Method for comprehensively processing brown coal and leonardite into humic fertilizers and preparations and into fuel briquettes, and mechanochemical reactor for processing highly-viscous media

Abstract

Method for converting brown coals, including leonardite, into humic fertilizers and fuel briquettes, comprising first grinding the raw material to less than 3 mm and subsequently treating it with water or water solutions, using liquid-phase mechanoactivation and/or mechanochemical activation, with a duty of water curve ranging from 0.9 to 2.5 and with reaction composition dispersion by chafing and dynamic shift by exposing the medium to a hydraulic impulse of sonic and infrasonic frequencies, by metered introduction of 10 to 40 MJ per cubic meter of mechanical energy, with automatic limitation of the energy in the sub-cavitation area for preventing the mechanochemical reactors from falling into cavitation modes; the method further comprises separation of converted suspension compositions into solid and liquid phases in the centrifugal force field, optionally acidizing the liquid phase with the withdrawal of humic acids from the liquid phase to the heavy phase and recycling of residual water.

Claims

1. A method for continuously converting raw material comprising brown coals, including leonardite, into humic fertilizers and fuel briquettes, wherein the humic fertilizers are selected from: ballast organic fertilizers in the form of suspended gels, ballast organomineral fertilizers in the form of suspended gels, ballastless solutions of humic acid, ballastless solutions of fulvic acid, ballastless dry humic acid salts and ballastless dry fulvic acid salts; wherein said method comprises first grinding the raw material to less than 3 mm, subjecting the ground raw material to two consecutive first and second liquid-phase mechanoactivation and/or mechanochemical activation treatments in a first mechanochemical reactor and a second mechanochemical reactor, respectively, wherein the first liquid-phase mechanoactivation and/or mechanochemical activation treatment in the first mechanochemical reactor comprises either liquid-phase oxidation with hydrogen peroxide or treatment with water and the second liquid-phase mechanoactivation and/or mechanochemical activation treatment in the second mechanochemical reactor comprises aqueous alkaline treatment; and wherein the first and second mechanoactivation and/or mechanochemical activation treatments are performed with dispersion of a medium being converted inside the first and second mechanochemical reactors by chafing and dynamic shift of layers of the medium by exposing the medium to hydraulic impulse with frequencies ranging in the sonic and infrasonic frequencies, by metered introduction into the medium of 10 to 40 MJ per cubic meter of mechanical energy, with automatic limitation of the energy in a sub-cavitation area for preventing the first and second mechanochemical reactors from falling into cavitation modes; the method further comprising mechanical phase division of converted suspension compositions into solid and liquid phases in a centrifugal force field, optionally acidizing the liquid phase with a withdrawal of humic acids from the liquid phase to a heavy phase, and recycling of residual water.

2. The method according to claim 1 wherein flows of compositions being converted are redirected, thus organizing process loops for manufacturing the humic fertilizers.

3. The method according to claim 1, wherein during the conversion of the raw material into the humic fertilizers and fuel briquettes, mineral fertilizers and/or micronutrients are added.

4. The method according to claim 1, wherein to accelerate the process of withdrawal of humic acids from the liquid phase to the heavy phase in the form of coagulated pulp, which is manifested in agglomeration, flocculants are used.

5. The method according to claim 1, wherein during preparation of fulvic preparations, the liquid phase is acidified to pH values in the range 1.5 to 2.5 with a withdrawal of humic acids from the liquid phase to the heavy phase in the form of coagulated pulp while fulvic acid remain dissolved in the liquid phase and gravitational division by density is used.

6. The method according to claim 1, wherein the obtained fulvic acid solution is filtered to remove particles larger than 40 m.

7. The method according to claim 1, wherein humic acid solutions and/or fulvic acid solutions obtained are concentrated by vacuum evaporation at 60 C., and before evaporation, the solutions are subjected to activation by applying high-pressure.

8. The method according to claim 1, wherein the recycling of residual water comprises processes of desalination of said residual water, which are solutions products of alkali and acid neutralization with a separation of salts.

9. The method according to claim 1, wherein during the treatments, volatile substances contained in the raw material component are discharged and the combustible part of the volatile substances is used for heat generation to be used in processes requiring heating.

10. The method according to claim 1, wherein an anti-foaming agent is introduced into a medium being converted.

11. The method according to claim 1, wherein the fuel briquettes being produced are used for process heat generation.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) The invention is explained with a structural process flow diagram and drafts of the design arrangements of the basic equipment.

(2) FIG. 1. The structural process flow diagram of technological processes with software-controlled kinetics of mechanoactivation and mechanochemical activation during the preparation of humic fertilizers, physiologically active salt preparations and fuel briquettes.

(3) FIG. 2. The design arrangement of the mechanochemical reactor for the conversion of high viscosity media with mechanoactivation energy regulation.

(4) FIG. 3. The design and arrangement flow diagram of the moving elements and movement of the mechanochemical reactor high viscosity media being converted.

(5) FIG. 4. The as-built drawing presenting the functional and design peculiarities of the hydraulic puller assembly ensuring the feed of high viscosity media into their conversion area in the mechanochemical reactor.

(6) FIG. 5. The as-built drawing presenting the basis of the design of the mechanochemical reactor rotor disks for cases of processing of anomalously viscous, slow-flowing media.

PREFERRED EMBODIMENT OF THE INVENTION

(7) The embodiment of the invention based on the method of comprehensive conversion of coal series caustobioliths, mostly brown coals and leonardite, into humic organic and organomineral fertilizers and into preparations with the recovery of salts and fuel briquettes is illustrated by the process flow diagram in FIG. 1. THREE SYSTEMS ARE REPRESENTED structurally in this flow diagram: the water treatment and desalination system 1, the fuel briquette preparation and process heat generation system is represented by heat dryer 2, screw extruder 33 and boiler 4, and the PROCESS SYSTEM of comprehensive COAL SERIES CAUSTOBIOLITH CONVERSION itself is represented in detail.

(8) According to the presented method, THE MANUFACTURING PROCESS OF BALLAST ORGANIC or ORGANOMINERAL FERTILIZERS as a product in the form of suspended gels is performed as follows.

(9) Water treatment and desalination system 1 is fed with water through damper 5 from an external water supply system. Based on the performance of the physical and chemical assays of the incoming water, it is treated and softened if necessary. Then, depending on the commercial requirements for the product, cavitation processing of the water may take place [42, 43, 44] with a view to raising its pH from 7 to 7.4 to 8.45 to 9 owing to the saturation of the water with OH hydroxide ions. In this case, HAs are extracted without adding alkalis, as, if the OH ion content in the water is over 10-7 mole/liter, it is an alkaline solution.

(10) However, in this case, to increase the HA yield, it is necessary to process the raw material, e.g. leonardite, before the leaching with a 3 to 5% hydrogen peroxide solution. While this is carried out, hydrogen peroxide concentrate is metered from reservoir 6, through valves 7 and 8, via line 9 to mixer 10, and the dose of treated water is transferred from system 1 through valve 11 and via line 12 to mixer 10 by means of regulating valve 13, whereupon mixer agitator 10 is started for 10 to 15 seconds. When the hydrogen peroxide solution is ready, raw material meter 14, crusher 15, main drives 16, 17 and feeding drive 18 of mechanochemical reactor 19 are started. The moment of the ingression of ground leonardite 20 into feeding drive 18 is recorded by means of sensors (not shown), and the feed of hydrogen peroxide solution into mechanochemical reactor 19 from mixer 10 is started at once by means of metering pump 21 via line 22, through valve 23 and valve 24 via line 25. In this case, the speeds of feeding the reaction components into mechanochemical reactor 19 are calculated in advance based on the indications of raw material 27 water content sensor 26. At the same time, potential metal inclusions 28 are separated from raw material 27 for the faultless operation of the equipment using magnetic separator 29, and purified leonardite 30 enters grinder 15, whereas potential metal inclusions 28 are collected in bowl 31.

(11) The reaction components are converted in mechanochemical reactor 19 at temperatures ranging from 20 to 60 C., with the duty of water curve ranging from 0.9 to 1.2 in OPTIMIZED MECHANOCHEMICAL ACTIVATION MODE INCLUDING:

(12) The automatic regulation of the restriction of the reaction composition by maximum allowable temperature using the opportunity to decrease the speeds of main motion drives 16, 17 of reactor 19 (the physical effect of mechanical equivalent of heat). Control over the temperature of the composition being converted is carried out at its output from reactor 19 by means of thermal sensor 32, and the speeds of drives 16 and 17 are decreased based on the results of this control by means of drive controllers 33. In this case, the speeds of raw material feeding drive 18 and meter 14 are also decreased, while also decreasing the feed of hydrogen peroxide solution into reactor 19 by means of meter pump 21.

(13) The automatic restriction of the shift of mechanochemical reactor 19 to cavitation mode using the opportunity to decrease the speeds of drives 16 and 17 of the main motion of reactor 19 if cavitation noises appear within the volume of the reaction area of the reactor. The control of cavitation noises is carried out by means of acoustic sensor 34, and once they appear, the speeds of drives 16 and 17 are decreased smoothly using drive controllers 33 until cavitation noises disappear. The noise signals from the reaction areas of mechanochemical reactors 19 and 35 obtained by means of acoustic sensors 34 and 71 are communicated to controllers 33 via lines 72 and 73.

(14) The change of the dynamic hydraulic impulse effect on the reaction composition with varying frequencies throughout the range, from 3200 to 16 Hz, for the time of 4 to 6 seconds, the time of the passage of the reaction composition REACTOR DOSE through the reactor. REACTOR DOSE SHALL MEAN THE VOLUME OF THE REACTION AREA of a mechanochemical reactor. In this case, shift speeds are changed from 100 to 0.5 meters per second. Thus, while the reaction composition is converted, each macromolecular cluster of the raw material component is sure to be subjected to mechanical exposure to the shift (with the application of friction forces at a certain path length to the elementary and hypothetical layers of the reaction composition), which is actually the introduction of mechanical energy into this reaction composition. The mechanical activation energy of the reaction composition at such reaction composition parameters amounts to approximately 20 MJ/m3.

(15) A more complete representation of the operation of mechanochemical reactors 19 and 35 may be understandable due to its description as a component of the group of the presented inventions.

(16) While the composition of leonardite with hydrogen peroxide solution is converted in mechanochemical reactor 19, the feed of the solution through the metering pump is controlled using flow meter 36. Converted composition 37 enters knockout drum 38, using which volatile substancesgases 39 forming as a result of chemical reactions and evolving from leonardite as a result of its mechanodestructionare withdrawn from this composition. These volatile substances 39 are collected, condensed and stored in a special gas subsystem (not shown), and then these gases 39 are burnt in boiler 4 with process heat recovered. Converted composition 40 cleaned from gases 39 enters buffer circulation tank 41, from which this composition is sent through valve 42, via line 43 and using feed pump 44 FOR CONVERSION BY LEACHING to mechanochemical reactor 35 while controlling the conversion feed of the composition using flow meter 45 and flow indicator 46.

(17) During the leaching process, the duty of water curve is increased to values ranging from 1.5 to 2.5 by adding an alkali water solution or pH-corrected water to the composition being converted. The liquid component being added is sent to mechanochemical reactor 35 via lines 47 and 164 using metering pump 48, through valves 49 and 165, from mixer 50, while controlling the feed of this component by means of flow meter 51. In this case, as it has been specified above, pH-corrected water rather than that containing chemical additives is fed using pump 52 from water treatment and water desalination system 1 via line 53 through valve 54, check valve 55 and through valve 56 into mixer 50. In this case, pH-corrected water transits alkali mixer 50.

(18) Depending on the commercial requirements to the product, in this case, the BALLAST ORGANIC FERTILIZER in the form of suspended gel, leaching can be optionally carried out using sodium or potassium hydroxides. In this version, alkali 59 metered on weighing unit 58 is loaded from warehouse bunker 57 to mixer 50, and treated (and softened if necessary) water is also metered into it via line 53. Then, mixer agitator 50 is started for 1 to 2 minutes, and the process alkaline solution is thus prepared. The amount of the water used in the process is calculated in advance based on the fact that the composition fed to mechanochemical reactor 35 for conversion already contains water and that the duty of water curve of its conversion in reactor 35 must range from 1.5 to 2.5.

(19) During the conversion of the reaction composition, mineral fertilizers and/or micronutrients 60 are introduced into mechanochemical reactor 35 if necessary.

(20) The operation of mechanochemical reactor 35 is similar to that of reactor 19, as it is described above. Temperature control in reactor 35 is carried out using thermal sensor 61.

(21) Using switch 62, finished products 63BALLAST ORGANIC OR ORGANOMINERAL FERTILIZERS in the form of suspended gelsare taken out of the process for packaging and warehousing (not shown).

(22) Switch 62 can also be used during start-up and commissioning to collect samples 64 during the experimental works to select the modes of raw material composition conversion. Mechanochemical reactor 19 for the collection of samples 66 is also equipped with a similar switch, 65.

(23) Valves 67 to 69 installed on the outlet nozzles of mixers 10, 50 and 70 are designed for the preventive flushing of these mixers in the time between the experimental selections of reaction components and equipment operation modes to preclude the potential undesirable mutual influence of some chemical substances or other on each other.

(24) During the recovery of some product or other from the supposed product range according to the presented invention, circulation cycles may be used in mechanochemical reactors 19 and 35, when the composition being converted is sent from reactor 19 to its inlet for repeated conversion. The number of such cycles can range from two to six.

(25) During this cyclic conversion of raw material compositions, the time of change in the frequencies of hydraulic impulse effect on these compositions being converted within the above frequency range is increased in accordance with the number of cycles. To complete the conversion of the raw material components using circulation cycles, suitable pipelines and valves (not shown in FIG. 1) are used. Furthermore, if a large-tonnage process unit is created on the basis of the presented invention, then cyclic circulation conversion (if necessary under the process operating procedure of the manufacturing of any product) is substituted with conversion in multiple mechanochemical reactors, when the composition being converted is consecutively transferred from one reactor to another. Such version of the process regarding reactors 19 and 35 is not shown in FIG. 1 due to its simplicity.

(26) According to the presented method, THE PROCESS OF PRODUCTION OF HUMIC BIOLOGICALLY ACTIVE PREPARATIONSBALLASTLESS SOLUTIONS OF HUMIC ACID COMPOSITIONS OF VARIOUS CONCENTRATIONS AND WITH VARIOUS MINIMUM RESIDUAL COMPOSITIONS OF SOLID FRACTIONS BY SIZEis carried out in TWO versions. The first version is as follows.

(27) In the first stage, ballast humates in the form of suspended gels are prepared as described above. In this case, suspension 130 obtained is sent using switch 62 to knockout drum 74 by means of which volatile substances are withdrawn from this composition suspensiongases 75 forming as a result of chemical reactions and evolving from leonardite as a result of its mechanodestruction. These volatile substances 75 are collected, condensed and stored in the special gas subsystem mentioned above, and then these gases 75 are burnt in boiler 4, yielding process heat.

(28) Converted suspension composition 76 cleaned from gases 75 and composed of HA water and alkaline solution and a solid fraction is sent to a special unitDISSOLVER-DESTABILIZER 77. While this unit is filled with suspension composition 76 and until it is removed from this unit, the operating mode of the mixer and high-speed mill of unit 77 is maintained, which continues the completion of the HA leaching process.

(29) The time of containment of the suspension composition in unit 77 in turbid condition is 1 to 5 minutes, after which this composition is subjected to mechanical division into solid and liquid phases on a high-speed centrifuge-decanter 78. For this, the suspension composition is sent to decanter 78 via line 79 using pump 80 and through valve 81.

(30) During this, decanter 78 is started, and the completeness of the composition's division into phases is controlled using flow meter 82 and the level meter embedded in unit 77. Separated solid phase 83 is sent from decanter 78 to dryer 2 of the fuel briquette preparation and process heat generation system, and liquid phase 84, which is an HA water and alkaline solution, is sent from decanter 78 to buffer reservoir 87. Then, this HA water and alkaline solution is sent from buffer reservoir 87 to dissolver-destabilizer 77 using pump 88, via lines 89 to 91, through valve 92, check valve 93, valve 94, and through valve 95. The completeness of the transfer of the HA water and alkaline solution from buffer reservoir 87 to dissolver-destabilizer 77 is controlled using the level meter embedded in reservoir 87 and using flow meter 96.

(31) Before the end of the process of transferring the water and alkaline solution to dissolver-destabilizer 77, a 10 to 20% process solution of an acid, e.g. hydrochloric acid, whose concentrate is stored in warehouse acid reservoir 97, is prepared. To this end, acid mixer 70 is first filled with a dose of water via lines 53 and 98, through check valve 99, through valves 54 and 100. Then the agitator of acid mixer 70 is switched on, and then, valves 101 and 102 are opened, and the acid is dosed (by gravity) via line 103 to mixer 70. The acid dose in this case is controlled by means of embedded level meters in warehouse acid reservoir 97 and in acid mixer 70. In 5 to 10 seconds, once the metering ends, the agitator of acid mixer 70 is stopped.

(32) Further on, while the agitator and high-speed mill of dissolver-destabilizer 77 work, the acid dose is transferred from mixer 70 to dissolver-destabilizer 77 by gravity via line 104, through valves 105 and 106, thus carrying out the process of acidification of the medium being converted with pH being decreased to 1.5 to 3, while the HAs withdraw from the solution to the heavy phase in the form of coagulated pulp. The dose of the acid solution introduced into dissolver-destabilizer 77 is controlled using flow meter 155. Flocculant 107 is added within 2 to 4 minutes after the introduction of the acid into dissolver-destabilizer 77 is completed if necessary, and its agitator and high-speed mill are stopped after 2 to 4 more minutes.

(33) For the next 5 to 20 minutes (depending on the use of the flocculant), the HA is sedimented in the form of a gel or large flocks. A part of the liquid phase, the mother solution, which is the solution of the products of alkali and acid neutralization, is withdrawn from a certain level of dissolver-destabilizer 77 by means of pump 108 via lines 109 and 110, through valve 111, to water treatment and water desalination system 1, where this solution is desalinated, and commercial-condition salts are produced, whereas the pure water is returned to the main technological processes.

(34) Then, the agitator and high-speed mill of dissolver-destabilizer 77 is started, and dry alkali 112 is introduced into it, raising pH to 8.5 to 10. Thus, the HAs are transferred from the heavy phase (within 1 to 2 minutes of the operation of the agitator and high-speed mill of dissolver-destabilizer 77) to a new secondary solutiona product which is now obtained with the HA concentration increased to 10 to 15%. In this case, the concentration of the HA solution obtained is determined not only by the HA content in the primary alkaline solution, but also by the amount of the mother solution collected from dissolver-destabilizer 77.

(35) The product thus obtainedA BIOLOGICALLY ACTIVE PREPARATION, BALLASTLESS HUMIC ACID COMPOSITION SOLUTIONis transferred to warehouse commercial reservoir 113 by means of pump 88, via lines 109, 114, 89, 90 and 115, through valves 111 and 116. In this case, the completeness of the transfer of the product to warehouse commercial reservoir 113 is controlled using flow meter 117 and the level meter embedded in dissolver-destabilizer 77. The product is taken from warehouse reservoir 113 for sale via line 118, through valve 119.

(36) The water solution of this product can be used for effective plant cultivation. In this case, to use the solution obtained in hydroponics processes, it is additionally purified at filter 120 and sent to warehouse commercial reservoir 121. In this case, the HA solution obtained and that in dissolver-destabilizer 77 is called a semi-product and sent to filter 120, also with pump 88, via lines 109, 114, 89 to 91 and 121, through valve 111, 94 and 122.

(37) The filtered solution is a product containing 0.5% of solid phase particles or less with sizes below 40 m and can be used in plant cultivation using hydroponics processes. This product is sent from filter 120 via lines 123 and 160, through valve 124, to warehouse reservoir 121. The product is sent for sale from warehouse reservoir 121 via line 125 and through valve 126.

(38) Residual solid phase 127 is sent from filter 120 using process transport 128 to the fuel briquette preparation system, where this solid phase 129 is loaded into dryer 2.

(39) In the second version according to the presented method, THE PROCESS OF PRODUCTION OF HUMIC BIOLOGICALLY ACTIVE PREPARATIONSBALLASTLESS SOLUTIONS OF HUMIC ACID COMPOSITIONS OF VARIOUS CONCENTRATIONS AND WITH VARIOUS MINIMUM RESIDUAL COMPOSITION OF FRACTIONS BY SIZE, is carried out as follows.

(40) At the first stage, a low concentration product is prepared, namely HA water and alkaline solution 84, which is taken from decanter 78 (liquid phase) as described above to buffer reservoir 87.

(41) Then, at the second stage of the process, this HA water and alkaline solution is sent from buffer reservoir 87 to vacuum evaporating apparatus 131 with a view to increasing its concentration. It is sent by means of pump 88, which performs the role of a charging pump for high-pressure pump 132 in this process version, via lines 89, 90, 133 and 134 through valves 92 and 135 and check valve 93. In this case, before sending the HA water and alkaline solution to vacuum evaporating apparatus 131, this solution is subjected to activation in ejector emulsifier 136 in hydrodynamic pre-cavitation mode. The operation of ejector emulsifier 136 in such mode is ensured by means of high-pressure pump 132, regulated throttle 137, with which the necessary back pressure is ensured, and a buffer reservoir (not shown). The completeness of the use of the HA water and alkaline solution taken from buffer reservoir 87 is controlled using flow meter 117.

(42) To prevent the thermal destruction of the HAs, the operation of evaporating apparatus 131 is maintained in water boiling mode on the level of 60 C. using vacuum pump 138 creating a pressure of 19.87 kPa in condenser 139 andvia vacuum line 140 respectivelyin evaporating apparatus 131.

(43) Pure water is pumped from condensate trap 141 with condensate pump 142 to buffer reservoir 143 for condensate via line 144, through valve 145. This pure condensate water is used further on if and when necessary by returning it to water treatment system 1 with a view to replenishing the process water consumption or preparing the hydrogen peroxide solution or while preparing fulvic preparations as will be described below. To this end, the water is sent from buffer reservoir 143 using pump 146, via lines 147 and 12 to water treatment system 1, through valves 148 and 11, check valve 149 and through valve 23. In another case mentioned above, the water from buffer reservoir 143 is sent using pump 146, via lines 147, 12 and 150 to mixer 10, through valves 148 and 13, check valve 149 and through valve 23. In yet another case mentioned above, the pure water from buffer reservoir 143 is sent using pump 146 and metering pump 21, via line 147, through a buffer reservoir (not shown) to mechanochemical reactor 19, through valves 148 and 24, as well as through check valve 149.

(44) The operation mode of evaporating vacuum apparatus 131 is also ensured by feeding warming vapor 151 into it from boiler 4. To regulate the feed of the warming vapor and stabilize the water boiling temperature on the level of 60 C. in this apparatus 131, thermal sensor 152 and adjustable valve 153 are used. In FIG. 1, the waste steam returned for heating from apparatus 131 to boiler 4 is shown as number 154.

(45) Thus, some of the water is removed from the HA solution using evaporating vacuum apparatus 131, which increases the HA content in the solution to the commercial condition required. The finished productthe HA solution from apparatus 131is taken to warehouse reservoir 113 or to warehouse reservoir 121 depending on the minimum allowable content of residual solid particles in the product.

(46) The finished HA solution is taken from apparatus 131 using a product pump and a buffer reservoir (not shown), via lines 156, 157, or via lines 156, 158 to 160 and using logistic valves 161 to 163.

(47) According to the presented method, THE PROCESS OF PRODUCTION OF HIGHLY BIOLOGICALLY ACTIVE PREPARATIONSBALLASTLESS SOLUTIONS OF FULVIC ACID COMPOSITIONS OF VARIOUS CONCENTRATIONS WITH THE MINIMUM RESIDUAL COMPOSITION OF SOLID FRACTIONS BY SIZEis carried out in two versions. Such raw material as leonardite is used due to the fact that leonardite is the richest raw material for humic preparation production, as its humic (protohumic) substance content reaches 90% [14, 32].

(48) According to the first version as the easiest one, FAs are extracted from leonardite using pure water and adaptively optimized mechanoactivation. The relative simplicity of the technological process consists in the fact that no chemical substances are used in this version.

(49) However, in this case, the HAs contained in the solid phase escaping the process are lost. At the same time, organic carbon is transferred to fuel briquettes, which results in the losses mentioned being replenished in terms of energy.

(50) The technological process is carried out as follows:

(51) Mechanochemical reactor 19 is started, and ground leonardite 20 prepared as described above is fed into it. At the same time, pure water is fed into reactor 19 via line 25 using metering pump 21, via valve 24.

(52) In this case, the flows of leonardite 20 and pure water are regulated based on the prescribed duty of water curve of 2 to 3, depending on the characteristics of raw material leonardite 27 and in view of its water content that is controlled using sensor 26. Leonardite is converted in adaptively optimized mechanoactivation modes and in mechanochemical reactor 35 as well. The volatile substances formedgases 39 and 75 which, as has been specified above, are used to generate process heatare removed.

(53) The process dose of reaction composition 76 is collected in dissolver-destabilizer 77, from where it is sent for mechanical phase division in decanter 78, via line 79, using pump 80, through valve 81. Solid phase 83 is sent from decanter 78 to dryer 2 of the fuel briquette preparation system, whereas liquid phase 84, which is a solution of FAs and a certain small part of water-soluble HAs, is collected in buffer reservoir 87. Then, the FA solution is subjected to filtration to make sure in contains solid particles with the maximum size of 40 m, and the filtered solution is sent to warehouse reservoir 167 from filter 120 or from filter 120 through vacuum evaporating apparatus 131, a concentrated FA solution thus obtained. The FA solution is fed to filter 120 from buffer reservoir 87 using pump 88, via lines 89, 91 and 121, through valves 92, 94 and 122 and through check valve 93. The completeness of the withdrawal of the FA solution for filtration is controlled using the level meter embedded in buffer reservoir 87 and according to the indications of flow meter 96.

(54) The filtered low-concentration FA solution is sent from filter 120 to warehouse reservoir 167 using the residual pressure after filter 120, via lines 123, 159 and 168, through logistic valves 124 and 163.

(55) In the other case, the filtered low-concentration FA solution is sent from filter 120 to vacuum evaporating apparatus 131 via lines 123, 133 and 134, through valve 169, using high-pressure pump 132 and through ejector emulsifier 136 and adjustable throttle 137, whose intended use and operation are described above. As a result of the operation of vacuum evaporating apparatus 131, the concentrated FA solution, a commercial product, is obtained. This product also contains a small amount of low-molecular, active, water-soluble HAs. The properties of this product in application are somewhat improved owing to the HAs. The finished product is sent to warehouse reservoir 167 via lines 156, 158 and 168, through logistic valves 161 and 162.

(56) According to the second version of the preparation of the FA solution, extraction is carried out by means of sodium or potassium hydroxide while also using adaptively optimized mechanoactivation. Hydrochloric or orthophosphoric acid is used in the technological process. The technological process according to this version ensures the production of not only the FA product solution, but also the HA solution which is also a commercial product.

(57) The technological process is carried out as follows:

(58) At the first stage of the technological process, a reaction composition is prepared from leonardite using leaching based on sodium or potassium hydroxide (otherwise, their pyrophosphates are used) or using no chemical substances and using the physical process of pH correction instead as it has been described above, and the reaction composition is concentrated in dissolver-destabilizer 77. In this case, the process of the liquid-phase oxidation of leonardite can be carried out in advance depending on its initial characteristics. The process of liquid-phase oxidation according to the presented invention is also described above. Then, the reaction composition is sent from dissolver-destabilizer 77 for phase division to decanter 78 as it has also been described above. Solid phase 83 is sent from decanter 78 to dryer 2 of the fuel briquette preparation system, whereas the liquid phase, which is a composition solution of HAs and FAs, is sent to buffer reservoir 87 via line 84. Then, this composition solution is transferred using pump 88 to dissolver-destabilizer 77 via lines 89 to 91, through check valve 93 and through valves 92, 94 and 95. The completeness of the transfer of the composition solution from buffer reservoir 87 to dissolver-destabilizer 77 is controlled using the level meter embedded in reservoir 87 and using flow meter 96.

(59) Further on, during the operation of the agitator and high-speed mill of dissolver-destabilizer 77, an acid solution is introduced into it, pH decreasing to 1.5 to 2.5, and the process of withdrawing the HAs from the liquid phase to the heavy phase in the form of coagulated pulp is carried out within 5 to 15 minutes. Hydrochloric acid or orthophosphoric acid is introduced into dissolver-destabilizer 77 from acid mixer 70 via line 104, through valves 105 and 106. In this case, the metering of the acid solution is controlled using the level meter embedded in acid mixer 70 and using flow meter 155. To accelerate the process of withdrawing the HAs from the liquid phase, flocculant 107 can be introduced into dissolver-destabilizer 77. As a result of the completion of the process of the transfer of the HAs to the heavy phase, the FAs remain dissolved in the liquid phase. The agitator and high-speed mill of dissolver-destabilizer 77 are stopped, and HAs in the form of gel-like flocks are sedimented at the bottom of dissolver-destabilizer 77 for 10 to 20 minutes.

(60) Then, using the technical capabilities of dissolver-destabilizer 77 (to be shown in detail below), the liquid phase from dissolver-destabilizer 77, which is an FA solution, is transferred to buffer reservoir 166 using pump 88, via lines 109, 114, 89 to 91 and 85, through valves 111, 94 and 86. The FA solution is sent from buffer reservoir 166 using pump 88 to filter 120, where solid particles 127 with sizes over 40 m are separated and sent to carrier 128 to be disposed of into the fuel briquette preparation system. The FA solution is fed to filter 120 via lines 170, 89 to 91 and 121, through valves 171, 94 and 122 and through check valve 172. The completeness of the withdrawal of the FA solution from buffer reservoir 166 for filtration and then for concentration is controlled using the level meter embedded in reservoir 166 and according to the data of flow meter 96.

(61) Then, the filtered FA solution is sent from filter 120 to vacuum evaporating apparatus 131, and the concentration of the product is increased as it has already been described above. The finished product (concentrated FA solution) is sent to warehouse reservoir 167.

(62) A water and alkaline solution which is metered from alkali mixer 50 by means of metering pump 48 is poured to the sedimented HAs in dissolver-destabilizer 77. This solution is sent via lines 47 and 173, through valves 49, 165 and 174. Metering is controlled using the level meter embedded in alkali mixer 50 and according to the data of flow meter 51. At the same time, the agitator and high-speed mill of dissolver-destabilizer 77 are switched on, and the HAs are dissolved in it within 1 to 2 minutes after the end of the introduction of the alkaline solution. Then the HA solution, as it has been described above, is sent to warehouse reservoir 113 or, using filtration, to warehouse reservoir 121.

(63) The FA solution obtained possesses extremely high biological activity and is of high commercial value. FAs have relatively small molecular weights and, consequently, they penetrate the roots, stalks and leaves of plants well. While penetrating, FAs bring micronutrients from the surfaces of plants to their tissues. When applied on the foliage, an FA transports micronutrients right into the metabolic centers of plant cells [31, 37].

(64) If potassium hydroxide and orthophosphoric acid have been used in the process of obtaining this product (as specified above), such product can be used in animal husbandry, poultry farming and fish farming.

(65) Humic biologically active preparationsballastless dry HA salts and highly biologically active ballastless preparationsdry fulvic acid salts, fulvates, are prepared according to the processes described above, the only difference being that products are dried in vacuum evaporating apparatus 131 to the water content corresponding to their commercial conditions. The withdrawal of finished products in FIG. 1 is marked with number 175.

(66) THE PREPARATION OF FUEL BRIQUETTES in accordance with the presented invention is carried out as follows:

(67) Residual (after the processes of preparation of humic and fulvic preparations) solid fractions 83 and 129, which consist mainly of organic carbon and 10 to 25% of mineral components, are sent to dryer 2 of the fuel briquette preparation system, where a part of moisture is removed from this material, its content being reduced from 40 to 60% to 15 to 20%. During the drying of this material, this dried material 176 is metered into extruder 3 in a continuous flow by means of turning and blowing with hot gases, for instance, like a fluidized bed. Extruder 3 is heated with hot flue gases 177 coming from boiler 4 when a part of fuel briquettes 178 being produced is burnt in it and the combustible part of volatile substances 179 (the total of volatile substances 39 and 75 withdrawn from the coal raw material while it is converted into humic fertilizers and humic and fulvic acid preparations) is burnt.

(68) The temperature of the flue gases heating the thermal contacting parts of extruder 3 with material 176 is regulated within the range of 600 to 650 C. according to the indications of a pyrometer (not shown) and by means of regulating valves 180 and 181.

(69) Other channels for the regulation of the temperature of gases 177 warming extruder 3 include the machines for fuel transfer (not shown) of briquettes 178 and volatile substances 179 to boiler 4. The potential excess heat of flue gases 182, of boiler 4 is vented to the atmosphere by means of regulating valve 181. Warming flue gases 177, while passing extruder 3, give up a part of their heat in it. And then, these gases 182, their temperature ranging from 400 to 450 C., are sent to dryer 2, where these gases give up the other part of their heat for the removal of moisture from the solid fractions of materials 83 and 129 and for their heating. Then, these flue gases 183, cooled to a temperature of 110 to 115 C., are removed from dryer 2 into the atmosphere.

(70) During the semi-coking of material 176 in extruder 3, a steam-and-gas composition [27, p. 197] whose gases partially consist of combustible substances, which results in off-gases 184 being sent from extruder 3 to boiler 4 for their combustible part to be burnt, is withdrawn from this material.

(71) After fuel briquettes 185 leave extruder 3, they are cooled and stockpiled 186, as well as packaged into commercial packaging.

(72) THE EMBODIMENT OF THE INVENTION REGARDING THE MECHANOCHEMICAL REACTOR for the conversion of high viscosity media including suspensions and pulps is illustrated with as-built drawings FIGS. 2 to 5. The design arrangement of the reactor is represented in FIG. 2. Here, the body of the reactor, which is mounted on fixed guides 188 using thread joints 189, is marked with number 187. In this case, reactor case 190, 191 is made split, consisting of the stationary part (case 190) and the movable part (case 191), which can be moved using wheels 192 on guides 188 to the preventive maintenance and repair position.

(73) An electric motor (not shown) driving rotor disk 193 fixed on supporting sleeve 194, which, in its turn, is rigidly connected with the hollow drive shaft 195 of the hydraulic puller, which is shown through case 196, shields 197, bearings 198 and load port 199, is placed on body 187. In this case, an autonomous screw adjustable drive (not shown) is installed on load port 199 from the top, and the internal surface of port 199 is equipped with insert 200 made of an anti-adhesion material.

(74) An electric motor (not shown) driving rotor disk 201 fixed on supporting screw sleeve 202, which, in its turn, is rigidly fixed on drive shaft 203 of supporting bearing assembly 204, is placed on movable case 191.

(75) Small console screw 206, which is axially inserted into hollow drive shaft 195 of the hydraulic remover, on whose internal surface radially embracing screw 207 is rigidly fixed, is fixed on supporting screw sleeve 202 using adapter sleeve 205.

(76) The distribution manifold ring of the hydraulic puller connected with load port 199 on the one side and connected to hydraulic valve gaps 209 made in the hollow drive shaft 195 of the hydraulic puller is shown as number 208. Here, the direction of the operating rotation of driving shaft 211, hollow drive shaft 195 of the hydraulic puller is shown as number 210. The operating direction of the rotation of driving shaft 203 is shown as number 212.

(77) Circular rows of bearing rods 214 and 215 respectively are fixed on rotor disks 193 and 201 using detachable fixings 213, e.g. collet closers.

(78) The distribution manifold ring of stationary case 190 connected to sleeve fitting 217 for introducing liquid components into the reactor on the one side and connected to valve ports 218 made in supporting sleeve 194 on the other side is shown as number 216. Pump-and-screw blades 219 ensuring the reliability of the casting of the flow of the medium being converted to the area of the activation interaction of rods 214 and 215 are fixed on this supporting sleeve 194.

(79) Fixed reflecting and directing blades 220 are placed in off-loading gap 221 of the reactor, and to ensure the reliability of the removal of the high viscosity media being converted from the reactor, these blades, as well as off-loading gap 221 itself, are connected with vibration impact electromagnetic device 222.

(80) Mini-screw, single-turn threads made on the cylindrical surfaces of the rotor disks, which actively reflect the materials being converted from the gaps between the rotor disks and the internal cylindrical surface of case 190 of the reactor when the rotors rotate, are shown as number 223.

(81) Acoustic signals, including cavitation-type noises, are picked up from the reaction area using acoustic sensor 224 embedded in case 190.

(82) The placement of cleaning mini-rotors 225 in case 190 of the mechanochemical reactor with cleaning rods 226 installed on them is shown in detail in FIG. 3. Here, the rotation direction of mini-rotors 225 is shown as number 227, and the rotation direction of rotor disk 201 with rods 215, whose peripheral row is the closest to cleaning mini-rotors 225, is marked with number 228. The rotation direction of rotor disk 193 (not shown) with rods 214 is shown in the same FIG. 3 as number 229.

(83) Directions 230 of the movement of the medium being converted under the influence of pump-and-screw blades 219 ensuring the reliability of the casting of the flow of this medium to the area of the activation interaction of rods 214 and 215 are marked. In this case, direction 231 of the rotation of pump-and-screw blades 219 coincides with the rotation direction of rotor disk 193 (not shown in FIG. 3). The rotation direction of supporting screw sleeve 202, which helps feed the medium being converted to pump-and-screw blades 219, is shown as number 232.

(84) The orientation and placement of valve gaps 209 made in hollow drive shaft 195 of the hydraulic puller are shown in FIG. 4 in detail. It is here that the distribution manifold ring of the hydraulic puller connected to load port 199 (not shown in FIG. 4) is shown as number 208. The same distribution manifold ring 208 is connected to valve gaps 209 as well. The sealing elements ensuring the water-proofing of bearings 198 of the hydraulic puller assembly from the media being converted are shown as number 233.

(85) The general layout of rodless rotor 234 with radial and wave surfaces 235 designed for the conversion of special anomalously viscous, slow-flowing media in the mechanochemical reactor is shown in FIG. 5.

(86) THE OPERATION OF THE MECHANOCHEMICAL REACTOR (with the exception of the chemistry of the processes, which is described above in detailfrom the perspective of mechanics) IS PERFORMED AS FOLLOWS.

(87) First of all, the main motion drives of the reactors are started with the rotation of shafts 203 and 211 and the respective rotor disks 193 and 201. Then, the main (viscous or highly viscous) component being converted is fed into the reactor through load port 199, and after a short delay time (0.5 to 2.5 seconds), a liquid component flow is directed into the reactor via sleeve fitting 217. The metering of the flows of the components being converted into the reactor, the speeds of its main motion drives and the delay time are according to the process operating procedure corresponding to the chemistry of the conversion process. Vibration-impact electromagnetic device 222 is switched on then, after the delay time, as well.

(88) The viscous or highly viscous component being converted is fed into distribution manifold ring 208 and through it, into hydraulic valve gaps 209 by means of screw drive 18. The surfaces of hydraulic valve gaps 209 are spatially oriented so that these surfaces form the pump reflecting forces affecting the flow of the component being converted (to the rotation axis of shaft 195 in the radial direction and to the area of the active interaction of rods 214 and 215 of the reactor in the axial direction of shaft 195) while hollow drive shaft 195 rotates. This ensures the advance of the medium being converted with the change in its direction and ensures the transfer of the flow of the component being converted from fixed load port 199 to the cavity of rotating drive shaft 195. Here, the viscous or highly viscous component being converted enters the field of the effect of the forces driving it on all sides: from axial small console screw 206 and from radially embracing screw 207, which is made in left-handed thread turns. Thus, guaranteed injection of the viscous or highly viscous component being converted into internal cavity 194 of supporting sleeve 194 is carried out. As a result of such injection, the component being converted that is in the internal cavity of supporting sleeve 194 is exposed to a certain pressure of the hydraulic puller, which results in it being picked up freely by supporting screw sleeve 202 and directed towards pump- and screw blades 219, with which the flow of the composition being converted is cast into the activation interaction area of rods 214 and 215. Here, the medium being converted is already called a composition, as the flow of the medium running to pump-and-screw blades 219 (right here) is where the liquid component is injected using meter pumps 21 or 48 via valve ports 218, which are fed from distribution manifold ring 216 of stationary case 190, which is, in its turn, fed through sleeve fitting 217.

(89) The mechanochemical conversion of the reaction components is carried out in the active interaction areas of the circular rows of rods 214 and 215 as described above owing to the static and dynamic adjustable parameters in accordance with the process operating procedure. During this conversion, the reaction components, affected by gravitational and centrifugal forces, advance over the reaction zone in radial directions relative to the rotation axes of rotor disks 193 and 201.

(90) Upon reaching the periphery of the rotor disks, the composition being converted is forced to move along the internal cylindrical surface of case 190 of the reactor, exposed to drawing friction forces acting from the peripheral row of rods 215, as shown in FIG. 3 with number 236. In this case, the vertical components of this movement, the one left of axis A, are favorably directed towards the withdrawal of the reaction component from the reactor, i.e. towards off-load gap 221. The vertical components of this circular movement (marked with number 237) right of axis A are directed opposite to off-load gap 221 and are a potential reactor contamination factor.

(91) Due to this fact, cleaning mini-rotors 225 with the following effect are applied and included in the design assembly in accordance with the inventive conception. In the areas of the minimum contact distances between rods 215 and cleaning rods 226, their speed vectors (tangential to the circles in which these rods move) coincide in their directions and are close in the angular directions 237 of the movement of the reaction composition. Due to this fact, a part of the moving (237) flow of the composition being converted is deflected next to each cleaning mini-rotor 225 (in directions 238) with no significant energy consumption and with no formation of pressure jumps localized there, owing to the drawing active friction forces of cleaning rods 226. And thus, the whole peripheral flow in direction 237 is re-formed to a new flow in direction 239, which in its turn, moves towards off-load gap 221, where it is withdrawn from the reactor in direction 241 under the effect of the gravitation force and favorably meeting the flow in direction 240. In this case, the flow in direction 240 mentioned is formed from the flow in direction 236 under the effect of centrifugal forces and the gravitation force.

(92) The major part of the flow in direction 240, as shown in FIG. 3, diverges additionally owing to the response of fixed reflecting and directing blades 220 and withdrawn from the reactor by this diverged flow in directions 242.

INDUSTRIAL APPLICABILITY

(93) The applied method of comprehensive conversion of coal series caustobioliths, mostly brown coals and leonardite, into products including humic organic and organomineral fertilizers and into humic and fulvic preparations with fuel briquettes being obtained can be applied for large-tonnage production of these products for commercial purposes in the field of agriculture for the production of environmentally friendly foodstuffs in animal husbandry, poultry farming and fish farming processes.

(94) Furthermore, the products manufactured according to the presented method can be used as components of artificial soils and ameliorants, as is, for instance, shown in [88], jointly with zeolite materials, with serpentinite and with mineral fertilizers.

(95) The majority of the equipment units associated with the processes of the preparation of the products obtained according to the presented invention in the industries of a number of countries has been tested and is in operation.

BIBLIOGRAPHIC DATA OF THE REFERENCES

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