CN107824124A - A kind of nano material preparation facilities and method - Google Patents

Abstract

The invention provides a nano-material preparation device and method, the device comprises an explosion-proof tank, the explosion-proof tank is connected to the output shaft of the motor, and the rotation of the motor drives the explosion-proof tank to rotate; the explosion-proof tank is detachably connected through a vacuum pump at the exhaust port; The explosion-proof tank is also provided with a pressure relief port, and the pressure relief port is connected with a pressure relief screw; the explosion-proof tank is also threaded with a seat body, and the seat body is respectively fixed in the explosion-proof tank with a mixed powder column, a pressure sensor, an electrode and a detonator. The base is located outside the explosion-proof tank and is also equipped with a power module, a constant current source, a controller and a wireless transceiver module. The pressure sensor, constant current source and wireless transceiver module are respectively connected to the controller signal, and the detonator is electrically connected to the constant current source. , the constant current source, the electrode and the controller are respectively electrically connected to the power module. The invention can overcome the disadvantages of complex and cumbersome synthesis technology, difficult control of process conditions, low output, large pollution and the like when the oxide nanometer material is prepared by the traditional chemical synthesis method.

Description

Apparatus and method for preparing nanomaterials

technical field

The invention relates to the field of nanomaterial preparation, in particular to a nanomaterial preparation device and method.

Background technique

Nano-oxide materials are the basic materials for preparing nano-devices. When using conventional chemical synthesis methods to prepare nano-oxide materials, there are many disadvantages, including complex and cumbersome synthesis techniques, difficult control of process conditions, low yield, and large pollution. In order to overcome the shortcomings brought about by conventional chemical synthesis, a detonation method has been developed to synthesize nanomaterials in recent years.

The detonation method refers to the technology of using the instantaneous high temperature and high pressure generated by the explosion of negative oxygen balance explosives to rapidly decompose the raw materials, and then aggregate and crystallize to form nanomaterials. It is a new research direction combining explosive mechanics and materials science, and the process is simple. It can effectively reduce the pollution to the environment, and it is easy to realize large-scale production. It is a green technology for preparing nano-powder and has good economic and social benefits. On the one hand, the mechanism of the explosion field is that the gas generated by the explosion and the high-temperature and high-pressure field provide materials and energy for the synthesis and phase transformation of nanoparticles. Surface deposition exerts steric hindrance effect and organizes the growth and agglomeration of nanoparticles. The detonation method is a cheap, easy-to-control process parameter and close to gas-phase synthesis. As a new synthesis technology, it has been widely studied by researchers due to its simple operation, low cost, suitable for the synthesis of various simple substances, oxides and composite oxides, and a wide range of applications. From the perspective of detonation synthesis technology itself, it can solve the problem of cheap, pollution-free, large-scale synthesis of nano-oxides and nano-composite oxides. Nanoparticles synthesized by detonation are actually rapidly generated in a high-pressure and high-density gas, and expand at a high speed with the subsequent detonation gas, which makes it easy to prepare nanoparticles with good dispersion.

Contents of the invention

The purpose of the present invention is to overcome the problems existing in the prior art, to provide a nanomaterial preparation device and method, to prepare oxide nanomaterials by detonation method, which can overcome the synthesis of oxide nanomaterials prepared by traditional chemical synthesis methods The technology is complex and cumbersome, the process conditions are difficult to control, the output is low, and the pollution is large.

The technical solution of the present invention is: a nanomaterial preparation device, including a base, two supports are arranged in the middle of the base, an explosion-proof tank is arranged between the two supports, and the left end of the explosion-proof tank is located on the left side. The supports are connected through the first rotating shaft, and the right end of the explosion-proof tank is connected with the supporting body on the right side through the second rotating shaft, wherein the second rotating shaft is fixedly connected with the explosion-proof tank, and the second rotating shaft passes through the The supporting body is connected with the motor shaft, and the rotation of the motor can drive the explosion-proof tank to rotate around the first rotating shaft and the second rotating shaft; the explosion-proof tank is also provided with an exhaust port, and the exhaust port is connected to the One end of the trachea is detachably connected, and the other end of the exhaust pipe is connected to a vacuum pump, which is used to vacuumize the inside of the explosion-proof tank through the exhaust pipe; The pressure port is connected with a pressure relief screw; the lower end of the explosion-proof tank is threadedly connected with a seat body, and the seat body is respectively fixed with a mixed powder column, a pressure sensor, an electrode and a detonator in the explosion-proof tank, and the seat body is located outside the explosion-proof tank. Also be provided with power supply module, constant current source, controller and wireless transceiver module, described pressure sensor, constant current source and wireless transceiver module are respectively connected with controller signal, detonator is connected with constant current source electricity, constant current source, electrode and The controllers are respectively electrically connected to the power supply module; the wireless transceiver module is used to wirelessly send the pressure signal detected by the pressure sensor to the wireless data acquisition terminal, and the wireless transceiver module is used to receive the external remote control wirelessly The detonation command sent from the terminal.

The device also includes a filtering and purifying device and a calcining device, the filtering and purifying device is used for filtering and purifying the detonation products produced in the explosion-proof tank, and the calcining device is used for calcining the filtered and purified detonation products, thereby The final desired nano oxide material is obtained.

The inner wall of the explosion-proof tank is covered with protruding structures for hindering the airflow generated by the detonation.

Above-mentioned detonator adopts electric detonation detonator.

The above-mentioned mixed powder column adopts the mixture of explosive and precursor pressed by the position pressing method.

A method for preparing nanomaterials, comprising the steps of:

1) Pressing the required ratio of explosives and oxide precursors into a mixed powder column of a certain density according to the positioning pressing method;

2) The seat body is disassembled from the explosion-proof tank, the mixed powder column is installed on the seat body, and the detonator is installed, the pressure sensor, constant current source and wireless transceiver module are respectively connected to the controller signal, and the detonator Electrically connect with the constant current source, set the trigger probe, and then electrically connect the constant current source, electrode and controller with the power module respectively; install the base on the explosion-proof tank;

3) Vacuum the inside of the explosion-proof tank through the vacuum pump. When the vacuum reaches the required vacuum degree, close the vacuum pump and the exhaust port, and separate the exhaust pipe from the exhaust port;

4) Start the motor to make the explosion-proof tank rotate at high speed driven by the motor;

5) Send the detonation command to the controller through the wireless transceiver module through the external remote terminal, and the controller controls the constant current source to detonate the detonator; the wireless transceiver module sends the pressure signal detected by the pressure sensor to the wireless data acquisition terminal in a wireless manner , record the burst pressure related data;

6) After the detonation is completed, turn off the motor, and after the explosion-proof tank cools down, clean the explosion-proof tank, collect detonation products, clean up impurities, perform filtration purification, calcination, etc., and conduct further characterization studies on the obtained nano-oxide materials to determine their shape. appearance, crystal structure and other parameters.

Beneficial effects of the present invention: In the embodiment of the present invention, a device and method for preparing nanomaterials are provided, and oxide nanomaterials are prepared by detonation, which can overcome the complexity of synthesis technology when preparing oxide nanomaterials by traditional chemical synthesis methods It is cumbersome, the process conditions are difficult to control, the output is low, and the pollution is large.

Description of drawings

Fig. 1 is the structural representation of device of the present invention;

Fig. 2 is the connection block diagram of the electric component on the explosion-proof tank of device of the present invention;

Fig. 3 is a block diagram of the electrical connection between the vacuum pump and the motor of the device of the present invention and an external power supply.

Detailed ways

A specific embodiment of the present invention will be described in detail below in conjunction with the accompanying drawings, but it should be understood that the protection scope of the present invention is not limited by the specific embodiment.

Referring to Fig. 1, Fig. 2 and Fig. 3, the embodiment of the present invention provides a nanomaterial preparation device and method, the main purpose of the present invention is to design an oxide nanomaterial explosive synthesis reaction device, using a solid mixture explosive as a precursor , different detonation parameters can be controlled during the synthesis process, such as the type of explosive, detonation performance, proportion in raw materials, charging method, etc., and can record detonation parameters, precursor ratio and form, and detonation products, etc. Experimental parameters. The device of the present invention comprises a base 1, the middle part of the base 1 is provided with two support bodies 15, an explosion-proof tank 2 is arranged between the two support bodies 15, and the left end of the explosion-proof tank 2 is connected to the support body 15 on the left side. Connected by the first rotating shaft 18, the right end of the explosion-proof tank 2 is connected with the support body 15 on the right side by the second rotating shaft 19, wherein the second rotating shaft 19 is fixedly connected with the explosion-proof tank 2, and the second rotating shaft 19 passes through the support body 15 on the right side and is connected with the motor 3 shaft, and the rotation of the motor 3 can drive the explosion-proof tank 2 to rotate around the first rotating shaft 18 and the second rotating shaft 19; An exhaust port 17 is provided, and the exhaust port 17 is detachably connected to one end of the exhaust pipe 14, and the other end of the exhaust pipe 14 is connected to the vacuum pump 4, and the vacuum pump 4 is used to pass through the exhaust pipe 14 to the described Vacuumize in the explosion-proof tank 2; the upper end of the explosion-proof tank 2 is also provided with a pressure relief port 13, and the pressure relief port 13 is connected with a pressure relief screw; A mixed powder column 7, a pressure sensor 12, an electrode 11 and a detonator 6 are respectively fixed in the explosion-proof tank 2, and a power module 10, a constant current source 9, a controller and Wireless transceiver module 8, described pressure sensor 12, constant current source 9 and wireless transceiver module 8 are connected with controller signal respectively, detonator 6 is electrically connected with constant current source 9, constant current source 9, electrode 11 and controller are connected with power supply respectively The modules 10 are electrically connected; the controller is specifically a single-chip microcomputer. The wireless transceiver module 8 is used to wirelessly send the pressure signal detected by the pressure sensor 12 to the wireless data acquisition terminal, and the wireless transceiver module 8 is used to wirelessly receive the detonation command sent by the external remote terminal . Pre-evacuating the explosion-proof tank before detonation can be more conducive to detonation to generate airflow, and can also pre-eliminate the adverse effects of the air inside the explosion-proof tank on detonation. The high-speed rotation of the explosion-proof tank driven by the motor during the detonation process can further make the particle powder produced in the detonation process form more complex collisions, so as to facilitate the production of nanoparticles.

Further, the device also includes a filtering and purifying device and a calcining device, the filtering and purifying device is used to filter and purify the detonation products produced in the explosion-proof tank 2, and the calcining device is used to filter and purify the detonation products Calcination is carried out to obtain the final desired nano oxide material.

Further, the inner wall of the explosion-proof tank 2 is covered with protruding structures 16 for obstructing the airflow generated by the detonation, so as to be more conducive to the formation of nanoparticles.

Further, the detonator 6 adopts an electric detonation detonator.

Further, the mixed charge column 7 adopts the mixture of explosive and precursor compressed by the position pressing method.

The nanomaterial preparation method provided by the invention comprises the following steps:

1) Pressing the required ratio of explosives and oxide precursors into a mixed powder column of a certain density according to the positioning pressing method;

2) The seat body 5 is disassembled from the explosion-proof tank 2, the mixed powder column 7 is installed on the seat body 5, and the detonator 6 is installed, and the pressure sensor 12, the constant current source 9 and the wireless transceiver module 8 are respectively connected to the control The device signal is connected well, and at the same time, the detonator 6 is electrically connected to the constant current source 9, and the trigger probe is set, and then the constant current source 9, the electrode 11 and the controller are respectively electrically connected to the power module 10; the base 5 is installed on the explosion-proof tank 2 on;

3) Vacuumize the inside of the explosion-proof tank 2 through the vacuum pump 4. When the vacuum reaches the required degree of vacuum, close the vacuum pump 4 and the exhaust port 17, and separate the exhaust pipe 14 from the exhaust port 17;

4) Start the motor 3 to make the explosion-proof tank 2 rotate at a high speed driven by the motor 3;

5) Send the detonation command to the controller through the wireless transceiver module 8 through the external remote control terminal, and the controller controls the constant current source 9 to detonate the detonator 6; the wireless transceiver module 8 sends the pressure signal detected by the pressure sensor 12 in a wireless manner To the wireless data acquisition terminal, record the data related to the explosion pressure;

6) After the detonation is completed, turn off the motor 3, and after the explosion-proof tank cools down, clean the explosion-proof tank 2, collect the detonation products, clean up impurities, perform filtration purification, calcination and other treatments, and conduct further characterization studies on the obtained nano-oxide materials to determine Its morphology, crystal structure and other parameters.

In summary, the present invention provides a device and method for preparing nanomaterials. The oxide nanomaterials are prepared by detonation, which can overcome the complex and cumbersome synthesis technology when preparing oxide nanomaterials by traditional chemical synthesis methods. Difficult to control, low output, large pollution and other shortcomings.

The above disclosures are only a few specific embodiments of the present invention, however, the embodiments of the present invention are not limited thereto, and any changes conceivable by those skilled in the art shall fall within the protection scope of the present invention.

Claims (6)

1. a kind of nano material preparation facilities, it is characterised in that including base (1), the middle part of the base (1) is provided with two branch Support body (15), anti-explosion tank (2), the left end of the anti-explosion tank (2) and the support positioned at left side are provided between two supporters (15) By first rotating shaft (18) connection, the right-hand member of the anti-explosion tank (2) and between the supporter (15) on right side between body (15) Connected by the second rotating shaft (19), wherein being fixedly connected between the second rotating shaft (19) and anti-explosion tank (2), the second rotating shaft (19) passes through Positioned at right side supporter (15) and with motor (3) axis connection, the anti-explosion tank (2) can be driven by the rotation of motor (3) Rotated around the first rotating shaft (18) and the second rotating shaft (19)；Exhaust outlet (17), the exhaust are additionally provided with the anti-explosion tank (2) Mouth (17) and one end of blast pipe (14) are detachably connected, and the other end of blast pipe (14) is connected with vavuum pump (4), the vacuum Pump (4) is used for by blast pipe (14) to being vacuumized in the anti-explosion tank (2)；The upper end of the anti-explosion tank (2) is additionally provided with pressure release Mouth (13), pressure relief opening are connected with pressure release screw on (13)；The lower end of the anti-explosion tank (2) is threaded with pedestal (5), pedestal (5) mixing powder column (7), pressure sensor (12), electrode (11) and detonator (6) are respectively fixed with anti-explosion tank (2), On the pedestal (5) power module (10), constant-current source (9), controller and wireless receiving and dispatching mould are additionally provided with outside anti-explosion tank (2) Block (8), the pressure sensor (12), constant-current source (9) and radio receiving transmitting module (8) are connected with controller signals respectively, thunder Pipe (6) electrically connects with constant-current source (9), and constant-current source (9), electrode (11) and controller electrically connect with power module (10) respectively； The radio receiving transmitting module (8) is used to wirelessly be sent to the pressure signal that the pressure sensor (12) detects Data acquisition end, while radio receiving transmitting module (8) is used to wirelessly receive that external remote control end is sent Quick-fried order.

A kind of 2. nano material preparation facilities as claimed in claim 1, it is characterised in that also include filtering purifying plant and Calciner plant, the filter purifying plant are used to filter and purify caused detonation product in anti-explosion tank (2), the calciner plant For being calcined to the detonation product after filtering and purification, so as to obtain final required nanometer oxide material.

3. a kind of nano material preparation facilities as claimed in claim 1, it is characterised in that on the inwall of the anti-explosion tank (2) Being covered with has for forming the bulge-structure (16) hindered to air-flow caused by detonation.

4. a kind of nano material preparation facilities as claimed in claim 1, it is characterised in that the detonator (6) uses electric initiating Detonator.

5. a kind of nano material preparation facilities as claimed in claim 1, it is characterised in that the mixing powder column (7) is using fixed The explosive and precursor mixture of position pressing method compacting.

6. a kind of preparation method of nano material, it is characterised in that comprise the following steps：

1) explosive of required ratio and oxide precursor are pressed into the mixing powder column of certain density according to positioning pressing method；

2) pedestal (5) is disassembled from the anti-explosion tank (2), and mixing powder column (7) is installed on pedestal (5), and is installed Detonator (6), pressure sensor (12), constant-current source (9) and radio receiving transmitting module (8) are connected with controller signals respectively, Detonator (6) is electrically connected with constant-current source (9) simultaneously, and triggering probe is set, then by constant-current source (9), electrode (11) and control Device electrically connects with power module (10) respectively；Pedestal (5) is installed on anti-explosion tank (2)；

3) by vavuum pump (4) to vacuumizing inside anti-explosion tank (2), when vacuumize reach needed for vacuum level requirements when, close true Empty pump (4) and exhaust outlet (17), and blast pipe (14) is separated with exhaust outlet (17)；

4) start motor (3), anti-explosion tank (2) is rotated at a high speed under the drive of motor (3)；

5) detonation order, controller control constant-current source (9) are sent to controller through radio receiving transmitting module (8) by external remote control end Detonator (6) is set to detonate；The pressure signal that radio receiving transmitting module (8) wirelessly detects the pressure sensor (12) Data acquisition end is sent to, records detonation pressure related data；

6) treat that detonation finishes, close motor (3), after anti-explosion tank (2) cooling, clear up anti-explosion tank (2), collect detonation product, cleaning Impurity, the processing such as filtering purification, calcining is carried out, further characterization research is carried out to gained nanometer oxide material, to determine it The parameters such as pattern, crystal structure.