JPS6138240B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to new and surprisingly different dispensing packages of heavy duty detergent compositions. More particularly, the present invention relates to bottled granular heavy duty detergents that can be easily dispensed like liquids, yet without the various disadvantages associated with liquids.

Granular detergent compositions based on synthetic organic detergents and builder salts that enhance their cleaning power are well known and have been commercially available for many years. In a preferred form, the particles may be round or spherical, or may be an agglomeration of a small number of spherical particles, such as those obtained by spray drying of clutch mechanics of its various components, followed by size screening. good. Post-spraying of liquid substances, especially heat-sensitive substances, onto the surface of spray-dried beads is also known. However, it is often difficult to obtain free-flowing products containing significant proportions of liquid to viscous synthetic organic detergents (eg, liquid nonionic detergents) and water-soluble builder salts.
For this reason, synthetic organic detergents with low viscosity, such as synthetic organic anionic detergent salts such as linear sodium tridecylbenzene sulfonate (which also serve to enhance the detergency of built detergent compositions), are widely used. For ease of dispensing, among other things, liquid detergents are often sold in plastic bottles (eg, single-piece hollow-handled bottles). However, prior to the present invention, it was not possible to package free-flowing, high bulk density heavy duty detergents in bottles that could be dispensed as easily as liquids and without suffering the various disadvantages associated with liquid detergents. unknown. For example, the bottled granular detergent of the present invention does not separate into different phases and therefore contains non-detergent ingredients (e.g. hydrotropes) to prevent separation into different phases.
does not need to exist. Moreover, since the granular products of the present invention are substantially dry, no aqueous or liquid phase decomposition reactions occur between the components, and therefore, special stabilizers can be incorporated or the formulation can be modified to react in an aqueous medium. There is no need to inactivate or eliminate substances that tend to Additionally, because the particulate builder detergent is dispensed as a solid particulate composition, there is no detergent gel or cement-like deposit that sometimes occurs in the neck of conventional liquid dispensing bottles. Thus, the present invention provides the advantages of granular or powdered detergents with packaging and dispensing conveniences that are equal to or superior to bottled liquid detergents.

According to the invention, the bottle comprises: a bottle having a neck for dispensing detergent from the bottle; and a free-flowing granular detergent composition within the bottle, which can be poured out through the neck; the particles comprising: a synthetic organic detergent; and its builders, of which at least 90% are American Sieve Series 8
Have a particle size that passes through a mesh screen and is retained on a 200 mesh screen, has a bulk density of at least 0.5 g/cc, and has a fluidity that is at least 70% of that of clean dry sand. A bottled granular detergent is provided. In various preferred embodiments of the invention, the cross-sectional area of the passage within the bottle neck is within a specified range and within a specified percentage range with respect to the bottle cross-sectional area; the bottle is integral therewith and communicates with the main interior of the bottle. The neck of the bottle is annular and has a hollow handle of specific dimensions, and a threaded cap of specific size to serve as a convenient metering cap for the detergent particles to be dispensed; is dust-free; the detergent composition is of a specific type;
Said properties exist within certain more limited ranges. A simple method for filling the bottle and its integral hollow handle is also within the scope of the invention.

Hereinafter, in order to facilitate understanding, the present invention will be described with reference to the accompanying drawings.

FIG. 1 is an enlarged side view of a bottled fluid detergent product (uncapped) of the present invention. In FIG. 1, a bottle 11 made of transparent polyvinyl chloride plastic has a body 13 having a handle 15 which is blown in one piece, and a neck 17 .
Although the bottle may have a variety of shapes, the preferred construction shown is one step that is substantially oval in cross-section (at least in its upper and lower portions) and that the length of the oval shape in the head of the bottle is It has a neck or spout portion near one end of the horizontal shaft, and a handle at or near the opposite end of the shaft. Also, the upper part 14 (the part near the end of the dispensing neck) of the body wall 12 is substantially vertical, that is, at about 70 to 90 degrees from the horizontal axis, and the upper part 16 (the part near the end of the handle) is less vertical. That is, it is also preferable that the angle is 30 to 60 degrees from the horizontal axis. The reason for this will be explained later.
Inside the bottle 11 are detergent composition particles 19 , which can be easily dispensed through a passageway 21 in the neck of the bottle by simply tipping the bottle and pouring out the granules. The above mentioned part is the second part.
This is suitably illustrated in FIG. FIG. 2 is a top plan view of the product of the present invention, and FIG. 3 is an enlarged side view of the product viewed from the handle side.

FIG. 4 is a sectional view taken along plane 4--4 of FIG. FIG. 4 shows a portion of the main interior 23 of the bottle and a portion of the internal passageway passing through the handle 15 , both of which are filled with granular detergent 19 as shown. has been done.

In Figures 1 to 4, the bottle is shown without a cap, but with a regular seal,
For shipping, an internally threaded screw cap is required, as shown in Figure 5 (enlarged side view of part of the head of the product of Figures 1-4 with sealing cap attached). It is suitably screwed into the threaded neck 17. Seal washers are usually not used if the bottle cap material is sufficiently resilient (seal beads are often sufficient), but may be used if desired. Since the cap 27 of FIG. 5 can of course also be considered to be in place on the threaded neck of the bottle of FIGS. 1-4, no alternative arrangement is shown.

Figure 6 is a photomicrograph (200x) of the main part of the spray-dried builder beads or particles before their surface is post-sprayed with a synthetic organic detergent (to make them free-flowing); The broken part of the bead in Figure 6 is shown (2000x magnification). The contents of Figures 6 and 7 are self-explanatory; the bright parts are reflections from the bead's skeleton (both the inside and outside of the bead help strengthen it), and the dark parts are the inside of the bead, the surface, and the void just below it. and the voids are made essentially free of detergent by spraying a liquid or dissolved synthetic organic detergent onto its surface or otherwise contacting the builder beads (e.g., the detergent covers less than 10% of the outer surface of the beads). can be introduced after producing the bead surface (coating). The beads shown in Figures 6 and 7 contain approximately 18.8 parts pentasodium tripolyphosphate hexahydrate, 7.6 parts sodium silicate ( _Na2O : _SiO2
= 2.4), which was obtained by spray-drying clutch materials containing 28.3 parts of pentasodium tripolyphosphate (anhydrous) and 49.6 parts of water until the water content was approximately 10%.

FIG. 8 is a partially enlarged layout of the filling means for filling a bottle with a free-flowing granular detergent composition, showing the sequence of filling operations and steps. FIG. 8 shows six steps (stages) when filling the bottle 11 with the granular builder-containing detergent 19 .
In the first step (left end of the figure), the control valve 33
A filling head 29 with an extendable filling nozzle 31 is placed above an empty bottle 11 of the same construction as shown in FIGS. 1-4. In the second step, the extensible nozzle 31 is lowered to a position where its bottom is within the neck 17 of the bottle 11 , but the introduction of the granular heavy detergent into the bottle has not yet begun. The next step shows the filling of granular detergent 19 into the bottle 11 , the height of the detergent particles being within the height of the handle opening into the main interior of the bottle, as indicated by position 35 . point, while in the channel 25 of the handle 15 of the bottle it is at a lower height 37 . In the fourth stage, the height of the granular detergent increases further,
Higher than the top of the passageway 25 , the granular detergent 19 fills the passageway and forms a positioning surface 39 approximately at the same height as the particles within the main interior of the bottle. In the fifth stage, particles
The nozzle 31 is filled up to a final filling height 41 of 19 , and the nozzle 31 is pulled up in the sixth stage. The next step in the fill and seal operation (not shown) is to cap the bottle either automatically (preferably) or manually.

The bottle used as the container for the product of the invention is one that allows easy dispensing of the granular heavy duty detergent and may be made of any suitable material of construction, but may be made of synthetic organopolymer plastic material, such as polyester. Preferred are vinyl chloride, polymethyl methacrylate, polyethylene terephthalate, polyethylene, polypropylene, polystyrene and polyester (preferably reinforced with glass fibers), and nylon. Glass bottles can also be used. The bottles used are preferably transparent, but it is also within the scope of the invention to use opaque or translucent plastics.
An important advantage of the bottle materials described above is that they have relatively thin walls, i.e., are essentially to completely water resistant even with a thickness of approximately 1 to 3 mm, and are typically impermeable to organic volatile substances (e.g. perfumes). This means that it becomes a barrier.

Bottles can take a variety of shapes, but unlike jars and other containers, they have a neck that is narrow compared to the average cross-sectional area of the bottle body and has a small opening or passageway therein. Generally its cross-sectional area is less than 40% of the average bottle cross-sectional area, preferably
It is less than 30%, more preferably less than 25%. For ease of pouring and good control of dispensing, the cervical passageway should be between 2 and 40 cm ² , preferably between 3 and 40 cm 2 .
It has a cross-sectional area of 20 cm ² , more preferably 5 to 15 cm ² . The neck is normally oriented so that its passageway and walls are parallel to the vertical axis of the bottle, but it can also be tilted (usually within 30° from the vertical axis, but can also be tilted further). be). The neck size depends in part on the bottle capacity and on the size of the cap desired for dispensing the detergent composition. I will say more about this later. 17 For auto or one size bottles, a neck height of 1 to 5 cm can be used, but usually 1.5 to 3 cm.
For larger sizes like 1/2 gallon, 2, and 1 gallon 4 bottles, the neck should be 1 to 5 cm.
High, preferably 2-5 cm high. When the bottle has the illustrated configuration with its improved configuration, other bottle dimensions are adjusted according to bottle capacity.

Although a variety of configurations and cross-sectional shapes can be used for the bottle, the most preferred cross-section is one that is substantially oval, and the bottle illustrated in the accompanying drawings falls within this category. In some cases, it may be desirable to cut such an egg-shaped round mirror surface into a square, and such a shape cut into a square is also considered to be oval in this specification and is included in the definition of oval. Instead of an oval cross-section, other curved shapes can also be used, such as a ring, an ellipse (included in the oval), a regular polygon, for example a rectangle with rounded corners, a square. The use of any such shape is within the scope of this invention.

Although not a necessary requirement for some embodiments of the invention, an important feature of a bottle with which the detergent compositions of the invention can be "combined" is that the bottle is often blown or otherwise molded. It is an integral hollow handle that is appropriately molded into the neck and main body. The interior of this handle communicates with the other interior of the bottle so that granular detergent can be loaded into the interior of the handle and flowed out of it. The handle is usually located on the side of the bottle away from the neck or spout and often does not protrude beyond the normal bottle wall.
In other words, the handle is not an appendage to the bottle; the handle and its opening are formed by "removal" of material within the general outline or silhouette of the bottle. The handle need not have regular cross-sections or internal passages, although substantially regular or uniform passages are preferred. The hollow handle has at least one section with an internal cross-sectional area in the range from 1 to 10 cm ² , preferably from 2 to 5 cm ² . Typically, the handle has a convenient length for easy gripping, and this length has been found to be approximately 8-12 cm, preferably 9-11 cm. A hollow handle section of such height is easily filled with the free-flowing, high bulk density, dust-free granular detergent of the present invention, which easily flows out of the section upon dispensing. From this point of view, it is advisable to have a free height of at least 1 cm, preferably at least 5 cm, higher than the neck of the handle channel and between the desired filling height of detergent particles and the head of the handle channel; A height of up to 10-15 cm is useful. The angle of inclination of the wall 16 is greater than or approximately equal to the normal resting angle of the granular detergent after deposition, during filling or after dispensing, thus facilitating the filling of the handle passageway and its discharge therefrom.

The granular detergent inside the bottle has improved flowability,
It has a high bulk density and a particle size distribution that facilitates flow and evacuation to minimize bridging tendencies within the container or within confined areas thereof. The particle detergent composition consists of a synthetic organic detergent and its builder,
It can also, of course, include various adjuvant materials that are normally present and desirable in detergent compositions, but which do not have properties that render the composition ineffective for the purposes of the present invention.

The synthetic organic detergent may contain any suitable anionic, nonionic, cationic, or amphoteric surfactant, but among these, anionic substances and nonionic substances are very preferable, and are suitable for the composition of the present invention. In this case, the nonionic type is most suitable. Generally, cationic detergents are excluded from the products of this invention. This is especially true when anionic detergents are used. Nonionic detergents are preferred, but in some cases mixtures of nonionic and anionic detergents are preferred.

Nonionic detergents may be liquid or semi-solid at room temperature and are typically liquid or viscous at temperatures slightly below 40°C. Nonionic detergent is about 5 to 30
Preferably, but not limited to, straight chain or branched chain (straight chain preferred) ethoxylated aliphatic alcohols having from about 8 to 22 carbon atoms having ethylene oxide units/molecule. A particularly suitable nonionic organic detergent of this type is manufactured by the Schiel Chemical Company and sold under the trade name Neodol. Among the Neodolls available, Neodoll 25-7 (average 7
fused with ethylene oxide units
C _12-15 higher aliphatic alcohol) and Neodol 45
~11 ( _C14-15 higher aliphatic alcohol condensed with an average of 11 ethylene oxide units) is particularly preferred. Another group of suitable ethoxylated fatty alcohol detergents is manufactured by the Continental Oil Company under the trade name Alfonic, the most preferred of which is Alfonic 1618-65, which is
It is a mixture of _C16-18 primary alcohols ethoxylated to contain 65 mole percent ethylene oxide.

Another example of a nonionic synthetic organic detergent is BASF
It is sold by Wyandotte under the trade name Pluronic. Such compounds can be produced by condensation of ethylene oxide with a hydrophobic substrate formed by condensation of propylene oxide and propylene glycol. The hydrophobic part of the molecule has a molecular weight of about 1500-1800, and adding polyoxyethylene (i.e. polyethylene oxide) to this part increases the overall water solubility of the molecule, and detergents are made with a polyoxyethylene content that is based on the total weight of condensed organisms. It remains liquid at room temperature until about 50%, and becomes solid at about 50%. Another useful nonionic detergent is a polyethylene oxide condensate of alkylphenols, such as alkylphenols in which the alkyl group contains about 6 to 12 carbon atoms in a straight or branched chain configuration and 5% per mole of alkylphenol.
It is a condensation product of ~25 moles of ethylene oxide. The alkyl group in the alkylphenol can be derived from polymerized propylene, and can also be, for example, diisobutylene, octene, nonene.

Typical anionic detergents are natural or synthetic C _5-20
Higher fatty acid soaps derived from higher fatty acids or their triglycerides, such as coconut oil, tallow, hydrogenated coconut oil, hydrogenated tallow and mixtures thereof; having 10 to 18 alkyl groups, preferably 12 to 18 alkyl groups;
Linear alkylbenzene sulfonates with 15 carbon atoms, such as linear sodium tridecylbenzene sulfonate; paraffin sulfonate; olefin sulfonate; and other organic sulfonates and sulfates (usually one C A lipophilic group containing _10-18 carbon chains is present). The various nonionic compounds described can be converted to anionic compounds by sulfation or sulfonation (usually the former) at the terminal hydroxyl group, in which case usually steps are taken to produce the initial nonionic condensation product. 3 as the proportion of ethylene oxide used is reduced.
~12 moles, preferably 5 to 10 moles of ethylene oxide are present per mole of anionic detergent.

The various anionic detergents mentioned above are preferably used as Na salts, but K salts and possibly small proportions of ammonium salts and triethanolamine salts can also be used.

Typical cationic detergents also usually have fiber softening properties and antimicrobial properties, which are particularly characteristic of quaternary compounds. Examples of such substances are distearyldimethylammonium chloride and 2-heptadecyl-sulfate.
1-Methyl-1-[(2-stearoylamido)ethyl]imidazolinium methyl. A variety of amphoteric detergents can also be used, and these generally contain cationic substituents such as amino groups that have been quaternized (e.g. with lower alkyl groups) or condensed with lower alkylene oxides (e.g. ethylene oxide). These are higher aliphatic carboxylates, phosphates, sulfates or sulfonates which may have a lower alkyl chain extended at the amino group site. Typical commercially available water-soluble amphoteric organic detergents are Deriphat 151 (sodium N-coco-β-aminopropionate manufactured by General Mills. Inc.) and Milanol.
C2M (MiranolC2M) (acid anhydride) [Miranol Chemical Company.inc]
Made in Japan.

A detailed description of various suitable detergents, including a description of the detergent groups to which the above detergents belong, is available at
Mc Cutcheon’s “Oetentents and
Emulsifiers," 1973 edition, and Schwartz, Perry and Berch, "Surface Active Agents," Volume (Interscence Publishers, 1958).

It is highly preferred that the builders in the compositions of the invention are inorganic substances, and among these the water-soluble salts, especially the phosphates, are highly preferred. However, organic builders such as sodium citrate, sodium gluconate, trisodium nitrilotriacetate, and other organic builders that are known to have builder activity and can be ingredients in free-flowing built detergent products. Compounds can also be used, often in admixture with inorganic substances. Usually the organic compound is present as a salt of Na or other alkali metal, but sometimes the free acid form can also be used. Although phosphates are highly preferred for producing exceptionally free-flowing, high bulk density granules containing large amounts of synthetic organic detergent (preferably post-added to the phosphate base beads), Other inorganic materials such as silicates, borates, carbonates, bicarbonates can also be used as builders alone or in combination with phosphates. Ion exchange clays such as type A (preferably 4A) or other suitable molecular sieves which act as builders in detergent compositions and also remove hard water ions from wash water are also used as builders, preferably with suitable phosphates. However, for non-phosphate detergents it can be used alone or with other non-phosphate builder salts in conjunction with other ion-exchange zeolites.

Regarding the phosphates and other inorganic water-soluble builder salts used, Na salts are usually used, but K
Salt also helps. Specific examples of phosphate builder salts are pentasodium tripolyphosphate and other sodium tripolyphosphates (trisodium tripolyphosphate, trisodium phosphate, disodium phosphate, monosodium phosphate, tetrasodium pyrophosphate, disodium pyrophosphate, etc.). be. Although these corresponding K salts can also be used, they are preferably used in combination with Na salts.

Preferred other builder materials are alkali metals which provide anti-corrosive properties to the detergent compositions of the present invention and which also serve to form builder beads desirable for overspraying or post-spraying onto the surface of the synthetic organic detergent liquid. silicates, typically about 40 to 60
It is supplied in the form of an aqueous solution containing silicate solids, typically about 50% by weight. Preferably, the silicate is sodium silicate;
The _Na2O : _SiO2 ratio is usually from 1:1.6 to about 1:3.4, preferably from 1:2 to 1:3, most preferably about 1:
The ratio is 2.35 to 1:2.4.

In addition to the synthetic organic detergent and builder components, various adjuvants can be present in the detergent compositions of the present invention and are usually spray dried (when they are heat sensitive) with the clutch materials particles. It is preferable to formulate them in a particle structure by post-addition. These adjuvants include common functional and aesthetic materials such as bleaching agents, e.g. sodium perborate; colorants, e.g. pigments, dyes, fluorescent brighteners; fragrances; foam stabilizers, e.g. lauryl myristyl diethanolamine. alkanolamides, such as enzymes, e.g. proteases, amylases; skin protection and conditioning agents, e.g. low molecular weight water-soluble proteins obtained by hydrolysis of proteinaceous substances such as animal hair, back hair, gelatin, collagen; foam-breaking Agents such as silicones; fabric softeners such as ethoxylated lanolin; disinfectants such as hexachlorophene; buffers such as alkali metal acetates and bisulfates; and flow improvers such as powdered clay. Additionally, filler salts such as sodium sulfate (usually anhydrous) and sodium chloride may be present, but are usually best avoided.

The builder detergent composition particles of the present invention typically contain about 50-98% builder, with the remainder of the synthetic organic detergent being water, ignoring the presence of all other materials. Considering the presence of other substances in the product,
Products typically contain 30-80% builder, 2-35% to 40% synthetic organic detergent, (excluding fillers) 0-20%
% adjuvant, 0-50% filler (preferably excluded) and 3-15% water. The granular detergent may be manufactured to meet the above specifications by any suitable means, including spray drying of heat-stable materials, but with the highest flowability, lowest dustiness, highest bulk density,
In order to minimize undesirable chemical reactions and degradation, base beads consisting essentially of builder alone (preferably with or without water) are prepared and treated with liquid nonionic or anionic detergents. Post-addition of detergents, such as mixtures with nonionic detergents (sometimes it is preferred to spray dry anionic detergents with builders) is preferred. Typically, when detergent particles are made by this preferred method, about 60-98% by weight of the basic beads are detergent builders with a porous exterior surface and a skeletal interior structure, and about 2-40% by weight are prepared at temperatures below 40°C. A synthetic organic detergent material is incorporated into the bead such that the outer surface of the bead is substantially detergent-free and therefore free-flowing. In a preferred embodiment of the invention, the granular detergent composition has a
95% basic beads are composed of 5-30% synthetic organic detergents, which consist of about 45-85% phosphoric acid builder salts, about 5-15% alkali metal silicates and about 5% synthetic organic detergents.
~15% water. In a highly preferred embodiment of the invention, the synthetic organic detergent contains about 8
Polyethoxylated nonionic detergents such as those derived from aliphatic alcohols containing ~22 carbon atoms by condensation with about 5 to 30 moles/mole of ethylene oxide. Preferably, the phosphate salt is a mixture of hydrated and anhydrous salts, hydrated phosphate (usually pentasodium tripolyphosphate hexahydrate) and anhydrous phosphate (usually anhydrous pentasodium tripolyphosphate hexahydrate). ) is about 0.3~0.7, preferably 0.4~
It is within the range of 0.6. Regardless of how the granular detergent is manufactured, to make the bottled product of the present invention, the final detergent product must contain at least
Clean, dry sand with a particle size such that 90% of the particles pass through an 8-mesh screen of the American Sieve Series and are retained on a 200-mesh screen, and a bulk density of at least 0.5 g/cc. It is important to have a liquidity of at least 70%. Preferably, at least 90% of the detergent composition passes through a 20 mesh screen and is retained on a 200 mesh screen, and at least 95% of the detergent composition passes through a 20 mesh screen and is retained on a 200 mesh screen.
More preferably, less than 0.5% passes through the 200 mesh sieve. The bulk density is preferably in the range 0.55 to 0.8 g/cc and the fluidity is preferably at least 75% of clean dry sand and may be close to or equal to 100%.

Particles are normally dust-free, so even after shaking them in a transparent container, the interior of the container higher than the particles will disappear after a short period of 1-2 seconds after shaking has stopped. It is clear and there are no particles attached to the inner wall of the container. This desirable dust-free property is due in part to the formulation of nonionic detergents, which are typically present in sufficient proportions to immobilize dust and prevent dust generation from particle movement. For example, in many cases, the amount of nonionic detergent used is
12 to 40%, sometimes as high as 20 to 25 to 40% of the final product, which can be absorbed into the interior of the detergent particles without making the surface sticky or low-flowing. Representative nonionic detergents which are particularly preferred to be used are condensation products of aliphatic alcohols with a C _10-18 carbon chain with 6-14 mol/mol of ethylene oxide, in this case especially at 20-40%. When present in a detergent composition, the proportion of particulate detergent passing through a 200 to 325 mesh screen is often zero. The presence of more absorbent detergent in the granular product, resulting in a higher bulk density product, allows for the use of smaller amounts of product per wash load, thereby making it easier to load into the bottle, and Naturally, it would be easier to dispense smaller amounts of detergent and measure it with a bottle cap.

If dust is generated, even if the amount is very small, coat the inner surface of the bottle with a thin layer of silicone or a quaternary ammonium salt as mentioned above, or both, to smooth the inner surface of the bottle. It may be desirable to promote the dispersion of electrostatic loads on the inner surfaces, thereby avoiding the adhesion of particulates to the inner surfaces of the bottle. Typically, the amount of such material used is sufficient to form a thin layer on the inner surface of the bottle, often only 1 to 10 molecules thick.

Bottle caps may be of any suitable construction and material, but screw caps are preferred because of their ready availability, ease of sealing, and ease of metering. However, since the contents are particulate solids rather than liquids, a perfect leak-tight seal is not always necessary, and other types of caps that do not have the sealing force of regular screw-on caps may be used. For example, a cap that is press fit in place may be used, and may have a slide valve mechanism to open the dispensing passageway. In this case, as well as in other cases, the neck can be flatter than the screw-on cap, and can also be a spout in the bottle wall. The cap may be made of any suitable material such as synthetic organic polymer plastic, rubber (especially hard rubber), metal, alloy, or the like. Useful synthetic organic polymers include melamine formaldehydes, phenol formaldehydes, nylon,
Mention may be made of polystyrene (obtained from dense or expanded beads), glass fiber reinforced polyester, polypropylene, polyethylene.

Preferred internally threaded caps form a leak-tight seal with the neck of the bottle when screwed in place to prevent loss of contents, prevent moisture and other foreign contaminants from accessing the contents, and prevent moisture from leaving the bottle. Prevent penetration. Thus, because of the screw-on construction and barrier properties of the bottle, an effective and inexpensive seal is obtained without the need for special barrier liners or coatings on permeable containers commonly used to package detergent powders. Additionally, although the cap is relatively small, it can be used to meter the desired amount of detergent particles of the present invention. However, as a practical matter, screw-on caps sized to help seal the mouths of bottles of useful sizes (e.g., 1 quart to 1 gallon; 1 pint bottles can also be used) are not suitable for automatic washing for a single wash. One cap, or even four caps, will not be large enough to fill the normal detergent particle capacity that must be used in the machine. That is,
For a typical spray-dried detergent powder having a bulk density of about 0.3 g/cc, with a small percentage of nonionic detergent post-sprayed on its surface, about 90 g or 300 c.c. of detergent particles can be washed in 17 gallons. It has to be placed in a tank, whereas a typical bottle cap has a capacity of only 5 to 15 c.c. Therefore, even if the capacity is 15 c.c., such low-density "normal" powder detergent must be measured using a cap 20 times, which is not acceptable to housewives, who also use a normal measuring cap. There would be no advantage to pursuing this method instead. but,
With the method of the invention, such weighing is possible using packages with only slightly larger caps. By increasing the amount of detergent (e.g. liquid non-ionic detergent) that can be incorporated into the beads of the present invention, it is possible to halve the amount of detergent product required per wash load, resulting in higher bulk densities (e.g. 0.6 The other half of the requirement is met by the use of beads. That is, by simply making the cap slightly larger so that it has a capacity of about 20 c.c. instead of 15 c.c., one regular load of toploading type can be obtained by measuring 4 caps of detergent powder. of laundry, and in the case of sideloading (usually about half the amount of detergent used in the former case) a two cap metering is sufficient. Furthermore, by adjusting the bulk density of the product, its synthetic organic detergent content, and the cap size, it is possible to use as little as 1 cap or as much as 3 caps of detergent per wash. Thus, the present invention provides a convenient method for easily metering bottled granular detergent in a bottle cap to provide a desired amount of detergent composition for a single typical wash load.

Methods for producing free-flowing, high bulk density granular detergents of desired particle size are well known to those skilled in the art and can be used in the present invention. For example, controlled spray drying, spray cooling, agglomeration, solidification, anti-friction crystalline materials, etc. have been previously described and are useful. The nonionic detergent may be included in the base particles and have the desired rounded structure sufficient for the particles to be free-flowing, and any liquid or sticky detergent may be contained within the interstices rather than on the surface of the particles. As long as it retains the material (usually less than 20%, preferably less than 10% is present on the surface) it can be integrally formed with the particle. After manufacture, the detergent particles are filled into the bottle and capped by a method such as that shown in FIG. 8 or an equivalent method, although other, more complex and less filling methods may also be used. The shelf life of the product after sealing in the bottle is almost unlimited, in fact in most cases for at least three years without any undesirable changes.

The product of the invention has a number of advantages, many of which have already been mentioned. Relatively inexpensive and readily available containers with integrally molded hollow handles can be used with conventional sealing means to provide a product with excellent storage properties. The particles are attractive because of their round, uniform shape and flow like a liquid. They weigh in relatively small caps and are dense enough to contain the amount needed for multiple washes (about 10-20 washes per quart, usually about 12 washes) in a reasonably sized bottle. . Commercially available liquid detergents can be used only eight times per quart (these numbers are for top-loading washing machines). Additionally, the cap can be graduated to allow for even finer measurements. The products are easily manufactured and can conveniently incorporate normally heat-labile ingredients. Also, during storage, it is highly stable due to the fact that it is not in a liquid phase. For this reason, specific cleaning ingredients that are typically less stable, but highly effective, can be included in the formulation.

The following examples illustrate the invention:
It is not limited. Unless otherwise indicated, all parts herein are by weight and all temperatures are in °C.

Example 1 14.5 parts of pentasodium tripolyphosphate powder (anhydrous), 15.2 parts of sodium silicate (Na ₂ O:SiO ₂ =
An aqueous slurry consisting of 1:24) 50% aqueous solution and 21 parts deionized water was prepared. Approximately 60% of this slurry
℃ and mixed well in a crutcher to form pentasodium tripolyphosphate hexahydrate salt. The preclutching mix thus produced was then heated to 88°C and maintained between this temperature and 93°C to prevent hydration of the anhydrous sodium tripolyphosphate powder that was then added. A total Klutchyer Mix was then prepared by adding 28.3 parts of pentasodium tripolyphosphate powder (anhydrous) and 21 parts of deionized water at a temperature within the range of 88 DEG to 93 DEG C. described above. The product mix is approximately
It contained 45-50% solids by weight.

The clutch mixture was pumped through a counter-current spray drying tower (8 feet high) using a Whirljet 15-1 spray nozzle at a manifold temperature of 82°C and an absolute pressure of about 54 Kg/ ^cm2 (about 750 psig). dry air (initial temperature when entering the spray tower is approximately 315
℃).

The spray-dried elementary beads produced have internal structure and external surface characteristics similar to the beads shown in FIGS. In contrast to spray-dried detergent beads, they are irregularly structured round solids with a spongy porous outer surface and a skeletal internal structure.

The spray dried base beads are 77% sodium tripolyphosphate, 13% sodium silicate, and 10%
Contains water. Its bulk density is 0.55g/cc,
The fluidity is 86% of that of dry sand and the product is completely non-stick. Sieve (American Sieve Series)
According to the analysis, No. 20 on 1%; No. 20 passed;
No.40 on 19%; No.40 passed, No.60 on 50%;
No.60 passed, No.80 on 20%; No.80 passed, No.100
On 6%; No.100 passed, No.200 on 3%;
1% passed No.200;

The basic beads were introduced into a batch rotary drum blender and post-sprayed with Neodol 25-7 and small amounts of colorants, fragrances and brighteners at 49°C, resulting in 78% basic beads and 19.7% Neodol 25-7. A final product consisting of 7% and 2.3% minor components was produced. In other experiments, liquids (Neodoll 25-7 and minor ingredients, or water-soluble or aqueous dispersions thereof) were mixed in a Patterson-Kelley twin shell and Zig blender.
The mixture was sprayed in the form of microdroplets or mist onto the surface of the oscillating elementary beads in Zag blenders.

The bulk density of the obtained product was 0.68g/cc, and the fluidity was
79%, and was completely non-adhesive. According to American Sieve Series, No.20 on 1%; No.40 on
20%; No.60 on 52%; No.80 on 20%; No.100
On 5%; No.200 on 2%; No.200 passing 0%;
was analyzed.

The final product obtained after only 10 minutes of mixing was filled at room temperature into bottles of the type shown in Figures 1-4 in the manner shown in Figure 8. The bottle is made of clear PVC and has a capacity of approximately 2
(1/2 gallon). They were gravity filled with product without difficulty. The average filling time was about 5 seconds or less per bottle, and hollow handles were also filled without problems. After filling, the bottles were appropriately mechanically capped and the manufactured product was packed into cases and sent to storage. Based on past experiments and tests on storage of heavy duty detergents, the manufactured product has a shelf life of over 3 years.

It takes 75 c.c. to reach 0.075% concentration in 17 gallons of laundry.
detergent is sufficient, which is approximately 5 cm in diameter and 4 cm in height.
With a cap of cm, the diameter is 4 cm and the height is 3 cm.
I was able to measure it twice using a cm cap. The former cap size was used in the bottles illustrated and described herein.

A normal laundry load (approximately 9 pounds) using detergent in a 17-gallon tank loading washer.
Good results were obtained by washing. Similarly, laundry was effectively cleaned when half the amount was used in a front-loading washing machine. During use, the product flowed freely from the bottle and from the handle hollow, but did not spill as easily as a liquid would, and did not leave an undesirable gel or cement-like coating on the bottle cap threads.

The products produced were attractive and some or all of the particles involved could be colored by known methods, for example by post-spraying some of the particles with a dye.

Instead of producing detergent composition particles by the method described above, a product having the same bulk density, particle size and flow properties, and also being non-stick, is used in the art for producing granular detergents. A useful bottled granular detergent having the desirable cleaning properties described above was obtained when manufactured by the spray cooling, agglomeration, and attrition methods described above. However, products made by the methods described earlier in this example appear to be superior to products made by these methods, and are generally more attractive and free-flowing than other products of the same composition. It also had a high bulk density.

Example 2 A product similar to that of Example 1 was mixed with 25 parts of hot water (60°C) in essentially the same manner as in Example 1.
Hydrate the phosphate using a clutcher primer of 3.5 parts sodium silicate solids and 13 parts pentasodium tripolyphosphate powder (anhydrous) and mix the slurry well in a vessel with a steam jacket. The hexahydrate was then heated with steam to 93°C, and then in a clutch mixture at this temperature, 13 parts of anhydrous pentasodium tripolyphosphate powder, 25 parts of water and a further 13 parts of anhydrous pentasodium tripolyphosphate were added. Powder and 7.5 parts of anhydrous sodium carbonate were added. During mixing, the temperature was not allowed to fall below 82°C to prevent hydration of the anhydrous pentasodium tripolyphosphate that was then added. The mix was sprayed at an absolute pressure of 57 Kg/cm ² (800 psig pressure) into a spray tower with an inlet dry air temperature of 343°C and an outlet air temperature of about 113°C. The builder particles produced had a particle size distribution in which 90% by weight passed through a No. 20 screen (American sieve series) and 90% by weight was retained on a No. 200 screen.
78 parts of the spray-dried beads were then mixed with Example 1 while rocking in a tilted cylindrical rocker for about 5 minutes.
19.5 parts of Neodol 27-4 and
2.5 parts of minor ingredients (fluorescent brightener and fragrance) were oversprayed. The bulk density of the removed product is approximately 0.75
g/cc, flow value was 75%, and water content was approximately 5%.
This was filled into the bottle according to the method of Example 1 and tested for suitability as a heavy duty detergent according to the method described above. That should be extremely satisfying,
It was found to have the desirable properties previously reported for the other Example 1 products produced by a similar method.

Example 3 Following the methods of Examples 1 and 2, 13 parts of sodium tripolyphosphate hexahydrate, 26 parts of anhydrous sodium tripolyphosphate, 47 parts of deionized water, and 7.5 parts of sodium tripolyphosphate hexahydrate were added.
Basic beads were prepared from 1.5 parts organic builder "M" (Monsant Chemical Company) and 6.5 parts sodium silicate solid (Na ₂ O; SiO ₂ =1:2.4). 85 parts of the resulting spray-dried builder beads were sprayed with Neodol 45-11 (12 parts) and minor ingredients (fluorescent brightener and fragrance; 3 parts total). The resulting detergent passed the tests described in Examples 1 and 2 and was a free-flowing, dust-free, attractive, high bulk density laundry detergent with good detergent power.

Example 4 The experiment of Example 1 was repeated using Alphonik 1618-65 as the nonionic detergent to produce a final granular detergent product containing 30% nonionic detergent (with correspondingly reduced proportions of other ingredients). Obtained. The resulting product was an excellent detergent and the corresponding bottled granular detergent had excellent stability and use properties as described above.

Example 5 The experiments of Examples 1 to 4 above were repeated using different bottles and caps and granular detergent contents, and varying the proportions of the composition components by ±10%, ±20%, ±30%, except that The bottles were filled and capped in a variety of bottles made of different materials and constructions (but within the limits already mentioned), maintaining the proportions and ratios already mentioned. Products that were free-flowing, of high bulk density, and easily meterable in the caps used were easily manufactured, and the detergents contained therein were attractive and useful. Detergents and corresponding bottled products made by other manufacturing methods as previously described had the same detergent particle properties and were equally satisfactory.

The present invention relates to a new commercial detergent product, a bottled granular heavy duty detergent. The present invention does not have the problems associated with the use of liquids, and allows for the commercially acceptable use of granular heavy duty detergent powders in a manner similar to that of heavy duty liquid detergents, but without the disadvantages associated with the use of liquids. made possible for the first time. The bottles used are water resistant, increasing storage stability. They were attractive, relatively small, resealable, easy to handle, and allowed the use of powdered detergents (traditionally only liquids could be used, and this included the inherent disadvantages of liquids). (accompanied by). The concept of the present invention, the embodiment of this concept to produce commercially usable products with individual desired properties of various compositional ingredients, has significant benefits to the heavy duty laundry detergent industry.

Although the present invention has been described above using illustrations and examples, those skilled in the art can make substitutions and changes to equivalent means without departing from the present invention based on the description of this specification. should not be limited to these.

[Brief explanation of the drawing]

FIG. 1 is an enlarged side view of a bottled granular detergent product of the present invention. FIG. 2 is a top plan view of the product of the present invention. FIG. 3 is an enlarged side view of the product of the present invention, viewed from the handle side. FIG. 4 is a cross-sectional view taken along plane 4--4 of FIG. Figure 5 shows
5 is an enlarged side view of a portion of the head of the product of FIGS. 1-4 with a seal cap attached; FIG. Figure 6 shows
Figure 2 is a photomicrograph (200x magnification) of the main part of the spray-dried builder beads or particles before the synthetic organic detergent is post-sprayed onto the surface. FIG. 7 is a micrograph (2000x magnification) showing the broken part of the bead in FIG. 6. FIG. 8 is a partially enlarged layout view of a filling means for filling a bottle with a free-flowing granular detergent composition. 11...Bottle, 13...Bottle body, 15...
... Bottle handle, 17 ... Bottle neck, 19 ... Granular detergent composition, 21 ... Channel, 23 ... Bottle main interior, 27 ... Cap, 29 ... Filling head, 31 ... Stretchable filling nozzle, 33...Control valve.

Claims (1)

[Scope of Claims] 1. A bottled granular laundry detergent consisting of a transparent bottle having a neck for dispensing detergent and a cap sealing the neck, wherein the bolt is made of an essentially water-resistant synthetic organic polymeric plastic with thin walls. , the neck is provided at the top of the bottle, adjacent to one side, the passageway has a cross-sectional area of less than 40% of the average cross-sectional area of the bottle, and the neck passageway has a cross-section of about 2-40 ^cm2. The bottle has an area of about 1-10 cm 2 , and the bottle is provided with an integral hollow handle on the opposite side of the bottle where the neck is provided, the interior of the handle communicates with the interior of the bottle, and the handle has an area of about 1-10 cm ² . having an internal cross-sectional area in the range, the handle is free-flowing in the bottle;
granular detergent pourable through the handle and the neck, the particles comprising about 2-40% by weight of a synthetic organic detergent selected from the group consisting of nonionic detergents and mixtures of nonionic and anionic detergents; and about 60-98 wt. selected from the group consisting of at least one sodium salt of carbonate, phosphate and silicate, the particles having at least 90% passing through an 8 mesh screen and passing through a 200 mesh screen (US sieve series). of a size maintained, have a bulk density of at least 0.5 g/cc, have sufficiently high flowability that the detergent flows freely from the neck of the bottle and the handle, and the particles are substantially The bottled granular laundry detergent is dust-free so that after pouring out some of the composition from the bottle, the bottle and the interior of the bottle above the level of the granular detergent composition return to clarity. 2. the cervical passageway has a cross-sectional area of about 3-20 cm ² , the organic detergent typically contains about 5-30% by weight of a sticky ethoxylated nonionic detergent, and the bulk density is about 0.55-
0.80 g/cc, and the laundry detergent and the sealed cap are adapted such that one or two cups of granular detergent is sufficient for a typical washer load. Contains granular laundry detergent. 3. The bottled granular laundry detergent contains at least about 12
A bottled granular laundry detergent according to claim 2, comprising % by weight of said nonionic detergent. 4. The bottled granular laundry detergent contains approximately 5-30% by weight.
4. The bottled granular laundry detergent according to claim 3, wherein the nonionic detergent is a polyethoxylated aliphatic alcohol or a polyethoxylated alkylphenol. 5 The bottled granular laundry detergent contains at least about 20
A bottled granular laundry detergent according to claim 4, comprising % by weight of said nonionic detergent. 6. The bottled granular laundry detergent of claim 5, wherein the granular detergent has a fluidity of about 70% or more. 7. The bottled granular laundry detergent of claim 6, wherein the bulk density is at least about 0.6. 8 the neck is threaded and the cap, when filled, contains about the same amount, about 1/2 amount, about the desired amount of granular detergent composition to be used to wash laundry in the washing machine; A bottled granular laundry detergent according to claim 1, which is a screw cap sized to measure 1/3 or about 1/4 of an amount. 9. The detergent builder is in the form of beads with a porous outer surface and a skeletal internal structure, and the synthetic organic substance is liquid or sticky at temperatures below 40°C, and the synthetic organic detergent is incorporated inside the beads. 2. A bottled granular laundry detergent as claimed in claim 1, wherein the outer surface of the beads is substantially free of the detergent. 10 The bottled granular laundry detergent is 70-95% by weight.
of basic beads and 5-30% by weight of a synthetic organic detergent, the basic beads comprising about 45-85% by weight of a phosphoric acid builder salt, about 5-15% by weight of an alkali metal silicate, and about 5-15% by weight of an alkali metal silicate. A bottled granular laundry detergent according to claim 9, comprising % by weight of water, and wherein the synthetic organic detergent is a nonionic polyethoxylated detergent.