Method of granulating particulates

FIELD: chemistry.

SUBSTANCE: method is carried out through the following consecutive steps: feeding, mixing, moistening with binder, preliminary granulation and granulation by pelletisation. The preliminary granulation step is carried out in a high-speed apparatus with mechanical activation of the initial mixture, to which the binder is added in an amount of 20-35 wt % of the total weight of the binder until establishing plastic strength of the mixture at a level of 20-30 kg/m2. The step for granulation by pelletisation is carried out by feeding microgranules obtained at the first granulation step onto the surface of a scuff plate rotating anticlockwise and at a rate higher than the critical rotation speed of the scuff plate. That step is carried out with simultaneous moistening by periodic fine spraying of the binder in amount of 4-15% of the total weight of the binder.

EFFECT: invention enables to granulate multi-component granular mixtures with particle size of 1-7 mm, and mixtures of enzymes and biologically active preparations.

1 tbl

 

The invention relates to the technique of granulation dispersible, granular materials and, in particular, can be used for the granulation of mixed fodder, enzymes and biologically active preparations.

One of the known methods of granulation is a method of digging. This granulation method described in known publications (Ipoin. Granulation. M.: Chemistry, 1991, 240 C.), whereby the dispersed product is served in a plate granulator where it is hydrated binder liquid (e.g. water) from nozzles and ukutyvaemsya to pellets of a given size. On granules located on the rotary plate, the forces of gravity, centrifugal force and friction force. During the rotation of the tilted plate due to the action of centrifugal force and friction force of the granules are pressed against side and bottom of the plate and rise to a certain height, and then under the action of gravity to slide down the bottom down. The shape of the trajectory of the pellet approaches the spiral. It is revealed that the granulation is carried out due to forces of surface tension and capillary pressure of a moving liquid film under the action of which particles are drawn together and form the primary agglomerates. The size of the primary agglomerates is determined by the size of the drops of water falling into the layer of material. Most of these agglomerate who is close to each other, and they are partially connected by water films. When moving moist agglomerate excess moisture is squeezed out to the surface, and the structure of the granules becomes more dense. Under the action of centrifugal forces arising from the rotation of the granulator, and the forces of surface tension of the liquid film of small agglomerates grow larger and, under certain conditions, become nuclei (sources granulometry). In the future anhydride (dry) particles accumulate on the moistened particles of retur. In this case, if the size dispersible drops large particles are formed internal retur 3-5 mm in diameter, but the mechanism for the enlargement of the granules remains the same. Further, the seal structure of the granules occurs in dense dynamic layers due to the forces of interaction of particles with each other.

One of the main problems when used for granulation method okutyvaya is strict regulation of the process of granulation on the angular velocity of rotation of the plate (ω), the angle (α), the place of supply of binder and input material, as well as limited areas of natural roll-off, low utilization ratio of the volume of the plate and wide particle size distribution of the finished product. Part of the task of narrowing of the particle size distribution is solved is by developing the design of a particular device - "disc granulator with activator", comprising a housing with a cover, which is installed with the possibility of rotation of the inclined plate and the cover, perpendicular to the bottom of the plate, set the trigger actuator (EN 2209662, B01J 2/14, 2003).

Shock blade activator, on the one hand, leads to the destruction of large granules and aggregates, and, on the other hand, initiates granulometrie in the original product. Active mixing of the activator by exposure to an activator for moving the plate a layer of granules increases the uniformity of the granules obtained from multicomponent mixtures, reducing the time of granulation compared to conventional Poppet granulator.

The disadvantage of this method of influence on the mechanism of granulometry is the narrow scope of the impact on the stratum granulosum and the low strength of the resulting pellets. To resolve some of the above problems when used during granulation method okutyvaya, there are various methods of granulation of dispersed materials in various fields.

So, for example, describes a method for the production of granular fertilizers from fine powdered materials, including batching, mixing, wetting and granulating by washing with or without additives, and granulating with okaty what W is performed using as the liquid phase of the aqueous extract soluble components of these fertilizers, having a temperature of 80-90°C (EN 2084276, B01J 2/14, 1995). The process in this case is carried out in a drum or disc granulator and of particles with micron size receive granules size 1-4 mm due to the introduction of aqueous extract soluble components of these fertilizers and due to crystallization put them in salt when carrying out granulation in this way increases the nutrient content and the strength of the granules.

The disadvantages of this method are:

high energy consumption caused by the need to introduce more energy-intensive stage of water extraction of soluble components;

the high sensitivity of the process to the dispersion of the spray binder;

a wide particle size distribution of the obtained granules;

narrow the scope of the process, excluding the granulating temperature-sensitive products (e.g., enzyme products, premixes and certain components of animal feed), not withstanding the elevated temperature, including at the level of 80-90°C.

Another known method the fine granulation of materials is carried out by feeding the humidified material on the rotating plate granulator, and before the presentation of the material on the plate to it with stirring embryonic particle fraction 50-300 μm in the amount of 25-30% of the volume of material (EN 2082491, B01J 2/14 1994). When implementing this method consistently perform stage batching, mixing the starting materials, the subsequent wetting with a binder and granulating the balling on a rotating inclined plate with simultaneous wetting by spraying a binder. The best results in performance and composition (dEQ=10-20 mm) is achieved when the diameter of the plate 0.7 m, an angle of inclination α of 55° and the rotation frequency n=22 min-1. From the description of the present invention, it follows that the hydration of fine material when mixed with Securom lead to a moisture content of 10-25%, and granulating the mixture should be performed within 5 min with additional hydration 2-5%.

The disadvantage of this method is the use of external large Remora (for example, marble chips), as well as introduce a limited amount of binding that does not allow you to pelletize fine powders to obtain granules with a narrow particle size distribution. In this way it is impossible to pelletize fine enzyme preparations and premixes with low bulk density.

Part of the task of narrowing of the particle size distribution is solved by exposure to an activator for moving the plate a layer of granules (EN 2209662, B01J 2/14, 2006). The disadvantage of this method of influence on the mechanism of granulometry is narrow blast impact on the stratum granulosum and the low strength of the resulting granules.

The closest in technical essence of the present invention is a method of granulating the fine materials that are implemented on a plate granulator, including stage batching, mixing, followed by wetting with a binder and granulating by rolling on a rotating inclined plate (EN 2410152, B01J 2/14, 2011). This granulation in this process is carried out in two stages, and the stage of wetting with a binder hold up to humidity 40-70% of the optimum moisture content of the mixture and simultaneously advanced granulation with reception centres granulation and subsequent input received microgranules on the surface area of the plate that constitutes 50-80% of its total surface. Stage granulation carried out at a speed exceeding the critical speed of rotation of the plate, while the ratio of the area of the spray binder in the zone of contact with the material is 0.4 to 0.7 of the working area of the plate, and the angle of elevation of the material on the peripheral area relative to the bottom surface of the plate is equal to 3-10° (EN 2410152, B01J 2/14, 2011).

The disadvantage of this method is the difficulty of granulation multicomponent, polydisperse materials (for example, feed mixtures)having high stickiness, as well as a wide granulometric composition of the obtained product. In addition, when this SP is the property obtained granules increased in size (>5 mm) and varying quality (in the form density and strength).

The technical task of the invention is the increase in the yield of marketable fractions, the increase in the uniformity of particle size distribution and strength of granular product using a wide class of binder.

The technical problem is solved by the proposed method of granulating polydisperse multicomponent mixtures, including batching, mixing, and subsequent hydration of the binder, prior to pelleting and pelleting the balling at this preliminary stage of the granulation is carried out in an apparatus of the high-speed type with mechanical activation of the mixture, which is added to the binder in a quantity amounting 18-30 wt.% from the total mass of the binder before the establishment of the plastic strength of the mixture at the level of 12-25 kPa, and the stage of granulation by balling carried out on a rotating inclined plate, for which the microspheres are injected on the surface of the inclined plate, rotating counterclockwise at a speed exceeding the critical speed of rotation of the plate, with simultaneous wetting by spraying a binder, and periodically carry out a fine spray of binder in the amount equal to 8-15% of the total mass of the granulated material, which is directed to the area of the plate, the composition of the managing 20-35% of the total area, and in the interval between inputs binder carry out periodic influence of the activators with the rotational speed of 600-1000 min-1on the layer of granules at the bottom of the plate, comprising 15-30% of the total area of the plate.

A significant feature of the proposed method are the conditions for the pre-granulation (regranulate), which is carried out in the apparatus of the high-speed type with mechanical activation with the introduction of the binder in the number of 18-30% of the total mass of the binder to the plastic strength of the mixture 12-25 kg/m2.. Enter a binder in the amount of 18-30% of the total mass of the binder provides the necessary plastic strength of the mixture. In the case of lowering the amount of typing binder below 18%, a decrease of density and strength of granules, and in case of exceeding the number above 30%, the product loses its flowability. The selected range set plastic strength of the mixture at the level of 12-25 kPa is chosen experimentally and it is at such a value obtained microspheres of the desired granulometric composition due to the interaction between the interacting particles.

In the proposed method, granulation is carried out already at the initial stage of preliminary granulation centre granulometry obtained by hydration in high-speed regranulate ramoc the CSO type. In regranulate is mixing, mechanical activation and the formation of germ granules (centers granulometry). Due to the intensive mixing in the volume of the mixture is a uniform distribution of particles, their partial grinding and mechanical activation with the formation of new specific contact surfaces. When declared sensitive parameters in the further processing are formed germ granules allocated to the disc pelletizer. Obtained at the stage of regranulate germ granules through the loading pipe is introduced to the rotating plate. As a result of granules on the surface of the inclined rotating plate, gravity, centrifugal, friction they are moved along a complex path around the zone of movement of the largest granules located inside the zones.

There is a critical frequency of rotation of the plate (n), in which there are large centrifugal force presses the layer of particles to the side of the plate and prevent the sliding of the particles down. In the proposed method is proposed to use the speed of rotation of the plate greater than critical. It is known that the critical speed depends on many factors, including the angle of repose of the material (φ0), the inclination of the plate (α), the diameter of the plate (D), in practice, for each material, e is the rate determined experimentally.

At speeds below the critical speed optimal mode when the separation of fines from the side of the rotating plate is at the top of their ascent on the surface of the pellet. In this case, is effectively used half or slightly more than half of the bottom area of the plate.

Actively rolling due to the natural sliding and rolling movement on the surface of the plate granules are coated in the liquid phase, for example a binder consisting of gelatino-sugar solution. In addition stuck to the bottom of the plate pellets difficultly enough cleaned off the bottom with a knife, mounted on a plate and sliding it towards the bottom of particles. Fan-shaped flow of pellets comes to the vertical wall of the knife set at an angle of 45° in the zone 10-11 o'clock He alters the trajectory of the layer of granules, and the area on which they move, is 75-90% of the area of the plate. Periodic effects of the activators with the rotational speed of nAK=600-1000 min-1the exposed layer of granules at the bottom of the plate, comprising 15-30% of the total area of the plate that is optimum conditions for mechanism granulometry. When the rotational speed is less than 600 rpm-1continued growth of the granules, and at speeds greater than 1000 rpm-1grinding granules, which does not allow for od is godnosti of granulometric composition.

With large granules, getting in the zone the activator, are being exposed to it, which leads to the destruction of large agglomerates of granules. After that, due to the centrifugal force of the granules reached a given size, rolled over the side of the plate in the discharge pipe and removed from the disc pelletizer.

Thus, the active mixing of the material activator increases the uniformity of the granules obtained from multicomponent mixtures (from 0.5 mm to 8.0 mm 1-3 mm), thus reducing the time of granulation. For example, the feed mixture in the presence of the activator plate granulator, time granulation is reduced from 15-20 minutes to 8-10 minutes the yield of granules of the desired class (commodity fraction, size 1-3 mm) increases to 90% against 55% in the conventional plate granulator without activator.

The activator provides intensive movement of particles between the blades at speeds greater than the speed of movement of the particles on the plate and their interaction with the Board plate. Given the placement of the activator, technological and operational parameters of his work provide the output from the plate receiving pellet density, durability and particle size distribution.

In the study of the process of granulation was carried out series of experiments. As source material COI is litovali hydrated granular chicken feed, contains 9 components with an average particle size of dEQ=3 mm Granulation is as follows. As a binder used gelatino-sugar solution. The original mixture is moistened and simultaneously granularit in the mixer speed type, with the amount of added binder is 18 wt.% of the total number of input binding (see experience No. 2 of the table). Then the resulting mixture, consisting of homogeneous crushed and activated microgranules (centers granulometry) when the plastic strength of 15 kPa, overload on the plate granulator. On moving along the surface of the plate layer of particles periodically serves the remainder of the binder, which is served in the lower area by the area of the plate constituting 30% of its total surface. These values affect the efficiency growth of the granules at this stage of granulation.

In the interval between inputs Vasudeva in the lower zone of the plate periodically affect the moving layer of the activator with the rotational speed of 800 rpm-1during the time average of 30-70% of the total time of the granulation on the plate.

After obtain pellets of the mixture is discharged, then dried and determine particle size distribution by sieving method on the sieve, and the granules for compression. The table shows the results of the research process Gras is lirovaniya on the plate (D t=350 mm) with activator depending on operating parameters of the process.

No.Process indicators granulationNumbers of experiments
123"prototype"
1Performance on the initial mixture (G), kg/h99,5108
2The amount of binder applied to regranulates, % from the total amount of the binder applied to the plate22183035
3Plastic strength of the mixture in regranulate Pm, kPa12152530
4The residence time of the mixture in regranulate τCR, min12 25
5The total amount of binder applied to the plate Wt, mass %8151514
6The residence time of the mixture on the plate τt, min9101215
7The working surface of the bottom plate %, of the total surface70908080
8The angle of the plate α, deg45485048
9The frequency of rotation of the plate nt, min-145607062
10The area of the spray S, in % of the total area of the bottom of the plate,20 303530
11Speed activators nAK, min-16008001000-
12The zone of influence of the activator on the layer of granules of the area of the plate SAK, %152030-
13While working activator of the total time of granulation τAK, min757-
14The strength of the dried granules σSG, MPa1,5210,8
15Output of marketable fractions (1-3) mm %90958055

In the above Table shows the performance of the inventive process and the appropriate show is whether the prototype method (EN 2410152, B01J 2/14, 2011). As follows from the description of the prototype method, in a known way to obtain granules with an average diameter of 5 mm, and in the present method, the average diameter is 1-3 mm, that is, the inventive method is achieved by narrowing of the granulometric composition of the product and is more monodisperse product. Confirmation of the achieved technical effect is the index of commodity output, which reaches maximum 95%, and in the method-prototype only 55%. In addition, when carrying out the granulation process of the inventive method compared with the method of the prototype increases the strength of the resulting pellets of 1.5-2.0 MPa, and the method prototype granule strength is 0.8 MPa.

Thus, when the aggregate of the stated essential features provided the stated goal of increasing the yield of marketable fractions, the increase in the uniformity of particle size distribution and strength of granular product using a wide class of binder. This technical result is achieved by using a combination of essential features that characterize the proposed method of granulating polydisperse multicomponent mixtures on the plate granulator. The claimed method allows you to pelletize multicomponent granular mixture with a particle size of from 1 to 7 mm (for example, curini the feed, contains 9 components), as well as mixtures of enzymes and biologically active preparations.

Method of granulating polydisperse multicomponent mixtures, including batching, mixing, and subsequent hydration of the binder, preliminary granulation and pelleting the washing carried out on a rotating inclined plate with a velocity exceeding the critical speed of rotation of the plate, with simultaneous wetting by spraying a binder, characterized in that the preliminary granulation is carried out in regranulate high-speed type with mechanical activation of the mixture, which is added to the binder in a quantity amounting 18-30 wt.% from the total mass of the binder before the establishment of the plastic strength of the mixture at the level of 12-25 kPa, after which the microspheres are injected on the surface of the plate, rotating counterclockwise and when periodic finely dispersed spray of binder in the amount of 8-15% of the total mass of the granulated material in the area of the plate which constitutes 20-35% of the total area of the bottom of the plate, while in the interval between inputs binder carry out periodic influence of the activator with the rotational speed of 600-1000 min-1on the bottom layer of granules comprising 15-30% of the total area of the plate.



 

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