CN212468054U - Continuous catalyst supply device for continuously preparing SiC nanowires - Google Patents
Continuous catalyst supply device for continuously preparing SiC nanowires Download PDFInfo
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- CN212468054U CN212468054U CN202020622647.9U CN202020622647U CN212468054U CN 212468054 U CN212468054 U CN 212468054U CN 202020622647 U CN202020622647 U CN 202020622647U CN 212468054 U CN212468054 U CN 212468054U
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Abstract
The utility model belongs to the technical field of solid catalyst continuous supply, in particular to a catalyst continuous supply device for continuously preparing SiC nanowires, which comprises a middle-path air inlet oil circulating heating device (1), a loop air inlet device (2), a cooling circulating water jacket (3) and a precursor evaporation device (4); the cooling circulation water jacket (3) is used for cooling the middle-path intake oil circulation heating device (1), and an interlayer between the cooling circulation water jacket (3) and the middle-path intake oil circulation heating device (1) forms a middle-path intake device (2); the middle-path gas-oil circulation heating device (1) is connected with the precursor evaporation device (4); the medium-path air inlet oil circulation heating device (1) comprises a medium-path air pipe (10) and an oil circulation heating device (11) arranged on the medium-path air pipe (10). The utility model provides a condition of reactant condensation under the low temperature transportation condition that gasification temperature is high.
Description
Technical Field
The utility model belongs to the technical field of solid catalyst supplies with in succession, in particular to catalyst continuous feeding device of continuous preparation SiC nano wire.
Background
Silicon carbide (SiC) nanowires and fibers are important high-temperature materials with high strength, corrosion resistance and good chemical stability, and are generally prepared by a carbothermic method at present. The SiC nanowires with higher major diameter can be generated by adopting chemical vapor deposition, but the prior method adopts a mode of loading materials once and fixing a catalyst, and the method can not realize continuous batch production. The main reason is that the catalyst is generally solid and needs to be fed into the fluidized bed reactor in a gaseous state, which cannot be stably supplied.
For example, ferrocene serving as a catalyst is high in gasification evaporation temperature and easy to condense in the experimental preparation process, so that ferrocene can be guaranteed not to condense in the conveying process only by heating in the ferrocene conveying process, the conveying process is guaranteed to be smooth, and the problem is solved by adopting a mode of heating medium path oil in a circulating manner.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is to design a catalyst that is suitable for continuous preparation SiC nano wire and supplies with in succession to solve the condition of the condensation of the reactant that gasification temperature is high under the low temperature transportation condition.
In order to solve the technical problem, the utility model provides a continuous catalyst supply device for continuously preparing SiC nanowires, which comprises a middle-path gas inlet oil circulation heating device, a loop gas inlet device, a cooling circulation water jacket and a precursor evaporation device;
the cooling circulation water jacket is used for cooling the middle-path air inlet oil circulation heating device, and an interlayer between the cooling circulation water jacket and the middle-path air inlet oil circulation heating device forms a loop air inlet device; the middle-path gas inlet oil circulating heating device is connected with the precursor evaporation device; the middle-path air inlet oil circulation heating device comprises a middle-path air pipe and an oil circulation heating device arranged on the middle-path air pipe.
Preferably, the oil circulation heating device comprises an oil circulation jacket, a sealed oil heater and a circulating pump, the oil circulation jacket is arranged on the middle gas pipe, and the oil circulation jacket is connected with the sealed oil heater through a pipeline to form an oil circulation loop; and an oil inlet pipeline of the oil circulation loop is provided with a circulating pump.
Preferably, an oil inlet is formed in an inner layer jacket of the oil circulation jacket, and an oil outlet is formed in an outer layer jacket of the oil circulation jacket.
Preferably, the oil inlet and the oil outlet are located on the same side of the oil circulation jacket, and the height of the oil inlet is lower than that of the oil outlet.
Preferably, a protective gas inlet is formed in the loop gas inlet device, and a protective gas outlet is formed in an interlayer between the cooling circulation water jacket at the gas outlet end and the middle path gas inlet oil circulation heating device.
Preferably, the cooling circulation water jacket is connected with a cooling circulation water source; the cooling circulation water jacket is of a jacket structure, a cooling water inlet is formed in an inner jacket of the cooling circulation water jacket, and a cooling water outlet is formed in an outer jacket of the cooling circulation water jacket.
Preferably, the precursor evaporation device is provided with a carrier gas inlet.
Preferably, the middle gas pipe is provided with a reaction gas inlet.
Preferably, the cooling water outlet is higher than the cooling water inlet, and the cooling water outlet is higher than the cooling water inlet and is positioned at the lower part of the cooling circulation water jacket and at the same side of the cooling circulation water jacket; the cooling circulation water jacket is cylindrical in shape.
Compared with the prior art, the utility model discloses following beneficial effect has:
firstly, the utility model comprises a middle-path gas inlet oil circulation heating device, a loop gas inlet device, a cooling circulation water jacket, a precursor evaporation device, a gas source and a cooling circulation water source; the gas source is used for providing protective gas, reaction gas and carrier gas; the cooling circulating water source is used for providing circulating cooling water; the medium-path gas oil circulation heating device needs an external sealing oil heating device and a high-temperature resistant circulation mechanical pump, and plays a role in heating the medium-path gas. A high-temperature resistant circulating mechanical pump is mainly used for circulating oil. The sealed high-temperature oil heater is mainly used for heating oil liquid.
Second, the utility model discloses an adopt the mode of giving way oil circulation heating, solved the condition of the high precursor of gasification temperature low condensation of temperature in transportation engineering to this device structure and simple process, easy to carry out and control, production efficiency is high.
Drawings
Fig. 1 is a perspective view of a continuous catalyst supply device for continuously preparing SiC nanowires according to the present invention;
FIG. 2 is a front view of a continuous catalyst supply apparatus for continuous production of SiC nanowires according to the present invention;
3 FIG. 3 3 3 is 3 a 3 cross 3- 3 sectional 3 view 3 taken 3 along 3 line 3 A 3- 3 A 3 of 3 FIG. 32 3; 3
FIG. 4 is a cross-sectional view taken in the direction B-B of FIG. 2;
in the figure: 1. the system comprises a middle-path gas inlet oil circulating heating device, a loop gas inlet device, a cooling circulating water jacket and a precursor evaporating device, wherein the middle-path gas inlet oil circulating heating device comprises 2 the loop gas inlet device, 3 the cooling circulating water jacket and 4 the precursor evaporating device.
Detailed Description
The following detailed description of the embodiments of the present invention is provided with reference to the accompanying drawings and examples. The following examples are merely illustrative of the present invention and are not intended to limit the scope of the present invention.
As shown in fig. 1-4, a continuous catalyst supply device, i.e. a gas inlet device, suitable for continuous preparation of SiC nanowires, comprises a medium-path gas oil circulation heating device 1, a loop gas inlet device 2, a cooling circulation water jacket 3, a precursor evaporation device 4, a gas source and a cooling circulation water source.
The medium-path air inlet oil circulation heating device 1 comprises a medium-path air pipe 10 and an oil circulation heating device 11 arranged on the medium-path air pipe 10. The oil circulation heating device 11 includes an oil circulation jacket 110, an external seal oil heater 111, and a high temperature resistant circulation pump 112. The middle gas pipe 10 is provided with a reaction gas inlet 101, and the reaction gas inlet 101 is connected with a gas source. The gas source enters the middle gas pipe 10 through the reaction gas inlet 101 and is sprayed out.
An oil circulation jacket 110 is arranged on the outer side of the air outlet end of the middle gas pipe 10 and used for heating the middle gas, an oil inlet 113 and an oil outlet pipe 114 are arranged on the oil circulation jacket 110, the oil inlet 113 is located at the lower end of the oil outlet 114 and is horizontally at an angle of 0 degree, an oil channel is formed by an internal interlayer, hot oil firstly flows on the inner side of the interlayer when entering, and then flows on the outer side of the interlayer through the top end. The oil outlet 114 is connected with the inlet end of the sealed oil heater 111, the outlet end of the sealed oil heater 111 is connected with the inlet end of the high-temperature resistant circulating pump 112, and the outlet end of the circulating pump 112 is connected with the oil inlet 113.
The main body of the sealed oil heater 111 is a sealed stainless steel tank body, is heated by an electric heating wire, is internally provided with a temperature thermocouple, is provided with an oil inlet and an oil outlet, and is mainly used for heating oil.
The high temperature resistant circulating pump 112, the main body material is stainless steel, mainly used for making the fluid circulation.
The cooling circulation water jacket 3 is arranged at the outer side of the middle path air inlet oil circulation heating device. The cooling circulation water jacket 3 has a cooling water inlet 31 and a cooling water outlet 32, and is connected to a cooling circulation water source. The cooling circulating water source is used for providing circulating cooling water. The cooling circulating water is a normal-temperature water source and plays a role in cooling. The cooling water outlet 32 and the cooling water inlet 31 are arranged at the lower part of the whole position of the cooling circulating water jacket, the cooling water inlet 31 is arranged at the lower end of the cooling water outlet 32, the horizontal angle is 0 degree, the water channel is realized through the inner interlayer, and when the cooling water enters, the cooling water firstly flows at the inner side of the interlayer and then flows into the outer side of the interlayer through the top end. The cooling circulation water jacket 3 has a cylindrical shape as a whole.
The cooling circulating water sleeve is always filled with cooling circulating water in the using process, so that the precursor is ensured to be directly heated to the reaction temperature from the evaporation temperature, and the protection is provided for the middle-way oil circulating heating device in the high-temperature environment.
The cooling circulation water jacket 3 is sleeved outside the middle path inlet oil circulation heating device 1, and a loop interlayer is arranged in the middle of the cooling circulation water jacket, so that the purpose of protecting the middle path inlet oil circulation heating device and the loop inlet device in a high-temperature environment is achieved.
An interlayer is arranged between the middle inlet oil circulating heating device and the cooling circulating water jacket to form a loop inlet device 2. The loop air inlet device is provided with a protective gas inlet 21, and a protective gas outlet is positioned at the air outlet end of the middle oil circulation heating device and the cooling circulation water jacket interlayer. And the loop air inlet device is positioned in the interlayer of the middle path air inlet oil circulating heating device and the cooling circulating water jacket, and an air source enters from the loop air inlet pipe and then is sprayed out from the interlayer.
The precursor evaporation device 4 is arranged at the bottom end of the middle oil circulation heating device 1, and a carrier gas inlet 41 is arranged on the precursor evaporation device 4. The main body of the precursor evaporation device 4 is a stainless steel sealed tank body, a carrier gas inlet 41 is arranged on the tank body, a gas inlet pipe extends into the upper part of the tank body, the catalyst vapor precursor evaporation device 4 on the upper part is carried to be carried away, heating wires are adopted for heating, and a temperature thermocouple is arranged in the precursor evaporation device.
Gas sources are used to provide shielding gas, reaction gas, and carrier gas, such as: argon, hydrogen, etc., for further processing.
The following describes in detail an operation method of a catalyst continuous supply apparatus for continuously preparing SiC nanowires:
1. and (3) loading the precursor into a precursor evaporator, assembling the precursor with a middle oil circulating heater, and assembling the whole equipment.
2. The equipment is assembled with the fluidized bed, an air source and a cooling circulating water source of the equipment are connected, a pipeline for circulating oil, a high-temperature-resistant oil circulating pump and a high-temperature oil heater are connected, and a heating power supply of the equipment is connected.
3. And turning on a power supply of the equipment, adjusting the temperature, starting heating, and enabling the temperature of the oil liquid and the precursor evaporator to reach the target temperature in the process of heating the fluidized bed.
4, vacuumizing the fluidized bed to-0.1 Kpa, introducing protective gas to normal pressure through equipment, and opening a gas outlet hand valve of the fluidized bed;
5. opening equipment to cool circulating water;
6. adjusting the temperature rising program of the fluidized bed, and starting to rise the temperature;
7. and after the temperature of the fluidized bed reaches the reaction temperature, introducing carrier gas into the precursor evaporation device, introducing the gasified precursor into the middle path along with the carrier gas, and introducing the gasified precursor into the fluidized bed along the middle path to start reaction.
8. And after the reaction is finished, stopping introducing the carrier gas.
9. Cooling the fluidized bed, and closing the protective gas and the circulating cooling water after the temperature is reduced to normal temperature;
the utility model discloses be suitable for fluidized bed-chemical vapor deposition's gas inlet equipment, solved current nozzle and condensed the problem that leads to the trachea not unobstructed at the transportation in-process of carrying the high precursor of gasification temperature, solved the condition of the high precursor of gasification temperature low condensation of temperature in transportation engineering. The utility model discloses an adopt the method of heating for well way reaction gas, improved the condition of the condensation of the high reactant of gasification temperature under the low temperature transportation condition greatly to this device structure and simple process, easy to carry out and control, production efficiency is high.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of modifications and replacements can be made without departing from the technical principle of the present invention, and these modifications and replacements should also be regarded as the protection scope of the present invention.
Claims (9)
1. A catalyst continuous supply device for continuously preparing SiC nanowires is characterized by comprising a middle-path gas inlet oil circulating heating device (1), a loop gas inlet device (2), a cooling circulating water jacket (3) and a precursor evaporation device (4);
the cooling circulation water jacket (3) is used for cooling the middle-path intake oil circulation heating device (1), and an interlayer between the cooling circulation water jacket (3) and the middle-path intake oil circulation heating device (1) forms a middle-path intake device (2); the middle-path gas-oil circulation heating device (1) is connected with the precursor evaporation device (4);
the medium-path air inlet oil circulation heating device (1) comprises a medium-path air pipe (10) and an oil circulation heating device (11) arranged on the medium-path air pipe (10).
2. The continuous catalyst supply device for continuous preparation of SiC nanowires according to claim 1, wherein the oil circulation heating device (11) comprises an oil circulation jacket (110), a sealed oil heater (111) and a circulation pump (112), the oil circulation jacket (110) is arranged on the middle gas pipe (10), and the oil circulation jacket (110) is connected with the sealed oil heater (111) through a pipeline to form an oil circulation loop; and a circulating pump (112) is arranged on an oil inlet pipeline of the oil circulating loop.
3. The continuous catalyst supply device for continuous preparation of SiC nanowires as claimed in claim 2, wherein the inner jacket of the oil circulation jacket (110) is provided with an oil inlet (113), and the outer jacket of the oil circulation jacket (110) is provided with an oil outlet (114).
4. The continuous catalyst supply device for the continuous preparation of SiC nanowires as claimed in claim 3, wherein the oil inlet (113) and the oil outlet (114) are located on the same side of the oil circulation jacket (110), and the height of the oil inlet (113) is lower than that of the oil outlet (114).
5. The continuous catalyst supply device for continuous preparation of SiC nanowires according to claim 1, wherein the loop gas inlet device (2) is provided with a shielding gas inlet (21), and an interlayer between the cooling circulation water jacket (3) at the gas outlet end and the medium-path gas inlet oil circulation heating device (1) forms a shielding gas outlet (22).
6. The continuous catalyst supply device for continuous preparation of SiC nanowires as claimed in claim 1, wherein the cooling circulation water jacket (3) is connected with a cooling circulation water source; the cooling circulation water jacket (3) is of a jacket structure, an inner jacket of the cooling circulation water jacket (3) is provided with a cooling water inlet (31), and an outer jacket of the cooling circulation water jacket (3) is provided with a cooling water outlet (32).
7. The continuous catalyst feeder for continuous SiC nanowire production according to claim 1, wherein the precursor evaporator (4) is provided with a carrier gas inlet (41).
8. The continuous catalyst supply apparatus for SiC nanowire production according to claim 1, wherein the central gas pipe (10) is provided with a reaction gas inlet (101).
9. The continuous catalyst supply device for the continuous preparation of SiC nanowires according to claim 6, wherein the cooling water outlet (32) is higher than the cooling water inlet (31), and the cooling water outlet (32) is higher than the cooling water inlet (31) and is positioned at the lower part of the cooling circulation water jacket (3) and at the same side of the cooling circulation water jacket (3); the cooling circulation water jacket (3) is cylindrical.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202020622647.9U CN212468054U (en) | 2020-04-22 | 2020-04-22 | Continuous catalyst supply device for continuously preparing SiC nanowires |
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| CN202020622647.9U CN212468054U (en) | 2020-04-22 | 2020-04-22 | Continuous catalyst supply device for continuously preparing SiC nanowires |
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| CN212468054U true CN212468054U (en) | 2021-02-05 |
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