DE1492841A1 - Free flowing, coated, particulate compositions and processes for their preparation - Google Patents

Description

B JiRLIN-Friedenau. i „- uäWQ ΒΙΚΓΗΚί ■ Pienzenauerstr. 2

(.aufersfraße 37 D Γ.- I Π g. Π A IN O K U O * -Π IVC patient attorney Grentzenberg

SÄ | ng.K.GRENTZEN

FATHER LAWYERS Bank account: -. ' ■ Bank accounts Bank for trade and industry ^ _1. , - - _n __ _and «" Dresdner Bank Deposit box 4 ___, - | Munich Berlin-Friedenau T ~ X ^. Li ^ rWI Dep.-Kassel Leopoldstrasse

sä ² ■ DrfcxpM

'■■■■■ P 440

The Pillsbury Gompany, Minneapolis, Minnesota, Y.St ₀ A ₀

Free flowing, coated particulate mixtures and Process for their manufacture

The invention relates to products existing by converting from a solid and a liquid phase mixtures or ₀ products in free-flowing, non-caking, easy dispersible agglomerates and consist of solid, coated with the originally liquid phase particles, as well as processes for their preparation " ,

The method according to the invention can be applied to any desired combination of a solid phase with any desired liquid phase, regardless of whether the products are naturally occurring, whether heterogeneous components are to be combined with one another or whether there are two or more products In any case acted practically dry, free-flowing stable products are obtained "Thus, the starting materials can or" solvent mixtures from which agglomerated products of the invention are produced initially, for example, _o

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in (1) granular form, whereby the individual grains consist of solid particles "which are coated with a liquid phase - such as a viscous syrup - (2) in the form of a practically solid, compact mass or _a caked mass (mass suite) of solid, in a viscous or syrupy liquid _o G-round mass embedded particles, which can then be transformed into an unstable, non-free flowing texlchenförmiges product, and (3) in the form of a physical mixture of a liquid and a solid substance

| present »

The solids / liquid starting mixture can also be prepared by mixing a liquid with a Peststoff and casting into blocks, which are then Z B are ₀ accommodated by grinding to particle shape and agglomerated _0, or be made from normally liquid products in a solid-liquid form can be transferred, which contains all the essential components of the original liquid and is comminuted and agglomerated in particle form. Typical examples are given below

"specified ,,

Under the term "liquid phase" or "liquid" as used herein, any liquid (flowable [but not gaseous]) or plastic substance that forms a permanent coating or "film" the solid particles can be sprayed on or deposited on them, whereby viscous or syrupy liquids, oils,

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Fats and the like are included. The term "liquid Phase "also includes water, fats, oils, or any other solvents in which substances such as vitamins, pharmaceuticals or other soluble substances are dissolved, as well as Liquids in which solid particles are dispersed «. However, the term does not include liquids of relatively high volatility under normal conditions evaporate and no coating or lilm on the solid Particles would be left behind as well as accidentally absorbed Humidity.

The liquid phase of the starting material, with which the solid particles which are to be present in the agglomerated products, are coated, can be non-crystallizable or not convertible into the solid state and on the individual coated particles from which the agglomerated end products exist, remain in liquid form, or after the formation of the coated particles can lose all of their solvent or liquid properties, whereby the particles from which the agglomerated products according to the invention consist, with the solid constituents of the originally liquid phase in a practically dry, are coated in a solid form »

Mixtures of this type have certain disadvantages or undesirable properties that limit their usefulness and / or manageability. These mixtures are fickle, flow, not free and, moreover, are often due to it

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characterized in that they baked into hard masses or only slowly dispersed and dissolved in a liquid can be.

The invention therefore relates very generally to novel products made from the aforementioned solid-liquid mixtures are produced and have improved properties, and which are characterized in that they are resistant, are free flowing, non-baking and rapidly dispersible and dissolvable in a liquid.

Furthermore, novel processes are proposed according to which these solid / liquid mixtures are agglomerated Products with the aforementioned properties can be converted and that allow these mixtures economically on a large scale with a minimum of pollution and the resulting decommissioning the equipment for cleaning or restoring the operational condition are handled and processed can.

The agglomerates according to the invention can generally be made up of loose, nested grapes from very small individual particles, which practically only touch at individual points, are described consisting, whereby there is one Liquid as a result of the numerous gaps and spaces in the agglomerates is allowed to form the agglomerate rasoh to penetrate and quickly every particle of the agglomerate to reach, disperse and bring into solution,

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OWGlNAL INSPECTED

whereby in most cases a product is obtained, which can be described as "instantly" wettable, dispersible and dissolvable.

The individual particles of the agglomerates preferably consist of the originally solid material that is in dust or Powder form is present, the powdery particles with a very thin film of the material or the substance, from which the originally liquid phase of the starting mixture consists, are coated. The coating or film in the agglomerated product according to the invention can be in liquid or non-flowable or solid form, if all or part of the solvent or liquid properties of the originally liquid phase have been lost are. The particles are arranged in a random manner to one another, which is why the agglomerates have a rough, Have irregular surface, which together with the relatively large grain size of the agglomerates Result in products that are free flowing and do not cake. So the particles of the agglomerate consist of one solid material of a certain composition that is permanent with a film - either a liquid or a solid, but applied as a liquid - with a are coated with different compositions, which is why the products according to the invention can be referred to as multiphase products.

The agglomerates according to the invention are further characterized

QBGlNAL INSPECTED

characterized as being free flowing, not caking, are friable and relatively uniform in structure and have a satisfactory appearance, wherein the liquid phase is evenly distributed over the agglomerates as a thin coating on the particles and not on individual points is present in high concentration.

Although the agglomerates are made from fine, powdery particles, when added to a liquid they do not agglomerate into practically impenetrable masses. By converting the finely ground dust-like particles into agglomerates, the advantages of the very small particle size are retained, which means that the particles can be dissolved quickly (and often immediately) in a liquid, since the speed of dissolution is inversely related to the particle size. _e h the dissolution rate increases with decreasing particle size while preventing the clumping or agglomeration to impermeable masses.

Even if the liquid phase in the agglomerates is quite viscous, the agglomerates are free-flowing and not caking. This is due to certain factors, such as the large dimensions of the agglomerates and the low layer thickness of the liquid film because of the distribution over all of the small solid particles, on that the Main amount of the liquid phase inside the agglomerates is

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ORIGINAL INSPECTED

finds, whereby their viscous properties have no influence on other agglomerates, and that most agglomerates have an irregular, rough shape, what leads to the fact that between the agglomerates in proportion to their size and weight only one little surface contact takes place and that the formation of a bond between the agglomerates that is strong enough is that the agglomerates do not crumble apart is prevented.

In the agglomerated ProdukW the original (solid and liquid phases are distributed thoroughly and evenly over the agglomerates, whereby all components of the agglomerates are uniformly when mixed with liquids and wetted immediately and go into solution and be dispersed rapidly in liquids.

The method according to the invention is general by dispersing a plurality of the aforesaid coated particles having adhesive surfaces and the dispersed particles coated with the sticky substance in tangled (random) contact with each other brings, whereby the particles then stick together and form the agglomerates according to the invention.

The formation of fine solid particles coated with a thin film of a liquid can affect any in a suitable manner. It is important that the liquid is in the form of a very thin film on the surfaces of the

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ORIGINAL INSPECTED

is sprayed on the solid particles _e In a preferred embodiment of the invention, this is achieved by a grinding or milling, the unagglomerated solids / liquid starting mixture is ground so zerkleinertoder regardless of its physical form such that the total surface of the solid phase or the solid Particles is greatly enlarged in order to distribute the liquid phase over a greatly enlarged solid surface. Preferably this will be to the point of apparent dryness

"carried out especially when using highly viscous liquids Find. If the solid phase is coated with the liquid phase before grinding, the grinding process becomes essential A decrease in the thickness of the liquid coating and a decrease in the apparent viscosity. That ground powdery material is usually very volatile. If this is the case, the invention should carried out agglomeration, in which the volatile coated particles are brought together and formed into persistent agglomerates

^ merged products are converted, connected almost immediately before the inconsistent, ground powdery material has a chance to cake together. the The first milling step is very important as it has been found that many solid / liquid mixtures do not can be successfully agglomerated into the desired product if not milled prior to the agglomeration step or be crushed »

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In some cases, however, the solid phase can first be crushed to the form of a dust, whereupon the fine particles then - e.g. by mixing with a Liquid in a mixer operating at high speed - coated with a thin film of liquid and eventually become agglomerated. It is recommended in the manufacture of the coated particles to be agglomerated that is, to sufficiently enlarge the total solid surface, so that the liquid can spread out into such a thin film that the coated mass practically becomes dry to the touch. On the size of the solid surface that the liquid is available, depends on the ratio of solid to liquid at which the substances are successful converted into coated particles and agglomerated. Conversely, determines the ratio of liquid to solid the minimum degree of fineness to which a given amount of the solid must be comminuted, whereby The larger the ratio of liquid to solid, the finer the particles have to be ground. The procedural stage, in which the liquid is applied as a thin film or the thickness of the film is reduced, alone is sufficient not enough to achieve a new and usable product, but is in connection with the subsequent agglomeration stage necessary so that the products according to the invention are obtained.

It has also been found in many cases

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It is preferable to carry out the above-mentioned milling or mixing under such conditions that a simultaneous drying of the liquid phase or a loss of solvent occurs. This allows the coated particles to be handled more easily and with less contamination of the apparatus used during the subsequent agglomeration stage; simultaneously can be applied in this way, larger quantities of the liquid phase to the solid particles and be incorporated into the agglomerates ultimately obtained _e drying and removal of solvent can be accomplished in any suitable manner, such as by grinding in the presence of excess air "

Except for those cases where the liquid is successfully applied as a thin film on top of what is already in the form of a dust present solids can be applied, it has been found that the liquid / solid mixtures that exist before the agglomeration were ground to the form of dust, manufactured agglomerated products are superior to such products are obtained from unground mixtures.

By distributing the liquid phase, Z ₀ Bo by grinding - preferably to a point of apparent dryness - over a large surface, the mixture to be agglomerated is melted into a state in which it can be handled during the agglomeration stage without excessive contamination of the apparatus can and in which the particles to be agglomerated are easily dispersed and then arbitrarily

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brought together to form porous, free-flowing agglomerates can be. In the case of some foods, the thinner liquid film changes and / or increases, such as it is achieved by the grinding process, the taste of the Starting material, as will be explained in more detail below.

As a result of the comminution of the material before agglomeration to the form of dust, agglomerates can be obtained which contain a very large number of these fine particles. Depending on the fineness to which the ' starting material was ground, and the following agglomeration process, the majority of the agglomerates according to the invention consists of about 5000 to 30,000 individual particles, the agglomerates as a whole having a size corresponding to 0.149-4.76 mm clear mesh size .

As a result of this large number of individual particles, which have been nested in a single agglomerate, the predominant part of the moisture changes as a result of the large solid surface exposed within the agglomerates g take place not outside, but inside the agglomerates. The comminution of the material to the form of dust also leads to the fact that the individual agglomerates acquire a very irregular, uneven outer surface and shape, especially when the individual particles are brought together at will, as described below. The irregular, uneven shape is essential contributes to the

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agglomerated products according to the invention free-flowing and are not caking.

The way in which a liquid phase located on a particle changes its layer thickness by grinding the solid and liquid phase - with the size of the solid particles or »the solid phase increasing the total surface is decreased so that the liquid phase can be distributed over a much larger surface - decreased is explained hypothetically in the following.

W A solid cube with an edge length of 0.127 cm should be assumed, on which there is a uniform syrup film with a thickness of 0.0254 cm, which completely covers the cube. If this hypothetical cube is divided into 125 cubes with an edge length of 0.0254 cm (approx. 250 Ii), the surface area is increased by 5 times compared to the original cube and the thickness of the syrup film is 0.00508 cm or 1/5 of that original thickness has been reduced.

^ Will use the same cube in 1000 smaller cubes

cut to an edge length of 0.0127 cm (about 125 Ii), so the total surface area is increased by 10 times compared to the original cube and the thickness of the syrup film is increased the original thickness by 10 times to 0.00254 cm decreased.

If the above hypothetical cube is converted into 125,000 smaller cubes with an edge length of about 0.00254 cm (or about

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; H92841

25 η t this value is in a range in which a particle of this size is no longer perceptible in the mouth), the total surface area is increased by 50 times compared to the original cube and the thickness of the syrup film to 0.000508 cm, ie reduced to 1/50 of the original thickness.

From these hypothetical considerations, it can be seen how much the thickness of the liquid film verrin- by milling of the coated with the liquid particles a may be siege and how / else a much thinner film on a highly elevated number νώη to this V smaller particles is produced. The value and importance of the milling process becomes even more apparent when one takes into account that in actual milling, the particles are not divided into cubes on flat cut surfaces. In reality, the smaller ground particles naturally have a very rough, irregular outer surface, which results in a much larger surface area than in the above explanations. Accordingly, the liquid film is many times thinner than in the above explanation.

To sum up, let me say once again that the Liquid film can be distributed by grinding the starting material and made to a very small thickness, the film thickness decreasing as the size reduction increases.

The grinding is to be applied to all solid / liquid starting materials that come into consideration within the scope of the invention.

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-H-

• rials applicable · The size up to which the starting material grinding depends on many factors, including the nature of the starting material and the intended use Intended use for the agglomerated product. In general, the more valuable the agglomerated product is the particle size is smaller, since the liquid film decreases and the rate of dissolution decreases with decreasing Particle size is increased. According to the invention, a depth Smaller size of 300 u or less preferred »For some of the foods and sugar products described below a particle size of 25-10Ou is preferable. For special purposes will have a particle size of 0.1 - 25 yes Recommended according to the invention, the whole range of 0.1-300 u is therefore preferred.

During the agglomeration stage, the powdery, coated particles are dispersed and then treated so that an adhesive surface is formed on the particles that is strong enough to be able to bind the particles together-P when they are brought into contact with one another will·

In a few cases, the surfaces of the milled coated particles are those after the milling step are already sufficiently sticky by themselves, so that the particles become after dispersion without any special treatment reunite. The particles can also be so hygroscopic that when dispersed in the ambient

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atmosphere absorb enough moisture so that your Surfaces become sticky. In such cases, the special treatment of the ground particles carried out to achieve the adhesive properties can be dispensed with. In most cases, however, the treatment carried out to form the adhesive layer is necessary to achieve successful agglomeration

laughs at the agglomeration of the coated particles the agglomerates can optionally be subjected to additional process steps, e.g. dried, cooled and sorted will·

It can be seen from the explanations at the gate, that the process according to the invention for converting τοη solid / liquid mixtures into stable, free-flowing, easily dispersible agglomerates is preferably carried out in such a way that fine solid particles are produced, them coated with a thin film of the liquid phase (such as by grinding the solid and the liquid together), disperses the coated particles, forms adhesive surfaces on the diapered coated particles, and finally brings the dispersed, coated with an adhesive layer into contact with one another, whereby the particles come together to form porous nested structures called agglomerates.

The individual stages of the actual agglomeration, like dispersing, producing the adhesive surfaces

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and bringing together into porous, interleaved formations can by any suitable means in any appropriate manner. It is preferred to have these steps concurrently in a single, uninterrupted operation to be carried out in a manner as already disclosed and briefly described below. The type and Way and the apparatus for carrying out the invention However, the method is not limited to this. For implementation

^ tion of the individual stages of the process according to the invention any suitable agglomeration device can be used.

The agglomeration device shown in the attached, somewhat schematic drawings consists of one Feed hopper 10 through which the coated, to be agglomerated Particles are supplied, which are the product of a previously carried out grinding of the used as starting materials Represent pesticides and liquids, and from which the material to be agglomerated is drawn off by the screw conveyor 11

P will move the material continuously into the elongated agglomerator 12 gives up, which has a sieve 13 on which the The bulk of the coated particles is initially deposited and on which they agglomerated during their conversion to the desired one Product migrates along the vessel from the inlet to the discharge end.

The agglomerator shown is arranged in a row

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the bordering work area, denoted by A, D and CS, in which the agglomeration, drying, cooling and sorting takes place.

There are also devices for vibrating the entire agglomerator, with which the general induces forward movement of the bed of coated particulate material which travels therethrough will. These VoÄchtungen include the supporting rocker arm 14 and the eccentric drive arm 15. In the ^ Migration of the material across the screen 13 is preferred kept in a practically flowable state by a stream of solvent vapor flowing onto the coated Particles can create sticky surfaces, such as moist air or water vapor, which settles on the coated particles can condense, is passed through. The steam is continuously fed into the lower part of the first compartment, i.e. the agglomeration section A, introduced through the inlet 16 and sweeps up through the sieve 13 and the bed with the material at a speed sufficient to I. the bed of the finely ground, powdery material in a practically flowable state and the particles in the near To keep in touch with each other. After the material has been wiped through the bed, the steam is passed through a suitable The outlet, i.e. the discharge opening 17, which is mounted on the top of the agglomerator, is discharged. To achieve

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of becoming flowable or of dispersing and mixing together however, means other than the upflow of steam may be used for the particulate material means other than a condensable one, as well as for forming the adhesive surfaces on the coated particles Steam come into embossing, e.g. an absorbable gas or heating.

To avoid contamination of the screen 13, the flow of humid air can be in any suitable Way to be overheated. Devices can also be provided which have an intermittent or uninterrupted Removal of the screen or parts thereof from the agglomeration zone, allow the screen to be washed and returned. If using superheated moist air, use the particles that are in the lower part of the bed near and adjacent to the sieve, the excess? / poor of the gas flow without condensation of moisture taking place on these particles, while those Particles that are in the upper parts of the bed take up the condensate, causing the formation of agglomerates is completed. Devices for repeated removal of the sieve without interrupting the work process agglomeration can consist in using a sieve in the form of an endless belt and cleaning devices, like spray nozzles, for automatic cleaning of all

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Parts of the sieve after it has come into contact with the adhesive material to be agglomerated. The bed of material in section A is vibrated by the agglomerator and the upward flowing feuohte Air in a dispersed, duro-stirred and practically flowable condition, with the moist 'not only serves to keep the bed of particles in! vr * is kept practically flowable state, but rather also to the fact that on the dispersed particles water | steam condenses, thus - as stated above - sticky Surfaces are formed. Ba the surfaces of the fine particles in the section A due to the condensation If the moisture become sticky, they become practically free flowing through the mixing and movement of the moisture Beds are arbitrarily brought into contact with one another, causing them to stick together and gradually separate from the particles nested structures, i.e. the agglomerates according to the invention, arise.

The agglomerated material migrates from section I A to the next stage, section D, in which the material dried and the moisture added in section A using a stream of hot air, the temperature of which depends on the amount depends on the water to be removed, is removed. In the apparatus shown in the accompanying drawings, strokes the hot drying air continuously through the screen 13 and through the bed of agglomerates in section D, whereby

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the agglomerates in de "Hare, as the moisture is removed from them to solidify and stiffen respectively, eretarr" n _t uad wherein the stream of hot air to the bottom of the sections D duroh the line reaches 18 and duroh the Ablafl5ffnung 19 escapes to the upper side · laughing the Drying, the hot, dried agglomerates pass the next or «last stage, the section CS, in which the agglomerates are optionally exposed to a cooling air stream which is fed through line 20 and through the drain opening 21 on the top and through which the agglomerates reach room temperature brought into a rigid, rigid state · In the last section CS, the agglomerates are also sorted during the cooling. The hot-dried agglomerates migrate from the sieve 13 to a coarser sorting sieve 22, the material falling through the sieve 22 coming to rest on the finer collecting sieve 23. The excess material remains on the sieve 22.Product and oversize material are discharged as indicated

The specific method and apparatus described for carrying out the agglomeration of the coated particles allows careful control of the agglomeration process, such as control of the addition of moisture and a Control of the activity of the particles and their contact.

The agglomerator can be tilted downward and vibrate or left to stand still during agglomeration will. Agglomeration is achieved in both cases.

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Sae method according to the invention proves to be particularly advantageous when Bau wants to coat a solid such as sucrose or dextrose with a heavy, viscous liquid, for example May syrup or invert syrup. A Gemisoh made of 1 part corn syrup or invert syrup with 3 parts sugar is a heavy, thick paste that has no practical application, since it is impossible to pack, handle and dissolve such a product, according to the method according to the invention, such a mixture is finely powdered Whereby the thickness of the viscous film is preferably reduced to the point of apparent dryness in accordance with the foregoing. Such a product, however, is not yet free-flowing or immediately soluble, but instead proves to be inconsistent on shipping and quickly turns into hard lumps which make it unsuitable for practical use _β

After agglomerating the ground mixture in accordance with the method of the invention However, a stable, free-flowing, non-caking and easily soluble product is obtained, which in spite of its high liquid content is apparently dry.

According to the method according to the invention, it is also possible to apply a substance in the form of a liquid coating apply another substance that is in finely divided form and acts as a carrier or diluent, and then to be converted into a free-flowing agglomerated product

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wandein, because Ia a liquid easily dispersible and / or is löelioh, the liquid coating during the agglomeration is dried, so that the end product is completely trooken and one of the porters is owing are covered with a dry coating of the originally liquid substance.

To explain the different types of solid / powdery substances that are produced according to the invention Process are known to be agglomerated, and the novel products obtained in this way are now followed by a series of examples, which, however, only the process according to the application should explain, but not limit.

The inventive method is particularly applicable and useful in improving physical Properties of certain sugar products

You products sugar, falling within the scope of the invention include all products that are made of a solid sugar, usually sucrose or dextrose, and egg ner liquid (usually non-crystallizing) phase, it jaich often containing in a sugar Low purity syrup. This class of substances includes sugar products such as "soft" sugar, solidified sugar cane juice, various confectionery products, fondant and over-sugar masses and dry, instantly soluble extracts for the preparation of non-alcoholic beverages, such as with cola or fruit flavors, etc., these

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OW <3> NAL INSPECTED

Ββ1βρ1 · 1 · only serve as an explanation and not as a Limitation should be understood as in this Stoffklaeee nooh more products fall

Soft zuoker

The distinction between τοη the "hard" Raffinadesunkern al · "soft" Zuoker designated products have eh ^v ., A lower degree of purity · The degree of contamination according to this term fall under this term the well-known light brown and yellow sugars, the dark brown sugars, the partially refined products and solo zuokers, which are referred to as raw or not yet refined zuokers. The sugar crystals are coated with a "tiscose syrup, the molasses. The molasses contain the natural impurities of the sugar, that is, the light-sugar components of the sugar cane juice in an enriched form of the uncritical part of the sucrose and the reducing sugars Sugars do not only include the natural white zuokers, which are intermediate products in the refining of the sugar, but also those white zuokers that have been artificially produced by overlaying or "coloring" τοη refined sugar crystals bit suitable molasses ·

Under the term "soft sugar" as used here is, however, other types of τοη "colored" sugars, where the refined sugar crystals are not aiii molasses,

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but old another film of syrup artificially covered over These syrups often have a fruit flavor, in contrast to the well-known Helasse flavor the brown and raw sugar.

The expression "soft sugar ¹¹ , as it is used here quite generally, however, only includes the above-mentioned common, molasses-coated sugars and colored sugars, but any sugar whose particles consist of a center or core made of sucrose or another -

"Ren sugar - coated with a film from the mother liquor, of added syrup or another liquid - consist · The hard core of refined sugar can consist of Dextrose or sucrose are made up · The soft film can be a have any composition and can be applied to the sugar grain by known methods

Since the common soft sugars are generally obtained from plants containing sucrose, i.e. sugar cane, Sugar beet and sorghum, represent the sugar crystal

^ Ie coated by these syrupy molasses, practically pure sucrose due to the viscous molasses film that is present on the crystals of the soft sugar, these sugars are not free-flowing and have a pronounced tendency when stored - especially when Loss of their moisture content - caking into hard, firm masses that are uncomfortable to handle and can only be broken with difficulty «The natural

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The stickiness of these soft sugars is further increased by the hygroscopic nature of these sugars or their molasses coating. Because of the pronounced inclination of these points Sugar, in storage and dehydration xu hard masses To bake them together, these sugars are currently available in very coarse-grained form, as attempts are being made to reduce caking in this way as much as possible. The coarseness of these sugars only counteracts these difficulties to a limited extent, as they do not prevent caking and neither do the sugars be mowed in a suitable manner in a free-flowing manner Due to the coarseness of this soft zuoker, the rate of dissolution in a liquid is considerably reduced, since the rate of dissolution is a function of the Particle size is. So are the soft sugars currently available, which normally contain 2-5 # moisture so designed that there is no method by which they can be treated in such a way that they are suitable for easy handling and storage. When these usual soft sugars are in | If kept in a warm, dry atmosphere, they will lose moisture and become very hard · Become in a If kept in a cool, humid atmosphere, caking into hard masses is prevented, but the zuokers are a consequence the absorption of extra moisture will become even more sticky and stiff and hard as the viscosity of the syrup increases the soft crystals increases. Take the chilled zuoker

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when heated to normal temperature in a humid atmosphere, their original properties, i.e. their normal sticky, non-free flowing state, while drying caused hardening more difficult is to be cared for. The property of these soft sugars, xu caking hard masses therefore poses a significant problem in terms of storage and handling Manufacturers, industrial consumers and the housewife represent "

In addition to the poor flow properties, the Stickiness, the tendency to stick together too hard and the storage problems mentioned above are further problems important disadvantages of the usual soft sugars in that they do not disperse easily in liquids and dissolve, especially not in cold liquids · This inability to rapidly disperse and dissolve in a liquid, combined with stickiness and the generally unsatisfactory appearance of soft sugars, has limited their usefulness and prevented that they are used in considerable quantities, e.g. as table sugar for sprinkling on the breakfast table, for fruit and other purposes where the characteristic taste of the soft sugar is desired. This inability to disperse and dissolve quickly is also of great concern in the field of the production of saccharified products and fondants, i.e. in a larger part of the confectionery industry.

The well-known soft sugars can not be in one

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Fondant or a "cooked icing ") by simply adding them to the required amount of liquid. The coated sugar product according to the invention, on the other hand, can - if it is made from Little rope with a grease that is no longer perceptible in the mouth of about 40 η or less - in a fondant • which can be transformed into an overcooking mass that has all the properties of a so-called "cooked fondant sugar mass", without the sugar being used for the purpose | crystallization to that for such fondant products required special fine grain size redissolved and has to be cooked.

In the confectionery industry, a fondant is made that is fat contains, called "fudge" · Bei Carrying out the method according to the invention, it is possible to add fat as the liquid phase or to add the fat to add to the liquid phase in connection with sucrose and / or dextrose as the solid phase of such sugar products · It is possible to produce dry, stable, free-flowing " de sugar by simply adding the appropriate amount of water or milk to a fat fondant immediately (Eng · "fudge") can be transformed. The soft sugars according to the invention have a taste compared to the usual soft sugar improved. This improvement in taste is due to the immediate solubility. A soft sugar produced according to the invention provides a novel one

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Direction of taste, since the taste buds of the tongue have all the components immediately and at the same time. In a conventional soft sugar act - when tasted in dry Fora - the individual components one by one to the ßeschmacksknospen, d _o h · the bitter and salty molasses is first added, while the large sugar crystals are subsequently dissolved, in which a predominantly savory and often unpleasant taste / remains, which is caused by the novel and uniform taste,

r is cause the soft sugar according to the invention, completely different, even though the actual composition of the sugar is identical.

When the method according to the invention is carried out using soft sugars, the particles are finely powdered soft sugar is joined together to form loose, nested, porous agglomerates and in this way a soft Obtained sugar product that is (a) free flowing, (b) practically non-caking, (c) both hot and auoh in cold liquids can be easily dispersed and quickly dissolved, and fudges, which contain an edible fat such as butter, can be transformed by adding the Agglomerates simply dispersed in the appropriate amount of liquid, (e) not in a cold, humid atmosphere or to be stored taking into account other and unusual features or to be packed in special containers needs to deal with the situation associated with the soft sugars

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overcoming problems; and (f) more satisfactory in appearance and has a better taste when tasted in dry form

The method of making these soft sugar agglomerates illustrates one of the preferred embodiments for making the "coated" particulate products of the invention. This process exists quite generally in the fact that the soft sugar is crushed to a fine dust or powder form, around the sugar particles to a much smaller size and thus the pilmdioke of the molasses as a result of the distribution on one to reduce a much larger area, that one creates adhesive surfaces on the finely ground particles and that one then arbitrarily bringing the tackified particles into contact with one another to create the loose, interleaved, porous To produce agglomerate * of the invention, the particles of soft sugar that form the agglomerates through leave gaps or spaces through all the agglomerates · |

In the case of the soft sugars, the distribution of the molasses over a much larger surface not only makes the material easier to handle and flows freely, but also means that the taste of the soft sugars is significantly improved because of the small thickness of the molasses film , which surrounds the sucrose parts after grinding - in contrast to the much more diocerous film like him

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Before the grinding is done - the sucrose is tasted at the same time as the thin molasses film, before the taste of the molasses and the sweet sugar are quickly mixed and the normally strong molasses taste of the usual soft sugars - in which the thick, strong molasses film must first be tasted and penetrated before you realize something of the sweet sugar - is no longer perceived _o this particular point is in relation to the raw sugar even more significant, since the usual raw sugar an even more bitter taste than the partially refined brown sugar have · by distributing this Melassefilmes a The much larger Saceharoseflache and the resulting reduction in film thickness to a minimum gives the raw sugars a very satisfactory taste, which in many cases enables such agglomerated raw sugar to be used as table sugar as a substitute for the usual refined granulated sugar Since raw sugar is considerably cheaper than granulated refined sugar, 'From the nutritional point of view, the constituents of sugar cane include some highly desirable non-sugar substances. Using the method according to the invention it is possible to obtain trooked, free-flowing and persistent cane sugars of any desired sucrose content and a content of these desired non-sugar substances

to manufacture

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In particular, there is the method according to the invention in that one grinds the sugar to be agglomerated to a single degree of fineness that practically all of the material has a diameter smaller than 300 ti, preferably less than 15On, the actual clay particle size depending on the intended use of the agglomerated product. If the coated sugar produced according to the invention is to be converted into a fondant product, a coking mass or a fat fudge mass (fudge) - duroh ■ simply adding the appropriate amount of moisture - to be transformed, the particles need to be down to one size ground that can no longer be perceived in the mouth, i.e. down to about 40 p. or below, as a suitably prepared fondant or saccharification mass should no longer have any noticeable graininess in the mouth. For other purposes, such as use as table sugar, the soft sugar can be ground to a coarser particle size than is used for fondant and topping masses is necessary, since in this use the graininess that is perceptible in the mouth is not important.

In the agglomeration of the soft sugars, the adhesive surfaces are preferably formed on the powdered, coated soft sugars by subjecting the particles to moistening or wetting, with each other A thin film of moisture forms on the surface of the individual small particles, which reduces the stickiness of the molasses increases or dissolves some of the sugar itself, thereby causing

909825/0624

Thus, with the help of the melee syrup or the saccharose itself, a sticky piIa forms on the surfaces of the particles. To achieve satisfactory results, the humidification must be carried out under carefully regulated conditions in order to avoid over-wetting or wetting of the sugar. Only very small amounts of moisture are required to achieve the desired agglomeration. An increase in moisture in sugar of $ 3> is usually considered sufficient, while the upper limit is around 6 % . The moistening must be carried out and regulated carefully in order to form a thin film of moisture evenly on a large number of τοη smallest particles with a minimal amount of moisture and to avoid over-moistening of the sugar, which leads to a complete or partial solution of the sugar to a sticky, wet mass - from which no porous agglomerates could be made - or the formation of so much excess syrup that the interstices between the agglomerates would be filled with the syrup, and / or would lead to the formation of hard shells on the agglomerates, de a penetration of a liquid into the interior impede.

As mentioned above, the carefully controlled deposition of moisture on the sugar powder particles can be carried out on can best be achieved by allowing water to condense from water vapor. In the preferred embodiment according to the invention

909825/0624

• -33-

drive to agglomerate soft sugars, therefore, the particles to be agglomerated are dispersed in the moist atmosphere of water vapor, with the Surface of the particles forms a thin film of water of the desired thickness, so that uniform wetting of the particles takes place. The particles must can of course be dispersed in the vapor at a temperature below the dew point · When performing the Moisture condensation on the particles can cause g only a limited amount of water will deposit on the particles, making it possible for it to get onto the surfaces of the particles to carefully regulate the amount of moisture to be applied without the risk of the above-mentioned over-wetting.

When the soft sugar particles have been wetted and given a sticky outer surface, will the whole mass of sticky, finely ground particles of soft sugar stirred - preferably proportionately moderate - to bring the particles into contact with one another. When the particles meet, they then adhere " together and form loose, interleaved, porous structures in which the individual particles are connected to one another by the sticky molasses film or the specially formed film of dissolved sugars. When the to be agglomerated Particles in a certain area, such as a fluidized bed, are kept close to each other, only needs to be stirred relatively little, since the sticky particles

909825/0624

then easily find others with whom they can connect to ₀ the more regular the emotion, the more porous and loose, the agglomerates and the lower the bulk density of the final product.

The degree of agitation desired for successful agglomeration of these soft sugars is through Suspending the particles to be agglomerated in a bed made practically flowable, wherein the Flow can be achieved in several ways. It It is preferred to achieve this flowability by venting the adhesive particles at a moderate rate Suspended gas stream, which keeps the bed in the practically flowable state until the agglomeration has ended. That through the amount of agitation induced by the fluidized bed provides agglomerates that are loose, interlaced, and porous, and a high Have the ratio of void to solid · Such agglomerates are not as dense and hard as those products obtained with a more violent and vigorous stirring } will.

The operations of dispersing, stirring and condensing Ens a moisture film on the dispersed particles can therefore with maximum effectiveness in the illustrated apparatus and can be carried out successfully in the manner described if the to be agglomerated Particles in a humid atmosphere caused by a water vapor Stream of grass - which is uninterrupted by the hatred

909825/0624

of the finely ground soft sugar - it is brought about, suspended and kept flowing, whereby the Humidification of the particles UAd the formation of the agglomerates practically effected at the same time Ia an eiAsigea operation will. With this method an even distribution and condensation of the moisture over the particles is achieved.

When the one of its particles of powdered soft sugar due to the addition of τοη moisture and the Formation of the adhesive surfaces jetted together and in porous, tersoha-sheathed agglomerates will be transformed the agglomerates are preferably dried by removing the added moisture in order to close the agglomerates formed solidify and stiffen, reduce their stickiness and make them easy to handle, pack, store and use Make adaptable »After drying, you can optionally be cooled and, if necessary, sorted

The agglomerated, molasses-coated soft Sugars have the typical properties of the agglomerates according to the invention, as mentioned above, and are also crumbly, have a relatively uniform shape and have a molasses film, which is evenly distributed without local overconcentration. The color of the soft zuoker produced according to the invention In contrast to soft sugars of the same degree of purity, which have been produced using conventional methods, it is drier

Shape lighter

90982S / 0624

Because the agglomerates of white sugar quickly and let them dissolve without lumps, these can Products are used as table sugar for sprinkling porridge, fruit and the like. Porous agglomerated sugar can be dispersed immediately in the appropriate amount of liquid »whereby a fondant or sickening mass is immediately formed in one operation · The invention Coated soft sugar agglomerates allow calibration #

^ Disperse and dissolve immediately, even if too cold Liquids are added, as in the preparation of quick-to-prepare beverages and the like · · As these Agglomerates of soft sugars are free-flowing, non-caking and crumbly, they can be stored under normal conditions · You don't need - like that non-agglomerated soft sugar - in a cool, To be stored in a humid atmosphere

)) are subject to normal humidity fluctuations, even if they are frequent and relatively drastic Will be exposed to changes in humidity - whereby the agglomerates are repeated one after the other in a very moist Atmosphere, then dried, stored moist again, etc.

As a result of the large internal surface area of these agglomerates, they have the ability to absorb large amounts of space

909825/0624

H92841

absorb or absorb moisture inside the agglomerates to be released so that most of the changes in fluidity are not outside, but inside the agglomerates takes place. The fluctuations between dry and humid air that occur in the atmosphere therefore occur no significant changes on the surfaces of the agglomerates

The following examples illustrate some typical applications of the process of the invention in the field the soft sugar. "

example 1 Experiment A (brown sugar)

In this experiment, a brown, soft sugar is ground to a particle size below 60 microns and then agglomerated in an apparatus corresponding to that illustrated in the accompanying drawings. The brown sugar is fed into the agglomerator at a rate of 45.4 kg / hour, the vibrating device | delivers a stroke of 1.27 cm and a frequency of 950 / minute. The agglomerating and flowable moist air which enters section A, which has a length of 30.5 cm, has a temperature of 71 ⁰ O when measured with a thermometer with a wetted ball, and a temperature when measured with a thermometer with a dry ball temperature of 138 ⁰ C and is conducted at a rate of about 2.38 OBM / minute through the bed "the Trookenabschnitt of

909825/0624

The agglomerator was about 1.50 m long and the temperature of the drying air was 149 ^° C. The agglomerates obtained in this experiment had the typical properties of agglomerated coated substances and soft sugars, as described above. Most of the agglomerates had a Size corresponding to 0.32 - 3.36 cm clear mesh size. In the meat industry it is customary to incorporate brown sugar in the presence of nitrate and other treatment agents in ham and other meat products. Such mixtures can be produced by the process according to the invention _e

Experiment B (raw sugar)

In this experiment, raw cane sugar is ground to a particle size below 50 ii and then agglomerated using the apparatus shown in the accompanying drawings. The ground raw sugar is fed into the agglomerator at a speed of 136 kg / hour and the vibration device is operated with an Hmb of 1.27 cm and a frequency of 850 / minute. The length of the agglomeration section was around 45 cm, and the moist air which made it flowable and agglomerated had a temperature of 79 ^° C. when measured with a thermometer with a wetted ball, and ^{a temperature of 143 °} C. when measured with a thermometer with a dry ball, and was passed through the bed at a rate of about 2.38 cbm / minute. the

909825/0624

Trookenzone was 137 whether long, and the drying air had a temperature τοη about 124 ⁰ C. The agglomerates obtained in this experiment showed all referred to in the desirable properties of the agglomerated soft sugar "such as may be achieved according to the invention. In addition, the agglomerated raw sugar, in contrast to non-agglomerated raw sugar, had a good taste. Most of the agglomerates had a size corresponding to 0.32-3.36 om the clear width. The agglomerated raw sugar had a bulk density τοη 0.40 g »

Example 2 Test; on caking and flowability

To explain the property of agglomerated soft sugars, as opposed to non-agglomerated ones To allow soft sugars to flow freely and not cake together, the following experiment was carried out: Agglomerated Brown sugar and common, non-aggloxnerized, unground brown sugar were served separately in open pans ben and heated to the same high temperatures with the same high humidity for 24 hours Samples dried in vacuo for 3 hours and left at room temperature overnight over a period of about 12 hours. When the tests were completed, it was found that the common, unground, non-agglomerated brown sugar was abundant had hard lumps that would not crumble,

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while the agglomerated brown sugar without oak any clumping remained free flowing

Example 3 Manufacture τοη instantly soluble »fondant from brown sugar

A soft brown sugar was chosen for this experiment. Special care was taken when grinding the sugar to a particle size τοη less than 40μ before agglomeration. A ground product of this type

"is highly volatile and tends to cake immediately," accordingly the ground product became instantaneous agglomerated after grinding and the agglomerated product by mixing τοη 100 parts of agglomerated brown Sugar converted into a fondant mass with 15 parts of warm water over a period of 1 minute. The fondant mass obtained was more identical to a cooked fondant mass Sugar composition in terms of gloss and smoothness, You can use the usual soft brown sugar to make a fondant

^ such properties cannot be produced.

Example 4

Dissolution rate of agglomerated soft brown sugars in water compared to the rate of dissolution of non-agglomerated soft browns Sugar

Three different samples were used in this experiment

soft sugar from above into a column of cold water

900825/0624

127 on length given. One of these samples consisted of common brown granular sugar, another sample of the same common brown granular sugar - but ground to powder form - and the third sample of this ground common brown sugar in agglomerated form. The samples were released through the column with cold The usual granular brown sugar was practically dissolved after a fall distance of 58.4 cn. The ground conventional sugar clumped together and reached the bottom of the tube undissolved. It remained partially unresolved even after a long period of time. The agglomerated brown sugar had completely dissolved after a fall distance of only 16.5 cm. This experiment illustrates the differences in dissolution rates between agglomerated brown sugars the usual granular brown sugars and the usual brown sugars that have been ground to the powder form, the agglomerated brown sugar having a larger dissolution rate than that of granular and powdered g.

Instantly soluble sugar cane juice in dry form

The method according to the invention is also applicable to the production of a dry, instantly soluble sugar juice powder in an agglomerated, stable, free-flowing form Form from the whole juice of plants containing sucrose, i.e. sugar cane, sugar beet and sorghum, applicable.

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The expression "whole juice ¹¹ , as it is used here, means that the whole juice of the sugar cane or the sugar beet or of sorghum is used without removing any of the original sugar constituents. The juice may, however, have been filtered or clarified by known methods. Whole Sugar cane juice and the products made from it have exceptional nutritional value · In most of the countries where sugar cane grows, sugar cane juice is generally used because of its high nutritional value.

P drunk »

In addition to the crystallizable sucrose, sugar cane juice contains a large, practically non-crystallizable one Part that is generally separated off in the form of molasses in conventional sugar production. In the Treatment of sugar cane juice to produce cane sugar is about 1 part molasses each in certain countries 2.5-3 parts of raw sugar obtained. Until now, the sugar industry has not been able to produce such large amounts of molasses

^ with the crystallized sucrose portion to a dry, In fact, even ordinary raw sugar is after centrifugation of the molasses does not flow freely and has a tendency to cake. According to the method according to the invention, it is now possible from the whole sugar cane juice to produce a stable, free-flowing, non-caking and immediately soluble product » According to the method according to the invention, a dry, stable, free-flowing, non-caking,

909825/0624

OWGiNAHNSPECTED

lends the dispersible and instantly soluble product from the whole Zuokerrohraaft produced by. First of all, the whole juice - preferably in clarified form - can be crystallized and solidified, for example by boiling in open pans or in a vacuum. The solidified Zuokerrohreaft is preferably poured into block form before grinding. If the end product is used as animal feed and not for human consumption, the unclarified juice can be used directly. Once the whole juice has solidified, it is in the general beeohrie- up * treated enclosed manner, as described in particular for the production of agglomerated soft sugars. So the solidified, crystallized whole sugar juice is ground or comminuted into powder form in order to enlarge the total surface of the sugar crystals and to distribute the non-crystallizable juice components in the form of a thin film on the fine sucrose particles, over a greatly enlarged area, preferably up to Point of apparent drought. g This intermediate product - apparently dry, powdered whole sugar cane juice - is extremely unstable and bakes together quickly. It is therefore immediately stabilized in accordance with the invention by converting the inconsistent powder particles into porous agglomerates by any suitable method, such as the method and apparatus described above, to form a dry, stable, free-flowing, non-caking, instantly soluble agglo-909825 / 0624

Manufacture merged product from whole zuoker cane juice.

The solidification can be carried out by first evaporating the juice by customary methods be »If the agglomerated product is to be used for direct human consumption, the juice is pre The juice is then thickened to about 92-98 ° Brix. Will the thickening carried out in open kettles, the thickened mass can granulated and partially crystallized by stirring »The granular mass can then still be in liquid state in preferably wooden molds are poured, where it solidifies instantly. The thickened clarified juice can also Boiled in conventional vacuum pans, granulated and crystallized into a hard mass (masseouite) of the appropriate density will. The hardened mass (masseeuite) can then be removed continuously and conveniently, either to Pouring in molds or for continuous consolidation. Depending on the composition of the juice, such as the ash content, the gum and other molasses-forming substances as well as the Brix value of the finished hard mass (masseouite), the hardening in the mold can be regulated so that it takes place within a few seconds or a few minutes or more. Haoh the solidification is practically the whole sucrose of the sugar cane juice in crystallized form. By varying the degree of oversaturation before Graining and crystallization and by varying the agitation speed the size of the sugar crystals can be

909025/0624

solid mass can be determined.

The whole zuoker cane juice agglomerated products of the invention contain, in addition to the sucrose, all of the original pulp components of the juice and have the same physical properties as are generally inherent in the agglomerated coated particulate products described above. So the lines of the sugar juice powder consist of a solid phase of sucrose and a thin film of non-crystallizable juice components. «The Λ particles are nested to form agglomerates, leaving a large number of gaps and spaces open, making the agglomerates easily dispersible in a liquid and immediately soluble In addition, as noted above, these whole sugar juice agglomerated products are free flowing and non-caking for the reasons given above. The agglomerated sugar juice product obtained according to the combined process steps of the present invention can immediately be converted back into the original zuoker cane juice by adding water. '

The dry agglomerated sugar juice products of the invention are stable and instantly soluble. However, the whole cane juice agglomerated products of the present invention have many other new and desirable properties and uses. For example, it has been found that acidic fruit juices with a pH of

909825/0624

ORIGINAL INSPECTED

have about 4, can be significantly improved in taste, when sweetened with the agglomerated cane juice product of the invention instead of refined sucrose These agglomerated sugar juice products can still be used in are used in the baking industry and other food industries

The agglomerated sugarcane juice product of the invention has a taste and aroma similar to ordinary ones Sugar is not to be found · Most zuoker cane juices have a high natural content of aconitic acid on ο The desired aroma of the aoonitic acid is however during the usual processing on! Raw sugar eliminated. During the baking process, the aconitic acid is converted into calcium aconitate and separated in the form of non-crystallizable molasses · However, the whole sugar cane juice is solidified and then pulverized and agglomerated according to the invention, the aoonitic acid originally present also remains in the end product · By treating the clarified juice with suitable ion exchange resins to release the original Aconitic acid content preferably at a pH of about 3.5 and to invert the juice to a suitable and desired invert sugar content, a constant, Instantly soluble, free-flowing product made from whole sugar cane juice of any desired invert sugar content and any desired pH value can be obtained,! fold treatment of the whole sugar cane juice in this way the product is then solidified, powdered and agglomerated according to the invention

909826/0624

OWGiNAL INSPECTED

When producing τοη agglomerated sugar cane juice powder as an additive for cattle feed, it is preferable to to use the raw, unclarified sugar cane juice at its original pH · Bas obtained product can be in Paper sacks are dispatched and thus saves the dispatch of liquid molasses · In addition, the cattle. those nutrients supplied with clarifying and liming normally destroyed or removed.

According to the invention, a dry, stable

get agglomerated sugar cane juice product that is free f fluent, non-caking, easily dispersible and is instantly soluble, has a high nutritional value, is cheaper than refined sugar, has a satisfactory taste or taste. has a satisfactory aroma and enables the sugar cane juice to have a wider and larger quantity Is used than before.

Confectionery products

Another important group of products that are used in The various confectionery products fall within the scope of the invention. Typical examples of these confectionery products, which can be successfully transformed into free-flowing, non-caking, easily dispersible and immediately soluble agglomerates are the various fondant preparations

As for the fondant preparations first, so it is currently common practice in the confectionery industry to

909825/0624

ORIGINAL INSPECTED

for the preparation of the various types of sweets, to prepare as fondant, Fettfondant (fudge), etc. _e, several homogeneous mixtures of dry sugars, including dextrose, and unkristallisierbaren liquid substances such as corn syrup or invert sugar, · This homogeneous mixture is normally boiled and recrystallized · According to the invention, the dry sugar (sucrose /, dextrose or their mixture) and the sugar syrup, such as corn syrup or invert sugar, are mixed homogeneously into a practically uniform mixture, after which the homogeneous mixture is pulverized - preferably in the presence of excess air in order to protect the surface of the To substantially enlarge sucrose crystals and to spread the uncrystallizable sugar syrup over this enlarged surface of the sucrose or dextrose crystals, which is preferably carried out up to the stage of apparent dryness, after which the powdered sugar particles coated with the syrup - preferably after The methods given above using the apparatus given - can be converted into the porous agglomerates according to the invention. With this procedure, the usual boiling and crystallization stages can be dispensed with, and the agglomerated mixture can be converted directly into a fondant or saccharification mass or another confectionery or A confectionery mix of this type can be made for use in industry as well as in the household; it can be used for an indefinite period of time without

909825/0624

OWGlNAL INSPECTED

bake lent stored, Ια paper sacks or cardboard boxes shipped and stored is in a liquid easily dispersible and soluble and for convenience for free-filling the consumer at any time "

This process is not only based on the usual homogeneous mixtures of Saooharose and a sugar syrup, but also on homogeneous mixtures of dextrose and sugar syrup, i.e. a system that consists entirely of dextrose. This agglomerated dextrose product can easily turned into a fondant product that sells at $ 100 | consists of dextrose. This represents a considerable advance in the fondant industry, as it is after the usual Cooking process was previously not possible to produce a fondant product consisting only of dextrose. Shark syrup that The hydrolysis product of corn starch, as is well known, consists of dextrose «

Example 5 Immediately soluble agglomerated fondant mixture (sucrose

and painting syrup)

The following is a typical example of making a persistent, free-flowing agglomerated fondant mix by the process of the present invention. A mixture consisting of 85 $> sucrose and 15 $> liquid corn syrup (43 ° Baume) is produced and finely ground, whereby the sucrose crystals are comminuted to a size of below 40 u. The fine saocharose powder particles that

909825/06 24 _0MGINAU , nspected

are then coated with a thin film of corn syrup according to the method according to the invention using an apparatus similar to that of the accompanying drawing - such as it was described above - resembles, agglomerated. The agglomeration section was approximately 45 cm long and the agglomerator was operated with a 1.27 cm stroke and frequency vibrates at 750 / second «The dusty, coated ones Particles were fed into the agglomeration section at a rate of 227 kg / hour.

^ Capable of solubilizing and moisturizing water vapor-containing air was passed at a rate of 2.77 cubic meters / minute after Dess deaf-shaped top through the left in the Agglomerierungsabsehnitt bed material and exhibited when measured with a thermometer with wetted ball a temperature of 71 ⁰ C and measured with a thermometer with a dry ball set a temperature of 149 ^° C. »The drying section was 206 cm long, and the drying air with a temperature of 132 ^° C. was passed through the drying zone at a rate of 5.55 cbm / minute

W agglomerates guided «The majority of the agglomerates had a size corresponding to 0.42 - 2.00 mm clear mesh size. The agglomerates were of good quality and were free-flowing, non-caking, easily dispersible and soluble in water and otherwise showed the typical Properties of the agglomerated products according to the invention · After adding the required amount of water, a fondant could also be produced from the agglomerates

909825/0624

INSPECTED

Quality was equivalent to a boiled fondant. Example 6

Immediately soluble agglomerated fondant mixture (sucrose and IiiTertzucker)

It was produced a mixture of 85 # sucrose and 15 ^ Invertzuckereirup and up to the dog no longer Vahrnehmbaren grain size τοη below 35 and ground · During the grinding process was for drying a stream of air with a temperature of 104 ⁰ C by the mixture | directed

The finely ground mixture, which is unstable and not free-flowing and immediately cakes together, was then introduced into an agglomerator similar to that described above at a temperature of 54 ^° C. at a rate of 182 kg / hour. The agglomeration section had a length of around 45 cm and a width of 15 cm. The agglomerated moist air has been given up by the Agglomerierungszone at a rate of 2.83 cubic meters / minute and had when measured with a thermometer ™ wetted-ball temperature of 68.5 ⁰ C and measured with a thermometer with dry ball a Temperature from 138 C to · The agglomerator was running at a frequency vibrates at a rate of 800 / minute and an amplitude of 1.59 cm. The drying air of 129.5 ⁰ C was through the drying zone (which had a length of 206 cm) with one speed

909Ö25 / 0624

ORIGINAL INSPECTED

of 5.66 obm / minute. It was a good agglomerated product - as is typical for the inventive process - formed that could be transformed into a finished fondant without boiling was required _f namely by 100 parts of the agglomerated product with 15 parts warm water 30 seconds! were mixed for a long time, the mixing being carried out in a water bath at 60 ^° C. In terms of gloss and breakage, the fondant obtained resembled a conventional cooked fondant of identical composition.

The inventive method can be applied to the processing of a stable, free-flowing, practically dehydrated Fondant product can be applied. For this purpose, a strongly cooked fondant is made of any desired Composition cooked and granulated in the usual way, preferably in such a way that that from sugar and mother liquor existing finished fondant has a minimum of moisture. As is well known, this can be easily checked. The brittle fondant obtained in this way is comminuted under suitable conditions, preferably by grinding in the presence of large amounts of excess cold air, which removes moisture during the milling step. The finely powdered fondant product is then immediately after agglomerated by the method according to the invention. The received, Fondant product consisting of free flowing, agglomerated particles can be added in the required amount Moisture can easily be turned into a damp fondant.

909825/0624

INSPECTED

Other instantly soluble products of this general type can be made with a combination of τοη sugar, either saooharose or dextrose, with another sugar-containing syrup, such as those syrups obtained from sugar cane (sugar cane syrup), with the sugar particles coated with the sugary syrup and then turned into agglomerates. Syrups of this type include sugar cane syrup, which is obtained by boiling down the whole zuoker cane juice to the syrup consistency, the "golden" syrup »obtained by mixing the second or third separation of the hard sugar mass (mass suite) during the refining of the raw cane sugar Mother liquor is obtained with invert sugar, and refined syrup, as is obtained from the refined raw cane sugar. Dextrose or sucrose can with other sugar syrups, such as lactose, maltose, Rafflnose and other natural in sugar beet and be coated contained in the sugarcane occurring sugar syrups, Malzsirupen, HonJLgsirup and maple syrup "Sämtliohe these different types of m sugary syrups are generally herein as Zuokersirupe designated.

The method described above can also be applied to dextrose that is obtained with the terminal molasses from the Dextrose can be coated. In a similar way So-called "No.70 zuoker" or other dextrose products of a low degree of purity, which are normally found in

909825/0624 originally inspected

Can be cast in block form, for more convenient use in the Brewing industry and for other purposes can be converted according to the invention into free-flowing products. Further products, which illustrate the process according to the invention, are fine sugar particles with a pondant mass or the whole Banana mass have been coated as if by grinding the Sugar with the fondant or banana mousse and subsequent agglomeration of the coated particles, like it Has been described above.

These examples merely illustrate some of the different types of confectionery industry products, such as they fall within the scope of the invention and can be easily converted into free flowing, instantly soluble agglomerated products.

Preparations for non-alcoholic beverages

Another area in which the method according to the invention is of particular usefulness and applicability is, lies in the production of non-alcoholic beverages. It was found that. according to the method according to the invention a dry, instantly soluble agglomerated syrup for the preparation of acidic and non-acidic non-alcoholic Beverages can be made. Most non-alcoholic beverages are made from a flavored syrup base made from zuoker (usually sucrose and sometimes a combination of sucrose with dextrose), com-

909825/0624

ORIGINAL INSPECTED

combined with various flavoring and coloring ingredients and an acid such as citric, lactic, tartaric, phosphoric acid or another organic or inorganic acid Acid. This syrup is then mixed with ordinary or carbonated water and made up Bottled bottles «These syrup bases for non-alcoholic beverages are produced in liquid form and dispatched, which results in certain disadvantages in handling and shipping, such as high costs, the use of glass containers and protective covers for them, and ™ Hernia. Sin syrup for non-alcoholic beverages that can be produced in dry, free-flowing, stable and non-caking form and in the Bottling is easy to disperse and instantly dissolve in the non-alcoholic beverage industry prove beneficial

When producing non-alcoholic beverages in powdered form, such as the well-known cola beverages, it is possible to combine all liquid components, such as the λ flavor and color components, and to mix them with all of the sugar, to pulverize the mixture - preferably in Presence of excess air to remove moisture - and then agglomerate as described above. The product obtained contains the non-sugar components of the non-alcoholic beverage in the form of a fine film, as it is with the hand of the

909825/0624

Examples dealing with soft sugars have been popularized.

Some of the non-sugar ingredients, like acids and often also dyes, often come in a dry form · In such cases, the inventive agglomerated Products are made by mixing all of the dry ingredients with the liquid ingredients mixed, the mixture ground to powder form and agglomerated.

As another possible method of making this

™ agglomerated products can be the usual flavored syrup for non-alcoholic beverages, * it sugar, acid, coloring and Contains flavor components, in liquid form as a film on powdered sugar (e.g. by grinding the sugar with the Syrup) are applied, whereupon the sugar particles coated with syrup are agglomerated.

The agglomerated syrup products of the invention for making non-alcoholic beverages can also be used for other purposes may be used. For example, the agglomeration

^ red product packaged and in concentrated, drier Form to dissolve into a non-alcoholic drink To be sold on the spot to the consumer. The agglomerated product can also be consumed directly in dry, agglomerated form can be packaged and sold as candy. The product can also be used for sprinkling ice cream, solid Ice cream and the like. Used and, if necessary, sprinkled from a shaker.

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Example 7

Dry, instantly soluble base for non-alcoholic beverages

A dry, immediately soluble agglomerated base for non-alcoholic beverages was made from 0.946 liters of syrup base flavored with "Wurxelbier" (English: root beer) and 35.4 kg of sucrose. 9.1 kg of powdered sugar were with the 0,946 liters of "root beer syrup ^w (English ·: root beer syrup) are homogeneously mixed and then mixed with 26.3 kg granulated sugar" The entire Gemisoh was finely ground and using similar equipment, The feed speed was 2.27 kg / minute and the vibration frequency was 800 / minute with an amplitude of 1.27 cm · The agglomeration section had a length of about 45 cm and a width of about 15 cm When measured with a thermometer with a wetted ball, air had a temperature of 85 ^° C. and when measured with a thermometer with a dry ball a temperature of 149 ^° C. and was passed through the bed in the agglomeration zone at a rate of 2.83 cbm / minute »The drying zone was ^{supplied with air at 135 °} C. A very good agglomerated product was obtained which, with water, quickly turns into a root beer drink he) transformed.

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Concentrated fruit juices

According to the invention, dry, stable, Produce free-flowing, easily dispersible and immediately soluble early morning juice preparations · With these products The individual particles that make up the agglomerates consist of solid sugar particles called bits a «natural, concentrated fruit juice, such as orange or raspberry juice, are coated. The agglomerated product is prepared as described above so that one first produces fine sugar particles with a thin film of the concentrated, liquid fruit juice are coated - as by mixing the sugar with the juice concentrate and grinding - and the fine coated particles are then agglomerated to form the agglomerates according to the invention. For example, an agglomerated product of this type can be prepared by starting from a starting mixture that contains 4 parts of sugar and 1 part of orange juice concentrate of 76 ° Briz. The concentrated fruit juice can advantageously be mixed with anhydrous dextrose anhydrous dextrose and sucrose or sucrose alone are added.

Mixed sugar

From the above description it can be seen that mixed sugars of different compositions can be obtained by the process according to the invention. In addition include mixtures of sucrose and dextrose or lactose

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u & d maltose in combination with corn syrups or similar Products obtained from the hydrolysis of corn starch, potato starch and the like, and liquid starch derivatives. The invention is also applicable to the agglomeration of raw corn sugars containing crystallized dextrose and corn syrup mother liquor are applicable. So it becomes a mixture pulverized from crystallized dextrose and corn syrup or dextrose mother liquor in order to coat the dextrose with a syrup or mother liquor film, after which the coated ones pulverized particles are agglomerated to form the free-flowing product according to the invention.

Softeners for textiles

The usefulness of the method according to the invention is further illustrated by a novel agglomerated Softening product for textiles which can be easily obtained according to the present invention

Certain nonionic and cationic compounds, such as quaternary ammonium compounds, act as fabric softeners or surfactants when they are Rinse water can be added to the fluff side of certain textiles. The new product according to the invention consists of a compound that softens textiles mixed with an inert, easily soluble diluent or carrier, such as sugar, and can easily be converted into a homogeneous, dry, persistent, free-flowing, easily dispersible

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and be brought into shape. The quaternary ammonium compounds that act as effective plasticizers. " are Available in both solid and liquid form, depending on γοη their particular composition. According to the invention, the softening quaternary Ammonium compound and the sugar acting as a diluent mixed together, ground to a dusty form and then after The processes described above are processed into agglomerated products with the properties characteristic for them. Becomes the active softener with the sugar particles mixed in liquid form, the sugar particles are coated with the plasticizer and these coated cords then agglomerated. In this case, the plasticizer containing the quaternary ammonium compound often loses solvent during and after the coating of the particles, whereby the sugar particles of the agglomerates are coated with the plasticizer in a practically dry form. The product can also contain small amounts of auxiliaries, such as coloring, Contains perfumes, irritants, blankophores, etc.

This novel agglomerated product and the process for its manufacture are described below:

Example 8

It was produced a mixture consisted of the 6 i "plasticizer in liquid form, less than 0.1 $> dye and perfume and 94 # sucrose. The active softener is a methylammonium sulfate from a fatty

. 909825/0624

acid amine with two hydrogenated Tallölfettsäureresten, the "Veri-soft-220" is commercially available under the name and consists of 80 io quaternary ammonium compound, 6 i »isopropanol and 14 # water. This mixture is ground to a particle size of about 60 microns or below and in an agglomerate or - similar to the apparatus described in the drawing - is given at a rate of 227 kg / hour. The agglomerator was vibrated at a frequency of 800 / minute and a stroke of 1.27 cm. The agglomeration section Λ was around 45 cm long and the dry section 206 cm long. The moist air making it flowable and agglomerating was passed through the material in the agglomeration section at a rate of 2.78 cbm / minute and had a temperature of 74 ^° C. when measured with a thermometer with a wetted sphere and a dry one when measured with a thermometer ball a temperature of 151.5 ⁰ C. the agglomerates were dried with air at 138 ⁰ C, which was passed through the drying zone at a rate of 5.55 cubic meters / minute. The agglomerates were of good quality W and were porous, stable, free-flowing, and easily dispersible and soluble in a liquid. The main part of the agglomerates had a particle size corresponding to 0.42-3.36 mm clear mesh size. The relative ratio of active plasticizer in liquid form to sugar at which agglomerates can be successfully made depends somewhat on the

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! * 3 L ö * I -62-

respective agglomeration device used. It has been found that the agglomeration can be carried out best when the amount of plasticizer is not more than 12 μl and is preferably in the range from 6 to 12 μl .

The advantages of the method according to the invention are readily apparent from the above description. After this The method according to the invention can be derived from a solid Phase and liquid phase mixtures that do not flow freely are difficult to disperse in a liquid and are to be dissolved and are difficult to pack and ship, in highly usable agglomerated, transform instantly soluble products that are free-flowing, non-caking, are easily dispersible and easily soluble in a liquid during handling, storage and Shipping do not pose any problems and in many cases open up new areas of application for the starting products or increase the usefulness and applicability in known areas considerably.

The various examples given above serve only to explain the types of products, that fall within the scope of the invention, i.e. the scope of the invention does not apply to these specific products limited. As emphasized above, the scope of the invention therefore includes all agglomerated products made from solid / liquid starting materials, both near

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as well as other products.

Among the term "agglomerated products" used in the preceding and following claims It is not just agglomerates »which are practically coated Particles are made up, but also agglomerates, which are composed of coated and uncoated particles adhering together such as particles of powdered brown sugar mixed with a dry flavoring in powdered and agglomerated form. The agglomerates according to the invention can also consist of mixtures of one or more solids and one or more liquids can be produced.

Numerous changes can be made to the details described above without this the scope of the invention is left.

- patent claims -

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Claims (1)

Patent claims: 1. Method of joining a solid and a liquid to a free-flowing, easily dispersible product, characterized in that the particles of the solid is surrounded by a film of the liquid and the coated particles are agglomerated to form porous agglomerates . 2. The method according to claim 1, characterized in that the particles to be agglomerated have a size of own below 300 u. 3. The method according to claim 1 or 2, characterized in that the liquid film is so thin that the coated particles feel practically dry. 4. The method according to claim 1 to 3, characterized in that the coated particles are thereby agglomerated that they are dispersed, that there are adhesive surfaces on the dispersed coated particles generated and that the dispersed coated particles are brought into contact with each other at random, whereby 'the Particles stick together to form porous agglomerates. 5. The method according to claim 4, characterized in that the particles are dispersed in an atmosphere, which produces surfaces that adhere to them, stirring the dispersed particles and thereby making them arbitrary 909825/0624 Contact and to be stored together to form nested structures brings. 6. The method according to claim 4, characterized in that that one creates a bed of the particles made practically flowable and the particles made flowable with it treated a medium containing a condensable vapor in order to the adhesive surfaces on the particles produce. 7. The method according to claim 1 to 6, characterized in that that part of the liquid is removed during the coating of the particles and the thus produced coated particles agglomerated. 8. The method according to claim 1 to 7, characterized in that that the solid particles and the liquid are mixed and ground together to form fine powdery To produce particles coated with a film of the liquid. 9. The method according to claim 7 and 8, characterized in that the material to be ground with a treated gaseous medium, with which part of the liquid can be removed. 10. The method according to claim 1 to 9, characterized in that that the coated particles are fine sugar-coated particles with a liquid film are coated. 11. The method according to claim 1 to 9, characterized in that 909825/0624 ORIGINAL INSPECTED I "T V 4U W -T I -If- 66 indicates that the coated particles are fine, rod-shaped sugar particles are coated with a film of a sugar syrup of lesser purity are. 12. The method according to claim 1 to 9, characterized in that that it is the coated particles are fine, powdery solid sugar particles, which with are covered with a fondant film. 13 »Method according to claims 1 to 9 for production dry, free-flowing, rapidly dispersible and instantly soluble mass for beverages that are easily transformed into a beverage with a liquid can, characterized in that the coated particles are fine, powdery sugar particles which are covered with a liquid film that contains the flavor components of the beverage. 14. The method according to claim 13, characterized in that that it is a non-alcoholic drink and that the fine, powdery sugar particles with are coated with a liquid film that contains the flavor components of the non-alcoholic beverage. 15. The method according to claim 1 to 9 for conversion from crystallized dextrose and dextrose mother liquor into dry, stable, rapidly dispersible, free-flowing ones Products, characterized in that the over- 909825/0624 pulled particles are fine, dust-like dextrose particles coated with a mother liquor film. 16. The method according to claim 1 to 9, characterized in that that the withdrawn particles are sugar particles with a film of a fruit juice are coated. 17. The method according to claim 16, characterized in that that the sugar particles with a film of the whole banana mass are stripped. \ 18. The method according to claim 1 to 9, characterized in that that it is in the coated particles to a Teilohenförmiges material with a film a plasticizer for textiles is coated. 19. The method according to claim 18, characterized in, that the particulate material is fine sugar particles covered with a liquid film are coated with a quaternary ammonium compound that acts as a softener for textiles. 20. The method according to claim 1 to 9 for the preparation of a dry, free-flowing, easily dispersible Product made from a normally plastic material, characterized in that it is the coated particles solid particles are covered with a film of the plastic material. 21. The method according to claim 10, characterized in 909825/0624 shows that the liquid film coating the fine sugar particles contains uncrystallized sugar. 22. The method according to claim 12, characterized in that that the liquid contains glucose. 23. The method according to claim 21, characterized in that that the liquid contains invert sugar. 24. The method according to claim 10, characterized in that that the liquid is molasses. 25. The method according to claim 1 to 24, characterized in that the coated particles are ground to the particle size and thus the film thickness of the liquid coating - because of the distribution of the liquid over a much larger surface * to reduce, and that the finer coated Particles agglomerate to form porous agglomerates. 26. Process for converting dust-like particles coated with a liquid into a free-flowing one, Easily dispersible product made from coated particles, characterized in that the coated particles dispersed, adherent to the dispersed coated particles Surfaces and that one disperses the adhered particles into random contact with one another by stirring, thereby forming porous agglomerates together. 27. The method according to claim 26, characterized 909825/0624 draws that a bed of coated particles is made and dispersing and stirring the coated particles of the bed to bring them into random contact with one another "Bring them to stick together and porous agglomerates which consist of nested structures of the interconnected particles and a network of interspaces exhibit. 28. Method according to claim 26 or 27, characterized in that that the dust-like particles are permanently coated with a film of an adhesive liquid. 29. The method according to claim 26 or 27, characterized in that the dust-like particles with a Liquid film are coated and that the surfaces of the particles are wetted while they are dispersed in the Condition so that they can be made adhesive. 30. The method according to claim 26 to 29, characterized in that the coated particles up to the form of dust be ground to the film thickness of the liquid coating due to the spreading over a much larger surface decrease and the fine particles with a liquid film to coat that is practically dry to the touch that the finer coated particles thus obtained in one Dispersed atmosphere that can produce adhesive surfaces on them, and that the dispersed, made adhesive Brings particles into random contact with one another, to 909825/0624 to store them together to form nested structures that form porous agglomerates. 31. The method according to claim 26 to 29, characterized that the coated particles are sugar particles with a syrup-like liquid film are coated so that the sugar is ground with the liquid to produce finer sugar particles and to distribute the syrup film over a much larger area, and that the finer particles are dispersed and treated to produce adhesive surfaces on them. 32. The method according to claim 26 to 29, characterized in that the coated particles are Sugar particles are coated with a molasses film that the molasses-coated particles are ground are ^ to get smaller sugar particles and the molasses film as a result to distribute it over a larger area and thus to reduce its film thickness and that the so obtained Particles are dispersed and treated to produce adhesive surfaces on them. 33. Process for converting a practically solid mass of a material from a solid and a liquid Phase consists in a free-flowing, rapidly dispersible product, characterized in that the mass to Milled particles, which consist of a solid phase and the liquid phase as a coating, around the liquid phase thereby 909825/0624 ORIGINAL INSPECTED -Jf- Ή over a much larger surface area of the solid distribute, and that the particles become porous agglomerates together. Process according to Claim 33, characterized in that the particles are agglomerated by dispersing the fine, dust-like coated particles, treating the dispersed particles in such a way that they form adhesive surfaces , and in that the dispersed, adhesive-like particles come into contact with one another and agglomerate to form porous agglomerates. 35. The method according to claim 33 or 34, characterized in that the solid Hasse comes from a liquid solution consisting of a crystallizable material and a non-crystallizable, liquid phase, and that this solution is transformed into a solidified mass before grinding contains the solid phase of the crystallizable material together with the liquid phase. 36. The method of claim 35, characterized in that it contains at the liquid solution to all the juice of a sugar-containing plant such as sugarcane, sugar beets and grain sorghum is that substantial amounts of sucrose than sugar. 37. The method according to claim 36, characterized in that the juice is clarified, except for the clarified juice 909Ö25 / 0624 OWGlNAL INSPECTED -JF- about 95 ° Brix thickens and the concentrated juice is oversaturated and crystallized to produce the finished mass. 38. A method for producing a dry, free-flowing fondant mass, characterized in that one Particles of a size no longer perceptible in the mouth, consisting of solid sugar and non-crystallized mother liquor consist, dispersed in a humid atmosphere in order to moisten the particles and to make surfaces sticky to them generate, and that the particles made adhesive are brought together and they are agglomerated to form porous agglomerates. 39. The method according to claim 38, characterized in that the sugar particles have a size below 40 u have and at least partially with a non-crystallizable Sugar syrup are coated, and that the dispersed, tackified particles together in Bringing arbitrary contact to agglomerate them into porous agglomerates. 40. Process for the production of a stable, free-flowing, easily dispersible and soluble fondant mass, characterized by converting fatty sugar into fine, Dust-like particles with the size of below 40 u, which can no longer be perceived in the mouth, are crushed and the sugar particles become coated with the liquid that is distributed over a larger surface during the grinding process, and that the coated particles are agglomerated to form porous agglomerates. 41. 909825/0624 41 ♦ Method according to claim 4-0, characterized in that that "the liquid is a non-crystallizable sugar syrup. 42. The method according to claim 40, characterized in that the sugar is sucrose and the liquid Contains glucose. 43. The method according to claim 40, characterized in that the sugar is sucrose and the liquid Phase contains invert sugar. ^ 44. The method according to claim 40, characterized in that the sugar is dextrose and the liquid phase also contains dextrose. 45. The method according to claim 40, characterized in that the sugar is dextrose and the liquid phase Contains invert sugar. 46. The method according to claim 40 for producing a fondant mass from soft sugar, characterized in that that the liquid is molasses. 47. Process for the production of a stable, M free-flowing, dry fondant mass, characterized in that a practically dehydrated, highly boiled-down fondant mass is ground and the milled particles are transformed into a porous, agglomerated product. 48. Free flowing, rapidly dispersible agglomerated Product, characterized in that it consists of particles 909825/0624 a substance coated with a second substance, which are assembled into nested structures leaving a multitude of gaps and spaces all over the agglomerated product. 49. Product according to claim 48, characterized in that the one substance consists of dust-like particles and the other substance is in the form of a thin coating which, prior to agglomeration, is in liquid form on the Particle has been applied. 50. Product according to claim 49, characterized in that the liquid with such a small layer thickness spread over the particles so that the particles are practically dry to the touch. 51. Product according to claim 48 to 50, characterized in that that the particles of the agglomerated product are about 300µ or less in size. 52. As a plasticizer for textiles suitable product, characterized in that it consists of a mixture of a active softener for textiles with a diluent and in the form of free-flowing, easily dispersible Agglomerates are present, which are made up of smaller, interleaved and connected particles. 53. Product according to claim 52, characterized in that the particles of the diluent with a thin Film of the effective plasticizer are coated. 54. 909825/0624 INSPECTED 54. Product according to claim 52 or 53, characterized in that that the effective plasticizer is a quaternary ammonium compound. 55. Product according to claim 52, 53 or 54, characterized in that the diluent is sugar. 56. Product according to claim 52 to 55, characterized in that the plasticizer in an amount of about 6 - 12 j £ and the diluent in an amount of etna $ 88-94. ( 909825/0624 -κ Blank page