CN108273467A - A kind of interior rotation homogeneous reaction device with positioning system - Google Patents

Abstract

An internal rotating homogeneous reaction device with a positioning system, including a box body, an electric blast heating device, a rotating device, a positioning device and a reaction kettle are arranged inside the box body; the rotating device is composed of a rotating motor, a central rotating shaft, a rotating bracket and several The card slot can be adjusted in size; the rotating motor is arranged on one side of the box body, and the rotating motor is connected to one end of the central shaft, which runs through the entire box. The card slot; the reactor is set in the card slot. The box body is made of high-quality cold-rolled steel plate, the surface is electrostatic powder sprayed, the coating is hard and firm, and has strong anti-rust ability. The studio is made of high-quality stainless steel plate with rounded corners, smooth, smooth and easy to clean. Between the cabinet and the working room, it is filled with ultra-fine glass wool insulation material, which has a good heat preservation function and effectively ensures the stability and accuracy of the temperature in the cabinet.

Description

An internal rotating homogeneous reaction device with a positioning system

technical field

The invention relates to a chemical reaction experiment device, in particular to an internal rotation homogeneous reaction device with a positioning system.

Background technique

Homogeneous reactors are widely used in chemical and chemical engineering and other experimental fields. Its main function is to test the reaction of the same component medium under different conditions or to test the reaction of different components of the medium under the same conditions. For example, in the process of preparing molecular sieves by hydrothermal crystallization, an aqueous solution is used as the reaction medium, and a high-temperature and high-pressure reaction environment is obtained by heating the reactor, so that insoluble or insoluble substances are dissolved and recrystallized to form dispersed nanocrystalline nuclei. At present, there are many types and structures of homogeneous reactors, but the basic principles are roughly the same. They all use the heating device to heat the box to keep the temperature constant, and the motor drives the stirring shaft in the box and the micro-reactor installed on the stirring shaft to rotate to achieve stirring reaction. the goal of.

The homogeneous reactor has a simple structure, less investment in manufacturing and installation, and is easy to operate and maintain; it has stable performance and large operating flexibility; it can realize complex physical and chemical reactions of homogeneous substances under different conditions, and its effect is better. Although the homogeneous reactor is widely used and has received a lot of research and development, there are still deficiencies, mainly including the poor temperature stability in the box, which causes the actual reaction temperature to not meet the standard; the external motor causes the motor to be corroded faster, The noise is loud, the fuselage is large, and it is inconvenient to place; the rotating bracket is in an active state when loading and unloading the reactor, which is not conducive to the loading and unloading of the reactor and other actual conditions.

Contents of the invention

In view of the defects and deficiencies in the prior art, the purpose of the present invention is to provide an internally rotating homogeneous reaction device with a positioning system, which solves the problem of uneven heating of traditional homogeneous reactors, external motors, and large noise. It is not easy to install, and the traditional homogeneous reactor cannot install and disassemble the reactor, and the rotating bracket is in a fixed state.

To achieve the above object, the technical scheme adopted in the present invention is as follows:

An internal rotating homogeneous reaction device with a positioning system, including a box body, an electric blast heating device, a rotating device, a positioning device and a reaction kettle are arranged inside the box body; wherein, the rotating device is composed of a rotating motor, a central rotating shaft, and a rotating bracket And a number of card slots that can be adjusted in size; the rotating motor is arranged on one side of the box body, and the rotating motor is connected to one end of the central rotating shaft. The central rotating shaft runs through the entire box. Adjustable card slot; the reaction kettle is set in the card slot, the side of the reaction kettle is provided with an electric blast heating device for heating the reaction kettle, and the output shaft of the rotating motor is provided with a positioning device for positioning the reaction kettle.

A further improvement of the present invention is that the positioning device includes a permanent magnet locator; a brake disc is arranged on the output shaft of the rotating electrical machine, and the permanent magnet positioner is arranged at the joint between the output shaft of the rotating electrical machine and the brake disc.

The further improvement of the present invention is that the other end of the central rotating shaft protrudes from the box body, a groove is opened on the central rotating shaft protruding from the box body, and a protrusion matching the groove is arranged on the rotating ferrule, so that the rotating ferrule It is arranged on the central rotating shaft, and the rotating ferrule is matched with the wrench, and by putting the wrench on the rotating ferrule, turning the wrench realizes the rotation of the central rotating shaft, thereby realizing the positioning of the reaction kettle arranged on the support.

A further improvement of the present invention is that the electric heating blower heating device is connected with several fan blades by a fan motor, and a circle of heating coils is arranged outside the several fan blades.

The further improvement of the present invention is that a control panel is provided on the upper front of the box body, a programmable temperature controller, a digital AC geared motor intelligent regulator and a main power switch are arranged on the control panel, and a box door is arranged on the lower part of the control panel. There are cooling holes on the upper part of one side of the body, exhaust holes on the lower part of the back of the box, and four adjustable instrument balance knobs on the bottom of the box.

The further improvement of the present invention is that the heating coil is connected with a programmable temperature controller, and the fan motor and the rotating motor are connected with a digital AC deceleration motor intelligent regulator.

The further improvement of the present invention lies in that a stainless steel jacket is provided outside the reactor.

The further improvement of the present invention is that 1 to 2 rectangular baffles are arranged inside the reaction kettle, the baffles are arranged vertically, the bottom of the baffle is connected with the cylindrical bottom, and the two ends of the baffle are connected with the inner wall of the reaction kettle.

The further improvement of the present invention is that the height of the baffle is 1/3 of the height of the reactor.

Compared with the prior art, the present invention has the following beneficial effects:

(1) The box body is made of high-quality cold-rolled steel plate, the surface is electrostatic powder sprayed, the coating is hard and firm, and has strong anti-rust ability. The studio is made of high-quality stainless steel plate with rounded corners, smooth, smooth and easy to clean. Between the cabinet and the working room, it is filled with ultra-fine glass wool insulation material, which has a good heat preservation function and effectively ensures the stability and accuracy of the temperature in the cabinet.

(2) The box is designed with a reasonable hot air circulation channel to make the temperature distribution in the box more uniform and the temperature rise faster; and an air outlet pipe is installed to discharge the air in the box in a small amount. If the gas discharged from the box has peculiar smell or is poisonous, the air outlet pipe can be conveniently connected to another pipe to discharge the gas to the designated place, avoiding the harm to the operator and reducing air pollution.

(3) The whole reaction device has a square closed design, which is small in size and easy to place. At the same time, it avoids many problems such as serious corrosion of the motor, loud noise, and low-speed vibration caused by the external motor.

Further, a permanent magnet positioning system is installed at the connection between the transmission shaft and the brake disc at the rear end of the motor of the equipment, or the ferrule positioning system installed outside the central rotating shaft extension box can prevent the rotating bracket from rotating freely when the reactor is installed and disassembled. The phenomenon.

Further, due to the rotation of the bracket, the reaction materials in the hydrothermal reaction kettle are fully mixed and reacted, thereby greatly reducing the crystallization time, making the crystal heated evenly, and greatly improving the product quality compared with a single constant temperature condition.

Furthermore, since 1-2 baffles are set in the homogeneous reactor, the heat transfer and mass transfer during the reaction process are further enhanced. This setup is complemented by a rotatable in-box stand.

Furthermore, there is a fixed position on the stirring rod (set according to the size of the reactor), which can fix multiple sets of miniature reactors of 50-100ml at the same time. The size, volume and quantity of the selected reactors can be designed and customized according to the needs of the experimenter. Increased practical operating range of the reactor.

Description of drawings

Figure 1 is a front view of the present invention.

Fig. 2 is a sectional view along line A-A in Fig. 1 .

Fig. 3 is a sectional view along line B-B in Fig. 1 .

Fig. 4 is a structural schematic diagram of the positioning device and the rotating device.

Figure 5 is a schematic structural view of the reactor.

Fig. 6 is a microscopic morphology diagram of HZSM-5 molecular sieve after 56 hours of reaction in a conventional homogeneous reactor.

Fig. 7 is a microscopic morphology diagram of the HZSM-5 molecular sieve after the reaction in the reaction device of the present invention.

Among them, 1. Programmable temperature controller; 2. Digital AC geared motor intelligent regulator; 3. Power switch; 4. Control panel; 5. Box body; 6. Box door closing valve; 7. Box bin; 8. Adjustable instrument balance knob; 9. Cooling hole; 10. Box door; 11. Center shaft; 12. Drive shaft; 13. Exhaust hole; 14. Fan motor; 15. Fan blade; 16. Heating coil; 17. Transmission shaft; 18. Rotating motor; 19. Permanent magnet locator; 20. Coupling; 21. Card slot; 22. Rotating ferrule; 23. Wrench; 24. Rotating bracket; 25. Stainless steel jacket; 26. Reactor; 27. Reactor internal baffle; 28. Reactor cover; 29. Allen wrench slot.

Detailed ways

The present invention will be described in further detail below in conjunction with the accompanying drawings and specific embodiments.

Referring to Fig. 1, Fig. 2, Fig. 3, Fig. 4 and Fig. 5, the internal rotation homogeneous reaction device with a positioning system of the present invention includes a box body 5, an electric blast heating device, a rotating device, a positioning device and a cylindrical poly Tetrafluoroethylene homogeneous reactor. The whole reaction device of the present invention is a cube-shaped closed design.

Among them, a control panel 4 is arranged on the upper front of the box body 5, and a programmable temperature controller 1, a digital AC geared motor intelligent regulator 2 and a main power switch 3 are arranged on the control panel 4, and a box door is arranged on the lower part of the control panel 4. 10. The middle part of the box door 10 is a visual panel, the upper part of the box body 5 is provided with cooling holes 9, the lower part of the back of the box body 5 is provided with exhaust holes 13, and the bottom surface of the box body 5 is provided with four adjustable instrument balance knobs 8.

The inside of the box body 5 is provided with an electric blast heating device. Specifically, the electric blast heating device is arranged in the area directly behind the inside of the box body 5. The electric blast heating device is connected to a plurality of fan blades 15 by a fan motor 14. A coil of heating coil 16 is arranged on the outer side of 15 .

Referring to Fig. 4, a rotating device is arranged inside the box body 5. Specifically, the rotating device is located in the middle of the box body 5. The rotating device consists of a rotating motor 18, a central shaft 11, a coupling 20, a rotating bracket 24, and a size-adjustable reaction kettle. The card slot 21 constitutes. Among them, the rotating motor 18 is located on one side of the box body 5 and is installed in a closed manner. The rotating motor 18 is connected to the central rotating shaft 11 through a coupling 20, the central rotating shaft 11 runs through the entire casing 5, and one end of the central rotating shaft 11 extends out of the casing 5 , and the protruding length is 1cm, the central rotating shaft 11 located in the box body 5 is provided with a rotating bracket 24, and the rotating bracket 24 is provided with several draw-in slots 21 of adjustable size reactors, the size of several draw-in slots 21 It can be adjusted, and reaction kettles 26 of different sizes can be fixed on the rotating bracket 24 through the slot 21 .

Referring to Fig. 4, a positioning device is provided inside the box body 5, and the positioning device includes a permanent magnetic positioner 19 and a ferrule positioning device. The output shaft of the rotating electrical machine 18 is provided with a brake disc, and the permanent magnet locator 19 is arranged at the joint between the output shaft of the rotating electrical machine 18 and the brake disc; A groove is provided on the central rotating shaft 11 protruding from the box body 5, and a protrusion matching the groove is provided on the rotating ferrule 22, so that the rotating ferrule 22 is arranged on the central rotating shaft 11, and the rotating ferrule 22 and the wrench 23, and by putting the wrench 23 on the rotating ferrule 22, turning the wrench 23 realizes the rotation of the central rotating shaft 11, thereby realizing the positioning of the reaction kettle 26 arranged on the support, so as to facilitate sampling. The positioning device and the permanent magnet locator form a positioning system, and the rotating ferrule 22 and the wrench 23 form a positioning system. The positioning device and the permanent magnet locator automatically brake when the power is suddenly cut off and the reactor power is turned off. When the reactor is braked and the position of the rotating bracket 24 is not conducive to the loading and unloading of the reactor, the clamping sleeve 22 and the wrench 23 can be used. Set the positioning device to manually adjust the position of the rotating bracket to a position that is convenient for loading and unloading the reactor. The above two positioning systems can be used alone, or they can be set together and used alone.

A stainless steel jacket 25 is arranged on the outside of the reaction kettle 26 , and a reaction kettle cover 28 is arranged on the top of the reaction kettle 26 . The middle part of the reactor cover 28 is provided with an Allen wrench slot 29. The function of the Allen wrench slot 29 is that the Reactor cover 28 needs to be tightened after the sample is added in the Reactor, and the Reactor cover 28 needs to be unscrewed after the reaction. These processes All need to use the hex wrench, so there is this design. There are 1 to 2 rectangular baffles 27 inside the reaction kettle 26. The baffles 27 are arranged vertically. The bottom of the baffle 27 is connected to the cylindrical bottom. It is 1/3 of the height of the reaction kettle 26, and by setting multiple baffles 27, the space of 1/3 volume in the reaction kettle 26 is set into multiple regions, which is beneficial to strengthen the heat transfer and mass transfer during the reaction process.

Referring to FIG. 2 and FIG. 3 , the heating coil 16 of the electric blast heating device is connected to the programmable temperature controller 1 , and the fan motor 14 and the rotating motor 18 are connected to the digital AC geared motor intelligent regulator 2 .

Working process of the present invention is as follows:

1. Open the reactor box door 10, put the reactor 26 to be processed (see FIG. 5 ) into the size-adjustable reactor slot 21 in the box body 5 and fix it, and close the box door 10 .

2. Turn on the power, insert the power plug into the 220V power socket, and set the power switch 3 on the right side of the control panel 4 to the "on" position. At this time, the instrument will display a digital display, indicating that the equipment is in working state.

3. By operating the programmable temperature controller 1 and the digital AC gear motor intelligent regulator 2 on the control panel 4, set the temperature and rotational speed required for the experimental reaction.

4. The instrument starts to work, the temperature and rotating speed in the box 5 gradually reach the set value, and after the required reaction time, the experiment is completed.

5. Turn off the power supply, and after the temperature in the box 5 is close to the ambient temperature, open the box door 10 and take out the reaction kettle 26.

The invention adopts an integrated box design, and the whole device is in the shape of a cube, which is small in size and easy to place. At the same time, it avoids many problems such as serious motor corrosion, loud noise, and low-speed jitter caused by the external motor of the traditional homogeneous reactor. . The programmable temperature controller is connected with the electric blast heating device, which can precisely control the experimental temperature. At the same time, different heating rates and different temperature gradients can be set according to the needs of the reaction for experiments, and the electric blast heating device can make the reaction The temperature in the reactor reaches the specified value in a short period of time and keeps the temperature uniform everywhere, avoiding the damage to the entire instrument caused by the locally high temperature in the reactor and the damage to the hydrothermal crystallization in the reactor. Compared with the traditional static reaction device, the whole set of rotating device can fully mix the reaction materials during the hydrothermal crystallization reaction, which greatly improves the reaction effect. At the same time, the digital AC geared motor intelligent regulator 1 adopts the high-efficiency single-phase AC motor speed control system with MCU as the core, uses the advanced zero-crossing power adjustment method, replaces the commonly used voltage adjustment with power adjustment, and performs calculations in combination with the digital PID method And control, realize the speed acquisition, calculation and display of the micro AC motor, achieve intelligent functions, have mature anti-interference ability, low-level operation without shaking, strong torque, easy to use and many other characteristics.

When the rotating electrical machine 18 is suddenly powered off or the reactor is shut down, the brake disc is also powered off at the same time. At this time, the spring presses the armature, forcing the brake disc to generate friction torque between the armature and the brake disc, so that the rotating electrical machine 18 The output shaft stops quickly, so that the rotating bracket can rotate freely when the reactor is installed and disassembled. It can be seen that the installation of the permanent magnet locator in the present invention avoids the phenomenon that the rotating bracket rotates freely when the reactor is installed and disassembled, and the positioning system formed by rotating the ferrule 22 and the wrench 23 further provides a more humanized dismounting position of the reactor. Created a relatively simple operating conditions. At the same time, there is a size-adjustable reactor card slot on the rotating support to adapt to different types of reactors for experiments, which greatly broadens the operating range of the reactor and enriches the design of experimental reaction conditions.

The present invention will be described in detail below by way of examples.

Example 1

HZSM-5 molecular sieves are usually synthesized in a conventional homogeneous reactor, and the synthesis conditions are:

First mix 12.50g Tetraethyl Tetrasilicate (silicon source), 12.00g Tetrapropylammonium Hydroxide (template), and 70g water (by adjusting the addition ratio of silicon source and water, the particle size of the synthetic molecular sieve can be changed) , stirred at 80°C, condensed and refluxed for 24 hours, then added 0.24g NaOH and 0.46g Al(NO ₃ ) ₃ 9H ₂ O (aluminum source) to the mixed solution, and transferred to a PTFE-lined stainless steel high-pressure reaction In the still, static hydrothermal synthesis at 170°C for 24h, after quenching, centrifuge and wash to the pH of the supernatant ≈ 7, then transfer to a blast drying oven to dry at 110°C for 12h, then transfer to a muffle furnace for calcination at 550°C for 6h Remove the template agent, take out the sample after cooling to obtain NaZSM-5 zeolite, and then use 1mol/L NH ₄ NO ₃ solution to carry out ion exchange three times at 80°C (the mass and volume ratio of molecular sieve and NH ₄ NO ₃ solution is 1 :30), obtain HZSM-5 molecular sieve.

It takes about 56 hours to react in a conventional homogeneous reactor, but the device of the invention can shorten the reaction time by more than 10-15 hours.

Referring to Figure 6 and Figure 7, by comparing the particle size distribution of the HZSM-5 molecular sieve obtained by the reaction between the conventional homogeneous reactor and the homogeneous reactor of the present invention, the particle size analysis of the molecular sieve obtained by the two devices was carried out by using a laser particle size analyzer, and the analysis found that The particle size distribution of the HZSM-5 molecular sieve obtained by synthesizing molecular sieves in a conventional homogeneous reactor is relatively wide (15-20 micron molecular sieve is D50), and the particle size distribution of the HZSM-5 molecular sieve obtained by the device experiment of the present invention is narrow (15-20 micron molecular sieve is D70), which shows that the present invention has a good control effect on the particle size of HZSM-5 molecular sieve.

Claims (9)

1. a kind of interior rotation homogeneous reaction device with positioning system, which is characterized in that including babinet (5), set inside babinet (5) It is equipped with electric heating air blowing heating device, rotating device and reaction kettle；Wherein, rotating device is by electric rotating machine (18), central rotating shaft (11), runing rest (24) and several card slots (21) adjusted that are sized to are constituted；Electric rotating machine (18) is arranged in babinet (5) Interior side, electric rotating machine (18) are connected with central rotating shaft (11) one end, and central rotating shaft (11) runs through entire babinet (5), center It is provided with runing rest (24) in shaft (11), several card slots (21) for being sized to adjust are provided on runing rest (24)； In card slot (21), reaction kettle (26) side is provided with the electric heating air blast for being heated to reaction kettle (26) for reaction kettle (26) setting Heating device is provided with the positioning device positioned to reaction kettle (26) on the output shaft of electric rotating machine (18).

2. a kind of interior rotation homogeneous reaction device with positioning system according to claim 1, which is characterized in that positioning dress It sets including permanent-magnetic positioner (19)；Brake disc is provided on the output shaft of electric rotating machine (18), permanent-magnetic positioner (19) setting exists The output shaft of electric rotating machine (18) and brake disc junction.

3. a kind of interior rotation homogeneous reaction device with positioning system according to claim 1, which is characterized in that center turns The other end of axis (11) stretches out babinet (5), stretches out on the central rotating shaft (11) of babinet (5) and opens up fluted, rotation cutting ferrule (22) On be provided with protrusion with groove match, to rotate in cutting ferrule (22) centrally disposed shaft (11), rotation cutting ferrule (22) match with spanner (23), and by the way that spanner (23) to be sleeved on rotation cutting ferrule (22), rotating spanner (23) realization pair The rotation of central rotating shaft (11), to realize the positioning to the reaction kettle (26) being arranged on holder.

4. a kind of interior rotation homogeneous reaction device with positioning system according to claim 1, which is characterized in that electric heating rouses Air heating device is connected by fan electromotor (14) with several flabellums (15), and a circle heating coil is provided on the outside of several flabellums (15) (16)。

5. a kind of interior rotation homogeneous reaction device with positioning system according to claim 4, which is characterized in that babinet (5) front upper is provided with control panel (4), and programmable temperature controller (1), digital is provided on control panel (4) AC gear motor intelligent regulator (2) and battery main switch (3), control panel (4) lower part are provided with chamber door (10), babinet (5) one upper lateral parts are provided with heat emission hole (9), and babinet (5) lower backside is equipped with vent (13), and babinet (5) bottom surface is equipped with four A adjustable instrument balance knob (8).

6. a kind of interior rotation homogeneous reaction device with positioning system according to claim 5, which is characterized in that heater wire Circle (16) is connected with programmable temperature controller (1), and fan electromotor (14) and electric rotating machine (18) are and digital AC Decelerating motor intelligent regulator (2) is connected.

7. a kind of interior rotation homogeneous reaction device with positioning system according to claim 1, which is characterized in that reaction kettle (26) outside is provided with stainless steel outer sleeve (25).

8. a kind of interior rotation homogeneous reaction device with positioning system according to claim 1, which is characterized in that reaction kettle (26) it is internally provided with 1~2 piece of rectangular baffle (27), baffle (27) is vertically arranged, baffle (27) bottom and cylindrical bottom Portion connects, and baffle (27) both ends are connected with reaction kettle (26) inner wall.

9. a kind of interior rotation homogeneous reaction device with positioning system according to claim 8, which is characterized in that baffle (27) highly it is the 1/3 of reaction kettle (26) height.