JPH03185099A - Bleaching agent particle filled in wax capsule and production thereof - Google Patents

Abstract

PURPOSE: To obtain bleaching agent particles which is stable when used in liquid and a granular detergent and does not cause environmental pollution problems by spraying molten paraffin wax sufficiently on the particles in a fluidized bed.

CONSTITUTION: Bleaching agent particles are suspended in a fluidized bed in which the temperature of the bed of at least 20°C is kept at the melting point or below of wax by passing air. Next, paraffin wax of 40-50°C melting point and of 10-60 mm penetration at 25°C which is heated above its melting temperature is sprayed sufficiently on the particles in the fluidized bed at a rate of 10-40 g/min per 1 kg of the particles to form a coat 100-1,000 μm thick, obtaining the intended particles.

COPYRIGHT: (C)1991,JPO

Description

DETAILED DESCRIPTION OF THE INVENTION INDUSTRIAL APPLICATION The present invention relates to paraffin wax encapsulated bleach particles that remain stable for use in liquid and granular detergents, and a method of encapsulating bleaching agents. Regarding.

Background of the invention Bleach particles have been coated with various materials.

In U.S. Pat. No. 3,908,045 (Allerm** et al.), bleach particles include fatty acids, polyvinyl alcohol,
or coated with polyethylene glycol.

U.S. Patent Nos. 4.078.009 and 4.126.71
No. 7 and No. 4, H6,052 (Ml!!611), bleach particles with 35-89% by weight of fatty acids and t-
It was coated with a mixture of 16% by weight fine quality wax (melting point 51-99°C). Other coating materials include:
Polymer latex, U.S. Pat. No. 4.759.956 (
Am*r etc.); polycarboxylate material, U.S. Pat. No. 4.762.637 (ArHson et al.); melting point 50
~65°C polyethylene wax, European Patent No. 132.
No. 184 (Scolle); and various waxes, U.S. Patent No. 4.421. fi69 (Br1chsrd
). The wax coating in the case of Br1eh*td constitutes O,Ql-10% of the weight of the bleach coated.

One disadvantage of conventionally coated bleach particles is the instability of the bleach in liquid aqueous cleaning compositions: water or other components of the composition that are incompatible with the bleach may mix with the bleach during storage. interact with each other. As a result, almost no bleaching activity remains as a detergent. Attempts have been made to increase the stability of encapsulated bleach particles using secondary coatings. for example,
taught the optional use of a secondary coating of soap in encapsulated bleach. Further, U.S. Pat. No. 4,657,784 (Olson) discloses that
It was taught to double coat the bleach core with an inner coat of paraffin or fine wax having a melting point of 94°C, and a secondary coat of a material having a higher melting point than the inner coat, such as sodium carbonate.

It has also been taught to encapsulate bleaching agents in an inner coating of fatty acids or waxes and an outer coating of water-soluble cellulose ether (European Patent Application No. 307, 58ff (O
lsom)). - The secondary coating is said to improve the stability of the bleach capsule, since cracks or gaps in the secondary coating can allow materials to contact and react with the bleach.

These secondary coatings are expensive to use and, while they add some stability to the bleach, they do not guarantee that the bleach can be used as a cleaning agent after storage.

Bleach has been encapsulated by various methods. U.S. Patent No. 3.847.830 (Willixms
et al.) describe several methods for encapsulating generally unstable peroxygen compounds in water-dispersible coatings, including paraffin waxes. A coating material is "water dispersible" if at least 75% of peroxygen is released within 30 minutes of adding 2 g of ambient peroxygen to lj of water at 15°C.

Three of the methods, such as Will 15m5, require an encapsulating agent that is melted before being sprayed onto the peroxygen particles in the fluidized bed. Two other methods involve dissolving the enveloping agent in an organic solvent and spraying the resulting solution onto the particles or immersing them in a large volume of solution to accomplish the coating.

The disadvantages of these two methods are the high organic solvent content and, more importantly, the associated environmental pollution problems.

U.S. Patent No. 3.856.699 (M i 7 * n
o etc.), the core particles are made into waxy material (wax) under heating.
A method is described for dispersing in a material, cooling the resulting dispersion, and crushing it into a powder. The powdered waxy material is then stirred in an aqueous medium at a temperature above the melting point of the waxy material. The waxed core material is then passed through an unstirred aqueous medium at a temperature below the melting point of the waxy material. Co-pending U.S. Patent Application No. 202,853 (K*me
1) disperses an active substance in a molten wax to form an active substance/wax dispersion;
2' to water containing a surfactant and aperture the active substance/wax dispersion for less than 4 minutes to form capsules therein; then immediately cool the capsules; and remove the cooled capsules from the water. Collect and improve capsule quality.

The bleach particles were also directly sprayed with the coating material in a fluidized bed apparatus, as in the case of Br1chsrd. In US Pat. No. 3,908,1145, a fatty acid coating material was sprayed onto the particles.

Also, in US Pat. No. 3,983,254, the height of the spray nozzle above the fluidized bed was considered to be important. In US Pat. No. 4,078,099, a rotating drum apparatus was used to apply the coating material.

Further, in US Pat. No. 4,759,956, a polymer latex was deposited onto a core material (such as bleach) in a fluidized bed operated in the Roadster J mode.

OBJECTS OF THE INVENTION One object of the present invention is to provide single coated wax encapsulated bleach particles with improved stability against degradation by ambient humidity or aqueous liquid media.

Another object is to provide wax-encapsulated bleach particles having a smooth, continuous coating with excellent surface safety.

It is further an object of the present invention to produce such encapsulated particles in a way that avoids the problems of improper coating and the resulting insufficient bleach stability and particle agglomeration.

Another object is to provide an encapsulated bleach having a coating that melts or softens sufficiently to release the bleach early in most automatic dishwashing wash cycles.

Furthermore, it is an object of the present invention to provide an encapsulation method that does not involve organic solvents that cause environmental pollution problems.

Another object of the invention is to provide a method that operates with a minimum of processing steps.

Yet another object of the present invention is to provide a liquid or solid cleaning composition containing the aforementioned single coated wax encapsulated bleach particles, which capsules do not leave waxy stains after cleaning. imparts stable bleaching activity.

More specific purposes include enzymes, fragrances, fabric softeners, structural agents,
and to provide stable bleaching activity in liquid dishwashing detergents or other hard surface cleaners that also contain oxidation-sensitive ingredients such as surfactants.

These and other objects of the invention are further elaborated in the following description and examples.

SUMMARY OF THE INVENTION In a first aspect, the invention encompasses encapsulated bleach particles suitable for use in household detergents. The bleach forms the core of these particles and constitutes 45-65% by weight, preferably 50-60% by weight of the final particle (i.e. core-coat). The single wax coating on the particles consists of 35 to 55%, preferably 40 to 55%, most preferably 45 to 55%, by weight of the particles, and about 40 to about 5% by weight.
Selected from one or more low melting point paraffin waxes having a melting point of 0°C and a penetration value of 10 to 60 m at 25°C. A single wax coating of 100 to ton microns thick is applied to the bleach particles. Preferably the coating thickness is between 2 [10 and 750 microns, most preferably 30
0 to 600 microns.

In a second aspect, the invention includes a method of making encapsulated bleach particles. This method has a low melting point, i.e. about 40
The process involves spraying molten paraffin wax having a melting point from 0.degree. C. to about 50.degree. C. onto the uncoated bleach particles in a fluidized bed. The bed temperature is 5°C to approximately 50°C above the wax melting point.
The temperature may be lower. The spray temperature of the molten wax applied to the particles is at least 5-40°C below the melting point of the wax.
expensive. A single wax coating with a thickness of lo [1 to 1.000 microns is applied to the bleach particles. The rate of application of the wax coating is lO per kg of bleach particles in the fluidized bed.
~40g/min.

The fluidized bed may be operated as a top-spray or a fuller-spray system. When using top spray, it is advantageous to have an annealing step after the coating step in order to impart a continuous surface and good surface integrity to the coating. If the fluidized bed is operated with one type of Wurs+er spray, no annealing step is required.

In a third aspect, the invention provides 0. 1 to 30% by weight of these encapsulated bleach particles. The composition may further include 0.1-15% surfactant, 1-75% builder, and other ingredients. These compositions leave little or no waxy stains on the surfaces they clean.

Encapsulated bleach particles of the present invention include particles with a single coating of 35-55% by weight paraffin wax and a core of 45-65% bleach suitable for use in household cleaning compositions. . Preferably, the paraffin wax coating constitutes 40-50% by weight of the particles and the core constitutes 50-60% by weight of the particles.

The bleaching agent encapsulated in the paraffin wax coating may be a chlorine or bromine releasing agent, or a peroxygen compound. Suitable reactive chlorine or bromine oxidizing substances include heterocyclic N-bromo and N-chloroimides such as trichloroisocyanuric acid, tribromoisocyanuric acid, dibromoisocyanuric acid, and dichloroisocyanuric acid, as well as potassium and sodium chloride. Mention may be made of its salts with water-soluble cations. Compounds such as 1.3 dichloro-5,5-dimethylhydantoin are also very suitable.

Dry, particulate, water-soluble anhydrous inorganic salts are likewise suitable for use herein, such as lithium, sodium or calcium hypochlorites and hypobromites. Trisodium chloride phosphate is another core material. However, chloroisocyanurate is the preferred bleaching agent.

Potassium dichloroisocyanurate is sold by Mon@*nje Col1psB as CL-59■. Sodium dichloroisocyanurate is also ^CL-
It is commercially available from 1Jons*nle as 60■,
In the dihydrate form, C1e*ron CDB-56■
As a powder form (particle diameter 15
media particle size (approximately 50-400 microns); coarse particle size (approximately 150-400 microns);
850 microns). Very large particles (850~!7
00 microns) have also been found suitable for encapsulation.

Organic peroxy acids may be used as the bleach core.

Peroxy acids useful in the present invention are solid, preferably substantially water-insoluble compounds. "Substantially water-insoluble" as used herein means water solubility of less than about 1% by weight at ambient temperature.

Generally, peroxy acids containing at least 7 carbon atoms are sufficiently insoluble in water for use herein.

Common monoperoxy acids useful herein include: (i) peroxybenzoic acid and ring-substituted peroxybenzoic acids, such as peroxy-alpha naphthoic acid; (11) aliphatic and substituted aliphatic monoperoxy acids; Examples include alkyl peroxy acids and aryl peroxy acids such as peroxylauric acid and peroxystearic acid.

Common diperoxy acids useful herein include: (iii) 1,12-diperoxidedodecanedioic acid; (i) 1,9-diperoxyazelaic acid; (v)
Diperoxybrassylic acid; diperoxysebacic acid; and diperoxyisophthalic acid; (Ma1) 2-decyldiperoxybutane-1,4-dioic acid.

Inorganic peroxygen generating compounds are also considered suitable as the core of the particles of the present invention. Examples of these substances include monopersulfate, perborate-hydrate, perborate tetrahydrate,
and percarbonates.

A suitable coating material for encapsulating the bleach core particles is a paraffin wax having a low melting point, ie, a melting point of about 35 to about 50°C, and a penetration value of 10 to 60 m at 25°C.

For coatings, melting points in this range are desirable for several reasons. First, any storage temperatures encountered by cleaning compositions are generally below a minimum of 40°C.

Therefore, the wax coating remains throughout storage of the cleaning composition.
Protect the bleach core. A 50°C melting point cap for the wax coating was selected as it provides a wax that melts or softens early in any automatic dishwashing cycle.

The operating temperature of automatic dishwashers is typically 40-70°C, so sufficient melting or softening occurs to release the bleach core. Thus, the paraffin wax of the present invention releases bleach when the capsule is exposed to a hot water bath, but not before.

Furthermore, the melted paraffin wax of the capsule of the present invention is
Remains substantially molten between 4a and 50°C.

Such molten waxes are readily emulsified by surfactant components in cleaning compositions. As a result, such waxes leave less undesirable waxy residue on the items being cleaned than high melting point waxes.

Paraffin wax as one type is about 30~
It has a melting point in the range of 80°C and consists primarily of normal alkenes with low levels of isoalkenes and cycloalkenes. Isoalkenes and cycloalkenes are responsible for the lack of order in the solid wax structure; when solid, paraffin waxes are often crystalline. Thus, the wax coating has a melting point substantially above 50° C. so that the high melting point components remain solid throughout the cleaning cycle and do not create invisible residues on the surfaces being cleaned. It should not contain any paraffin.

The amount of solids in the wax at any indicated time may be measured with a differential scanning calorimeter. At room temperature, the more solids present in the wax, the better the wax is for the present invention: such solids strengthen the wax coating and make the particles less susceptible to ambient temperature or liquid aqueous environments. On the other hand, "oil"
Or the liquid wax softens the wax, thereby rendering it less protected against bleach particles. Wax solids content as measured by differential scanning calorimetry for suitable paraffin waxes is 100-40% at 40°C, optimum 100-75%. The temperature at 50°C is 0 to 15%, preferably 0 to 5%.

In contrast to paraffin wax, fine quality wax is −
Numerically high molecular weight and melting point. Therefore, the melting point range for fine quality waxes is from about 50 to about 100<0>C. Furthermore, fine quality waxes have a higher viscosity than paraffin waxes in the molten state and are softer than paraffin waxes when solid.

Particles coated with fine quality wax therefore have a poor protective coating and it is highly unlikely that the wax coating melting from such particles will emulsify in the cleaning composition. Therefore, fine grade waxes are not considered to be within the scope of operation of this invention.

The Penetration Test (ASTM D-13211) is a standard industrial test for wax hardness. This test measures the depth (1 Paraffin wax suitable for use in encapsulating bleach particles has a penetration value of 10 to 60 degrees at 25°C.

Commercially available paraffin waxes suitable for encapsulating bleach particles include Merck 715G and 71
51 (Sold by West Germany Dsrmsjxdl E, Me
tek) ;Refer 1397 (Seller Bol
er) (penetration value 40 m5 at 25°C); Rots fully purified paraffin wax its/12G
<Seller Freak D, Ross Co,, I
nc, ) (25'C penetration value 40~5G theory) HAlts
Mouth “0ketin-2N!” (Seller Dw
r+chem Inc, ) (25℃ teno penetration value! 5
~26 theories) can be mentioned. The most preferred is 1o1er
It is Nu.

Method for Encapsulating Bleach Particles The manufacturing process for encapsulating bleach particles is: Hata) suspending the bleach particles in a fluidized bed; h) having a melting point of about 40-50°C to provide a coating; 1 whose penetration value is Ill~60~ at 25°C
selecting one or more paraffin waxes; C) heating the one or more paraffin waxes to a temperature well above the melting temperature to melt all the waxes; d) raising the bed temperature to at least -5°C. Fluidize the bed by passing warm air through the bleach particles to maintain a temperature below 50°C; C) Spray the bleach with molten paraffin wax for sufficient time to bring the melting temperature of the wax to at least 5°C. Continuous, adhesive (co
forming a paraffin wax coating of the present invention.

The amount of coating applied to the bleach core particles is generally about 35-55%, preferably about 45-50% by weight of the total particle (ie core+coating).

The coating is applied in a fluidized bed. There are several ways to operate a fluidized bed. - In numerical fluidized bed operation, air is pumped into the bed from below, while the coating material is blown onto the fluidized material from above. In this upward spray operation, the particles move randomly through the bed.

If care is not taken in applying molten coating materials in a fluidized bed, the resulting material may be poorly coated or may clump together. Both of these undesirable results derive from the temperature settings when operating the fluidized bed. For example, if the bed temperature is much lower than the temperature of the molten wax, the molten wax will begin to solidify as soon as it enters the cold bed region.

The wax then loses some of its ability to adhere to the surface of the bleach particles, and the wax itself solidifies immediately. When this happens, the fluidized bed in operation for spraying dries the wax and produces little or no coating on the bleach. Bleach particles that are not sufficiently coated consequently exhibit little stability to ambient temperature or aqueous liquid conditions. Alternatively, if the bed temperature is too high, the wax that is not in contact with the bleach particles will not be cooled and dried and will therefore remain soft and sticky. As a result, the bleach particles agglomerate and form clumps. The size of the resulting clumps becomes difficult to control. These large clumps are too large to melt during the cleaning cycle, where they remain as solid soil on the material being cleaned. Therefore, improper control of fluidized bed temperature can produce encapsulated bleach that does not meet one of the objectives of the present invention.

The inventors have shown that even with coatings up to 1,000 microns thick, if bed temperature and atomization temperature in the fluidized bed are properly controlled, agglomeration and insufficient coating will not occur. I found out that. Thus, "spray drying" of the wax and agglomeration of the coated bleach particles is reduced if the bed temperature is between 20 DEG C. and below the melting point of the wax. Preferably the bed temperature is between 20 and 35°C, most preferably between 25 and 32°C.

The inventors have further found it beneficial to maintain the atomization temperature, or the temperature at which the wax is sprayed from the nozzle onto the fluidized bed, at least about 5-10° C. above the melting temperature of the wax.

When using the top spray method, the maximum atomization temperature is approximately 35° C. above the wax melting point; above this temperature, the percentage of particle agglomeration becomes too large. Wwtsj
When coating particles using the er method, the spray temperature is 5
The temperature may be 0° C. and even higher than the melting point of the wax. This has been found to be a practical atomization temperature, even though it is expected that partially coated particles with a fused coating will stick to the spray nozzle. Instead, the air flow is strong enough to pull these partially coated particles apart. Alternatively, the inventors have discovered that the temperature of the molten wax may be maintained at a temperature substantially above the melting point of the wax, ie 50-100°C above the melting point. In this case, the spray temperature is preferably about the melting temperature of the wax, or even below, in order to reduce the wax temperature sufficiently to cause immediate solidification onto the bleach particles in the fluidized bed.

There are a number of commercially available fluidized bed devices suitable for use in the process of the invention; examples include the G11ll AirTec
GPCG-50 type and GPCG-60 of hnqaes
There is a type.

These can coat loads of bleach particles of 10 to sob in 0.5 to 3 hours. Table top encapsulation is
It may also be carried out in laboratory scale equipment, such as in the case of the Grxnallsll model number WSG-3 (sold by GhN Ait Tsehniqaes).

The inventors have surprisingly found that the encapsulated particles produced by the method of the invention exhibit excellent stability against ambient humidity when used in powdered detergents and against aqueous media when used in liquid detergents. It was found that the stability against

This increased stability occurs whether the bleach is encapsulated in the fluidized bed by the top spray method or by the Wmrgler method. Increased stability is
Examples are shown in ■ and ■.

An alternative to top spraying fused coating material is the warster spray system.

This method is described in detail in US Pat. No. 3.03.944, which is incorporated herein by reference. Generally, fluidized beds are characterized by randomness of particle movement. Random motion is undesirable when coating particles because of the resulting slow coating speed. To overcome this problem,
By controlling the speed difference, a circular (c7clic) flow pattern is established in the hth 1cr spray method. The Wwtsjer system involves the use of a vertically arranged coating column, where the particles are suspended in an upwardly flowing air stream that enters the bottom of the column. Inside the column, this air stream is divided into a portion of the suspended bed that flows upwardly,
and outside the tower, by another part flowing downwards.
Imparts controlled circular motion to particles.

All of the Kotobuki coating material is directed into a high velocity air stream to provide a coating of particles moving upward within the cylinder. The liquid coating solidifies on the surface of the particles as the air stream removes them from the nozzle. The particles are carried to the top of the tower and from this point fall along the outer path of the tower to the bottom of the tower. At the bottom, the particles exit through the opening and travel upwards again in the air stream inside the column. This cycle is repeated until the desired amount of coating is deposited on the particles.

In the case of the Wwtsler process, the W-neck+er system was certainly not suitable for encapsulating bleach particles in wax. The spray nozzle in the Wwtslet is at the bottom of the fluidized bed and sprays the coating material upwards. This configuration of the spray nozzle was certain to cause clogging of the spray nozzle if coated and agglomerated particles fell into the nozzle area from the upper air spray. This risk appeared to be particularly high since the nozzle temperature exceeded the melting point of the wax coating within the film. However, the inventors
Surprisingly, we have discovered that the use of the Wurster spray system offers many advantages.

Therefore, agglomeration of coated bleach particles can be further reduced when operating a fluidized bed in the Wwtwjet process.

Approximately 5-15% of particles covered by top spray
Wwt in the fluidized bed, on the other hand, aggregates and is therefore unusable.
The level of agglomerated particles using the ster system typically does not exceed 5%.

Furthermore, the coating time according to the Wmrsler method is
As shown in Example I below, even with substantially lower airflow speeds, it can take half or less of the time required for a single top spray method.

Although the batch size is often smaller than in the top-spray one-way system, and although the rate of wax spraying onto the core is virtually no higher than in the Warster system, the production rate of encapsulated bleach particles is still L
In the r5ter system, it is 2-3 times higher. This high production rate can be maintained even when the air flow rate through the fluidized bed is lower than the top spray method. Therefore, Wmrst
The high production rate with low airflow velocity in the ET system produces particles that are less agglomerated than the top spray system.

The inventors have further found that performing an additional annealing step after coating the bleach particles in a top-spray fluidized bed further improves the capsules. "Annealing" is a term that refers to further heating the wax-encapsulated bleach particles at a temperature above room temperature but below the wax melting point. This heating step is carried out using a fluidized bed, ie with hot air flowing through it; however, there is no molten wax being blown onto the particles during annealing.

The annealing process allows the wax to move enough to fill the crevices and crevices on its surface, thus better sealing the bleach inside.

The temperature chosen for the annealing is one that softens the wax without making it sticky. Generally, this temperature is
5-15°C above the bed temperature during coating and 3-15°C below the melting point of the wax coating. For example, if the melting point of the wax is 46°C, the annealing temperature is about 33-34°C.

The bed temperature during spraying is only about 31-32°C, 32
Above 0.degree. C., there is an opportunity for the particles to agglomerate: the high temperature of the molten wax and the annealing temperature soften the wax and cause the particles to agglomerate in the fluidized bed. however,
If hot melt wax is not sprayed onto the particles, the annealing temperature in the bed alone will not be hot enough to cause agglomeration.

Most preferably, annealing should be carried out for 10 minutes to 48 hours, optimally about 1 to 24 hours. capsule,
Incorporation of inert materials such as amorphous silica, alumina or clay can prevent the capsule from sticking at annealing temperatures. When mixed with inorganic annealing additives,
Since high temperatures can be used during the annealing process,
Therefore, the annealing period can be shortened. The additives may be used in amounts of 1:200 to 1:20, preferably t:too, based on the total capsule weight.

When using the Wmtrler spray system, we have further made the beneficial discovery that an annealing step is not necessary. More precisely, when using the Wmtsler method, cell annealing occurs automatically as part of the coating process.

When hot melt wax droplets are contacted with partially coated bleach particles, the wax on the already solid particles melts and fills any cracks in the wax surface. Unlike the spray-coated particles in the top-spray system, which fall into the crowding ring of other particles in the fluidized bed, the particles in the wsrster system exit the spray tower and fall through a low crowding gap outside the tower. . In this gap, the particles are gradually cooled. The reduced loading of bleach particles coated in the Wirstedt method also reduces the possibility of contact with other particles during cooling. The result is annealing as part of the coating process.

Cleaning Compositions Including Encapsulated Particles The wax-encapsulated bleach capsules of the present invention may be included in a variety of cleaning compositions. These compositions include powder and liquid compositions for textile cleaning, textile softening, automatic dishwashing, light duty dishwashing, and hard surface cleaning. Most of these compositions are approximately 75
% builder component, and 0.001-5% fragrance component. Some of the aforementioned types of products contain about 0.0% of the composition.
Some contain 0.01-15% by weight of surfactant, preferably about 0.5-10% by weight. Wax encapsulated chlorine bleach is particularly suitable for automatic dishwashing liquid or "gel" detergents, where the capsules contain 0.0% of the composition.
Present in an amount of 1-15% by weight. The automatic dishwashing horizontal detergent powder and detergent liquid have the compositions shown in Table 1.

Table I Automatic Dishwashing Detergent Composition Weight % Ingredients Formulation Formulation Builder 5-70 10-611 Nonionic Surfactant! -1s O, 01~
Trisilicate 1-20
S-211 Bulking Agent Toro 0 Bleach 0.1-20
0.1-20 thickener o-
so-s fragrance
0-5 0-5 water
The total value is 100.The total value is 100.Gels, unlike liquids, are mainly composed of polymeric substances.
Contains only low levels of clay.

Detergent Bilgoo Materials The cleaning compositions of the present invention may contain any type of detergent bilgoo commonly taught for use in automatic dishwashing or other cleaning compositions.

Builders include conventional inorganic and organic water-soluble bilgoux salts, or mixtures thereof. Builders may constitute from about 5 to about 10% by weight of the cleaning composition.

Generally well-known inorganic building blocks include the sodium and potassium salts of: pyrophosphate;
Tripolyphosphates, orthophosphates, carbonates, bicarbonates, sesquicarbonates and borates. Other non-phosphorous salts may be used as well, including crystalline and amorphous aluminosilicates.

Particularly preferred builders are sodium tripolyphosphate,
selected from the group consisting of sodium carbonate, sodium bicarbonate, and mixtures thereof. When present in these compositions, the sodium tripolyphosphate concentration ranges from about 2% to about 40%
%, preferably about 5% to about 30%. Sodium carbonate and sodium bicarbonate, if present, represent about 10-50% by weight of the cleaning composition, preferably about 20-40%.
is within the range of

Potassium pyrophosphate is a preferred builder in gel formulations, where it may be used at about 3 to about 30%, preferably about 10 to about 20%.

Organic detergent builders may also be used in the present invention. They are - numerically the sodium and potassium salts of: citrate, nitrilotriacetate, phytate, polyphosphonate, oxydisuccinate, oxydiacetate, carboxymethyloxysuccinate, tetra Carboxylate salts, starches, oxidized heteropolymerizable polysaccharides, and polymeric polycarboxylate salts such as polyacrylates of molecular weight s, ooo to about H6,01111. Polyacetal carboxylates such as those described in U.S. Pat. Nos. 4,144,225 and 4,148.495 may also be used.

Sodium citrate is a particularly preferred builder.

If included, it is preferably used in an amount of about 1 to 35% by weight of the detergent composition. The detergent builders described above are for illustrative purposes only, and the builders that can be used in the present invention are not limited to these types.

Surfactants Surfactants may be included in household detergents containing encapsulated bleach particles. Useful surfactants include anionic, nonionic, cationic, amphoteric, zwitterionic, and mixtures of these surfactants. Such surfactants are well known in the detergent art and are
ad DeterHe+j” (Vol.

II, b75ehvsrlt, Perr7 & H
itch, I+1erscie++cePIbli
Shers, Inc., 1959), the contents of which are hereby incorporated by reference.

Anionic synthetic detergents can be broadly described as surfactants having one or more negatively charged functional groups.

Soap is also included in this range of rumors. The soap is a 08-C2 alkali metal, alkaline earth metal, ammonium, alkyl-substituted ammonium or alkanol ammonium salt.
It is a 2-alkyl fatty acid salt. Sodium salts of tallow and coconut fatty acids, and mixtures thereof, are the most common. Another important class of anionic compounds is
Water-soluble salts, especially alkali metal salts, of organic sulfur reaction products having an alkyl group containing up to 22 carbon atoms and a group selected from the group consisting of sulfonic ester groups and sulfuric ester groups. Organic sulfur-based anionic surfactants include C10"-016" alkylbenzene sulfonate, C1°-C22 alkanesulfonate, C
1o~C22 alkyl ether sulfate, Cll1~c2
2-alkyl sulfates, C4-C1o dialkyl sulfosuccinates, cto-C22 acyl isethionates, alkyl diphenol oxide sulfonates, alkylnaphthalene sulfonates, and 2-acetamidohexadecane sulfonates. Two commercially available suitable anionic surfactants are [F] Dov+*x 2^-1 and nov+xx 3B-2 from Dow Chemicll Co.
Mono- and G-C8-C14 sold under the trade name
Alkyldiphenyl oxide mono- and/or di-sulfates. Organophosphate-based anionic surfactants include organophosphate esters, such as complex mono- or di-ester phosphates of hydroxy-terminated alkoxide condensates, or salts thereof. Examples of organic phosphate esters include phosphoric acid ester derivatives of polyoxyalkylated alkylaryl phosphoric acid esters, phosphoric acid ester derivatives of ethoxylated linear alcohols, and ethoxylates of phenol. Particularly suitable surfactants for inclusion in cleaning compositions with wax-encapsulated bleaches include complex mono- or nonionic alkoxylates of ethoxylated nonylphenols having sodium alkylene carboxylates attached to the ester-terminated hydroxyl groups. It will be done. Counterions for all the salts mentioned above are alkali metals, alkaline earth metals,
It may also be of the ammonium, alkanol ammonium, and alkylammonium classes.

Nonionic surfactants are broadly defined as compounds formed by the condensation of an alkylene oxide group with an organic hydrophobe that may be aliphatic or alkyl aromatic in nature. The length of the hydrophilic group or polyoxyalkylene group condensed with any specific hydrophobic group can be easily adjusted to produce a water-soluble compound having a desired degree of equilibrium between the hydrophilic component and the hydrophobic component. can be generated. Various suitable nonionic surfactants include, but are not limited to: (Turtle) Containing about 8 to about 18 carbon atoms in the aliphatic chain and containing 5 to about 5 G Polyoxyethylene or polyoxypropylene condensates of linear or branched saturated or unsaturated aliphatic carboxylic acids containing ethylene oxide and/or propylene oxide units.

Suitable carboxylic acids include "coco" fatty acids (obtained from coconut oil) containing on average about 12 carbon atoms, "tallow" fatty acids (obtained from tallow fat) containing on average 18 carbon atoms, Palmitic acid, myristic acid, stearic acid, and lauric acid.

(bl contains about 6 to about 24 carbon atoms, about 5 to about 5
Polyoxyethylene or polyoxypropylene condensates of linear or branched saturated or unsaturated fatty acid alcohols containing 0 ethylene oxide and/or propylene oxide units. A suitable alcohol is “Cocoyashi”
Includes fatty alcohols, one-tallow, one-fatty alcohol, lauryl alcohol, myristyl alcohol, and oleyl alcohol. A particularly preferred nonionic surfactant compound in this class is the 5hsll Ch*m
“Neodoll N” is a registered trademark of 1cxlCoapsB.
eod+1” type product.

Also included within this class are those of the formula: where R is a straight chain alkyl hydrocarbon having an average of 6 to 10 carbon atoms, and R' and R' each have about 1 to 4 carbon atoms. a linear alkyl hydrocarbon having carbon atoms, X is an integer from 1 to 6, y is an integer from 4 to 15, and 2 is an integer from 4 to 25) It is. A particularly preferred example of this category is OliIIICorportal
Po17-T! is a registered trademark of iom (NtvHsvea, Coma, ). rltalSLF-18. P++17-TtBea electron 5LF-18 has the above formula (wherein R is a C6-Clo linear alkyl mixture, R'
and R' is methyl, X has an average of 3, y has an average of 12, and 2 has an average of 16).

Further suitable are alkylated nonionic substances,
This is disclosed in U.S. Pat. No. 4,877,544 (Gxbrie
1, etc.), the content of which is incorporated herein by reference.

(c) About 6~! Contains 2 carbon atoms, from about 5 to about 25
Polyoxyethylene or polyoxypropylene condensates of linear or branched, unsaturated or saturated alkylphenols containing moles of ethylene oxide and/or propylene oxide.

(d) Polyoxyethylene derivatives of mono- and trifatty acid esters of sorbitan in which the fatty acid component has 12 to 24 carbon atoms. Preferred polyoxyethylene derivatives are sorbitan monolaurate, sorbitan trilaurate, sorbitan monopalmitate, sorbitan tripalmitate, sorbitan monostearate, sorbitan monoisostearate, sorbitan tristearate, sorbitan monooleate, and sorbitan triolein. It is a derivative of The polyoxyethylene chain is about 4
It may contain up to 30, preferably about 20, ethylene oxides. Sorbitan ester derivatives contain 1°2 or 3 polyoxyethylene chains, depending on whether they are monoesters, diesters or triesters.

(0th order formula: % formula % (2) where a, b and C are integers reflecting the oxidized polyethylene and oxidized polypropylene blocks, respectively, of the above polymer) Block Copolymer. The polyoxyethylene component of the block polymer constitutes at least about 40% of the block polymer. The material preferably has a
0. More preferably, it has a molecular weight of about 3,000 to about 6,000. These materials are well known in the art. They are "BASF under the Plaronics trademark"
- Commercially available from WTlndolle Cotpot*tioa.

Amphoteric synthetic detergents are broadly described as derivatives of aliphatic and tertiary amines, where the aliphatic groups are straight or branched, and some of the aliphatic substituents contain from about 8 to about 18 carbon atoms, and some contain anionic water-soluble groups, ie, carboxy, sulfo, sulfato, phosphate, or phosphono. Examples of compounds within this definition include sodium 3-dodecylaminopropionate and sodium 2-dodecylaminopropanesulfonate.

Zwitterionic synthetic detergents can be broadly described as derivatives of aliphatic quaternary ammonium, phosphonium, and sulfonium compounds, where the aliphatic groups are straight or branched and where the aliphatic substituents are One contains about 8 to about 18 carbon atoms, and the other contains an anionic water-soluble group, such as carboxy, sulfo, sulfato, phosphato, or phosphono. These compounds are often called betaines. In addition to alkylbetaines, alkylaminos and alkylaminobetaines are included within the invention. Cocoamido-propyl dimethyl betaine is a particularly useful surfactant.

After melting the wax capsule, it either remains melted or reassimilates depending on the temperature of the washing liquid. However, in the molten or solidified state, the wax is deposited as rivers on the surface of the pieces being cleaned and gives them a veneer, striation, or film appearance. Wax can also accumulate on surfaces that are being cleaned, ie, sinks, bathtubs, and automatic dishwashers.

This staining from wax coatings may be reduced by including one or more surfactants in the cleaning composition. The inventors have found that certain surfactants prevent wax residue better than others.

These surfactants are Po17...1...5LF-18■
(Olin Corp8jeon), and Eiph
os O5-H61 (Wilc.

Chew...1), and Dovfsx2^-1■ and Dov+st3to2■.

Thus, preferred embodiments of the cleaning composition include: 0.1 to 15% by weight wax encapsulated bleach as described above;
1-75% builder; and polyoxyalkylated alkylaryl phosphates, mono- and di-C8
~C14 alkyl diphenyl oxide mono- and/or di-sulfate, and of the following formula: where R is a C6-C1o linear alkyl mixture, R and R' are methyl, and X is on average 3; y has an average of 12 and 2 has an average of 1
6) of nonionic surfactants.

Silicates The compositions of the present invention may contain sodium or calcium silicates at a level of about 1% to about 40% by weight of the cleaning composition. This substance is used as a cleaning agent, an alkaline earth metal corrosion inhibitor, and a polish protector for ceramic tableware surfaces. Particularly effective ones have a SiO:N a 20 ratio of about 1.
．． 0=about 3.3, preferably about 2:about 3.2 sodium silicate. Some of the silicates may be in solid form.

Bulking Agents Water-soluble, inert particulate bulking agents may be present in the cleaning composition in powder form. The material should not precipitate calcium or magnesium ions at filler usage levels.

Suitable for this purpose are organic or inorganic compounds. Organic fillers include sucrose esters and urea. Representative inorganic fillers include sodium sulfate, sodium chloride, and potassium chloride. A preferred filler is sodium sulfate. Its concentration is 0-60%, preferably about 10-20% by weight of the cleaning composition.
is within the range of

Thickeners and Stabilizers Thickening agents are often desired for liquid cleaning compositions. Thixotropic thickeners such as montmorillonite (bentonite), hectorite, saponite, etc. may be used to impart viscosity to the liquid cleaning composition. silica,
Silica gels and aluminosilicates may also be used as thickeners.

Polyacrylic acid (molecular weight 300,
000 to 6 million) may be used alone or in combination with other thickeners. The use of clay thickeners for automatic dishwashing compositions is described, for example, in U.S. Pat.
No. 4.752.409. The use of salts of polymeric carboxylic acids is described, for example, in British Patent Application No. 2.164.
．． No. 350A. Commercially available bentonite clays include Kor (buxH) and YWH (Comb
wsmouthoa EBiaeeriB, l+c,),
PolxBelT(Ametiexn Co11oid
Co, ), and Ge1vbije clay (particularly Ge1
vhite GP and H) (Ealish Chin
@Cl*YCo, ) is mentioned. Po1irlel
T is preferred if it imparts a greater apparent whiteness to the composition than other clays.

For liquid formulations with the appearance and rheological characteristics of ``Bl'', chlorine-stable polymeric thickeners are particularly useful, especially when transparent gels are desired. U.S. Pat. No. 4,260.
No. 528 discloses natural rubbers and resins for use in clear automatic dishwashing detergents, which are not chlorine stable. B, F.

A cross-linked acrylic acid polymer manufactured by Goodrich and sold under the trademark "C!rbopol" is effective in producing transparent gels and has a C5 molecular weight of approximately 4.000.000.
rbopor 94 (l) is particularly preferred because it maintains high clay over long periods of time and has excellent chlorine stability.A further suitable chlorine-stable polymeric thickener is described in U.S. Patent Application No. 15
No. 7.42 (Ellio H et al., submitted February 17, 1988). The contents of this specification are hereby incorporated by reference.

The amount of thickener used in the composition is 0-5%, preferably 1-3%.

Long chain calcium and sodium soaps and C12~
Stabilizers and/or co-structuring agents such as 018 sulfates (co
-sjrwctwrsajs) is disclosed in U.S. Patent No. 3,9S
No. L 158 and No. 4.271.0311, and the use of other metal salts in long chain strata is detailed in U.S. Pat. No. 4.752.40. The amount of stabilizer that may be used in a liquid cleaning composition is about 0.0% of the composition.
0.01 to about 5% by weight, preferably 0.1 to 2% by weight. Such stabilizers are optionally present in the gel formulation. Co-structuring agents that have been found to be particularly suitable for gels include 0.01-4% trivalent metal ions and/or 1-60% water-soluble structural chelators of the composition. These co-structuring agents are described in co-pending U.S. Patent Application No. 1N, 49
No. 2 (Cotrial et al., filed December 30, 1987), the contents of which are hereby incorporated by reference.

Liquid and one gel two formulations of cleaning compositions that include defoamer surfactants may further contain a defoamer (de+osset). Suitable defoamers include mono- and di-stearyl phosphates, silicone oils, and mineral oils. Even when the cleaning composition contains only defoaming surfactants, defoamers help minimize foam that creates food contamination. The composition may contain from 0.2 to 2% by weight, preferably from 0.05 to 1.11%, of a defoamer.

Minimal amounts of various other ingredients may be present in the cleaning composition. These include flow control agents (in granular form), soil repellents, anti-resoiling agents, anti-fogging agents, enzymes (e.g.
．． 05-2% by weight, preferably 0.5-1.5% by weight of protease, amylase and/or lipase), as well as other functional additives and fragrances. The pH of the cleaning composition may be adjusted by adding strong acids or bases.

The following examples further illustrate the compositions of the invention. All parts, percentages, and proportions in the description and appended claims are by weight unless otherwise indicated.

Example! Two batches of wax encapsulated bleach particles are made using a low melting point wax in a GIxN WSG-5 fluid bed. Batch A is Hot with a ratio of 7154/H, 4G.
r941/AIts! Coat with a mixture of in 125 paraffin wax. Batch B is 100% Bol*
r! 141. Using the following conditions, CIe
*Coat roa CD 5G bleach particles.

Batch A Fluidized bed device Glut WSG-5 Spray one-way top spray nozzle
Intermediate opening width 11' expanded nozzle tip diameter
1.2 ■ Capacity 22 liters Floor weight
11 lbr.

Air flow rate 400-450 cle inlet air temperature 27-32℃ bed temperature
28-32℃ coating speed 52g/
min coating temperature 75-80℃ atomization air pressure
5-bar spray air temperature 80~90℃ batch time
Batch produced using top spray installed for 148 minutes,
Generally, there is a 15-20% loss as agglomerated material. 11 lb (Jkg) C1esro
n CDB-5ii bleach particles, 79.54/20.4
It is coated in batch A with 6 kg of a mixture of Hoter 941 and A 5 h 125 paraffin. The resulting encapsulated bleach particles have excellent stability in automatic dishwashing fluids.

Batch B was applied in a fluidized bed with the following settings: Nispre coated with 100% Bolsr H97 wax One-way Partition Height Nozzle Tip Diameter Capacity Bed Weight Air Flow Rate Inlet Air Temperature Bed Temperature Batch B orker Glstj (d 'CG-5 t,o' 2m 10.5 liters 17.51bs 20G-270cam 1g-24℃ 3G-31'C Coating speed 72g/min Coating temperature 75-80℃ Spraying air pressure
Spraying 1.5B* Air temperature 80
~90°C Batch Time 70 min Batch B encapsulated CDB-56 at 4t1°C;
It has excellent stability in automatic dishwashing liquids at pH 12.3.

Example ■ The solubility of a coating composition made from fine quality wax and fatty acids in an alkaline medium has a melting point of 40-5.
Compared to the solubility of coating compositions made from certain paraffin waxes at 0°C can show a significant difference. 4
Two different coating compositions are prepared from fine waxes having a set of fatty acids in the proportions shown below. Two different paraffin waxes are selected for comparison. The 4 fatty acids/waxes and 2 waxes are placed in separate beakers that already contain 2.8717 ttle of a 0.02% aqueous solution of Empho@C5-1361. The contents of each beer barrel were heated to 49°C and held at this temperature with stirring for 45 minutes, then cooled to room temperature and
Pour through a USA standard metal sieve having a mesh size of 8 (300 microns).

The solid wax captured on the sieve was dried and weighed to determine the amount of wax that remained as a solid residue after heating with the surfactant.

Table ■ 62.0% Lauric acid 9 78.1% Myristic acid 1 5゜72.2% Myristic acid 1 Boler paraffin 1397 (3, Rost's fully purified paraffin its/
12G Melting point of capric acid Lauric acid Myristic acid MIllivsx W-145^ = 31.2°C = 43.9°C = 54.1°C = 66-71'C 34.4% Capric acid 62]% Lauric acid 2, 11 % MIllivsx W-145^3g,
8% capric acid 5■, 4% lauric acid 3, 3.6% M1 eyes 1 vsx W-145AI8.
3% capric acid 711% myristic acid 4, 81% Mwlltwo W-145^! 9.0%
Capric acid 72.2% Myristic acid 5, 5olar paraffin + 317 ・, 1315 1632 ・, 267g 0.0001 51.7・ ! 0.44 11.1! 6.1・■ fully purified paraffin II5/+2
1111.0092 Fine quality wax/fatty acid compositions leave large amounts of wax residue. A comparison of Samples 1 and 2, and 3 and 4 shows that coating compositions containing low levels of 1vsx W145-A deposit less wax.

When comparing coating compositions 1 to 4, the melting point is 40
Paraffin wax at ~50°C leaves very little residue and is therefore highly preferred as a coating for bleach particles.

Example ■ Bleach was mixed as in Example I, but with wax (30% Epoleac C-16/70% B) melting at 72°C.
olctPzrslfi111426), 52℃ (^
ll*+ia 125/No) or 46'C (Less
115/12G) without a coating consisting of a wax that melts at 115/12G). Capsules coated with high melting point wax are coated in a fluidized bed analogously to the capsules of Batch A in Example I, except that Epole
For capsules coated with ae, the bed temperature is 60-6
5°C, and for capsules coated with A11s+ia 125/NO, the bed temperature is 40-45°C. R
Capsules coated with oss 115/12G are prepared analogously to Batch B of Example I. All three capsule batches are coated with a core:coat ratio of 47:53. For example, for a 1 gram capsule, the wax is 0.5
It should be 3 grams.

1.88 grams of each type of capsule is placed into 40 grams of an automatic dishwashing liquid composition containing:
Quality Weight%45%Kon
1.10 Laponite clay
0.02TUFF
4.00C*rbopol 941
1.0GSTP
1.0060% TKPP solution 25.0
On-silicate 17.0012Co
3 (47% sol+) 12.77L S7'F-181,00 Coloring agent 0.5 Fragrance
O,OS water
The method for making the automatic dishwashing gel formulation in 36.5 is as follows: Add water to a container. 1
Add the KOH with stirring for a minute, then add the clay with stirring for an additional 10 minutes. A mixture of TKPP, STP and C5rbopol 941 is then added over 12 minutes, followed by stirring for 30 minutes. Then, the TKPP solution is added and the mixture is stirred for 30 minutes. D-silicate, K2CO3 and 5ty-ta are then each added separately and each is stirred for 5 minutes.

The automatic dishwashing liquid composition containing the bleach capsules is then placed into the dispenser cup of the Keamore automatic dishwasher. A 40 gram sample of the automatic dishwashing liquid composition is placed at a time into the dispenser cup of the dishwasher and the machine is run empty for one cycle.

At the end of the wash cycle, strain the waste water from the machine through a 43 mesh U, S, standard metal sieve into a bucket.

Film melting point Retained wax Retained edge wax ('C)
Weight %72
0.28g 211%52
0.17g 1746
0 0 Example ■ The same three types of capsules prepared in Example ■ are now tested for spotting prevention on glassware being washed in an automatic dishwasher. At 140'F, hardness 120p
A visual test of the glass is performed in a Bosch S-512 dishwasher using p-water.

For testing, two dishwashers are loaded with 10 clear glass dishes and glasses (all clear and without specks). Next 4
Apply 0g fat stain to the inside of the washer door. Dirt: 4 lbs. Imptri*LV-Galin and 4 packets (12.8 oz. each) of C5tns
Mix and form the lioa non-fat dry milk until smooth. Next, 40 grams of an automatic dishwashing liquid composition containing one coated bleach capsule is placed into the cup dispenser of the dishwasher.

The glassware is then placed in a short wash cycle.

After the wash cycle, each glassware is removed from the dishwasher and evaluated for spotting according to the following rating: Spotting grade 0 = no spots 1 to almost no spots 2 = - 1/3 of the glassware has spots 3 = Spotting on 273 of the glass 4 = It is shown that the spots completely cover the glass and melt easily, thus releasing a large amount of bleach and improving the spotting score.

Example ■ In order to compare the stability in alkaline medium of a bleach coated with paraffin wax with a melting point of 40-50 °C with a bleach coated with a mixture of fine wax and fatty acids, C1esroa CDB-56 Bleach particles (Qli
ll Corporations a11) are coated with coating composition 3.4.5 or 6 as described in Example 2.

The capsules are manufactured on a Grs*B15ll machine WSG-31F with the following settings: Spray one-way Warster initial bed load
1,600g air temperature 16
-20℃ bed temperature es, 1g-22
℃ Coating speed 6G-80g/min Coating temperature 75-80℃ Atomizing air pressure
1.5 bar atomizing air temperature 79-88
℃ Batch Time 2G-28 minutes 1.11 grams of each capsule is then uniformly dispersed in the automatic dishwashing liquid of Example 2. In this way, six automatic dishwashing liquid compositions containing capsules are produced, each stored at 40°C.

Samples are prepared in triplicate in 4 oz glass jars.

1, 2. 7.14.28.42. and chlorine analysis is performed after 56 days.

A 5 ml aliquot is removed from each of the six automatic dishwashing fluid samples and filtered through a USA standard metal sieve (48 mesh) to remove the capsules. The wax coating is dissolved from each capsule by gentle stirring in hexane for 20 minutes. The amount of active chlorine remaining is then measured by standard iodometric titration. The results are summarized in the table below.

Table 6 100, 0 47.6 Capsules 3 and 4 have a melting point of 50° C. and exhibit coating levels of 57 and 54% by weight of total capsules, respectively.

Capsule 4' has the same composition as capsule 4, except that its coating level is higher, 66%. Capsules 1 and 6 have a coating level of 54%. The results show that the fatty acid/fine wax coating protects bleach poorly in alkaline media.

These coating materials are therefore not suitable for use in aqueous alkaline media. In comparison, when the coating is a paraffin wax with a melting point of 40-50°C, the bleach level retained in the alkaline medium is excellent.

Example ■ The stability of bleach encapsulated in a single wax coating of different thicknesses is determined as follows: C
A batch of 1...oa CDII H■ is placed in a fluidized bed and coated with sufficient Bolxr paraffin 1397 so that the coating constitutes 35% of the encapsulated bleach (Batch A), C1exroa CDB 56@) A second batch of (Batch B) is coated with enough Boler 1397 so that the coating covers 55% of the particles. Approximately Ig of each bleach encapsulation was then added to the automatic dishwashing composition of Example 40. and stored at 40°C.

Samples were prepared in triplicate in 4-ounce glass jars and heated to 40.2°C.
Store in. Chlorine analysis is performed at 1.2.4 and 6 weeks.

At the time intervals shown in Table V below, 5 ml aliquots are removed from each automatic dishwashing liquid sample. Filter these through a USA standard metal sieve (48 mesh) to remove the capsules. The amount of active chlorine remaining is determined by standard iodometric titration.

The results are summarized in the table below.

Table V Storage stability of remaining raw chlorine activity in ADL gel (%)
) Batch A Batch B Time (35% B) (55% training) 1 week 100.0 100.0 6 weeks + 63.0 8
2.0 This indicates that the thicker the coating, the more the bleach particles are protected in aqueous media.

Example ■ The capsules of Example ■ are included in the automatic dishwashing liquid composition of Example ■. 40 g of each composition was added to Il:e++mot
ePut it in the dispenser cup of the automatic dishwasher, 46
Run the machine for one wash cycle at .

Remove 5 ml aliquots from the wash solution every 20 minutes during the wash cycle. The amount of useful chlorine released from the capsules is determined by standard iodometric titration.

The results (Figure 3) showed that the capsules with the low melt coating released the bleach more quickly and completely. These capsules therefore exhibit a high degree of efficiency.

The above description and examples are selected embodiments of the invention. In light of this, various modifications may be suggested to those skilled in the art, all of which are within the spirit and scope of the invention.

[Brief explanation of drawings]

FIG. 1 is a graph of the amount of wax coating that remains unemulsified through an automatic dishwashing cycle, as described in Example 1. FIG. 2 is a graph of the spotting performance of automatic dishwashing liquids containing bleach encapsulated in waxes with different melting points, as described in Example 1. FIG. 3 is a graph of chlorine isolated by bleach encapsulated in waxes of different melting points, as described in Example 3. TT, embedded patent attorney Jun Sakai [[[I No CAPSULES

Claims (12)

[Claims] (1) A method for forming a coherent continuous coating around bleach particles suitable for use in a cleaning composition, comprising: a) suspending the bleach particles in a fluidized bed; b) Melting point approximately 40-50℃, penetration value at 25℃ 10-6
c) heating the one or more paraffin waxes to a temperature above their melting temperature to sufficiently melt all the wax; d) fluidizing the bed by passing air through the bleaching particles to maintain a bed temperature of at least 20° C. below the wax melting point; and e) transferring the molten paraffin wax onto the fluidized bed in the fluidized bed. 1 at a rate of 10 to 40 g/min per kg of bleaching particles.
spraying for a period of time sufficient to form a coating with a thickness of 0.00 to 1,000 microns. (2) Paraffin wax by the Wurster process, which involves suspending the particles in an upwardly flowing air stream that enters the bottom of the fluidized bed to impart controlled cyclical motion to the particles as well as a portion of the upwardly flowing bed. 2. A method according to claim 1, wherein the fluidized bed is sprayed with: (3) further comprising annealing the coated particles at a temperature of 5 to 15 degrees Celsius above the bed temperature during coating and at a temperature of 3 to 15 degrees Celsius below the melting point of the wax coating for 10 to 45 minutes after completion of spraying. The method described in Section 1. (4) The average diameter of the encapsulated particles is 800 to 4,000
2. The method of claim 1, in the range of 0 microns. (5) The solid content of paraffin wax is 40~40℃ at 40℃
2. The method according to claim 1, wherein the concentration is 100% and 0 to 15% at 50<0>C. (6) Wax encapsulated bleach particles suitable for incorporation into cleaning compositions comprising: a) a solid particulate core of bleach of 45 to 65% by weight of the final encapsulated particles; b) a solid particulate core of bleach of 45 to 65% by weight of the final encapsulated particles 35-55% by weight wax coating having a melting point of about 40°C to about 50°C and a penetration value of 10-60 mm at 25°C.
, and a coating having a thickness of 100 to 1,000 microns. (7) The encapsulated particles of claim 6, wherein the coating has a thickness of 200 to 750 microns. (8) The encapsulated particles of claim 6, wherein the bleaching agent is selected from the group consisting of chlorine releasing agents, bromine releasing agents, and organic and inorganic peroxygen generating compounds. (9) Claim 8 wherein the bleaching agent is chloroisocyanurate.
Encapsulated particles as described. (10) the following: a) 0.1-15% by weight of the encapsulated bleach of claim 6; b) 1-75% by weight of a builder; c) 0.1-15% by weight of a surfactant; d) Liquid cleaning compositions containing 15-95% water. (11) The composition has: a) 10-60% builder; b) 0.01-2% nonionic surfactant; c) 5-2
d) 0.1 to 15% of the encapsulated particles of claim 6; e) 0 to 5% of clay; and f) a residual amount of water. 10. The cleaning composition according to 10. (12) The surfactant is mono- and di-C_8 to C_1
_4 Alkyldiphenyl oxide mono- and/or di-
Sulfate, polyoxyalkylated alkylaryl phosphate ester, the following formula: ▲Mathematical formula, chemical formula, table, etc.▼ (wherein, R is a C_6~C_1_0 linear alkyl mixture, R' and R'' are methyl, 11. The cleaning composition of claim 10, wherein the cleaning composition is selected from the group consisting of surfactants and mixtures thereof, wherein x has an average of 3, y has an average of 12, and z has an average of 16.