CN115870052B - Preparation method and production device of nano magnesium hydride - Google Patents
Preparation method and production device of nano magnesium hydride Download PDFInfo
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Abstract
A method for preparing nano magnesium hydride and a production device thereof, which comprises the following steps: the device comprises a feed inlet, a grinding bin, a heating bin, a guide channel and a reaction bin; the multi-angle repeated grinding is finished on the horizontal plane through multi-layer multi-granularity grinding and intelligent grinding control, and the uniformity of the particles is subjected to supplementary grinding on the vertical plane; the application achieves better particle uniformity with higher efficiency; avoiding losses due to ineffective grinding; the heat energy consumption is less, the environment is protected, and the production cost is reduced.
Description
Technical Field
The application relates to the field of magnesium hydride preparation, in particular to a preparation and production device of nano magnesium hydride.
Background
Magnesium hydride (MgH 2), also known as magnesium hydride, is an inorganic salt, and has an off-white appearance, a tetragonal crystal structure and a density of 1.45g/cm3.MgH2 is covalent hydride, its formation enthalpy is-74.5 kJ/mol, its stability is high at normal temperature and pressure, and its hydrogen absorption and desorption temperature is up to 623-673K. MgH2 is decomposed under vacuum at 280 ℃. MgH2 is weak alkaline, insoluble in common organic solvents, inflammable and irritating. The hydrogen content of MgH2 is up to 7.65%, so that the method has wide potential application; from the theoretical hydrogen storage capacity, it is the first choice in metal hydrogen storage materials; the method is used for preparing hydrogen, can generate hydrolysis reaction at normal temperature to release hydrogen, and the hydrogen energy has the advantages of rich resources, high heat value, environmental protection and the like, and is considered as an optimal substitute of fossil energy in the future.
The hydrogen storage material is nanocrystallized, so that the operating temperature can be effectively reduced, and the hydrogen absorption and desorption rate can be improved. The nano hydrogen storage material can be carried by chemical products or industrial waste with high specific surface area. At present, the main preparation methods of the magnesium hydride nanoparticle material are a mechanical ball milling method, a physical/chemical vapor deposition method, a pyrolysis method, an electrochemical deposition method, a plasma method and the like. These methods have various features and advantages, and the more common method is the ball milling direct method.
In the prior art, a ball-milling direct method is often adopted, the ball-milling direct reaction method is simple in process, but the ball-milling time of the ball-milling direct method is long, the ball milling time is as long as hundreds of hours, the obtained magnesium hydride particles are larger in size, mostly larger than about 100nm and even thousands of nm, most importantly, the obtained particles are quite different in size and mostly about hundreds of nm, the later hydrogen production capacity is greatly influenced, and the raw material conversion rate is lower; therefore, based on the above-mentioned technical problems, there is a need to provide a device for preparing and producing nano magnesium hydride, which can grind and mix particles in a proper manner, reduce the difference between the overall particle size and the size, and reduce the ball milling time, thereby improving the reaction rate and the raw material conversion rate.
Disclosure of Invention
The technical scheme adopted for solving the technical problems is as follows:
a production device for preparing nano magnesium hydride, which comprises: the device comprises a feeding port, a grinding bin, a heating bin, a guide channel, a reaction bin, a discharge pipe, an air inlet pipe, a grinding bin bottom plate and a heating plate;
wherein, the feed inlet is arranged above the grinding bin, is in a cone shape, gradually extends towards the direction of the grinding bin and continuously reduces in diameter; the grinding bin is arranged below the feeding hole; the raw magnesium powder particles are conveyed into the grinding bin along the circumference of the barrel by the feeding port, and the raw magnesium powder particles can be subjected to repeated mechanical grinding with multiple granularities through multi-layer grinding in the grinding bin; the heating bin is arranged below the grinding bin and is directly connected with the grinding bin; the fine magnesium powder particles fall to the bottom of the heating bin through the opened grinding bin bottom plate; the heating bin is connected with the reaction bin through a guide channel, and the magnesium powder fine particles obtained by grinding enter the reaction bin along the guide channel under the heating of the heating plate and directly react with hydrogen entering from the air inlet pipe to prepare nano magnesium hydride;
the grinding bin comprises a plurality of grinding plate groups which are connected from top to bottom through a rotating shaft, and the grinding plate groups rotate around the rotating shaft; specific: each of the polishing sheet groups includes 3 polishing sheets tightly coupled to each other, an upper polishing sheet, a middle polishing sheet, and a lower polishing sheet; wherein, the two sides of the middle grinding disc are provided with hemispherical grinding balls which are annularly arranged, and a plurality of circles of grinding balls are outwards arranged along the axis of the rotating shaft;
the center positions of the upper grinding disc, the middle grinding disc and the lower grinding disc are provided with circular gaps, and the sizes of the circular gaps on the upper grinding disc and the lower grinding disc are larger than those of the circular gaps in the middle grinding disc; a plurality of hollowed guide grooves are uniformly distributed on the middle grinding disc, and middle magnesium powder fine particles formed in the grinding process enter a coupling gap between the upper grinding disc and a grinding ball of the middle grinding disc along a circular notch on the upper grinding disc; and finally along the guide grooves in the middle blade into the coupling gap between the lower blade and the middle blade grinding balls; after being fully ground, the polishing solution falls on the next grinding sheet group; the last grinding sheet group obtains magnesium powder fine particles to drop on a grinding bin bottom plate at the bottom of the grinding bin;
the grinding bin bottom plate is movable, and when the grinding cut-off condition is met, the movable grinding bin bottom plate moves out, so that fine magnesium powder particles on the grinding bin bottom plate fall to the bottom of the reaction bin.
Further, the inner and outer rings of the middle grinding plate are provided with non-through guide grooves in a staggered manner, so that fine particles of the middle magnesium powder are guided to a coupling gap between the lower grinding plate and the grinding ball of the middle grinding plate from the periphery of the middle grinding plate.
Furthermore, the inner ring and the outer ring of the middle grinding disc are alternately provided with non-through guide grooves, so that the guide grooves of the middle magnesium powder fine particles are hollow arc-shaped guide grooves and are not radial through grooves.
Further, 4-8 arc-shaped guide grooves are arranged on each middle grinding disc, and the radian is 90-180 degrees.
Further, the width and area of the guide groove at the outer ring are larger than those of the guide groove at the inner part.
Further, the size of the grinding balls gradually increases in a direction in which the diameter extends outward.
Further, the reacted nano magnesium hydride is discharged through a product discharge pipe, and then is subjected to subsequent condensation and collection of the nano magnesium hydride.
Further, the bottom plate is grid-shaped after being opened, so that fine magnesium powder particles uniformly fall to the bottom of the reaction bin.
Further, the bottom plate is formed by splicing two or more grid-shaped plates, and after the bottom plate is opened, the grids are exposed so that the magnesium powder fine particles above the bottom plate fall off.
The preparation method of the nano magnesium hydride preparation production device comprises the steps of firstly, primarily crushing a metal magnesium raw material to obtain magnesium powder raw particles, and putting the magnesium powder raw particles into a grinding bin through a feed inlet.
The preparation and production device of the nano magnesium hydride provided by the application can realize the following technical effects:
1) The multi-angle repeated grinding is finished on the horizontal plane through multi-layer multi-granularity grinding and further intelligent grinding control, and the uniformity of the particles is subjected to supplementary grinding on the vertical plane, so that the better uniformity of the particles is achieved with higher efficiency;
2) The adjustment of the grinding gap, namely the coupling degree, is realized through the integral independent control of the similar grinding sheets; by adopting the mode, the uniformity and the size of the particles can be adjusted, the reduction of the grinding performance caused by abrasion resistance can be prevented, the controllability of the production process is improved, and the service life of production equipment is prolonged;
3) The grinding efficiency is greatly improved by setting the intelligent grinding cut-off condition and matching with a multi-level multi-granularity grinding mode, and further, the grinding sequence is adjusted by intelligently controlling and selecting a proper grinding sheet group, so that the loss caused by ineffective grinding is avoided; the heat energy consumption is less, the environment is protected, and the production cost is reduced.
Drawings
Fig. 1 is a schematic structural diagram of a device for preparing and producing nano magnesium hydride.
Fig. 2 is a schematic view of a grinding bin of a production device provided by the application.
Fig. 3 is a schematic view of an abrasive sheet in an abrasive sheet set according to the present application, wherein fig. 3A is a schematic view of a middle abrasive sheet, and fig. 3B is a schematic view of an upper abrasive sheet and a lower abrasive sheet.
FIG. 4 is a schematic diagram of a coupling mode of the polishing plate set according to the present application, wherein FIG. 4A is a schematic diagram of a close-coupled section, and FIG. 4B is a schematic diagram of a close-coupled projection.
Fig. 5 is a schematic diagram of a detachable connection mode capable of being controlled independently and integrally of a device for preparing and producing nano magnesium hydride.
Fig. 6 is a schematic view of a polishing sheet guiding groove in a polishing sheet set according to the present application.
Fig. 7 is a schematic diagram of nano magnesium hydride prepared by the apparatus for preparing and producing nano magnesium hydride provided by the application.
Detailed Description
The apparatus for preparing and producing nano magnesium hydride according to the present application will be described in further detail.
The present application will be described in more detail below with reference to the attached drawings, in which preferred embodiments of the present application are shown, it being understood that one skilled in the art can modify the present application described herein while still achieving the beneficial effects of the present application. Accordingly, the following description is to be construed as broadly known to those skilled in the art and not as limiting the application.
In the interest of clarity, not all features of an actual implementation are described. In the following description, well-known functions or constructions are not described in detail since they would obscure the application in unnecessary detail. It will be appreciated that in the development of any such actual embodiment, numerous implementation details must be made in order to achieve the developer's specific goals.
In order to make the objects and features of the present application more comprehensible, embodiments accompanied with figures are described in detail below. It should be noted that the drawings are in a very simplified form and use non-precise ratios for convenience and clarity in assisting in the description of embodiments of the application.
The application provides a production device for preparing nanometer magnesium hydride, which is shown in figure 1 and comprises: a feed inlet 1, a grinding bin 2, a heating bin 3, a guide channel 4, a reaction bin 5, a discharge pipe 6, an air inlet pipe 7, a grinding bin bottom plate 21 and a heating plate 33;
wherein, the feed inlet 1 is arranged above the grinding bin 2, is in a cone shape, gradually extends towards the direction of the grinding bin 2 and continuously reduces in diameter; the grinding bin 2 is arranged below the feed inlet 1; the raw magnesium powder particles are conveyed into the grinding bin 2 along the circumference of the barrel by the feeding port 1, and can be subjected to repeated mechanical grinding with multiple granularity through multi-layer grinding in the grinding bin 2, so that fine magnesium powder particles with proper particle uniformity and size are obtained; the heating bin 3 is arranged below the grinding bin 2 and is directly connected with the grinding bin 2; the fine magnesium powder particles fall to the bottom of the heating bin 3 through the opened grinding bin bottom plate 21; the heating bin 3 and the reaction bin 5 are connected through a guide channel 4, and the ground magnesium powder fine particles enter the reaction bin 5 along the guide channel 4 under the heating of the heating plate 33 and directly react with hydrogen H2 entering from the air inlet pipe 7 to prepare nano magnesium hydride; the nano magnesium hydride after the reaction passes through a product discharge pipe 7, and then is subjected to subsequent condensation and collection of the nano magnesium hydride;
as shown in fig. 2-4, the grinding bin 2 comprises a plurality of grinding disc groups connected from top to bottom through a rotating shaft 23, and the grinding disc groups rotate around the rotating shaft 23; specific: each of the grinding sheet groups includes 3 grinding sheets tightly coupled to each other, an upper grinding sheet 81, a middle grinding sheet 82, and a lower grinding sheet 83; wherein, two sides of the middle grinding disc 82 are provided with hemispherical grinding balls which are annularly arranged, and a plurality of circles of grinding balls are outwards arranged along the axle center of the rotating shaft 23; the size of the grinding balls gradually increases along the direction of the outward extension of the diameter;
as shown in fig. 3A to 3B and fig. 6, further, the center positions of the upper and lower blades 81, 82 and 83 are provided with circular notches, and the size of the circular notches on the upper and lower blades 81 and 83 is larger than that of the circular notches in the middle blade 82; a plurality of hollowed guide grooves 84 are uniformly distributed on the middle grinding piece 82, and middle magnesium powder fine particles formed in the grinding process enter coupling gaps between the upper grinding piece 81 and grinding balls of the middle grinding piece 82 along circular gaps on the upper grinding piece 81; and finally enters the coupling gap between the lower blade 83 and the grinding balls of the middle blade 82 along the guide groove 84 in the middle blade 82; after being fully ground, the polishing solution falls on the next grinding sheet group; the last grinding sheet group obtains magnesium powder fine particles which fall on a grinding bin bottom plate 21 at the bottom of the grinding bin 2;
two types of guide slots 84 are shown in FIG. 6, one of which may be selected or both of which may be simultaneously selected for placement on the center plate; the guide grooves are hollow arc-shaped guide grooves 84 and are not radial through grooves, so that excessive reduction of the strength of the grinding sheet is avoided; by staggering the non-through guide grooves 84, the fine particles of the intermediate magnesium powder are guided from the outer periphery of the intermediate grinding plate to the coupling gap between the lower grinding plate 83 and the grinding balls of the intermediate grinding plate 82; the width and area of the guide groove 84 in the outer race is greater than the width of the guide groove in the interior;
preferably: 4-8 arc-shaped guide grooves are arranged on each middle grinding disc, and the radian is 90-180 degrees;
according to the application, multi-level multi-granularity grinding and further intelligent grinding control are adopted, multi-angle repeated grinding is completed on a horizontal plane, and uniformity of particles is supplemented on a vertical plane, so that good particle uniformity is achieved with high efficiency, and most of particle sizes are controlled to be 2-50 mu m; the problems that the hydrogen production cannot be directly used due to the excessive size of particles, and the magnesium hydride is low in yield and severe and dangerous in reaction conditions due to the excessively small particles are solved;
further, the grinding bin bottom plate 21 is movable, and when the grinding cut-off condition is met, the movable grinding bin bottom plate 21 is moved out, so that the magnesium powder fine particles positioned on the grinding bin bottom plate 21 fall to the bottom of the reaction bin 5; the heating plate 33 at the lower part of the heating bin 3 heats the bottom of the heating bin 3;
preferably: the bottom plate 21 is opened to be in a grid shape, so that fine magnesium powder particles uniformly fall to the bottom of the reaction bin; specific: the bottom plate 21 is formed by splicing two or more grid-shaped plates, and after the bottom plate is opened, the grids are exposed so that magnesium powder fine particles above the bottom plate fall off;
the weight sensor is connected with a control device (not shown) in a wireless or wired way, and sends the weighed weight to the control device; the control device judges whether the cut-off condition is met or not based on the received weight data;
further, the production device further comprises a weight sensing device 32, and the weight sensing device 32 is made of a high-temperature resistant material; the weight sensing device 32 is arranged at the lower part of the grinding bin bottom plate 21 and is used for detecting the weight of the magnesium powder fine particles falling on the grinding bin bottom plate 21;
preferably: the grinding cut-off condition is that the weight of magnesium powder raw particles put into a grinding bin 2 is equal to the weight of obtained intermediate magnesium powder fine particles falling down at the bottom of the grinding bin 2;
specific: the production device further comprises a weight sensor 32, wherein the weight sensor 32 is connected with a control device (not shown) in a wireless or wired way and is used for continuously detecting the weight of the magnesium powder fine particles and sending continuously detected weight data to the control device; the control device judges whether the cut-off condition is met or not based on the received weight data; when judging that the cut-off condition is met, controlling the grinding bin bottom plate 21 to move out, retract or open so that the grinding bin 2 is communicated with the heating bin 3, and enabling fine magnesium powder particles at the bottom of the grinding bin 2 to fall onto the bottom of the heating bin 3;
preferably, the coupling mode is a coupling relation formed by grinding balls on the middle grinding disc, grinding balls on the lower surface of the upper grinding disc and grinding balls arranged on the surface of the lower grinding disc, wherein the coupling relation is formed by mutual running-in;
preferably, the grinding balls of the same circle on each grinding disc have the same size;
specifically, the middle grinding disc 82 is provided with 2 circles of grinding balls along the axis of the rotating shaft 23 outwards; the upper grinding disc 81 and the lower grinding disc 83 are outwardly provided with 3 circles of grinding balls along the axis of the rotating shaft 23, and the sizes of the grinding balls on the middle grinding disc are larger than or equal to those of the grinding balls on the upper grinding disc 81 and the lower grinding disc 83; the difference of the sizes leaves necessary space for grinding to avoid that grinding cannot be performed normally;
as shown in fig. 2 and 3A-3B, the number of the polishing pad sets is preferably 3, including: a 1 st polishing sheet group, a 2 nd polishing sheet group and a 3 rd polishing sheet group arranged from top to bottom; the coupling tightness of the grinding sheets in the grinding sheet group is increased from top to bottom in sequence; as shown in fig. 2, the coupling tightness of the upper grinding plate group is loose from that of the lower grinding plate group; for each abrasive sheet group, the degree of tightness of coupling between the upper and middle abrasive sheets 81, 82 is loose or equal to the degree of tightness of coupling between the lower and middle abrasive sheets 83, 82; that is, the looser the grinding gap, the larger, and conversely, the tighter the inter-grinding gap, the smaller; specifically, h1 in FIG. 2>
=h2, h3> =h4, h5> =h6; h1> h3> h5; h2> h4> h6; wherein: h1 H2, h3, h4, h5, h6 are the vertical distances between the upper and middle plates in the 1 st plate group, the middle and lower plates in the 1 st plate group, the upper and middle plates in the 2 nd plate group, the middle and lower plates in the 2 nd plate group, the upper and middle plates in the 3 rd plate group, and the middle and lower plates in the 3 rd plate group, respectively;
one manner of coupling the abrasive sheet set is shown in FIGS. 4A and 4B; the coupling degree is tight, and the section surfaces among the grinding balls of the grinding sheet are tightly attached; thereby forming a strong polishing capability over the entire polishing sheet;
preferably: the middle grinding piece 82, the upper grinding piece 81 and the lower grinding piece 83 are all made of steel materials;
preferably: the upper grinding piece 81 and the lower grinding piece 83 are made of steel, and the outer surfaces of the steel are plated with hard anti-wear materials or catalyst materials;
preferably: the size of the grinding ball of the same grinding disc along the radial inward direction gradually changes from large to small; because the grinding balls of the middle grinding disc 82 are larger and have higher hardness, the grinding balls are not easy to wear, or the influence of the wear is small, the grinding balls of the upper grinding disc and the lower grinding disc are small, and the grinding balls are easy to wear, when the wear occurs, the spherical structure is easy to maintain because the spherical structure has no edges and corners, and when the size of the grinding balls is reduced, the design of the application can save the consumable materials of the grinding discs by replacing the upper grinding disc and the lower grinding disc among different grinding disc groups, and prolong the service life;
preferably: the middle, upper and lower blades 82, 81 and 83 are detachable;
preferably: the upper abrasive plates in all the abrasive plate groups can be independently and integrally controlled, the gaps can be reduced by integrally moving downwards, the lower abrasive plates in all the abrasive plate groups can be independently and integrally controlled, and the gaps can be increased by integrally moving upwards, so that the coupling tightness is increased; adjusting the coupling relationship by moving up and down as a whole; the service life of the grinding sheet is greatly prolonged; based on such a design, in the case that the coupling relationship between the polishing sheets can be adjusted according to the size of the finished magnesium hydride particles, when the uniformity of the magnesium hydride particles is poor, the distance between the polishing sheets is increased to reduce the coupling degree, and when the size of the magnesium hydride particles is large, the distance between the polishing sheets is reduced to increase the coupling degree;
FIG. 5 illustrates a removable, integrally independently controllable connection structure; taking the upper grinding plate 81 as an example; the arrangement of the middle and lower blades 82, 83 is also similar; the rotating shaft 23 is sleeved with a collar 92, the collar 92 is connected to the inner side surface of the circular notch of the upper grinding disc 81 through a connecting piece 91, and the rotating shaft 23 drives the grinding disc to rotate and grind by taking the rotating shaft 23 as the center;
preferably: the rotating shaft is fixedly connected with a rotating motor (not shown), and the connection mode can be welding, riveting and the like; 3-5 connectors 91;
preferably: the overall control of the upper plates in all the plate groups, and the overall control of the lower plates in all the plate groups, is achieved by the vertical connection between the collars 92, while the middle plates in all the plate groups remain unchanged with respect to the shaft 23; the relative positions of the middle grinding disc and the upper and lower grinding discs in the vertical direction are adjustable through the integral control, so that the grinding clearance, namely the coupling degree, is adjusted; in this way, not only the uniformity and size of the particles can be adjusted, but also the reduction of the grinding performance caused by abrasion can be resisted;
the preparation method of the nano magnesium hydride provided by the application, as shown in figure 1, specifically comprises the following steps:
step S1: preliminary crushing a magnesium metal raw material to obtain magnesium powder raw particles, and putting the magnesium powder raw particles into a grinding bin 2 through a feed inlet 1; wherein: the particle size of the magnesium powder raw particles is between 1 and 1000 um;
step S2: under the protection of inert gas, carrying out multi-layer grinding on magnesium powder particles to obtain magnesium powder fine particles; wherein: the multi-layer grinding is mechanical grinding with multiple granularities; wherein: the magnesium powder fine particles are mechanically ground; the grain diameter is between 1um and 200um; the rotating speed is 40-100 rpm;
preferably: the inert gas is argon or helium and the like;
the magnesium powder particles are subjected to multi-layer grinding, and the method specifically comprises the following steps: carrying out multi-layer grinding on the raw particles of the magnesium powder by adopting the grinding bin 2 in the production device;
step S3: judging whether the grinding cut-off condition is met, if so, obtaining the obtained intermediate magnesium powder particles as final magnesium powder particles, entering the next step, otherwise, collecting the intermediate magnesium powder particles, and re-executing the step S2 on the intermediate magnesium powder particles;
preferably: the grinding cut-off condition is that the weight of the magnesium powder raw particles put into the grinding bin 2 in the step S1 is equal to the weight of the obtained intermediate magnesium powder fine particles;
in the prior art, fixed time is often adopted, grinding is stopped by experience, large-particle magnesium powder particles generated by insufficient grinding are caused, because raw materials are different, the feeding mode is dynamically changed, and the weight relationship between output and input reflects whether the grinding is sufficient or not to a certain extent; when the magnesium powder particles fall off too quickly, the weight of the magnesium powder particles is increased very quickly, improper grinding is caused, intelligent control with a certain tolerance degree can quickly find out the situation, and the secondary adjusted multi-level grinding is started;
further: the equality is approximately equal, and is determined to be equal when a×w2> =w1 > =bxw2; wherein: w1 is the weight of the intermediate magnesium powder fine particles, and W2 is the weight of the magnesium powder raw particles; wherein a > b;
preferably, a=98%, b=92%;
preferably, a=95%, b=90%;
wherein: the grain diameter of the fine magnesium powder is 1um to 200um; more preferably, the grain diameter is 0.1 um-20 um;
guiding grinding to be an innovative cut-off control mode based on big data information;
further, judging whether the grinding cut-off condition is met or not, specifically, starting a weight sensor to collect the weight of middle magnesium powder fine particles on the bottom of a grinding bin after each collection interval from the first grinding time interval, sending the weight to a control device, obtaining the weight by the control device, calculating the ratio of the weight to magnesium powder raw particles, and storing the ratio as a ratio sequence according to the time sequence; comparing the ratio sequence with a standard ratio sequence set to judge whether the cut-off condition is met or not;
preferably: the first grinding time interval is 1-5h;
preferably: the acquisition interval is a preset value; for example: 10-30min;
comparing the ratio sequence with a standard ratio sequence set, wherein the standard ratio sequence set comprises a plurality of standard ratio sequences; comparing the ratio sequence with each of the plurality of standard ratio sequences in turn and calculating the difference distance between the ratio sequence and the standard ratio sequence; if the difference distance between the standard ratio sequence and the ratio sequence is within the distance threshold, determining that the cut-off condition is met, otherwise, determining that the cut-off condition is not met;
the difference distance is calculated by adopting the following formula (1) to calculate the difference distance between the specific value sequence and the ith standard specific value sequence;
(1)；
wherein the ratio is the kth ratio in the ith standard ratio sequence; is the kth ratio in the ratio sequence; lth is the length of the sequence;
preferably, lth=12 to 24;
preferably: the distance threshold is a preset value;
preferably: the standard ratio sequence is obtained by experiments according to the obtained ratio sequence corresponding to the grinding process of the uniformity and the granularity range of the magnesium powder particles meeting the standard requirements of the final magnesium powder fine particles; a plurality of ratio sequences corresponding to the production process meeting the standard requirements are obtained through a large number of repeated experiments, and the ratio sequences are subjected to similarity comparison and combination to obtain a plurality of obvious representative ratio sequences which are used as standard ratio sequences to be put into a set to form the standard ratio sequences;
preferably: the experiment is a field experiment or a test experiment; the experiment times are 10000 times;
the difference distance is calculated by adopting the following formula (2) to calculate the difference distance between the specific value sequence and the ith standard specific value sequence;
(2)；
wherein the weight value is the weight value of the kth ratio;
preferably, the first time interval is 4-12 h; the acquisition interval is 10-20 min, and the lth=20-50;
collecting the middle magnesium powder fine particles, and re-executing the step S2 on the middle magnesium powder fine particles; collecting middle magnesium powder fine particles, and re-throwing the middle magnesium powder fine particles into a feed inlet 1;
alternatively, the following is used: judging whether the grinding cut-off condition is met, if yes, entering the next step, otherwise, collecting middle magnesium powder fine particles, and re-executing the step S2 on the middle magnesium powder fine particles; the method specifically comprises the following steps:
step S31, each ratio sequence and each first standard ratio sequence set are sequentially compared and a difference distance is calculated; if one or more first standard ratio sequences exist and the difference distance between the ratio sequences is within the distance threshold, determining that the cut-off condition is met, ending the step S3 and entering the step S4; otherwise, determining that the cutoff condition is not satisfied, and proceeding to step S32;
wherein: the first standard ratio sequence set and the standard ratio sequence set are obtained in the same way;
step S32, each of the ratio sequence and the second standard ratio sequence set is sequentially compared and a difference distance is calculated; selecting a second standard ratio sequence corresponding to the smallest difference distance from the first standard ratio sequences;
preferably: the second standard ratio sequence is obtained by obtaining a ratio sequence corresponding to the grinding process of the uniformity and the granularity range of the magnesium powder particles which do not meet the standard requirements of the final magnesium powder fine particles according to experiments; obtaining a plurality of ratio sequences which are obtained through experiments and do not meet the standard requirements through a large number of repeated experiments, performing similarity comparison and combination on the ratio sequences to obtain a plurality of remarkable representative ratio sequences which are used as second standard ratio sequences and are put into a set to form the second standard ratio sequences; the fact that the standard requirement of the final magnesium powder fine particles is not met refers to the fact that the standard requirement of the final magnesium powder fine particles is not met, and the typical situation that the standard requirement of the final magnesium powder fine particles is not met is several conditions;
preferably: the similarity comparison and merging are followed by clustering operation;
s33, acquiring a branch feed inlet corresponding to a second standard ratio sequence corresponding to the smallest difference distance; the branch feed inlets are respectively arranged between the grinding sheet groups; for example, in the example of FIG. 2, 2 branch feed inlets may be provided, between the 1 st polishing pad set and the 2 nd polishing pad set, and between the 2 nd polishing pad set and the 3 rd polishing pad set, respectively;
specifically, a branch feeding port (not shown) is positioned above a corresponding grinding sheet group on the barrel wall of the grinding bin 2;
alternatively, the following is used: presetting a corresponding relation between a second standard ratio sequence and a grinding gap adjustment mode; acquiring a grinding gap adjustment mode corresponding to a second standard ratio sequence corresponding to the smallest difference distance, and adjusting the vertical positions of an upper grinding plate and a lower grinding plate of the grinding plate group based on the adjustment mode so as to adjust the gap;
step S34, collecting middle magnesium powder fine particles, and putting the middle magnesium powder fine particles into the corresponding branch feed inlets again; and returns to step S2;
alternatively, the following is used: adjusting vertical positions of an upper polishing sheet and a lower polishing sheet of the polishing sheet group based on the adjustment manner to adjust a gap; then, the middle magnesium powder fine particles are re-put into the feed inlet 1;
according to the application, through setting the intelligent grinding cut-off condition and matching with a multi-level multi-granularity grinding mode, the grinding efficiency is greatly improved, and further, through intelligently controlling and selecting a proper grinding sheet group, the loss caused by ineffective grinding is avoided;
step S4: starting a heating bin to collect fine magnesium powder particles to a reaction bin; specifically, the heating plate 33 is started to heat the heating bin 3;
preferably, the heating temperature is 400-700 ℃;
preferably, the heating is performed by adopting a coil heating mode, and the position is the bottom of the heating bin 3;
step S5: the reaction bin 5 receives magnesium powder, hydrogen is introduced into the reaction chamber under the protection of inert gas, and the magnesium powder reacts with the hydrogen to obtain magnesium hydride particles, wherein the reaction time is 8-40h.
Preferably: the temperature in the reaction bin is 200-600 ℃;
preferably, the pressure in the reaction bin is 0.1-6 MPa. The particle diameter is 20-500nm, most of which is less than 100nm and about 100 nm.
Effect experiment:
adding 10kg of magnesium powder raw material with the average particle size of 1-1000 um into the production device, grinding for 24 hours by using a starting grinding bin under the condition of room temperature, re-feeding the magnesium powder raw material into a feeding hole 1 once at 8 hours, re-feeding the magnesium powder raw material into a branch feeding hole once at 8 hours (between a 1 st grinding disc group and a 2 nd grinding disc group), re-feeding the magnesium powder raw material into the feeding hole 1 once at 12 hours, re-feeding the magnesium powder raw material into the branch feeding hole once at 16 hours (between the 2 nd grinding disc group and the 3 rd grinding disc group), obtaining magnesium powder fine particles at the rotating speed of 80 revolutions per second, heating the magnesium powder fine particles to 220 ℃, guiding the magnesium powder fine particles into a reaction bin for reaction, setting the temperature of the reaction bin to 400 ℃, and setting the pressure to 2MPa to obtain final magnesium hydride particles; as can be seen from fig. 7, the magnesium hydride particles are uniform in size, spherical in particle morphology and have a particle size ranging from 20 nm to 250 nm; most of them are around hundred nm and within;
the production device provided by the application has the following beneficial effects:
1) The multi-angle repeated grinding is finished on the horizontal plane through multi-layer multi-granularity grinding and further intelligent grinding control, and the uniformity of the particles is subjected to supplementary grinding on the vertical plane, so that the better uniformity of the particles is achieved with higher efficiency;
2) The adjustment of the grinding gap, namely the coupling degree, is realized through the integral independent control of the similar grinding sheets; by adopting the mode, the uniformity and the size of the particles can be adjusted, the reduction of the grinding performance caused by abrasion resistance can be prevented, the controllability of the production process is improved, and the service life of production equipment is prolonged;
3) The grinding efficiency is greatly improved by setting the intelligent grinding cut-off condition and matching with a multi-level multi-granularity grinding mode, and further, the loss caused by ineffective grinding is avoided by intelligently controlling and selecting a proper grinding sheet set; the heat energy consumption is low, the environment is protected, and meanwhile, the production cost is reduced;
the foregoing has outlined and described the basic principles, features, and advantages of the present application in order that the description that follows is merely an example of the present application. It will be understood by those skilled in the art that the present application is not limited to the embodiments described above, but rather that the foregoing embodiments and description illustrate only the principles of the application, and that the application is susceptible to various equivalent changes and modifications without departing from the spirit and scope of the application, all of which are intended to be within the scope of the application as hereinafter claimed. The scope of the application is defined by the appended claims and their equivalents.
Claims (10)
1. A production device for preparing nano magnesium hydride, which comprises: the device comprises a feeding port, a grinding bin, a heating bin, a guide channel, a reaction bin, a discharge pipe, an air inlet pipe, a grinding bin bottom plate and a heating plate;
wherein, the feed inlet is arranged above the grinding bin, is in a cone shape, gradually extends towards the direction of the grinding bin and continuously reduces in diameter; the grinding bin is arranged below the feeding hole; the raw magnesium powder particles are conveyed into the grinding bin along the circumference of the barrel by the feeding port, and the raw magnesium powder particles can be subjected to repeated mechanical grinding with multiple granularities through multi-layer grinding in the grinding bin; the heating bin is arranged below the grinding bin and is directly connected with the grinding bin; the fine magnesium powder particles fall to the bottom of the heating bin through the opened grinding bin bottom plate; the heating bin is connected with the reaction bin through a guide channel, and the magnesium powder fine particles obtained by grinding enter the reaction bin along the guide channel under the heating of the heating plate and directly react with hydrogen entering from the air inlet pipe to prepare nano magnesium hydride;
the grinding bin comprises a plurality of grinding plate groups which are connected from top to bottom through a rotating shaft, and the grinding plate groups rotate around the rotating shaft; specific: each of the polishing sheet groups includes 3 polishing sheets tightly coupled to each other, an upper polishing sheet, a middle polishing sheet, and a lower polishing sheet; wherein, the two sides of the middle grinding disc are provided with hemispherical grinding balls which are annularly arranged, and a plurality of circles of grinding balls are outwards arranged along the axis of the rotating shaft;
the number of the grinding sheet groups is 3, and the grinding sheet groups comprise: a 1 st polishing sheet group, a 2 nd polishing sheet group and a 3 rd polishing sheet group arranged from top to bottom; the coupling tightness of the grinding sheets in the grinding sheet group is increased from top to bottom in sequence; the coupling tightness of the grinding sheet group positioned at the upper part is looser than that of the grinding sheet group positioned at the lower part; for each abrasive sheet set, the degree of tightness of coupling between the upper and middle abrasive sheets is loosely greater than or equal to the degree of tightness of coupling between the lower and middle abrasive sheets; the looser the grinding gap is, the larger, and conversely, the tighter the gap is; h1> =h2, h3> =h4, h5> =h6; h1> h3> h5; h2> h4> h6; wherein: h1 H2, h3, h4, h5, h6 are the vertical distances between the upper and middle plates in the 1 st plate group, the middle and lower plates in the 1 st plate group, the upper and middle plates in the 2 nd plate group, the middle and lower plates in the 2 nd plate group, the upper and middle plates in the 3 rd plate group, and the middle and lower plates in the 3 rd plate group, respectively; the fine magnesium powder particles in the middle formed in the grinding process enter a coupling gap between the upper grinding disc and the grinding ball of the middle grinding disc along a circular notch on the upper grinding disc; and finally along the guide grooves in the middle blade into the coupling gap between the lower blade and the middle blade grinding balls; after being fully ground, the polishing solution falls on the next grinding sheet group; the last grinding sheet group obtains magnesium powder fine particles to drop on a grinding bin bottom plate at the bottom of the grinding bin;
the size of the grinding ball of the same grinding disc along the radial inward direction gradually changes from large to small; the upper abrasive plates in all the abrasive plate groups can be independently and integrally controlled, the gaps can be reduced by integrally moving downwards, the lower abrasive plates in all the abrasive plate groups can be independently and integrally controlled, and the gaps can be increased by integrally moving upwards, so that the coupling tightness is increased; adjusting the coupling relationship by moving up and down as a whole; the vertical connection between the collars realizes the integral control of the upper grinding plates in all grinding plate groups and the integral control of the lower grinding plates in all grinding plate groups, and the middle grinding plates in all grinding plate groups are kept unchanged relative to the rotating shaft;
the grinding bin bottom plate is movable, and when the grinding cut-off condition is met, the movable grinding bin bottom plate moves out, so that fine magnesium powder particles positioned on the grinding bin bottom plate fall to the bottom of the reaction bin; when the grinding cut-off condition is not met, collecting middle magnesium powder fine particles, and re-throwing the middle magnesium powder fine particles into a feed inlet;
judging whether the grinding cut-off condition is met or not, specifically, starting a weight sensor to collect the weight of the middle magnesium powder fine particles on the bottom of a grinding bin after each collection interval from the first grinding time interval, sending the weight to a control device, obtaining the weight by the control device, calculating the ratio of the weight to the weight of the magnesium powder original particles, and storing the ratio as a ratio sequence according to the time sequence; comparing the ratio sequence with a standard ratio sequence set to judge whether the cut-off condition is met or not; the standard ratio sequence is obtained by experiments according to the obtained ratio sequence corresponding to the grinding process of the uniformity and the granularity range of the magnesium powder particles meeting the standard requirements of the final magnesium powder fine particles;
comparing the ratio sequence with a standard ratio sequence set, wherein the standard ratio sequence set comprises a plurality of standard ratio sequences; comparing the ratio sequence with each of the plurality of standard ratio sequences in turn and calculating the difference distance between the ratio sequence and the standard ratio sequence; if a standard ratio sequence exists and the difference distance between the ratio sequences is within the distance threshold, determining that the cut-off condition is met, otherwise, determining that the cut-off condition is not met.
2. The production device according to claim 1, wherein: the inner and outer rings of the middle grinding disc are alternately provided with non-through guide grooves, so that fine particles of the middle magnesium powder are guided to a coupling gap between the lower grinding disc and the grinding ball of the middle grinding disc from the periphery of the middle grinding disc.
3. The production device according to claim 2, wherein: the guide groove is a hollowed arc guide groove and is not a radial through groove.
4. A production device according to claim 3, wherein: 4-8 arc-shaped guide grooves are arranged on each middle grinding disc, and the radian is 90-180 degrees.
5. The production device according to claim 4, wherein: the width and area of the guide groove on the outer ring are larger than those of the guide groove on the inner part.
6. The production device according to claim 5, wherein: the size of the grinding balls gradually increases along the direction in which the diameter extends outward.
7. The production device according to claim 6, wherein: the nano magnesium hydride after the reaction passes through a product discharge pipe, and then is subjected to subsequent condensation and collection of the nano magnesium hydride.
8. The production apparatus as claimed in claim 7, wherein: the bottom plate is latticed after opening for the even dropping of magnesium powder fine particles is in reaction bin bottom.
9. The production device according to claim 8, wherein: the bottom plate is formed by splicing two or more grid-shaped plates, and after the bottom plate is opened, the grids are exposed so that magnesium powder fine particles above the bottom plate fall off.
10. A preparation method of a preparation production device using the nano magnesium hydride according to any one of claims 1-9, firstly, preliminary crushing a metal magnesium raw material to obtain magnesium powder raw particles, and putting the magnesium powder raw particles into a grinding bin through a feed inlet.
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