Method of obtaining crystalline substances

FIELD: chemistry.

SUBSTANCE: method includes crystallisation, further separation and drying of crystals with an application of vibration fluctuations in the range of fluctuation accelerations 20-70 m/s2 and amplitude 2-5 mm, with separation of crystalline substances from a liquid phase being carried out by the supply of the suspension to filtering partitions, installed with a clearance one under another in a descending order of the cell size and performing directed fluctuations at an angle from 30° to 60° to horizontal.

EFFECT: invention makes it possible to obtain monodisperse fractions of crystalline substances of a specified granulometric composition, which results in an improvement of quality of the target crystalline products and increases efficiency of processes of drying and filtration, to eliminate additional operations of grinding or crushing.

3 dwg, 3 tbl, 3 ex

 

The invention relates to methods for dispersed crystalline substances and can be used in chemical, pharmaceutical and other industries. The most expedient is the use of this method in the pharmaceutical industry in the production of montmorillonite and synthetic substances of medicines.

A method of obtaining crystalline products, which consists in conducting the processes of crystallization, separation and drying of the crystals when applying vibratory oscillations, which is carried out in an apparatus for obtaining crystalline substances (see Avts of the USSR №1570740, CL B01D 9/00. B. I. No. 22. 1990; Avsw of the USSR №1773431, CL B01D 9/00. B. I. No. 41, 1992; RF Patent No. 2 287354, B. I. No. 32, 2006).

The disadvantage of this method is that its implementation is impossible to obtain a monodisperse fraction of the crystalline product of the specified particle size distribution. High residual humidity polydisperse precipitate after filtering reduces the efficiency of drying, this can form agglomerates, which causes the need for additional operations of milling and grinding of the final crystalline product.

It is known that in some cases the grinding causes the destruction of the internal structure of a material, for example, montmor is lonita - one of the most popular finely dispersed materials. Montmorillonite is a unique clay natural aluminosilicate, which allows you to create different types of polymer nanocomposites is a strategic raw material for nanotechnology of any state. Also used in the pharmaceutical industry, is a natural enterosorbent, contains in ionic form almost all macro - and micronutrients needed by the human body, has a protective effect against intestinal mucosa, selective sorption properties, which are explained discode-crystal structure, is a donor colloidal silica to humans. Getting montmorillonite responsible pharmacopeial purity standards and granulometric composition, has a number of additional limitations of technological nature, which makes it difficult for its industrial production by known methods. So, in conclusion, Kharkiv national University of pharmacy, the drying temperature, which is not disturbed crystal lattice of montmorillonite and retains its natural properties, should not exceed 35°C.

In addition, it is known that dry grinding affects the structure of montmorillonite (Boev NM, below AM, Nasedkin CENTURIES Mat. The 2nd international. proc. The industrial minerals and scientific-technical progress". Moscow, may-June, 2007. M: GEOS, p.26-28).

A method of obtaining crystalline substances, such as substances of synthetic drugs, including when applying vibratory oscillations of crystallization, separation and drying of the crystals in the range of accelerations of vibrations 20-70 m/s2and the amplitude of 2-5 mm (Patent RF №2132714, bull. No. 19, 1999). This method is the closest to the claimed method according to the totality of symptoms and was selected as a prototype.

The main disadvantage of the prototype is that during its implementation, it is impossible to obtain a monodisperse fraction of the crystalline product of the specified particle size distribution, for example, montmorillonite, supersewn polystyrene, etc. in Addition obtained after filtration of polydisperse sediment has a high residual moisture. This is because the separation of the dispersed crystalline substances from the liquid phase is carried out by feeding the suspension into committing vertical oscillations of the filter wall, the cell size which is smaller than the smallest particles of the solid phase of polydisperse suspensions. When this filter partition holds both large and small solid phase of the suspension, forming a layer of sludge, the height of which in the process is constantly increasing. Polydispersities contributes to the formation of dense packing of the particles of the solid phase, smaller elementary then, the increase in hydraulic resistance and capillary forces clutch which holds the liquid phase in the sediment and which must be overcome to dehydration under the action of vibration. This reduces the effectiveness of subsequent drying, but because of the possible formation of agglomerates necessary additional operations of milling, grinding and classification the final crystalline product.

The present invention is to provide a method which would allow to obtain monodisperse fractions of crystalline substances specified particle size distribution.

The solution of this problem is achieved by the claimed method of obtaining crystalline substances, including crystallization, separation and drying of the crystals when applying vibratory oscillations in the range of accelerations of vibrations 20-70 m/s2and the amplitude of 2-5 mm, and the separation of crystalline substances from the liquid phase is carried out by feeding the suspension into a filtering partition, installed with a clearance of one below the other in descending order of the sizes of cells and performing directional oscillations at an angle from 30° to 60° to the horizontal.

The technical result of the invention is to provide a monodisperse fractions of crystalline substances desired particle size distribution and the mouth of Annie additional operations of refining and/or grinding.

The inventive method of obtaining crystalline substances is carried out in the apparatus shown in figures 1-3. Figure 1 shows the position of the apparatus during the process of crystallization, figure 2 - position of the apparatus in the separation of crystalline compounds obtained by crystallization or other method from the liquid phase, and figure 3 shows the position of the apparatus when carrying out drying the obtained monodisperse crystalline product specified size.

The device consists of vibrooccasion 1, a cylindrical working chamber 2 with a heat exchange jacket 3, the filter element 4. Cylindrical working chamber 2 is installed on the vibrooccasion 1 with the possibility of a coup by 180° about the horizontal axis, as shown in figures 1 and 2. The pipe 5 is coolant, pipe 6 to the substrate, through the pipe 7 unload the target product, through pipe 8 unload the coarse fraction and impurities, the nozzle 9 is designed for removal of filtrate. The filter element 4 is made in the form of a set of filter partitions 10, 11, 12 and 13, as shown in figure 2, installed with a clearance of 20 mm one below the other in order of decreasing cell size. Inclined plate 14 is intended for feeding the suspension through the filler neck 15 on the filter septum. The inclined plate 16 is intended for the drainage of the filtrate cher the h pipe 9. The vibrooccasion 1 allows you to change the angle of application of directional fluctuations and transmitted to the working chamber 2.

The inventive method of obtaining crystalline substances is as follows. When the position of the working chamber of the apparatus shown in figure 1, and the angle of application of directional fluctuations of α=90° through the pipe 6 download raw vibratory influence conduct the process of obtaining crystalline substances by crystallization or other means, for example, suspensionen. Then, the separated crystalline substance from the liquid phase. For this purpose, the working chamber is turned 180°, and the angle of application of directional fluctuations α deviate from the vertical, as shown in figure 2. The suspension on the inclined plate 14 through the filler neck 15 is supplied to a filtering partition 10, 11, 12 and 13. In the feed area of the suspension below the filler neck 15, there is a separation of the solid phase fractions. On the filter wall 10 delayed the largest particles and directional oscillations immediately discharged from the service zone of the suspension, not forming a precipitate and not preventing the free passage of the liquid phase with the smaller particles to the next filter wall 11 and further partitions 12 and 13. Directional vibrations vibrotransporter sediment for each of istrouma partitions. Through the nozzles 8 of the apparatus is removed coarse unconditioned sludge. Target crystalline product specified dispersion is delayed by a partition 13 with the finest cells and acts on the heated bottom of the working chamber 2. Drying of the target crystalline product specified dispersion is performed during the vertical direction fluctuations in librarybased layer, as shown in figure 3.

A causal relationship between the set of features listed in the claims, and the above technical result is the following. In the present method of obtaining crystalline substances, including crystallization, separation and drying of the crystals when applying vibratory oscillations in the range of accelerations of vibrations 20-70 m/s2and the amplitude of 2-5 mm, the separation of crystalline substances from the liquid phase carried out petroccione, feeding polydisperse suspension for a few vibrating filter partitions arranged with a gap under one another in descending order of the sizes of cells and performing directional fluctuations. This allows each of the filtering partitions sequentially extracted from the incoming stream of the suspension, only the solid phase particles that are larger than the cell size of this filtering partition. As shown the respective partitions make directional oscillations, then hold each partition of the particles of the solid phase under the action of vibration is continuously discharged from the zone of the feed suspension, not forming a precipitate and not preventing the free passage of the liquid phase together with smaller particles of the solid phase to the next filter wall. Directed called oscillations, having vertical and horizontal components. The removal of particles of the solid phase from the zone of the feed suspension occurs under the action of the horizontal component of the acceleration of the oscillations is equal to Aω2cosα, where A is the amplitude, ω is the circular frequency, ω=2πf, where f is the frequency (Hz), α is the angle of application of horizontal directional oscillations (deg.) (S.M. Chistovalov, E. Melnikov, "Kinetics of the process of continuous vibratory separation of coarse suspensions". Chemical and petroleum engineering, No. 11, 1990, p.12-13).

Monodisperse layer of residue on each of the partitions is formed only at the exit from the zone of the feed suspension and directional fluctuations of sediment transported by each of the filtering walls. Simultaneously with vibrotransporter sediment is the extraction of capillary bound moisture and fracture patterns of sediment under the action of vibration. Sediment is an unconsolidated porous structure with winding then is, permeating layer in all directions. The liquid phase filling the pore space of the layer of sediment is retained therein by the forces of capillary adhesion and surface tension. Under the action of the vertical component of the directional oscillations, namely acceleration fluctuations Aω2sinα, extracts moisture from the layer of sediment (E.A. Nepomnyashchy, S.M. Chistovalov. "Patterns of entrainment of moisture from the layer of granular material under the influence of vibration". Russian journal of applied chemistry, No. 1, 1985 press, p.104-109). The efficiency of the separation of the suspension is determined by the amount of the residual moisture content of sludge. For monodisperse sediment density of packing of the particles and the magnitude of the capillary forces of adhesion that must be overcome for its dehydration, lower than the polydisperse sedimentation. Therefore, improving the efficiency of the separation of the suspension and drying the crystalline substance.

The invention is illustrated by the following examples of its implementation.

Example 1. Obtaining monodisperse crystalline montmorillonite (particle size 40 μm)

Montmorillonite, meet pharmacopoeial requirements, dispersion of 40 μm obtained from bentonite clay of Kurinskogo field, containing up to 90% montmorillonite.

The method is carried out in the above-described apparatus for obtaining crystalline substances, shown in figures 1-3. On shaking prevod 1, ensuring creation aimed at an angle α° to the horizontal) and regulated (in terms of frequency f, amplitude A and the acceleration Aω2vibrations set with the possibility of a coup by 180° working chamber 2 with a heat exchange jacket 3, a filter element 4, the technological connections 5-9.

When the position of the working chamber, shown in figure 1, through the pipe 6 into the working chamber 2 serves feedstock lump bentonite clay and ethanol in a weight ratio to 1:20, in the heat exchange jacket 3 through pipe 5 serves the coolant with a temperature of 35°C. Include vibrooccasion and in the specified range of vibration parameters in the vertical direction fluctuations suspension bentonite clay in ethanol for 0.5-1.5 hours.

After suspending the working chamber is turned by 180° and place it in the position shown in figure 2, and the angle of application of directional fluctuations α deviate from the vertical, to separate the crystalline monodisperse montmorillonite dispersion of 40 μm from the liquid phase. When working vibrooccasion suspension by an inclined plate 14 through the filling neck 15 is supplied to a filtering partition 10, 11, 12 and 13. In the area of flow of the liquid phase of the suspension passes freely through the filter septum due to the fact that the swelling of the solid phase particles continuously re is out of the zone under the action of directional fluctuations. Hold on the filter walls 10, 11 and 12 (cell size 140, 71, 56 μm, respectively) particles of montmorillonite, sand and impurities are transported along the walls under the action of the horizontal component directed vibrations and removed from the apparatus through the pipe 8. On the filter septum 13 delayed the solid phase particles size of 40 μm, which are transported on the wall and act on the heated bottom of the working chamber 2. The filtrate on the inclined plate 16 is removed from the apparatus through the pipe 9 into the receiving tank. The process of separation and fractionation of the suspension is from 10 to 25 minutes. Further drying monodisperse montmorillonite specified particle size distribution until a constant weight is performed during the vertical direction of the oscillations, as shown in figure 3, in librarybased layer at a temperature of 35°C. the drying Time is from 11 to 27 minutes. Dry monodisperse montmorillonite discharged through pipe 7, connected by a flexible chute with the receiving tank of the finished product.

Example 2. Obtaining monodisperse crystalline KNO3 (dispersion (40 μm)

In the position of the working chamber, shown in figure 1, through the pipe 6 in 2 working chamber is poured a saturated solution of KNO3. The temperature of the coolant in the jacket at the time of fill is 70°C. To the installization conduct when working vibrooccasion and vertical oscillations, the temperature of the coolant in the jacket reduced from 70°C to 10°C. the Time for crystallization is 0.5; 2 and 5 hours in each experiment. Then carry out the separation of a crystalline substance from the liquid phase, for which the working chamber is turned 180° and deviate from the vertical, the angle of application of α oscillations. The suspension on the inclined plate 14 through the filling neck 15 is supplied to a filtering partition 10. 11, 12 and 13. In the area of flow of the liquid phase of the suspension passes freely through the filter septum due to the fact that the swelling of the solid phase particles are continuously discharged from the zone under the action of directional fluctuations. Hold on the filter walls 10, 11 and 12 (cell size 140, 71 and 56 μm, respectively) particles KNO3larger than 40 μm under the action of the horizontal component directed vibrations are transported on the walls and removed from the apparatus through the pipe 8. On the filter septum 13 delayed the solid phase particles size of 40 μm, which are transported on the wall and act on the heated bottom of the working chamber 2. The filtrate on the inclined plate 16 is removed from the apparatus through the pipe 9 into the receiving tank. The time of the separation and fractionation of the suspension ranges from 18 to 30 minutes. Subsequent conductive drying KNO3given the granulomas the historical composition is performed during the vertical direction of the oscillations, as shown in figure 3. in librarybased layer at a temperature of coolant in the jacket 70°C. the drying Time is from 30 to 47 minutes. Dry KNO3unloaded through the pipe 7, connected by a flexible chute with the receiving tank of the finished product.

Example 3. Obtaining monodisperse crystalline inderal (40 μm)

In the position of the working chamber, shown in figure 1 through the pipe 6 in 2 working chamber is poured a saturated solution of inderal Temperature of the coolant in the jacket at the time of casting is 90°C. Crystallization was carried out at the working vibrooccasion and vertical oscillations, the temperature of the coolant in the jacket reduced from 90°C to 5°C. the Time for crystallization is 0.5; 2 and 5 hours in each experiment. This is followed by separation of the crystalline inderal from the liquid phase, for which the working chamber is turned 180° and deviate from the vertical, the angle of application of α oscillations. The suspension on the inclined plate 14 through the filling neck 15 is supplied to a filtering partition 10, 11, 12 and 13 installed with a clearance of 20 mm one below the other in order of decreasing cell size. In the area of flow of the liquid phase of the suspension passes freely through the filter septum due to the fact that the swelling of the solid phase particles are continuously discharged from the zone under the action aimed Coleman the th. Hold on the filter walls 10, 11 and 12 (cell size 140, 71 and 56 μm, respectively) particles inderal larger than 40 μm under the action of the horizontal component directed vibrations are transported on the walls and removed from the apparatus through the pipe 8. On the filter septum 13 delayed the solid phase particles size of 40 μm, which are transported on the wall and act on the heated bottom of the working chamber 2. The filtrate on the inclined plate 16 is removed from the apparatus through the pipe 9 into the receiving tank. The time of the separation and fractionation of the suspension ranges from 18 to 30 minutes. Subsequent conductive drying inderal specified particle size distribution is performed during the vertical direction of the oscillations, as shown in figure 3, in librarybased layer at a temperature of coolant in the jacket 90°C. the drying Time is from 30 to 47 minutes. Dry inderal discharged through pipe 7, connected by a flexible chute with the receiving tank of the finished product.

The results of the experiments are presented in tables 1-3, where the sign "+" denotes positive results - obtaining a crystalline substance (montmorillonite KNO3and anaprilin) of a given particle size distribution; the sign "-" denotes experiments in which failed to obtain a crystalline substance of ass is Noah dispersion.

Table 1
The results of experiments on the separation of the montmorillonite dispersion of 40 μm from ethanol at f=15 Hz and A=1, 2, 3, 4, 5, 6, 7 mm
Aw2(m/s2) α (°)1020304050607080
10--------
20--------
25--------
30-++++++-
35-++++++-
40-++++++-
45-++++++-
50-++++++-
60-++++++-
70--------
80--------

Table 2
The results of experiments on the separation KNO3(particle size 40 μm) from the liquid phase at A=3 mm and f=8, 12, 15, 20, 22 and 25 Hz
Aw2(m/s2) α(°)1020304050607080
10--------
20--------
25--------
30-++++++-
35-++++++-
40 -++++++-
45-++++++-
50-++++++-
60-++++++-
70--------
80- -------

Table 3
The results of experiments on the separation of inderal (40 μm) from the liquid phase at A=4 mm and f=7, 10, 15, 18, 20 and 22 Hz
Aw2(m/s2) α(°)1020304050607080
10--------
20--------
25-- ------
30-++++++-
35-++++++-
40-++++++-
45-++++++-
50-++/td> ++++-
60-++++++-
70--------
80--------

Thus, it was found that, in contrast to known methods, the inventive method of obtaining crystalline substances, use of vibration exposure in the range of accelerations from 20 to 70 m/s2when the amplitudes from 2 to 5 mm, and the above described apparatus, including several filter partitions mounted with clearance one below the other in descending order of cell size and sovershaem the x-directional vibrations at an angle from 30° to 60° to the horizontal, allows to obtain monodisperse crystalline substances desired particle size distribution. Monodisperse fractions easier dehydrated, consequently, increases the efficiency of the separation of the suspension and drying the crystalline substances and does not require additional grinding of the target product, aggravating its structure.

It is shown that under vertical vibrations, and when you use one of the filtering partitions cannot obtain a crystalline substance of a specified particle size distribution, i.e. only the combination of all the features of the invention enables the achievement of a technical result.

The method of obtaining crystalline substances, including crystallization, subsequent separation and drying of the crystals when applying vibratory oscillations in the range of accelerations of vibrations 20-70 m/s2and the amplitude of 2-5 mm, characterized in that the separation of crystalline solids from the liquid phase is carried out by feeding the suspension into a filtering partition, installed with a clearance of one below the other in descending order of the sizes of cells and performing directional oscillations at an angle from 30° to 60° to the horizontal.



 

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