CN107224949B - Method for preparing nano material by using high-gravity field microreactor and liquid-phase precipitation method - Google Patents
Method for preparing nano material by using high-gravity field microreactor and liquid-phase precipitation method Download PDFInfo
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Abstract
A high-gravity field micro-reactor for preparing nano materials comprises a micro-reaction component, a material receiving groove provided with a discharge hole, a first motor, a transmission system, a feeding system and a supporting system, wherein the micro-reaction component consists of an upper disc and a lower disc, the central parts of the upper disc bottom surface and the lower disc top surface, which are distributed with a micro-groove and a lower disc, are provided with feeding micro-channels, a gap of 0.03-0.1 mm is formed between the upper disc bottom surface and the lower disc top surface after combination, and the transmission system operates under the driving of the first motor, so that the upper disc and the lower disc in the micro-reaction component rotate in opposite rotating directions. In order to adjust the gap between the upper disc and the lower disc in the micro-reaction assembly and clean the upper disc and the lower disc, an upper disc lifting system can be additionally arranged. The super-gravity field microreactor is used for preparing the nano material by adopting a liquid phase precipitation method, so that the nano material has high dispersity and uniform particle distribution, the treatment capacity is increased, and the blockage of a micro-reaction assembly is avoided.
Description
Technical Field
The invention belongs to the technical field of chemical reaction, and particularly relates to a super-gravity-field micro-reactor for preparing a nano material and a method for preparing the nano material by a liquid phase precipitation method.
Background
The nano material is paid much attention in recent years, and shows important application value in various fields by virtue of surface effect, volume effect, quantum size effect, macroscopic quantum tunneling effect and the like which are different from the conventional material.
In the preparation process of the nano material, the characteristic time t of particle nucleation N 1ms grade, micro-mixing homogenization characteristic time t m ＝k m (v/ε) 1/2 (k m Is constant), t is required to ensure high dispersibility and uniform distribution of the particle size m <t N Whereas in a conventional mechanically stirred tank reactor, t m = 5-50 ms, greater than t N Thus seriously affecting the nucleation effect. In order to solve the above problems and to prepare a nanomaterial with highly dispersed and uniformly distributed particle sizes, vapor deposition methods, plasma methods, super-gravity methods, ultrasonic methods, microwave methods, microreactor methods, and the like have been developed in succession. Wherein, the micro-reactor method limits the chemical reaction in a limited space by virtue of micro-scale effect, shortens the contact distance of reactants by increasing the surface area of a body, greatly improves the mass transfer speed, and further t m <t N The prepared nanometer material has high dispersivity, excellent distribution homogeneity, fining and controllability, and is widely concerned.
At present, the microreactor for preparing nano materials mainly comprises a membrane hole type, a T type, a Y type, a hydraulics focusing type, a thin layer crossing type, a recombination type, a multi-branch injection type and an external field force coupling type. However, these microreactors still have two problems in industrial application: firstly, the processing capacity is small, the industrial amplification is difficult, the micro-channel or membrane pore size is usually in a micron order, the flow capacity is limited, the single-channel processing capacity is extremely small, the micro-reactor is usually amplified in parallel to achieve the industrial processing capacity, and when the micro-channel number is increased sharply, the detection and control complexity of the micro-reactor is increased; and secondly, the micro-channel or the membrane hole is easy to block and difficult to clean, a plurality of micro-channels or membrane holes are generally integrated in a closed cavity of the micro-reactor, the inner diameter of the micro-channel or the pore diameter of the membrane hole is narrow, and nano particles formed by reaction or impurities in raw materials easily cause the micro-channel to block and difficult to clean. In order to prevent the blockage, an external connection processing device, such as a Flow Plate micro-reactor designed by Lonza and the like, is generally used for generating ultrasonic cavitation action on the inside of the fluid through an external connection ultrasonic device, so as to prevent the blockage, but the structure is complicated and the cost is increased due to the blockage prevention through the external connection device, so that the blockage is not beneficial to industrial popularization.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-gravity-field microreactor for preparing nano materials and a method for preparing the nano materials by a liquid-phase precipitation method, which can increase the treatment capacity and avoid the blockage of a micro-reaction assembly while keeping the high dispersibility and the uniform particle distribution of the nano materials so as to meet the industrial production requirement of preparing the nano materials by the liquid-phase precipitation method in the chemical field.
The invention relates to a high-gravity-field microreactor for preparing nano materials, which comprises a micro-reaction component, a material receiving groove provided with a discharge hole, a first motor, a transmission system, a feeding system and a supporting system; the micro-reaction component consists of an upper disc and a lower disc, wherein micro-grooves are distributed on the bottom surface of the upper disc, a buffer groove is arranged at the central part of the bottom surface of the upper disc, the micro-grooves are distributed on the top surface of the lower disc, and a feeding micro-channel is arranged at the central part of the lower disc, wherein the number of the feeding micro-channels is more than or equal to the type of raw material liquid forming reaction products; the transmission system comprises a transmission, a first transmission shaft, a second transmission shaft, a third transmission shaft, a fourth transmission shaft, a first synchronous belt, a gear transmission pair, a second synchronous belt and a plurality of bearing assemblies for being combined with the transmission shafts, wherein the first synchronous belt consists of a first synchronous belt driving wheel, a first synchronous belt driven wheel and a first transmission belt; the supporting system comprises a bottom frame, a middle frame, an upper frame, a first support and a joint body, wherein the joint body is provided with a central hole matched with the lower section of the fourth transmission shaft, the inner wall of the central hole is provided with a bearing combined with the fourth transmission shaft and feeding chambers matched with the feeding channel in the shaft body of the fourth transmission shaft in position and in the same number, the feeding chambers are provided with feeding holes penetrating through the inner wall and the outer wall of the central hole, and a sealing ring is arranged between the bearing and the feeding chambers; the feeding system is composed of a feeding hole and a feeding cavity which are arranged on the connector body, a feeding channel which is arranged in the shaft body of the fourth transmission shaft and a feeding micro-channel which is arranged at the central part of the lower disc.
The combination mode of the components is as follows:
the bottom frame, the middle frame and the upper frame are overlapped and connected into a whole, the first support is installed at one end of the upper surface of the top plate of the upper frame, the speed changer and the first motor are installed on the first support, and a power output shaft of the first motor is connected with a power input shaft of the speed changer; the upper end of the first transmission shaft is connected with a power output shaft of the transmission, the lower end of the first transmission shaft is combined with a bearing assembly arranged on a bottom plate of the bottom frame, the upper end of the second transmission shaft is combined with the bearing assembly arranged on a top plate of the upper frame, the lower end of the second transmission shaft is combined with the bearing assembly arranged on the bottom plate of the upper frame, two ends of the second transmission shaft are parallel to the center line of the first transmission shaft after being combined with the bearing assembly, the upper end of the third transmission shaft is combined with the bearing assembly arranged on the top plate of the upper frame, the lower end of the third transmission shaft is positioned below the bottom plate of the upper frame, the center line of the third transmission shaft is parallel to the center line of the second transmission shaft after being combined with the bearing assembly, the distance between the center line of the third transmission shaft and the center line of the second transmission shaft meets the installation requirement of a gear transmission pair, the joint body is arranged on the bottom plate of the bottom frame, the center line of the third transmission shaft and the center line of the third transmission shaft are positioned on the same straight line, the lower section of the fourth transmission shaft is arranged in an inner hole of the joint body, and the upper end of the bottom plate of the middle frame; the first synchronous belt driving wheel is arranged at the upper section of the first transmission shaft, the first synchronous belt driven wheel is arranged at the upper section of the second transmission shaft, the driving gear is arranged at the lower section of the second transmission shaft, the driven gear is arranged on the third transmission shaft, the second synchronous belt driving wheel is arranged at the lower section of the first transmission shaft, and the second synchronous belt driven wheel is arranged on the fourth transmission shaft; the receiving groove is arranged on the top surface of the bottom plate of the middle frame, and the mounting position of the receiving groove ensures that the upper end of the fourth transmission shaft is positioned in the center of the inner cavity of the receiving groove; the lower disc of the micro-reaction assembly is fixed at the upper end of the fourth transmission shaft and is positioned in the material receiving groove, each feeding micro-channel arranged at the center of the lower disc is respectively connected and communicated with a corresponding feeding channel arranged in the shaft body of the fourth transmission shaft, the upper disc of the micro-reaction assembly is fixed at the lower end of the third transmission shaft and is positioned in the material receiving groove, and a gap of 0.03 mm-0.1 mm is formed between the bottom surface of the upper disc and the top surface of the lower disc.
After the combination according to the above-mentioned mode, the transmission system operates under the drive of the first motor, thereby making the upper disk and the lower disk in the micro-reaction assembly rotate in opposite rotating directions, and the structure of the transmission system can make the upper disk and the lower disk rotate in opposite directions at the same rotating speed, and also can make the upper disk and the lower disk rotate in opposite directions at different rotating speeds.
In order to adjust the gap between the upper disc and the lower disc in the micro-reaction assembly and clean the upper disc and the lower disc, the invention adopts the technical scheme that an upper disc lifting system is additionally arranged. The upper disc lifting system comprises a second motor, a bevel gear transmission pair, a lifting shaft, a second support, a ball spline, a positioning block and a cylindrical supporting cylinder, wherein the upper section of the lifting shaft is a screw rod section, the lower part of the lifting shaft is provided with a spline section, the central hole of a driven bevel gear of the bevel gear transmission pair is a screw hole matched with the screw rod section arranged on the lifting shaft, and the second support is provided with a through hole for the screw rod section of the lifting shaft to pass through. In order to adapt to the structure and the function of the upper disc lifting system, the lower part of the third transmission shaft is provided with a spline section which is combined with a female rotary ball spline arranged on the bottom plate of the upper frame. The mounting position and the mounting mode of each component of the upper disc lifting system are as follows: the supporting cylinder is arranged on the upper surface of the top plate of the upper frame, and the central line of the supporting cylinder and the central line of the third transmission shaft are in the same straight line; the lower end of the lifting shaft is connected with the upper end of the third transmission shaft through a coupler, the upper end of the lifting shaft extends out of the supporting cylinder, the ball spline is installed on the spline section of the lifting shaft, at least two positioning blocks are arranged, one end of each positioning block is installed around the outer side face of the ball spline at equal intervals, and the other ends of the positioning blocks are in movable fit with the inner wall of the supporting cylinder; the second support is sleeved with the screw rod section of the lifting shaft and fixed at the upper end of the supporting cylinder, the second motor is installed on the second support, a driving bevel gear of the bevel gear transmission pair is installed on a power output shaft of the second motor, and a driven bevel gear of the bevel gear transmission pair is installed on the screw rod section of the lifting shaft and combined with the driving bevel gear.
The upper disc of the high-gravity-field microreactor for preparing the nano-materials is in a shape of a truncated cone, a stepped truncated cone with a large lower part and a small upper part, or a truncated cone with a large lower part and a small upper part, and the lower disc of the high-gravity-field microreactor for preparing the nano-materials is in a shape of a truncated cone, a stepped truncated cone with a large upper part and a small lower part, or a truncated cone with a large upper part and a small lower part.
The high gravity field micro-reactor for preparing the nano material is characterized in that a feeding micro-channel arranged at the central part of a lower disc is preferably a round hole, a feeding channel penetrating through the upper end surface and arranged in a shaft body of a fourth transmission shaft is preferably a round hole, and the feeding micro-channel and the feeding channel have the same aperture and are 0.45-4 mm.
The microgravity field micro-reactor for preparing the nano material has the advantages that the micro-grooves on the bottom surface of the upper disk and the top surface of the lower disk are distributed in a spiral shape, an arc shape, a sector shape or a honeycomb shape. The width of the micro-groove on the bottom surface of the upper tray and the top surface of the lower tray is 0.01 mm-0.80 mm, and the depth is 0.05 mm-0.75 mm.
The method for preparing the nano material by the liquid phase precipitation method uses the high gravity field microreactor with the structure and has the following operation:
(1) Starting a first motor, and driving a transmission system to operate under the driving of the first motor, so that an upper disc and a lower disc in the micro-reaction assembly rotate in opposite rotating directions, and the separation factor is controlled to be 15-250;
(2) Feeding each raw material liquid into a feeding channel arranged in the shaft body of a fourth transmission shaft through a feeding hole and a feeding cavity arranged on a joint body respectively, feeding each raw material liquid into a feeding micro-channel arranged on a lower disc in a micro-reaction assembly through the feeding channel, and then feeding each raw material liquid into a space between an upper disc and a lower disc of the micro-reaction assembly through the feeding micro-channel, wherein each raw material liquid is milled to continuously update a contact interface and strengthen mass transfer to complete reaction under the action of the overweight force generated by the upper disc and the lower disc through micro-groove layer layers on the bottom surface of the upper disc and the top surface of the lower disc to form nano granular reaction products, and slurry containing the reaction products is thrown into a material receiving groove under the action of centrifugal force and is discharged from a discharge hole arranged on the material receiving groove;
(3) And (3) filtering, cleaning and drying the slurry containing the reaction product discharged from the discharge hole of the material receiving groove, or cleaning, filtering and drying the slurry, or cleaning and drying the slurry while filtering to obtain the nano material.
The super-gravity field micro-reactor and the liquid phase precipitation method are used for preparing the nano material, and the processing amount is related to the feeding flow of each raw material liquid and the radius of an upper disc and a lower disc in the micro-reaction assembly.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention discloses a high-gravity field micro-reactor, wherein micro-grooves are distributed on the bottom surface of an upper disc and the top surface of a lower disc of a micro-reaction component, a stable and adjustable high-gravity field is constructed by rotating the upper disc and the lower disc in opposite rotating directions, the generated high gravity pushes reactants to the outer edge from the centers of the two discs, in the process, fluid continuously collides with the micro-grooves and is further dispersed and crushed to form a continuously updated surface under the combined action of shearing force and the high gravity, the mass transfer effect is greatly enhanced, the flow velocity of the fluid is increased, the reaction residence time of the fluid in the micro-reaction component is rapidly reduced, and simultaneously, under the micro-scale effect generated by micro-gaps of the upper disc and the lower disc of the micro-reaction component, the surface area between the fluid is increased, the mass transfer distance is reduced, and t is reduced, so that t m ＜t N And moreover, the supersaturation degree of the reaction product in the reaction solution is improved, according to the classical nucleation theory, the supersaturation degree of the reaction product is increased, the nucleation rate is increased rapidly, and the critical nucleation size is reduced, so that the particle size distribution of the reaction product is narrowed, and the nano material with high dispersity and uniform particle size distribution is obtained.
2. The high-gravity-field micro-reactor adopts an active mixing mode, and a high-gravity field is formed by reversely rotating the upper disc and the lower disc, so that the flow velocity of fluid is greatly improved, and meanwhile, the micro-reaction componentFor a non-closed system, the fluid can be thrown out from the periphery of the upper and lower disc edges, so the handling capacity per unit time is greatly improved (taking example 3 as an example, the handling capacity is 0.018m 3 H), and the reactor breaks through the quantity amplification mode of the parallel superposition of the conventional microreactor, and experiments show that the handling capacity of the device is in positive correlation with the third power of the radius of the upper disk and the lower disk, so that the nano material prepared by using the microreactor and the method can reach the industrial production level standard.
3. According to the high-gravity-field microreactor, under the action of a coupling high-gravity field, a raw material liquid quickly passes through the micro-gap sections of the upper disc and the lower disc in the micro-reaction assembly, and the distance between the micro-gap sections can be changed through online adjustment of the upper disc lifting system according to actual reaction requirements, so that impurities and generated precipitates are timely and quickly thrown out of the micro-reaction assembly along with liquid after reaction, in addition, after the reaction is finished, the upper disc can be integrally lifted through the upper disc lifting system, the distance between the upper disc and the lower disc is increased, and the micro-reaction assembly is convenient to clean and remove impurities. Experiments show that the blocking phenomenon does not occur when the micro-reactor is continuously and stably operated for 72 hours, and the blocking problem of the micro-reactor is effectively solved.
4. Because the upper disc and the lower disc of the micro-reaction component rotate reversely, the relative acceleration can be improved, the mixed mass transfer effect is enhanced, and the energy consumption can be reduced.
Drawings
FIG. 1 is a schematic diagram of a first structure of a high gravitational field microreactor for preparing nanoparticles according to the present invention;
FIG. 2 is a schematic diagram of a second structure of a high gravitational field microreactor for preparing nanoparticles according to the present invention;
FIG. 3 is a schematic diagram of a bottom frame in a high gravitational field microreactor for the production of nanoparticles in accordance with the present invention;
FIG. 4 is a schematic diagram of a middle frame in a high gravitational field microreactor for producing nanoparticles according to the present invention;
FIG. 5 is a schematic diagram of an upper frame in a high gravitational field microreactor for producing nanoparticles according to the present invention;
FIG. 6 is a schematic view of a first transmission shaft in a high gravitational field microreactor for producing nanoparticles according to the present invention;
FIG. 7 is a schematic representation of a first synchronization zone in a high gravitational field microreactor for the production of nanoparticles according to the present invention;
FIG. 8 is a schematic diagram of a gear pair in a high gravitational field microreactor for producing nanoparticles according to the present invention;
FIG. 9 is a schematic diagram of a third drive shaft in a high gravitational field microreactor for producing nanoparticles in accordance with the present invention;
FIG. 10 isbase:Sub>A sectional view A-A of FIG. 9;
FIG. 11 is a cross-sectional view B-B of FIG. 2;
FIG. 12 is a schematic diagram of a fourth transmission shaft in a high gravitational field microreactor for producing nanoparticles according to the present invention;
fig. 13 is a schematic diagram of a fourth transmission shaft and a joint body in a high gravitational field microreactor for producing nanoparticles according to the present invention;
FIG. 14 is a schematic diagram of a second timing belt in a high gravitational field microreactor for producing nanoparticles according to the present invention;
FIG. 15 is a schematic view of a discharge chute in a high gravity field microreactor for producing nanoparticles in accordance with the present invention;
FIG. 16 is a schematic diagram of a lifting shaft in a high gravitational field microreactor for the production of nanoparticles according to the present invention;
FIG. 17 is a cross-sectional view C-C of FIG. 16;
FIG. 18 is a schematic view of a lifting shaft spline segment and a ball spline in a high gravity field microreactor for preparing nanoparticles according to the present invention;
FIG. 19 is a schematic top plate view of a micro-reaction module in a high gravitational field microreactor for producing nanoparticles according to the present invention;
FIG. 20 is a top view of FIG. 19;
FIG. 21 is a schematic bottom-wall view of a micro-reaction module in a high gravitational field microreactor for producing nanoparticles according to the present invention;
FIG. 22 is a top view of FIG. 21;
FIG. 23 is a schematic view showing a first form of micro grooves provided on the bottom surface of the upper plate or the top surface of the lower plate of the micro reaction module, the micro grooves being spirally distributed;
FIG. 24 is a schematic view showing a second pattern of micro-grooves formed on the bottom surface of the upper plate or the top surface of the lower plate of the micro-reaction module, the micro-grooves being distributed in a fan shape;
FIG. 25 is a schematic view showing a third form of micro grooves formed on the bottom surface of the upper plate or the top surface of the lower plate of the micro reaction module, the micro grooves being distributed in an arc shape;
FIG. 26 is a schematic view showing a third form of micro grooves provided on the bottom surface of the upper plate or the top surface of the lower plate of the micro reaction module, the micro grooves being distributed in a honeycomb shape.
In the figure, 1-a bottom frame, 1-a rectangular bottom plate, 1-2-a curved bracket, 2-a middle frame, 2-1-a bottom plate, 2-a curved bracket, 3-an upper frame, 3-1-a bottom plate, 3-2-a top plate, 3-a curved bracket, 4-a supporting cylinder, 5-a second support, 6-a first support, 7-a transmission, 8-a first motor, 9-a first transmission shaft, 10-a first synchronous belt driving wheel, 11-a first synchronous belt driven wheel, 12-a driving gear, 13-a driven gear, 14-a third transmission shaft, 14-1 connecting section, 14-2 spline section, 15-an upper plate, 15-1-a groove, 16-a female rotary ball spline, 17-a second synchronous belt driving wheel, 18-a second synchronous belt driven wheel, 19-a fourth transmission shaft, 19-1-a first feeding channel, 19-2-a second feeding channel, 20-a lower disc, 20-1-a first feeding microchannel, 20-2-a second feeding microchannel, 21-a joint body, 21-1-a gland, 21-2-a hydrostatic bearing, 21-3-a sealing ring, 21-4-a feeding chamber, 21-5-a deep groove ball bearing, 21-6-a rear end cover, 22-a first feeding port, 23-a second feeding port, 24-a receiving groove, 25-a discharging port arranged in the receiving groove, 26-a second motor, 27-a lifting shaft, 27-1-a screw rod section, 27-2-a spline section, 28-a ball spline, 29-a coupling, 30-a positioning block, 31-a plane bearing, 32-a bearing assembly, and 33-a second transmission shaft.
Detailed Description
The method for preparing the nano material by the high gravitational field microreactor and the liquid phase precipitation method is further explained by the embodiments and the attached drawings.
Example 1
In this embodiment, the high gravity field microreactor for preparing nanomaterials is shown in fig. 1, and comprises a micro-reaction assembly, a material receiving groove 24 provided with a material outlet 25, a first motor 8, a transmission system, a feeding system and a supporting system.
The micro-reaction component consists of an upper disc 15 and a lower disc 20, wherein the upper disc 15 is in a shape of a stepped circular truncated cone with a large lower part and a small upper part as shown in figures 19 and 20, a spiral micro-groove as shown in figure 23 is distributed on the bottom surface, a buffer groove 15-1 is arranged at the central part of the bottom surface of the upper disc, the lower disc 20 is in a shape of a stepped circular truncated cone with a large upper part and a small lower part as shown in figures 21 and 22, a spiral micro-groove as shown in figure 23 is distributed on the top surface, and two feeding micro-channels which are named as a first feeding micro-channel 20-1 and a second feeding micro-channel 20-2 are arranged at the central part of the lower disc; the radius of the bottom surface of the upper disc and the top surface of the lower disc is 5cm, the width of the spiral micro-groove on the bottom surface of the upper disc and the width of the spiral micro-groove on the top surface of the lower disc are 0.5mm, the depth of the spiral micro-groove is 0.5mm, the first feeding micro-channel 20-1 and the second feeding micro-channel 20-2 are round holes with the same aperture, and the aperture of the round holes is 2.5mm.
The transmission system comprises a speed changer 7, a first transmission shaft 9, a second transmission shaft 33, a third transmission shaft 14, a fourth transmission shaft 19, a first synchronous belt, a gear transmission pair, a second synchronous belt and a plurality of bearing assemblies for being combined with the transmission shafts; the first synchronous belt is composed of a first synchronous belt driving wheel 10, a first synchronous belt driven wheel 11 and a first transmission belt as shown in fig. 7; the gear transmission pair is composed of a driving gear 12 and a driven gear 13 as shown in fig. 8; the second synchronous belt is composed of a second synchronous belt driving wheel 17, a second synchronous belt driven wheel 18 and a second transmission belt as shown in fig. 14; as shown in fig. 12 and 13, the fourth transmission shaft 19 is provided with two feeding channels penetrating through the upper end surface in the shaft body, which are named as a first feeding channel 19-1 and a second feeding channel 19-2, the first feeding channel 19-1 and the second feeding channel 19-2 are circular holes with the same aperture, and the aperture of the circular hole is 2.5mm.
The supporting system consists of a bottom frame 1, a middle frame 2, an upper frame 3, a first support 6 and a joint body 21; as shown in fig. 3, the bottom frame 1 is composed of a rectangular bottom plate 1-1 and arc-shaped supports 1-2 symmetrically arranged at two ends of the rectangular bottom plate; as shown in fig. 4, the middle frame 2 is composed of a bottom plate 2-1 with two arc-shaped ends and two plane sides and arc-shaped supports 2-2 symmetrically arranged at the two ends of the bottom plate, and the bottom plate 2-1 is provided with a through hole for the first transmission shaft 9 and the fourth transmission shaft 19 to pass through; as shown in fig. 5, the upper frame 3 is composed of a bottom plate 3-1, a top plate 3-2 and an arc-shaped bracket 3-3 for connecting the bottom plate and the top plate, wherein the bottom plate 3-1 and the top plate 3-2 have the same shape and size, both ends of the bottom plate and the top plate are arc surfaces, and both sides of the bottom plate and the top plate are planes, and through holes for the first transmission shaft 9 and the third transmission shaft 14 to pass through are arranged on the bottom plate and the top plate; the joint body is provided with a central hole matched with the lower section of the fourth transmission shaft 19, a hydrostatic bearing 21-2 combined with the fourth transmission shaft is arranged at the upper end of the inner wall of the central hole, a deep groove ball bearing 21-5 combined with the fourth transmission shaft is arranged at the lower end of the inner wall of the central hole, two annular feeding chambers 21-4 matched with the feeding channel in the shaft body of the fourth transmission shaft are arranged at the section between the hydrostatic bearing and the deep groove ball bearing, a first feeding hole 22 and a second feeding hole 23 penetrating through the inner wall and the outer wall of the central hole are respectively arranged at the two feeding chambers, and sealing rings 21-3 are arranged between the hydrostatic bearing and the feeding chambers, between the two feeding chambers and between the deep groove ball bearing and the feeding chambers.
The feeding system is composed of a feeding hole and a feeding cavity which are arranged on the connector body, a feeding channel which is arranged in the shaft body of the fourth transmission shaft and a feeding micro-channel which is arranged at the central part of the lower disc.
The combination mode of the components is as shown in fig. 1, the bottom frame 1, the middle frame 2 and the upper frame 3 are overlapped and connected into a whole through a threaded connecting piece, the first support 6 is arranged at the left end of the upper surface of the top plate 3-2 of the upper frame, the speed changer 7 and the first motor 8 are arranged on the first support 6, and the power output shaft of the first motor is connected with the power input shaft of the speed changer; the upper end of the first transmission shaft 9 is connected with a power output shaft of the transmission, the lower end of the first transmission shaft is combined with a bearing assembly 32 arranged at the left end of the bottom frame bottom plate 1-1, and the bearing assemblies 32 combined with the first transmission shaft 9 are respectively arranged at through holes arranged on the middle frame bottom plate 2-1 and the upper frame bottom plate 3-1 and used for the first transmission shaft 9 to pass through; the second transmission shaft 33 is positioned at the right side of the first transmission shaft, the upper end of the second transmission shaft is combined with the bearing assembly 32 arranged on the upper frame top plate 3-2, the lower end of the second transmission shaft is combined with the bearing assembly 32 arranged on the upper frame bottom plate 3-1, and the central line of the second transmission shaft 33 is parallel to the central line of the first transmission shaft 9 after the two ends of the second transmission shaft are combined with the bearing assemblies; the third transmission shaft 14 is positioned at the right side of the second transmission shaft, the upper end of the third transmission shaft is combined with a bearing assembly 32 arranged on the top plate of the upper frame, the lower end of the third transmission shaft is positioned below a bottom plate 3-1 of the upper frame, the upper end of the third transmission shaft 14 is parallel to the central line of the second transmission shaft after being combined with the bearing assembly, and the bearing assembly 32 combined with the third transmission shaft 14 is arranged at a through hole arranged on the bottom plate 3-1 of the upper frame and used for the third transmission shaft 14 to pass through; the lower section of the fourth transmission shaft 19 is arranged in an inner hole of the joint body and is positioned by a pressure plate 21-1 and a rear cover plate 21-6, the upper end of the fourth transmission shaft 19 is positioned on a bottom plate 2-1 of the middle frame, and a bearing assembly 32 combined with the fourth transmission shaft 19 is arranged at a through hole arranged on the bottom plate 2-1 of the middle frame and used for the fourth transmission shaft 19 to pass through; the first synchronous belt driving wheel 10 is arranged at the upper section of the first transmission shaft, the first synchronous belt driven wheel 11 is arranged at the upper section of the second transmission shaft, the driving gear 12 is arranged at the lower section of the second transmission shaft, the driven gear 13 is arranged on the third transmission shaft, the second synchronous belt driving wheel 17 is arranged at the lower section of the first transmission shaft, and the second synchronous belt driven wheel 18 is arranged on the fourth transmission shaft; the material receiving groove 24 is arranged on the top surface of the bottom plate 2-1 of the middle frame, and the mounting position of the material receiving groove is that the upper end of the fourth transmission shaft 19 is positioned at the central part of the inner cavity of the material receiving groove; the lower disc 20 in the micro-reaction assembly is fixed at the upper end of a fourth transmission shaft 19 and is positioned in a material receiving groove, a first feeding micro-channel 20-1 and a second feeding micro-channel 20-2 arranged at the center of the lower disc are respectively connected and communicated with a first feeding channel 19-1 and a second feeding channel 19-2 arranged in a shaft body of the fourth transmission shaft, an upper disc 15 in the micro-reaction assembly is fixed at the lower end of the third transmission shaft and is positioned in the material receiving groove, and a gap of 0.08mm is formed between the bottom surface of the upper disc and the top surface of the lower disc.
Example 2
In this embodiment, as shown in fig. 2, the super-gravity-field microreactor for preparing nanomaterials is composed of a micro-reaction assembly, a receiving groove 24 provided with a discharge hole, a first motor 8, a transmission system, a feeding system, a support system and an upper disk lifting system. The difference from the embodiment 1 is that: an upper disc lifting system is added; the lower part of the third drive shaft 14 in the drive train is provided with a splined section 14-2 (see fig. 9) which is combined with a female rotary ball spline 16 (see fig. 2) mounted on the upper frame bottom plate 3-1; the micro-grooves distributed on the bottom surface of the upper plate 15 and the micro-grooves distributed on the top surface of the lower plate 20 in the micro-reaction assembly are fan-shaped micro-grooves as shown in figure 24, the width of the fan-shaped micro-grooves on the bottom surface of the upper plate and the fan-shaped micro-grooves on the top surface of the lower plate are 0.06mm, the depth of the fan-shaped micro-grooves is 0.10mm, and the pore diameter of the first feeding micro-channel 20-1 and the second feeding micro-channel 20-2 is 1.0mm; the aperture of a first feeding channel 19-1 and a second feeding channel 19-2 on the shaft body of the fourth transmission shaft is 1.0mm; a gap of 0.05mm is reserved between the bottom surface of the upper disc and the top surface of the lower disc.
In this embodiment, the upper disc lifting system is shown in fig. 2, and includes a second motor 26, a bevel gear transmission pair, a lifting shaft 27, a second support 5, a ball spline 28, a positioning block 30, and a cylindrical support cylinder 4, where the lifting shaft 27 is shown in fig. 16 and 17, the upper section of the lifting shaft is a screw rod section 27-1, the lower section of the lifting shaft is provided with a spline section 27-2, a central hole of a driven bevel gear in the bevel gear transmission pair is a screw hole matched with the screw rod section 27-1 provided on the lifting shaft, and the second support 5 is provided with a through hole for the screw rod section 27-1 of the lifting shaft to pass through; the mounting position and the mounting mode of each component of the upper disc lifting system are as follows: the supporting cylinder 4 is arranged on the upper surface of the top plate 3-2 of the upper frame, and the central line of the supporting cylinder is in line with the central line of the third transmission shaft 14; the lower end of the lifting shaft 27 is connected with the upper end of the third transmission shaft 14 through a coupler 29, the bearing in the coupler is a plane bearing 31, the upper end of the lifting shaft extends out of the supporting cylinder 4, the ball spline 28 is installed on the spline section 27-2 of the lifting shaft, the number of the positioning blocks 30 is three, one end of each positioning block is installed around the outer side surface of the ball spline 28 at an interval of 120 degrees, and the other ends of the positioning blocks are movably matched with the inner wall of the supporting cylinder 4; the second support 5 is sleeved with the screw rod section 27-1 of the lifting shaft and fixed at the upper end of the supporting cylinder 4, the second motor 26 is installed on the second support, a driving bevel gear in the bevel gear transmission pair is installed on a power output shaft of the second motor, and a driven bevel gear in the bevel gear transmission pair is installed on the screw rod section 27-1 of the lifting shaft and combined with the driving bevel gear.
Example 3
In this example, the super-gravity field microreactor described in example 2 is used to prepare nano strontium carbonate, and the operation is as follows:
(1) 321.56g strontium chloride is weighed and prepared into 2000mL strontium chloride solution with distilled water, and the solution is marked as solution A; weighing 189.74g of ammonium bicarbonate, adding distilled water to dissolve the ammonium bicarbonate, adding 664.2mL of ammonia water and 333.4mL of absolute ethyl alcohol, adding distilled water to enable the total liquid amount to reach 2000mL, and uniformly stirring to prepare 2000mL of mixed solution, wherein the mixed solution is marked as liquid B;
(2) Starting a first motor, and driving the transmission system to run by the first motor, so that the upper disk and the lower disk in the micro-reaction component rotate in opposite rotating directions at the rotating speed of 1000rad/min (the separation factor is 219);
(3) Feeding the prepared liquid A and liquid B into a feeding channel arranged in a shaft body of a fourth transmission shaft through a feeding hole and a feeding cavity arranged on a joint body at a flow rate of 150mL/min respectively, feeding the liquid A and the liquid B into a feeding micro-channel arranged on a lower disc of a reaction assembly through the feeding channel, and then feeding the liquid A and the liquid B into a space between an upper disc and a lower disc of a micro-reaction assembly through the feeding micro-channel, grinding the liquid A and the liquid B through micro-groove layers on the bottom surface of the upper disc and the top surface of the lower disc under the action of overweight force generated by the upper disc and the lower disc to continuously update contact interfaces and strengthen mass transfer to complete reaction to form nano granular strontium carbonate, throwing slurry containing the strontium carbonate into a material receiving groove under the action of hypergravity, and discharging the slurry from a discharging hole arranged on the material receiving groove;
(4) Filtering the slurry discharged from the discharge port, and adjusting with cleaning solution (NH) with pH not less than 10.5 with ammonia water 4 OH and NH 4 HCO 3 ) Washing until the filtrate is free of chloride ions through silver nitrate detection;
(5) Removing water from the washed filter cake by azeotropy with n-amyl alcohol, and drying at 150 ℃ to obtain a white powder product;
(6) The white powder product is detected by a transmission electron microscope, the crystal particles are uniform, the particle size is 50nm at most, 15nm at least, and the average particle size is 28nm, which shows that the prepared nano strontium carbonate has narrow particle size distribution and good particle dispersibility.
In this example, the processing amount of the raw materials was: 150mL/min X2X 60X 10 -6 ＝0.018m 3 /h。
Claims (10)
1. A high gravity field micro-reactor for preparing nano materials is characterized by comprising a micro-reaction component, a material receiving groove (24) provided with a discharge hole, a first motor (8), a transmission system, a feeding system and a supporting system;
the micro-reaction component consists of an upper disc (15) and a lower disc (20), wherein micro-grooves are distributed on the bottom surface of the upper disc (15), a buffer groove (15-1) is arranged at the central part of the bottom surface of the upper disc, the micro-grooves are distributed on the top surface of the lower disc (20), a feeding micro-channel is arranged at the central part of the lower disc, and the number of the feeding micro-channels is more than or equal to the type of raw material liquid forming a reaction product;
the transmission system comprises a transmission (7), a first transmission shaft (9), a second transmission shaft (33), a third transmission shaft (14), a fourth transmission shaft (19), a first synchronous belt, a gear transmission pair, a second synchronous belt and a plurality of bearing assemblies for being combined with the transmission shafts, wherein the first synchronous belt consists of a first synchronous belt driving wheel (10), a first synchronous belt driven wheel (11) and a first transmission belt, the gear transmission pair consists of a driving gear (12) and a driven gear (13), the second synchronous belt consists of a second synchronous belt driving wheel (17), a second synchronous belt driven wheel (18) and a second transmission belt, a shaft body of the fourth transmission shaft (19) is internally provided with a feeding channel penetrating through the upper end face, and the number of the feeding channels is the same as that of feeding micro-channels arranged at the central part of the lower disc;
the supporting system comprises a bottom frame (1), a middle frame (2), an upper frame (3), a first support (6) and a joint body (21), wherein the joint body is provided with a central hole matched with the lower section of a fourth transmission shaft (19), the inner wall of the central hole is provided with a bearing combined with the fourth transmission shaft and feeding chambers (21-4) matched with the feeding channel in the fourth transmission shaft in position and in the same number, a feeding hole penetrating through the inner wall and the outer wall of the central hole is formed in the feeding chamber, and a sealing ring is arranged between the bearing and the feeding chambers;
the feeding system consists of a feeding hole and a feeding cavity which are arranged on the joint body, a feeding channel which is arranged in the shaft body of the fourth transmission shaft and a feeding micro-channel which is arranged at the central part of the lower disc;
the combination mode of the components is as follows:
the bottom frame (1), the middle frame (2) and the upper frame (3) are overlapped and connected into a whole, the first support (6) is installed at one end of the upper surface of the top plate of the upper frame (3), the speed changer (7) and the first motor (8) are installed on the first support (6), and a power output shaft of the first motor is connected with a power input shaft of the speed changer; the upper end of the first transmission shaft (9) is connected with a power output shaft of the transmission, the lower end of the first transmission shaft is combined with a bearing assembly arranged on a bottom plate of the bottom frame, the upper end of the second transmission shaft (33) is combined with a bearing assembly arranged on a top plate of the upper frame (3), the lower end of the second transmission shaft is combined with a bearing assembly arranged on a bottom plate of the upper frame (3), the two ends of the second transmission shaft (33) are combined with the bearing assemblies and then the central line of the second transmission shaft is parallel to the central line of the first transmission shaft (9), the upper end of the third transmission shaft (14) is combined with the bearing assembly and then the central line of the third transmission shaft is parallel to the central line of the second transmission shaft, the distance between the central line of the third transmission shaft and the central line of the second transmission shaft is required to meet the installation of a gear transmission pair, the joint body (21) is arranged on the bottom plate of the bottom frame (1), the central line of the third transmission shaft and the central line of the third transmission shaft (14) are in a straight line, the lower section of the fourth transmission shaft (19) is arranged in an inner hole of the joint body, and the middle of the bottom plate (2) of the fourth transmission shaft (19) is arranged on the bottom plate of the bottom frame; the first synchronous belt driving wheel (10) is installed on the upper section of the first transmission shaft, the first synchronous belt driven wheel (11) is installed on the upper section of the second transmission shaft, the driving gear (12) is installed on the lower section of the second transmission shaft, the driven gear (13) is installed on the third transmission shaft, the second synchronous belt driving wheel (17) is installed on the lower section of the first transmission shaft, and the second synchronous belt driven wheel (18) is installed on the fourth transmission shaft; the material receiving groove (24) is arranged on the top surface of the bottom plate of the middle frame (2), and the mounting position of the material receiving groove enables the upper end of the fourth transmission shaft (19) to be positioned at the central part of the inner cavity of the material receiving groove; the lower disc (20) in the micro-reaction assembly is fixed at the upper end of a fourth transmission shaft (19) and positioned in a material receiving groove, each feeding micro-channel arranged at the center of the lower disc is respectively connected and communicated with a corresponding feeding channel arranged in the shaft body of the fourth transmission shaft, the upper disc (15) in the micro-reaction assembly is fixed at the lower end of the third transmission shaft and positioned in the material receiving groove, and a gap of 0.03-0.1 mm is formed between the bottom surface of the upper disc and the top surface of the lower disc.
2. The high gravitational field microreactor for preparing nanomaterials of claim 1, further comprising an upper disk lifting system, wherein the upper disk lifting system comprises a second motor (26), a bevel gear transmission pair, a lifting shaft (27), a second support (5), a ball spline (28), a positioning block (30) and a cylindrical supporting cylinder (4), the upper section of the lifting shaft (27) is a screw rod section (27-1), the lower part of the lifting shaft is provided with a spline section (27-2), a central hole of a driven bevel gear of the bevel gear transmission pair is a screw hole matched with the screw rod section (27-1) arranged on the lifting shaft, and the second support (5) is provided with a through hole for the screw rod section (27-1) of the lifting shaft to pass through;
the lower part of the third transmission shaft (14) is provided with a spline section (14-2) which is combined with a female rotary ball spline (16) arranged on a bottom plate of the upper frame (3);
the supporting cylinder (4) is arranged on the upper surface of a top plate of the upper frame (3), and the central line of the supporting cylinder and the central line of the third transmission shaft (14) are in the same straight line; the lower end of the lifting shaft (27) is connected with the upper end of the third transmission shaft (14) through a coupler (29), the upper end of the lifting shaft extends out of the supporting cylinder (4), the ball spline (28) is installed on a spline section (27-2) of the lifting shaft, at least two positioning blocks (30) are arranged, one end of each positioning block is installed around the outer side surface of the ball spline (28) at equal intervals, and the other ends of the positioning blocks are in movable fit with the inner wall of the supporting cylinder (4); the second support (5) is sleeved with the screw rod section (27-1) of the lifting shaft and fixed at the upper end of the supporting cylinder (4), the second motor (26) is installed on the second support, the driving bevel gear of the bevel gear transmission pair is installed on the power output shaft of the second motor, and the driven bevel gear of the bevel gear transmission pair is installed on the screw rod section (27-1) of the lifting shaft and combined with the driving bevel gear.
3. The high gravity field microreactor for preparing nanomaterials according to claim 1 or 2, wherein the feeding micro-channel provided at the center of the lower disk (20) is a circular hole, the feeding channel provided in the shaft body of the fourth transmission shaft (19) and penetrating through the upper end surface is a circular hole, and the feeding micro-channel and the feeding channel have the same pore diameter, both of which are 0.45mm to 4mm.
4. The high gravity field microreactor for preparing nanomaterials as claimed in claim 1 or 2, wherein the micro-grooves on the bottom surface of the upper plate (15) and the top surface of the lower plate (20) are distributed in a spiral, arc, sector or honeycomb shape.
5. The high gravitational field microreactor for the preparation of nanomaterials of claim 3, wherein the micro-grooves on the bottom surface of the upper plate (15) and the top surface of the lower plate (20) are distributed in a spiral, arc, sector or honeycomb shape.
6. The high gravitational field microreactor for the production of nanomaterials according to claim 1 or 2, wherein the microgrooves on the bottom surface of the upper plate (15) and the top surface of the lower plate (20) have a width of 0.01mm to 0.80mm and a depth of 0.05mm to 0.75mm.
7. The high gravitational field microreactor for preparing nanomaterials as claimed in claim 3, wherein the microgrooves on the bottom surface of the upper plate (15) and the top surface of the lower plate (20) have a width of 0.01mm to 0.80mm and a depth of 0.05mm to 0.75mm.
8. The high gravitational field microreactor for preparing nanomaterials as claimed in claim 4, wherein the microgrooves on the bottom surface of the upper plate (15) and the top surface of the lower plate (20) have a width of 0.01mm to 0.80mm and a depth of 0.05mm to 0.75mm.
9. The high gravitational field microreactor for preparing nanomaterials as claimed in claim 5, wherein the micro-grooves of the bottom surface of the upper plate (15) and the top surface of the lower plate (20) have a width of 0.01mm to 0.80mm and a depth of 0.05mm to 0.75mm.
10. A method for preparing nano-materials by liquid phase precipitation, characterized in that the high gravity field micro-reactor of any of claims 1 to 9 is used, and the operation is as follows:
(1) Starting a first motor, and driving a transmission system to operate under the driving of the first motor, so that an upper disc and a lower disc in the micro-reaction assembly rotate in opposite rotating directions, and the separation factor is controlled to be 15-250;
(2) Feeding each raw material liquid into a feeding channel arranged in the shaft body of a fourth transmission shaft through a feeding hole and a feeding chamber arranged on a joint body respectively, feeding each raw material liquid into a feeding micro-channel arranged on a lower disc in a micro-reaction assembly through the feeding channel, and then feeding each raw material liquid into a space between an upper disc and a lower disc of the micro-reaction assembly through the feeding micro-channel, wherein each raw material liquid finishes reaction through grinding and constantly updating a contact interface and strengthening mass transfer of a micro-groove layer on the bottom surface of the upper disc and the top surface of the lower disc under the action of overweight force generated by the upper disc and the lower disc to form a nano granular reaction product, and slurry containing the reaction product is thrown into a material receiving groove under the action of centrifugal force and is discharged from a discharge hole arranged on the material receiving groove;
(3) And (3) filtering, cleaning and drying the slurry containing the reaction product discharged from the discharge hole of the material receiving groove, or cleaning, filtering and drying the slurry, or cleaning and drying the slurry while filtering to obtain the nano material.
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| CN110882663B (en) * | 2018-09-10 | 2021-07-27 | 临沂大学 | Hypergravity micro-reaction device |
| CN110883339B (en) * | 2018-09-10 | 2022-09-09 | 临沂大学 | Method for preparing superfine metal powder |
| CN111437783A (en) * | 2020-05-19 | 2020-07-24 | 福州大学 | Continuous generation device for accurately controlling shape and size of high-viscosity fluid |
| CN112657517B (en) * | 2020-12-29 | 2023-07-25 | 北京化工大学 | Preparation method of molybdenum disulfide-based nano catalytic material |
| CN113041971B (en) * | 2021-03-24 | 2022-08-09 | 青岛科技大学 | Anti-blocking microchannel reactor |
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