RU2576438C1 - Method of producing granular regenerative product using roller compactor - Google Patents

Abstract

FIELD: technological processes.

SUBSTANCE: invention relates to production of products for air regeneration used in life support systems. Method of producing granular regenerative product using roller compactor includes loading of charge into roller compactor, having a number of rollers rotating in opposite directions, and pressing the mixture between rolls. Difference of the proposed method is that charge in roller compactor is supplied by screw feeder, a spacer pressing force is regulated by changing the rotation speed of the feeding auger, clearance between rolls is set in the range from 3 to 12 mm with linear speed of pressing from 2 to 12 m/min, molded tiles are crushed in the sieve mill, followed by fractional sieving on vibrating screen. Pressing rollers during the pressing process are cooled to 15-25°C. Granules after screening are subjected to thermal treatment at temperature of 150±10°C.

EFFECT: continuous process of granulation, increased efficiency and reduced costs.

6 cl, 1 dwg, 3 tbl

Description

The invention relates to methods for producing products for air regeneration used in human life support systems.

A known method of granulation of dispersed materials, according to which the granulation is carried out in the following successive stages: dosing, mixing, subsequent wetting with a binder, preliminary granulation and granulation by rolling. In this case, the preliminary granulation stage is carried out in a speed-type apparatus with mechanical activation of the initial mixture, to which a binder is added in an amount of 20-35 wt. % of the total mass of the binder to establish the plastic strength of the mixture at the level of 20-30 kg / m ² . The pelletizing step by rolling is carried out by introducing the microgranules obtained in the first granulation step onto the surface of the plate rotating counterclockwise and at a speed exceeding the critical speed of rotation of the plate. This stage is carried out with simultaneous wetting by periodic fine dispersion of the binder in an amount of 4-15% of the total binder mass (RF patent No. 2515293, IPC B01J 2/14, 2014).

The invention allows to granulate multicomponent granular mixtures with a particle size of 1 to 7 mm, as well as a mixture of enzymes and biologically active preparations. The main disadvantage of this solution is the unsuitability of the known method for granulating regenerative products, the processing of which requires at least the presence of a protective medium that excludes the contact of the product with water vapor and acid gases in the air. In addition, the known method does not achieve the specified density of granules, particle size distribution of the product, bulk density of the product and mechanical strength or resistance to abrasion.

Currently, the following technologies are used to produce regenerative products:

- static pressing of multi-channel blocks and briquettes;

- static pressing of tablet blocks with subsequent crushing to obtain granules of irregular shape;

- tableting using tablet machines.

The disadvantages of the technology for producing grain products are as follows:

- low productivity due to restrictions on the speed of pressing (slow stroke of the press, the need for exposure);

- restrictions on the thickness of the layer of the pressed block (tablet, briquette), uneven distribution of density with a layer thickness of more than 20 mm;

- significant pressing efforts due to losses to overcome the friction created by the walls of the molds, which requires the use of large-sized presses and equipment;

- multistage grinding of tablets to obtain the target grain fraction, and there is a high degree of substandard fractions, up to 45% of the amount of product fed to the crushing;

- repeated return of a large fraction to re-crushing (up to 5 times) manually;

- long-term presence of superexide compounds in the open air, leading to interaction with water vapor and carbon dioxide (especially in the summer), deterioration of chemical properties (Technological regulations inv. No. 73 kt, CKTE. 154.2003 from 2004).

Known adopted for the prototype method of producing multiparticles using a roller compactor. Roller compactors are widely used for dry granulation. The roller compactor pushes the smallest particles from the pharmaceutical mixture between the rotating rollers (rollers) in order to compact and compact the powders to a smaller volume, forming a compact (pressed powder blank) or a thin sheet. Then these compacts or thin sheets are crushed to form granules, from which tablets can then be compressed.

A feature of the known invention is the use of roller compactors for direct molding of multiparticles, eliminating the need for a separate tablet press or tabletting device. Roller compactors provide the possibility of implementing a continuous production method instead of a batch process based on the use of tablet presses (RF patent No. 2451504, IPC A61K 9/20, 2012).

In General, the known invention provides a method for the production of pharmaceutical compositions in the form of multi-particles (consisting of many particles). A feature of this method is the compaction (pressing) of the pharmaceutical mixture in a roller compactor with rollers rotating in opposite directions. The surfaces of the rollers have recesses (recesses) or molds in order to obtain multi-particle compacts of the desired shape and size from the mixture.

According to a known method, a pharmaceutical mixture containing a therapeutically active compound suitable for administration to a mammal and at least one pharmaceutically acceptable excipient is loaded into a roller compactor having a series of rolls rotating in opposite directions, each roll having a plurality of recesses for receiving said mixture, which correspond to recesses of exactly the same shape on the roll rotating in the opposite direction, and this mixture is pressed between rotating in in opposite directions by rollers with the direct formation of symmetrical mini-tablets without the need for a separate stage of pressing on a tablet press.

The objective of the invention is to obtain a granular regenerative product using a roller compactor.

The technical result is to ensure the continuity of the granulation process, which minimizes the duration of the granulation process, provides increased productivity and reduced costs.

The solution to this problem is provided by the fact that according to the method for producing a granular regenerative product using a roller compactor, in which the charge is loaded into a roller compactor having a series of rolls rotating in opposite directions, and this mixture is pressed between the rollers rotating in opposite directions, the charge being the roller compactor is fed by a screw feeder, the magnitude of the spacer force during pressing is controlled by a change in the rotational speed of the feeding screw, p between the rolls is set in the range from 3 to 12 mm with a linear pressing speed of 2 to 12 m / min, the molded tile is crushed in a sieve mill, after which fractional sieving is carried out on a vibrating screen.

The granules after sieving are subjected to heat treatment at a temperature of 150 ± 10 ° C and the exposure time at a given temperature of 6 ÷ 10 hours

Pressing rolls during the pressing process are cooled to a temperature of 15-25 ° C.

The preparation of a granular regenerative product is carried out upon reaching a relative humidity of 10-12% and an air temperature of 23 ± 2 ° C.

In automatic mode, the number of revolutions of the feed screw is adjusted, receiving data from the pressure force sensor mounted on the compactor roll.

Granules have an average particle size of greater than 1 to about 6.5 mm.

Feeding the batch to the roller compactor with a screw feeder, adjusting the spacer force during pressing by changing the speed of the feed screw, setting the gap between the rolls from 3 to 12 mm at a linear pressing speed of 2 to 12 m / min, followed by crushing the molded tile in a sieve the mill and fractional sieving on a vibrating screen ensure the achievement of the optimal ratio between the density of the granules from the regenerative product and their mechanical strength and resistance to abrasion. The density of the moldable tile depends on the properties of the initial charge, the size of the gap between the rolls, the frequency of rotation of the rolls and the pressure developed by the screw feeder and depending on the frequency of rotation of the screw. By selecting the optimal values of these parameters, it is possible to obtain a product suitable for outfitting respiratory protective equipment with a maximum protective action time. When crushing and fractional sieving, the particle size distribution and bulk density of the product are achieved, which allows to achieve the required packing density and reduce breathing resistance when used in respiratory protection. Setting the gap between the rolls in the range from 3 to 12 mm ensures uniform density of the pressed tiles from the regenerative product, while at a thickness of less than 3 mm, to achieve the required strength, it is necessary to increase the density, which affects the stoichiometric properties of the product, the same thing happens when the gap between the rolls is greater 12 mm due to uneven thickness.

At a linear pressing speed of less than 2 m / min, tile overconsolidation occurs, and at a speed of more than 12 m / min, a uniform density of the product is not achieved. The thickness of the pressed tile is selected within the specified range so that the density of the tile is as uniform as possible over the layer, which ensures the stability of the properties of the final granules. In this case, unlike static pressing in the mold, the pressing forces in the compactor are directed to the material layer from two opposite sides, which additionally ensures uniform distribution of density across the layer. In a sieve mill, which is hermetically mounted on the discharge opening of the compactor, the pressed tile is rotor pressed through holes of a given size in the mill grid, therefore granules are not formed larger than the holes in the sieves. A classifier or screen installed under the discharge opening of the sieve mill separates the main fraction from the fine reture, which is collected in a container and returned to the preparation of the charge. The combination of all plant elements in a single line, as well as the high productivity of the line minimizes the time the product is in the open air, thereby reducing the sorption of moisture and carbon dioxide by the mixture and granules.

The heat treatment of granules after sieving at a temperature of 150 ± 10 ° C and the exposure time at a given temperature of 6-10 hours provides an increase in the mechanical strength of the granules without increasing their density by relieving internal stresses arising from pressing and crushing.

The cooling of the press rolls during the pressing process to a temperature of 15-25 ° C ensures that product does not stick to the surface of the press rolls and prevents the particles from sticking to the surface of the tile.

Carrying out the production of a granular regenerative product upon reaching a relative humidity of 10-12% and a temperature of 23 ± 2 ° C, which corresponds to a calculated moisture content of 2.47 g / cu. meter (2.076 g / kg of dry air), provide the ability to leave the unit without washing for at least 7 days. During this time, no “saponification” of the product is observed, the color of product residues inside the unit remains yellow after 7 days, which indicates a slight absorption of moisture from the room air.

Correction in the automatic mode of the number of revolutions of the feed screw according to the data from the pressing force sensor installed on the compactor roll ensures the correction of the number of revolutions of the screw. In this case, the fluctuations in the pressing force are smoothed out, increasing the uniformity of the pressed tile. The time to reach the regime and the amplitude of the oscillations depend on the uniformity of the supply of material to the pressing zone.

Obtaining granules with an average particle size of from more than 1 to about 6.5 mm ensures optimal resistance of the granular product in the apparatus and increases its packing density in the apparatus.

In the diagram of FIG. 1 shows a scheme for producing a granular regenerative product.

The list of items indicated in the diagram

1 - the capacity of the prepared starting components;

2 - charge mixer;

3 - screw feeder;

4 - roller compactor;

5 - pressure sensor (spacer pressure);

6 - control unit;

7 - connecting element;

8 - sieve mill;

9 - vibrating screen;

10 - the capacity of the finished granules;

11 - line return retur to mix.

The method is implemented as follows.

Potassium superoxide-based components were fed from the container of prepared initial components 1 to mixer 2. After the mixture was mixed with the screw feeder 3, which precompressed, the mixture was fed into the space between the rollers of the roller compactor 4. The pressing was carried out under the action of the forces created by the rollers at rotation towards each other and measured by the sensor pressing forces (magnitude of spacer pressure) 5, connected to the control unit 6. Compressed tile made of rollers of the compactor 4 through the connecting element 7, made in the form of a flat shell of optically transparent material (for example, silicone rubber), was fed into a sieve mill 8. In a sieve mill 8, crushed pressed tiles were crushed with a rotor equipped with percussion elements that push material through holes of a predetermined size in the grid of the mill (5 mm), so granules larger than holes in the sieves are not formed. The obtained granules were fed into a vibrating screen 9 installed under a discharge opening of a sieve mill 8, in which the main fraction was separated from a shallow retura through a grid installed in a vibrating screen with a mesh size of 2.0 mm. Finished granules entered the container of finished granules 10. Fine retur at the line of returning the retur to mixing 11 was returned to the preparation of the mixture.

In the automatic operating mode of the installation, the screw speed was adjusted, receiving data from the pressing force sensor 5 mounted on one of the rollers of the compactor 4. The program ensures maximum smoothing of fluctuations in the actual values of the pressing force and at the same time brings them closer to the set value. The time to reach the regime and the amplitude of the oscillations depend on the uniformity of the supply of material to the pressing zone.

Examples.

In total, 5 compacting operations were carried out:

Example 1, the gap between the rollers is 2 mm, the feed material is a charge;

Example 2, the gap between the rollers is 4 mm, the feed material is a charge;

Example 3, the gap between the rollers is 5 mm, the feed material is a charge;

Example 4, the gap between the rollers is 5 mm, the feed material is the charge + retur after the third operation (50/50);

Example 5, the gap between the rollers is 14 mm, the feed material is a charge.

In the process of pressing, the following performance indicators of the compacting unit, shown in Table 1, were determined and recorded.

Table 1 Example Number The gap between the shafts, mm Auger, rpm (set values) Rollers, rpm Mill rpm Set pressing force, kN one 2 fifteen 10 one hundred 45 2 four eleven 10 one hundred 40 3 5 25 10 one hundred 45 four 5 twenty 10 one hundred 45 5 fourteen 25 10 one hundred 40 Parameters 3 and 4 of the tests are listed in the electronic database of recipes for the compactor

Samples were taken from the products obtained during the tests and sent for analysis.

Test results.

The particle size distribution and mechanical strength of the products are shown in table 2:

table 2 Example Number Fractional composition,% Strength (3.5-5.5),% More than 5.5 mm 3.5-5.5 mm 2.0-3.5 mm 1.0-2.0 mm Less than 1.0 mm one - - 72.00 18.00 10.0 88,20 2 - 27.14 63.70 7.58 1,58 76.78 3 0.60 42.80 50.80 4.80 1.00 75.70 * four 0.20 37.00 56,20 5.50 1.10 75.30 5 30,0 60.00 10.00 - - 62.00 Note - * After heat treatment, the strength of the sample was 88.32%.

The product obtained during the tests according to examples No. 3 and No. 4, was thermally processed in accordance with the requirements of the technological regulations of the CTKE. 154-2003 (PRZ), after which samples were taken to equip two SPI-20 self-rescue cartridges and tests were carried out on the time of the protective effect on the artificial lungs installation. The product obtained according to example No. 1, was characterized by high density, and according to example No. 5 - low mechanical strength.

The test results are shown in table 3. For comparison, the test results of the PRZ serial product and the requirements of TU for SPI-20 are given.

Table 3 Sample No. (batch, packaging) PDR in SPI-20 at 35 l / min, min Resistance mm water Art. T _vd ° C C (CO ₂ ),% Experimental product one 25 75/80 46.4 2.40 2 25 55/60 48.8 2.27 PRZ Series Product n. 2 pack. 47 25 45/45 49.2 2.27 n. 2 pack. 48 25 50/60 47.1 2.29 n. 2 pack. 49 25 50/55 47.0 2,38 TU requirements - Not less than 20 No more than 80 No more than 50.0 No more than 3,00

Note: The product of examples 1 and 5 was not tested.

The invention provides a continuous granulation process, an increase in productivity and a reduction in costs.

Claims (6)

1. A method of producing a granular regenerative product using a roller compactor, in which the charge is loaded into a roller compactor having a series of rolls rotating in opposite directions, and pressing this mixture between the rolling rolls in opposite directions, characterized in that that the charge is fed to the roller compactor by a screw feeder, the amount of spacer force during pressing is controlled by changing the speed of the feeding screw, the gap between the rollers is set from 3 to 12 mm at a linear pressing speed of 2 to 12 m / min, the molded tile is crushed in a sieve mill then carry out fractional sieving on a vibrating screen. 2. The method according to p. 1, characterized in that that the granules after sieving are subjected to heat treatment at a temperature of 150 ± 10 ° C and the exposure time at a given temperature of 6 ÷ 10 hours 3. The method according to p. 1, characterized in that the press rolls during the pressing process are cooled to a temperature of 15-25 ° C. 4. The method according to p. 1, characterized in that that obtaining a granular regenerative product is carried out upon reaching a relative humidity of 10-12% and an air temperature of 23 ± 2 ° C. 5. The method according to p. 1, characterized in that in automatic mode, the number of revolutions of the feed screw is adjusted, receiving data from the pressure sensor installed on the compactor roll. 6. The method according to p. 1, characterized in that that the granules have an average particle size of greater than 1 to about 6.5 mm.

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