CN113750910A

CN113750910A - Alkali metal carbon preparation facilities in supercritical fluid reaction system

Info

Publication number: CN113750910A
Application number: CN202110997662.0A
Authority: CN
Inventors: 孙俊杰; 周美成; 杨艳慧
Original assignee: Nanjing Gongcheng Energy Saving New Material Research Institute Co ltd
Current assignee: Nanjing Gongcheng Energy Saving New Material Research Institute Co ltd
Priority date: 2021-08-27
Filing date: 2021-08-27
Publication date: 2021-12-07

Abstract

The invention discloses a base metal carbon preparation device in a supercritical fluid reaction system, which comprises a bottom frame, wherein L-shaped supports are welded on two sides of the top of the bottom frame, which are close to the middle position, two mounting frames are welded on one side of each L-shaped support, one side of each mounting frame is connected with a reaction barrel through a bolt, a heating mechanism is arranged at the bottom of each reaction barrel, an inlet pipe and an outlet pipe are welded on the top of each reaction barrel, a sealing cover is inserted into the top of each inlet pipe and the top of each outlet pipe, a motor is connected to the top of each sealing cover through a bolt, and a rotating shaft is welded on an output shaft of each motor. According to the invention, under an scCO2 system, safe and nontoxic C02 is used as a carbon source, metal sodium is used as a reducing agent, CO2 is reduced into colorless transparent basic metal carbon under the supercritical condition of 440 ℃ and 80MPa for 12 hours, the activity performance of the metal sodium is increased, the metal sodium is fully and rapidly contacted with CO2, and the speed of the reduction reaction is increased.

Description

Alkali metal carbon preparation facilities in supercritical fluid reaction system

Technical Field

The invention relates to the technical field of supercritical fluid reaction systems, in particular to a device for preparing base metal carbon in a supercritical fluid reaction system.

Background

Any substance can correspondingly present three phases of solid, liquid and gas along with the change of temperature and pressure. The temperature and pressure of the mutual transformation between three states are called three-phase points, besides the three-phase points, a critical point exists in stable substances with not too large molecular weight, the critical point is composed of critical temperature, critical pressure and critical density, when the substances in gas-liquid equilibrium are heated and pressurized, the liquid density is reduced due to thermal expansion, the interface of the gas phase and the liquid phase disappears due to the pressure increase, and a homogeneous system is formed, and the critical point is formed. Fluids above the critical temperature and critical pressure are supercritical fluids. The supercritical fluid is in a gas-liquid state, and is neither liquid nor gas. The supercritical fluid has low viscosity, high density, good flowing, mass transfer, heat transfer and dissolving performances, and can be widely used in the fields of energy conservation, natural product extraction, polymerization reaction, production of superfine powder and fiber, and the like.

There are many ways of chemical reduction of carbon dioxide, but all have some disadvantages. For example, the conversion rate of photocatalytic reduction of CO2 is very low, and is influenced by many reaction factors, and the understanding of the mechanism only reaches the consensus of the 'free radical mechanism'. However, the carbon-based material is synthesized by a supercritical fluid reaction system (scCO 2), namely the carbon-based material is synthesized by scCO2, safe and nontoxic C02 is used as a carbon source, and metallic sodium is used as a reducing agent, and the carbon-based material undergoes a long-time chemical reaction under certain supercritical conditions.

Disclosure of Invention

The invention aims to solve the defects in the prior art and provides a device for preparing base metal carbon in a supercritical fluid reaction system.

In order to achieve the purpose, the invention adopts the following technical scheme:

a base metal carbon preparation device in a supercritical fluid reaction system comprises a bottom frame, wherein L-shaped supports are welded on two sides of the top of the bottom frame, which is close to an intermediate position, two mounting frames are welded on one side of each L-shaped support, a reaction barrel is connected on one side of each mounting frame through a bolt, a heating mechanism is arranged at the bottom of each reaction barrel, an inlet pipe and an outlet pipe are welded on the top of each reaction barrel, sealing covers are inserted into the tops of the inlet pipes and the outlet pipes, a motor is connected on the top of each sealing cover through a bolt, a rotating shaft is welded on an output shaft of the motor, a bearing seat is welded on the outer wall of each rotating shaft, connecting rods distributed at equal intervals are welded on the outer wall of each bearing seat, an object placing pot is connected at the bottom of each connecting rod through a bolt, a first supporting plate is welded on one side of the inner wall of the bottom frame, a first through hole is formed in one side of the top of the first supporting plate, and the inner wall of the first through hole is connected with a booster pump through a bolt, the top of booster pump has the pressure boost pipe of grafting in the reaction vessel through bolted connection, the welding of the inner wall opposite side of underframe has the second backup pad, and the top of second backup pad has the gas holder through bolted connection, and the one end of gas holder has the intake pipe of grafting in the reaction vessel through flange joint.

Preferably, the positioning seats are welded on two sides of the inner wall of the reaction barrel close to the bottom, the positioning holes are formed in one side of the top of each positioning seat, the positioning rods inserted into the positioning holes are welded on two sides of the bottom of the storage pot, the rotating shaft extends into the outer wall of the storage pot and is welded with arc-shaped stirring thin rods in an equidistance distribution mode, and the stirring balls are welded on the bottoms of the stirring thin rods.

Preferably, one side of the tops of the two L-shaped supports is connected with the same T-shaped plate through a bolt, the bottom of the T-shaped plate is connected with the top of the motor through a bolt, and a handle is welded to the top of the T-shaped plate.

Preferably, the top of one side of reaction barrel welding has the atmospheric pressure detection pipe, and the one end of atmospheric pressure detection pipe has the manometer through bolted connection, all has the valve through bolted connection on atmospheric pressure detection pipe, the pressure boost pipe and the intake pipe.

Preferably, the heating mechanism comprises a heater which is connected to the bottom of the reaction barrel through a bolt, and the top of the heater is connected with a heating coil which is inserted into the reaction barrel through a bolt.

Preferably, a second through hole is formed in the other side of the top of the first supporting plate, a protective ring is welded to the inner wall of the second through hole, and the heater is inserted into the protective ring.

Preferably, the underframe has all welded the stabilizer blade near the top of first backup pad both sides, and the top laminating of stabilizer blade is in the bottom both sides of retort, and the top one end welding of underframe has the push rod, and the bottom four corners of underframe all has the universal wheel through bolted connection.

Preferably, two there is a control box one side of mounting bracket through bolted connection, and electric connection between control box and motor, booster pump, manometer and the heater.

Preferably, the inner wall of the bottom frame is connected with a heat conduction cover wrapped on the periphery of the heating coil through a bolt, and the heat conduction cover is arranged to be of a spherical structure.

The invention has the beneficial effects that:

1. in the invention, a sodium metal material is placed in a placing pot, the placing pot is extended into a reaction barrel through a handle, a T-shaped plate is combined at the top of an L-shaped support, a sealing cover is combined in an inlet and outlet pipe, a positioning rod penetrates through the positioning hole, the whole reaction barrel is in a sealing state at the moment, the reaction barrel enters the reaction barrel through an air inlet pipe by releasing nontoxic CO2 in an air storage tank, the inside of the reaction barrel is heated to 440 ℃ through a heater and a heating coil pipe under an scCO2 system, the inside of the reaction barrel is pressurized to a supercritical condition of 80MPa through a booster pump, a booster pipe and a pressure gauge, and CO2 is reduced into colorless transparent basic metal carbon after 12-hour reduction reaction.

2. In the invention, in the process of carrying out reduction reaction, the rotating shaft is driven to rotate by the motor, the stirring fine rod and the stirring ball are driven to stir in the storage pot, and the mobility of the metal sodium is improved by the stirring fine rod and the stirring ball, so that the metal sodium is fully and quickly contacted with CO2, the speed of the reduction reaction is improved, and the efficiency of synthesizing the basic group metal carbon is improved.

3. In the invention, when the inside of the reaction barrel is heated by the heater and the heating coil, the CO2 and the heating coil can be isolated by the heat conduction cover, so that the problem of rapid expansion when the CO2 is directly contacted with the heating coil is avoided, and the problem of instability of the air pressure in the reaction barrel due to the change of carbon dioxide is prevented.

Drawings

FIG. 1 is a schematic view showing the overall configuration of an apparatus for producing a metal base carbonate in a supercritical fluid reaction system as set forth in example 1;

FIG. 2 is a schematic structural view of an inlet tube and a pressure gauge of an apparatus for preparing a metal-based metal carbon in a supercritical fluid reaction system as set forth in example 1;

FIG. 3 is a schematic sectional view showing the structure of a reaction vessel of an apparatus for preparing a base metal carbon in a supercritical fluid reaction system according to example 1;

FIG. 4 is a schematic diagram showing the structure of a placing bowl and a stirring pin of the apparatus for preparing a metal-based metal carbon in a supercritical fluid reaction system according to example 1;

fig. 5 is a schematic structural diagram of a heat conduction cover of an apparatus for preparing a metal base carbon in a supercritical fluid reaction system according to example 2.

In the figure: 1. a bottom frame; 2. a first support plate; 3. a guard ring; 4. a support leg; 5. an L-shaped bracket; 6. a second support plate; 7. a gas storage tank; 8. a control box; 9. a push rod; 10. a T-shaped plate; 11. a handle; 12. a motor; 13. a reaction barrel; 14. a booster pump; 15. a mounting frame; 16. an air inlet pipe; 17. a pressure gauge; 18. a sealing cover; 19. an inlet pipe and an outlet pipe; 20. a rotating shaft; 21. placing the article in a bowl; 22. positioning seats; 23. a heater; 24. a heating coil; 25. a connecting rod; 26. agitating the pin; 27. positioning a rod; 28. a heat conducting shield.

Detailed Description

The technical solution of the present patent will be described in further detail with reference to the following embodiments.

Reference will now be made in detail to embodiments of the present patent, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are exemplary only for the purpose of explaining the present patent and are not to be construed as limiting the present patent.

In the description of this patent, it is to be understood that the terms "center," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientations and positional relationships indicated in the drawings for the convenience of describing the patent and for the simplicity of description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the patent.

In the description of this patent, it is noted that unless otherwise specifically stated or limited, the terms "mounted," "connected," and "disposed" are to be construed broadly and can include, for example, fixedly connected, disposed, detachably connected, disposed, or integrally connected and disposed. The specific meaning of the above terms in this patent may be understood by those of ordinary skill in the art as appropriate.

Example 1

Referring to fig. 1-4, a base metal carbon preparation device in a supercritical fluid reaction system comprises a bottom frame 1, wherein L-shaped supports 5 are welded on two sides of the top of the bottom frame 1 close to a middle position, two mounting frames 15 are welded on one side of each L-shaped support 5, one side of each mounting frame 15 is connected with a reaction barrel 13 through a bolt, a heating mechanism is arranged at the bottom of each reaction barrel 13, an inlet pipe 19 is welded on the top of each reaction barrel 13, a sealing cover 18 is inserted on the top of each inlet pipe 19, the top of each sealing cover 18 is connected with a motor 12 through a bolt, a rotating shaft 20 is welded on an output shaft of each motor 12, a bearing seat is welded on the outer wall of each rotating shaft 20, connecting rods 25 distributed equidistantly are welded on the outer wall of each bearing seat, an object placing pot 21 is connected on the bottom of each connecting rod 25 through a bolt, the object placing pot 21 is of a net type structure, and a proper amount of sodium metal is placed in the object placing pot 21, the inner wall one side welding of underframe 1 has first backup pad 2, and open first through-hole in top one side of first backup pad 2, the inner wall of first through-hole has booster pump 14 through bolted connection, the top of booster pump 14 has the booster pipe of pegging graft in reaction vessel 13 through bolted connection, the pressure boost reading of booster pump 14 is 80MPa, the inner wall opposite side welding of underframe 1 has second backup pad 6, and the top of second backup pad 6 has gas holder 7 through bolted connection, the one end of gas holder 7 has air inlet pipe 16 of pegging graft in reaction vessel 13 through flange connection, the inside of gas holder 7 fills C02, under scCO2 system, use safe nontoxic C02 as the carbon source, sodium metal is as the reductant, under the supercritical condition of 440 ℃ and 80MPa, after 12 hours of reduction reaction, reduce CO2 into colorless transparent basic group metallic carbon.

Further, positioning seat 22 has all been welded to the inner wall both sides that reaction barrel 13 is close to the bottom, and open positioning seat 22's top one side has the locating hole, the bottom both sides of putting thing alms bowl 21 all weld the locating lever 27 of grafting in the locating hole, pivot 20 extends to go into the outer wall welding of putting thing alms bowl 21 in and has equidistance and be curved stirring pin 26, stirring pin 26's bottom has all welded the stirring ball, in the in-process of carrying out the reduction reaction, accessible motor 12 drives pivot 20 and rotates, drive stirring pin 26 and stir the ball and stir the processing in the inside of putting thing alms bowl 21, utilize the activity ability of stirring pin 26 and stirring ball increase metallic sodium, make metallic sodium abundant and quick contact with CO2, the speed of reduction reaction is improved, the efficiency of synthetic basic group metallic carbon is improved.

Furthermore, one side of the tops of the two L-shaped supports 5 is connected with the same T-shaped plate 10 through a bolt, the bottom of the T-shaped plate 10 is connected with the top of the motor 12 through a bolt, and a handle 11 is welded to the top of the T-shaped plate 10.

Further, an air pressure detection pipe is welded at the top of one side of the reaction barrel 13, one end of the air pressure detection pipe is connected with a pressure gauge 17 through a bolt, and valves are connected to the air pressure detection pipe, the pressure increasing pipe and the air inlet pipe 16 through bolts.

Further, the heating mechanism comprises a heater 23 which is connected to the bottom of the reaction barrel 13 through a bolt, the top of the heater 23 is connected with a heating coil 24 which is inserted into the reaction barrel 13 through a bolt, and the heating temperature of the heating coil 24 is 440 ℃.

Furthermore, a second through hole is formed in the other side of the top of the first supporting plate 2, the inner wall of the second through hole is welded with the protective ring 3, and the heater 23 is inserted into the protective ring 3.

Further, the underframe 1 has all welded stabilizer blade 4 near the top of 2 both sides of first backup pad, and the top laminating of stabilizer blade 4 is in the bottom both sides of retort 13, and the top one end welding of underframe 1 has push rod 9, and the bottom four corners of underframe 1 all has the universal wheel through bolted connection.

Further, one side of the two mounting frames 15 is connected with a control box 8 through bolts, and the control box 8 is electrically connected with the motor 12, the booster pump 14, the pressure gauge 17 and the heater 23.

The working principle is as follows: when in use, a user places a sodium metal material in the placing bowl 21, the placing bowl 21 extends into the reaction barrel 13 through the handle 11, so that the T-shaped plate 10 is combined at the top of the L-shaped bracket 5, the sealing cover 18 is combined in the inlet and outlet pipe 19, the positioning rod 27 passes through the positioning hole, the whole reaction barrel 13 is in a sealing state, the non-toxic CO2 in the gas storage tank 7 is released to enter the reaction barrel 13 through the gas inlet pipe 16, under the scCO2 system, the safe and non-toxic C02 is used as a carbon source, the sodium metal is used as a reducing agent, the interior of the reaction barrel 13 is heated to 440 ℃ through the heater 23 and the heating coil pipe 24, the pressure inside of the reaction barrel 13 is increased to the supercritical condition of 80MPa through the booster pump 14, the booster pipe and the pressure gauge 17, after 12 hours of reduction reaction, the CO2 is reduced into colorless transparent basic metal carbon, and in the process of reduction reaction, accessible motor 12 drives pivot 20 and rotates, drives to stir pin 26 and stirs the ball and stir the processing in the inside of putting thing alms bowl 21, utilizes to stir pin 26 and the mobility of stirring ball increase metallic sodium for metallic sodium is abundant and quick contacts with CO2, improves reduction's speed, improves the efficiency of synthetic basic group metal carbon.

Example 2

Referring to fig. 5, in a device for preparing a metal base carbon in a supercritical fluid reaction system, in this embodiment, compared to embodiment 1, a heat conduction cover 28 wrapped around a heating coil 24 is connected to an inner wall of a bottom frame 1 through a bolt, and the heat conduction cover 28 is configured as a spherical structure.

The working principle is as follows: when the reactor is used, when a user heats the inside of the reaction barrel 13 through the heater 23 and the heating coil 24, the CO2 and the heating coil 24 can be isolated through the heat conduction cover 28, the problem of rapid expansion when the CO2 is directly contacted with the heating coil 24 is avoided, and the problem of instability of the air pressure inside the reaction barrel 13 due to the change of carbon dioxide is prevented.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims

1. The base metal carbon preparation device in the supercritical fluid reaction system comprises a bottom frame (1) and is characterized in that L-shaped supports (5) are welded on two sides of the top of the bottom frame (1) close to an intermediate position, two mounting frames (15) are welded on one sides of the L-shaped supports (5), a reaction barrel (13) is connected to one side of each mounting frame (15) through a bolt, a heating mechanism is arranged at the bottom of the reaction barrel (13), an inlet pipe (19) and an outlet pipe (19) are welded on the top of the reaction barrel (13), a sealing cover (18) is inserted into the top of the inlet pipe (19), a motor (12) is connected to the top of the sealing cover (18) through a bolt, a rotating shaft (20) is welded on an output shaft of the motor (12), bearing seats are welded on the outer walls of the rotating shaft (20), connecting rods (25) distributed equidistantly are welded on the outer walls of the bearing seats, and object placing bowls (21) are connected to the bottoms of the connecting rods (25) through bolts, the welding of inner wall one side of underframe (1) has first backup pad (2), and open top one side of first backup pad (2) has first through-hole, and the inner wall of first through-hole has booster pump (14) through bolted connection, and the top of booster pump (14) has the booster pipe of pegging graft in reaction barrel (13) through bolted connection, the welding of the inner wall opposite side of underframe (1) has second backup pad (6), and the top of second backup pad (6) has gas holder (7) through bolted connection, and the one end of gas holder (7) has intake pipe (16) of pegging graft in reaction barrel (13) through flange joint.

2. The device for preparing the alkali-based metal carbon in the supercritical fluid reaction system according to claim 1, wherein the positioning seats (22) are welded on both sides of the inner wall of the reaction barrel (13) near the bottom, the positioning holes are formed on one side of the top of the positioning seat (22), the positioning rods (27) inserted in the positioning holes are welded on both sides of the bottom of the placing pot (21), the arc-shaped stirring thin rods (26) are welded on the outer wall of the rotating shaft (20) extending into the placing pot (21), and the stirring balls are welded on the bottoms of the stirring thin rods (26).

3. The apparatus for preparing a base metal carbon in a supercritical fluid reaction system according to claim 2, wherein one side of the top of each of the two L-shaped supports (5) is connected with the same T-shaped plate (10) by a bolt, the bottom of the T-shaped plate (10) is connected with the top of the motor (12) by a bolt, and the handle (11) is welded on the top of the T-shaped plate (10).

4. The apparatus for preparing a base metal carbon in a supercritical fluid reaction system according to claim 3, wherein a pressure detecting tube is welded to a top of one side of the reaction barrel (13), and one end of the pressure detecting tube is connected to a pressure gauge (17) by bolts, and valves are connected to the pressure detecting tube, the pressurizing tube and the gas inlet tube (16) by bolts.

5. The apparatus for preparing a base metal carbon in a supercritical fluid reaction system according to claim 4, wherein the heating mechanism comprises a heater (23) bolted to the bottom of the reaction vessel (13), and a heating coil (24) bolted to the top of the heater (23) and inserted into the reaction vessel (13).

6. The apparatus for preparing a base metal carbon in a supercritical fluid reaction system according to claim 5, wherein the first support plate (2) has a second through hole formed at the other side of the top thereof, and the guard ring (3) is welded to the inner wall of the second through hole, and the heater (23) is inserted into the guard ring (3).

7. The apparatus for preparing a base metal carbon in a supercritical fluid reaction system according to any one of claims 1 to 6, wherein the bottom frame (1) has support legs (4) welded to the top portions of both sides of the first support plate (2), the top portions of the support legs (4) are attached to both sides of the bottom of the reaction barrel (13), the push rod (9) is welded to one end of the top portion of the bottom frame (1), and universal wheels are connected to four corners of the bottom frame (1) through bolts.

8. The apparatus for preparing a base metal carbon in a supercritical fluid reaction system according to claim 6, wherein one side of the two mounting frames (15) is connected to the control box (8) by bolts, and the control box (8) is electrically connected to the motor (12), the booster pump (14), the pressure gauge (17) and the heater (23).

9. The apparatus for preparing a base metal carbon in a supercritical fluid reaction system according to claim 4, wherein the bottom inner wall of the bottom frame (1) is bolted with a heat conduction cover (28) wrapped around the heating coil (24), and the heat conduction cover (28) is provided in a spherical structure.