If the amount of anionic surfactant is less than 30% by weight, the amount of active agent will be small and the detergent will lose its advantage as a concentrated type high bulk density detergent, and if it exceeds 45% by weight, it will be difficult to manufacture.

As the anionic surfactant, for example, α-olefin sulfonate, linear alkylbenzene sulfonate, polyoxyethylene alkyl ether sulfate, soap, etc. are preferably used, and the salts include sodium salt, potassium salt, etc. .

In addition to anionic surfactants, zeolites, and carbonates, bicarbonates, fluorescent agents, and pigments are optional ingredients.

Sulfates, sulfites, etc. can be used.

Silicates cause deterioration of solubility over time, so it is desirable not to use them or to limit their usage.

Spray drying can be carried out by a conventional method, and is carried out by drying a detergent slurry containing 50 to 100 parts by weight of water based on 100 parts by weight of the above detergent components in a countercurrent type spray drying tower. It will be done. When preparing a slurry, it is desirable to neutralize the linear alkylbenzenesulfonic acid salt directly in a blending tank using NaOH or KOH.

The moisture content of the resulting spray-dried product is preferably 10 parts by weight or less based on 100 parts by weight of the detergent component, from the viewpoint of powder physical properties in consideration of handling in subsequent steps.

Then, the spray-dried product and the nonionic surfactant are uniformly mixed and kneaded to form a kneaded product.

As the nonionic surfactant, a primary one is preferably used.

(1): An EO-added nonionic surfactant prepared by adding an average of 8 to 30 moles of ethylene oxide (EO) to a primary or secondary alcohol having an average carbon number of 8 to 18.

(2): An EO-PO addition type nonionic surfactant in which an average of 8 to 20 moles of EO and an average of 3 to 15 moles of propylene oxide (PO) are added to a primary or secondary alcohol with an average carbon number of 8 to 18.

The EO-added nonionic surfactant has a poor solubility improvement effect when the number of moles of EO added is less than 8;
If the amount exceeds the molar amount, kneading becomes difficult, which is not preferable in terms of production. The same applies to the EO-PO addition type nonionic surfactant, and if the number of moles of EO or PO added is too small, manufacturing problems will occur.

The preferable number of EO addition moles of the EO addition type nonionic surfactant is 10 to 20, and the preferable addition number of EO addition moles of the EO-PO addition type nonionic surfactant is EO=8 to 15 and PO=5 to 15.

Furthermore, (b) nonionic surfactant is (a)/(b) with respect to (a) anionic surfactant in the spray-dried product.
= 20/1-3/1, preferably 1O11-4/
It is necessary to mix them in a ratio of 1:1. This value is 207
If it is less than 1, the effect of improving solubility is poor.

On the other hand, if it exceeds 3/1, the foaming power decreases, which is not preferable, and also makes production difficult.

In order to fully exhibit the solubility improvement effect of the nonionic surfactant, it is necessary to microscopically uniformly mix it with the anionic surfactant in the spray-dried product. Therefore, the spray-dried product and the nonionic surfactant are uniformly mixed and kneaded under strong shearing force. This mixing and kneading can be performed using a kneader, and a continuous kneader is preferred. In particular, in the subsequent crushing process, in order to reduce the load on the crusher, it is preferable to supply the kneaded material in the form of pellets. Preferably 5, for example, from Kurimoto Iron Works, K
It is commercially available as an RC kneader.

Although a normal extruder applies pressure, it is insufficient in terms of uniform mixing, and a sufficient solubility improvement effect cannot be obtained.

Moreover, in this mixing-kneading step, the above-mentioned optional components can also be added in addition to the spray-dried product and the nonionic surfactant. In addition, since nonionic surfactants have poor thermal stability, it is inappropriate to mix them into a detergent slurry and spray dry them, and it is preferable to add them during the kneading process.

The obtained kneaded material is crushed in multiple stages using a cutter mill type crusher having screen classification capability, and sequentially supplied from a crusher with a large screen hole diameter to a crusher with a small screen hole diameter.

By sequentially feeding from a cutter mill type crusher with a large screen hole diameter to one with a small hole diameter and crushing in multiple stages until granules with the desired particle size are obtained, the average particle size ratio before and after entering the crusher becomes smaller. , the amount of fine powder is reduced and the yield is improved without being subjected to excessive crushing.

In addition, due to the combination of not being subjected to excessive crushing and the fact that it receives a lot of centroid effect (grading) in the crushing chamber, it has a sharp particle size distribution and an improved shape with almost no flat particles or acicular particles. This is an industrially effective method for granulating high bulk density detergents that produce crushed granules and have high commercial value.

Furthermore, the crushing capacity can be improved compared to the case where the same number of crushers used in multi-stage crushing and granulation are arranged in parallel as in the single-stage crushing method of the prior art. In this case, in each stage of the crusher, by setting the average particle size ratio at the entrance and exit of the crusher to an appropriate value and allocating the required degree of crushing (reduction in particle size) to each stage, the crushing capacity can be improved. can be improved even more effectively.

The kneaded material is crushed before being crushed using a cutter mill.

It is appropriate to form pellets by the above-mentioned continuous kneader, extrusion molding, or the like. The diameter of the pellet is suitably 2 to 10 mm, preferably 4 to 7 mm. If the pellet diameter becomes too small, problems such as deformation of the die attached to the extruder may occur due to an increase in extrusion pressure. On the other hand, if the pellet diameter is too large, the load on the crusher will increase. In addition, the length of the pellet is 5 to 30 mm, taking into consideration the adhesion to the pellet cutting knife and the load on the crusher.
m is suitable, preferably 5 to 15 mm.

The pellets are crushed in multiple stages using a cutter mill type crusher equipped with a classification screen, and then crushed and granulated.

The average particle size of the final crushed granules is preferably 300 to 1500 μm, preferably 500 to too μm. If the particle size is large, the solubility during washing will be slow, causing problems such as adhesion to fabrics and reduced detergency, while if the particle size is small, on the other hand, the amount of dust generated will increase due to an increase in fine powder, and the crushing yield will decrease.

A cutter mill type crusher has multi-stage rotating crushing blades and discharges crushed materials through a 360° release screen, and is commercially available as, for example, New Speed Mill (Maguchi Seiko ■). An arbitrary upper limit particle size can be set by adjusting the opening diameter of the screen.

The screen is not particularly limited, such as a wire mesh type, a herringbone type, a punched metal type, etc., but a punched metal type is preferable in consideration of the screen strength and the shape of the crushed material.

Since the crushers are connected in series, it is preferable that the crushing capacity in multi-stage crushing of high bulk density detergent be large and common to each stage. In order to achieve this, it has been found that there is an optimal value for the ratio of average particle diameters at the crusher inlet and outlet, which can be obtained by selecting the screen hole diameter.

dPz: Average particle diameter of particles discharged from the crusher Once the average particle diameter at the start of the crushing process and the average particle diameter of the desired crushed granule are set, the number of crushing stages is automatically determined according to these. At that time, if the relationship between the screen hole diameter and the average particle diameter of the crushed material obtained is determined in advance by experiment,
Even more effective.

Furthermore, as can be seen from the above relationship, when the particle size is large, the surface area of the powder is small and the load on the crusher is small, so the ratio of the average particle size at the inlet to the outlet can be widened. Therefore, in multi-stage crushing, it is desirable to reduce the crushed particle size as much as possible in the upper-stage crusher.

When performing multi-stage crushing, it is possible to install a sieve at the discharge port of the crusher in each stage and supply only the crushed material of the desired particle size to the next stage crusher, but this can lead to clogging of the sieve, complication of the system, and installation. This is disadvantageous in terms of increased area. Therefore, a direct-coupled type is preferable, in which the discharged material (crushed material) from the first-stage crusher is directly supplied to the second-stage (and sequentially from the third stage onwards) crushers.

During crushing, it is preferable to add a crushing aid.

Grinding aids are generally known as grinding aids, and when added in small amounts into a grinder, they have effects such as reducing grinding power, improving grinding particle size, and improving properties of ground products.

The particle size of the crushing aid is suitably 50 μm or less, preferably 20 μm or less. Moreover, the addition amount is preferably 0.5 to 10% by weight based on the crushed amount.

Types of crushing aids include stearate, aluminosilicate such as A-type zeolite, calcium carbonate, magnesium carbonate, and magnesium silicate.

Silicon dioxide, titanium dioxide, finely divided sodium carbonate, and sodium sulfate are preferred. These crushing aids adhere to the surface of the crushed material and reduce the surface activity of the crushed material, thereby preventing adhesion to the crusher, thereby reducing the crushing power, and improving the fluidity of the crushed material. It will be done.

Methods for adding the auxiliary agent include a method in which it is mixed in advance before crushing, a method in which the entire required amount is added at once in the first stage of multi-stage crushing, and a method in which it is added in portions for each stage. The selection is arbitrary, but it is preferable to add them all at once from the viewpoint of the auxiliary effect and economical efficiency. Furthermore, by directly connecting the crushers to each other and creating a system in which the spaces between each stage are sealed (closed direct connection type), the loss of the auxiliary agent is reduced, and the amount of the auxiliary agent added can be effectively applied.

In order to prevent crushed materials from softening due to crushing heat and sticking to the crusher, it is desirable to introduce cold air into the crusher. The temperature of the cold air is suitably 10 to 25°C, preferably 15 to 20°C. In addition, the amount of cold air is 0.1~5m'
/)cg (crushed material) is suitable. If the amount of cold air is too large, the temperature of the crushed material will drop significantly and the crushed material will become hard and brittle, resulting in over-pulverization, resulting in an increase in fine particles and deterioration in shape.

The method of introducing the cold air may be either by introducing the required amount into the first stage all at once or by dividing it into each stage. Furthermore, it is economical to recycle the cold air discharged from the crusher after separating it from the powder.

The resulting crushed granulated particles may be coated with a water-insoluble powder to further modify the powder properties.

According to the present invention, the solubility in cold water is good and! This method is suitable as an industrial production method because it allows mass production of high bulk density granular detergents with a two-product shape close to a sphere and excellent powder physical properties and appearance at a high yield.

Example The following composition was adjusted to have a slurry moisture content of 45%, and then dried to a moisture content of 5% using a countercurrent spray drying tower. The temperature of the hot air used was 380°C.

The obtained spray-dried product had an average particle size of 350 μm and a bulk density of 0.
．． The fluidity was also good at 35 g/cc and an angle of repose of 45°.

Next, the above spray-dried product, sodium bicarbonate, a nonionic surfactant to which a blue dye was added (15 moles of ethylene oxide added to a primary alcohol with 12 to 13 carbon atoms), and water were mixed in a continuous kneader ( Kurimoto Iron Works, KRC Kneader Model I2) was used to obtain a dense and uniform kneaded product.

A perforated plate (thickness: 10 re) with 80 holes of 5 nnφ was installed at the outlet of the kneader, and the kneaded material was approximately 5 aa thick.
It was made into a cylindrical pellet with a diameter of 10 mm. The pellets had a uniform blue color, indicating that the nonionic surfactant and the spray-dried product, that is, the anionic surfactant, were uniformly mixed.

Cold water at 5° C. was flowed through the jacket of the kneader to remove heat of kneading and the like. The temperature of the obtained pellets was 50°C.

The obtained pellets were introduced into a crusher (Speed Mill ND-10 model, Maguchi Seiko ■) together with twice the amount (weight ratio) of 15° C. cooling air. At this time, 4 parts by weight of zeolite (moisture 15%) with an average particle size of 1 μm (minus particle size) was added as a grinding aid per 100 parts by weight of the pellets.

The crusher is 15C long! It has 11 cutters in 4 stages, rotates at 3000 rpm, and has 3 screens.
Made of 60° punched metal. Three stages of these crushers are connected in succession, and the discharged material (crushed material) from the first stage crusher is supplied to the second stage crusher, and then similarly to the third stage crusher. Step) Crushed. The hole diameter of the punching metal is 1st stage: 3.5+pφ, 2nd stage: 2Iφ, 3
Row: 1.5nynφ.

The particles that passed through the three stages of the crusher were separated from the cooling air to form a product (high bulk density detergent).

The detergent composition, manufacturability, and product properties are shown in Table 1.

Comparative Example 1 The same procedure as in Example 1 was carried out except that the continuous kneader was changed to an extruder (manufactured by Fuji Paudal; Pelleter Double EXD-60 type). The color of the extruded granules was non-uniform, and adhesion occurred on the second and subsequent stages of the crusher, causing the crusher to stop after 10 minutes. Table 1 shows the properties of the small amount of sample collected.

Example 2 In Example 1, the crusher was operated at the upper limit as shown in Table 1 below.

Example 3 In Example 1, the crusher was made into two stages, the first stage had a screen hole diameter of 2.5 rrnφ, the second stage had a screen hole diameter of 1.5 mmφ, and the crusher was operated at the upper limit of its capacity.

Example 4 In Example 1, the nonionic surfactant was
Average of 9 moles of EO in secondary alcohol, p.

was added to an average of 5 moles, and anion/
By changing the nonionic surfactant ratio as shown in Table 1,
A high bulk density detergent was produced in the same manner as in Example 2.

Comparative Example 2 In Example 1, as a crusher, the screen hole diameter was 1.
A specimen of 5 mm diameter was used, and the operation was performed by crushing at the upper limit of capacity.

Example 5 In Example 1, sodium carbonate having an average particle size of about 30 μI was used as the grinding aid, and operation was performed at the upper limit of capacity.

The above results are shown in Table-1.

In addition, the product shape of the single granular detergent in Examples 1 to 4 is almost spherical with no corners, whereas in Comparative Example 2, there are many flat or forest-like particles and the particle size distribution is broad. Ta.

In addition, solubility was evaluated as follows.

Water 12 at 25° C. is placed in a beaker, and a cell for measuring conductivity is inserted into the water. Then, 0.83 g of each high bulk density detergent composition was added to the water and washed at 250 g using a low speed Starsea.
The time required for 90% of the added detergent particles to dissolve was measured from the change in conductivity by stirring at a speed of 100 rpm.
UCTIVE METERDS-8F type was used.

(Left below) Procedural amendment 1. Description of the case 19861 Patent Application No. 298455 2 Name of the invention Method for producing a high bulk density detergent composition 3 Person making the amendment Relationship to the case Patent applicant 1-3-7 Honjo, Sumida-ku, Tokyo (676) Lion Co., Ltd. Representative Atsushi Kobayashi 4, Agent 6 Contents of amendment (1) On page 2, line 6 of the specification, the statement "Town...Togireiteiori, Takataka Mitsu" has been changed to r... ...and the bulk density is corrected to J.

that's all

Claims (1)

[Claims] 1. A dry product obtained by spray-drying a slurry of a detergent raw material composition containing 30 to 45% by weight of an anionic surfactant and 45 to 65% by weight of a detergent pilder made of zeolite and carbonate, and a nonionic surfactant. are uniformly mixed and kneaded under strong shearing force in an anionic surfactant/nonionic surfactant ratio of 20/1 to 3/1 (weight ratio), and then the kneaded product is screened. 1. A method for producing a high bulk density detergent composition, which comprises using a cutter mill-type crusher having a classification function, and carrying out multi-stage crushing by sequentially feeding from a crusher with a large scoop hole diameter to a crusher with a small scoop hole diameter.