Laboratory reaction kettle for preparing transformer oil desulfurization adsorbent and application of laboratory reaction kettle

Abstract

The invention discloses a laboratory reaction kettle for preparing a transformer oil desulfurization adsorbent and application of the laboratory reaction kettle. A kettle body comprises a shell and fire-resistant steel pipes symmetrically arranged on the two sides of the shell, the shell is provided with a first gas inlet, the gas inlet is provided with a valve, the valve is communicated with a first gas inlet pipe through a copper sleeve, and the first gas inlet pipe is connected with a reducing gas steel cylinder; the bottom of the shell is detachably connected with a steel cover; each fire-resistant steel pipe is detachably connected with a temperature-resistant cover, a second gas inlet and a gas outlet which are communicated with the temperature-resistant covers are respectively formed in the middle of the two temperature-resistant covers, the second gas inlet is communicated with a second gas inlet pipe through a copper sleeve, and the second gas inlet pipe is connected with an inert gas steel cylinder; handles are arranged on the two sides of the temperature-resistant cover respectively. The reaction kettle disclosed by the invention is resistant to high temperature, and materials of the reaction kettle are prevented from being deformed or oxidized; through full protection of inert gas, oxygen is prevented from permeating and oxidizing; meanwhile, the adsorbent is convenient to load and unload.

Description

Technical Field

[0001] The invention relates to the field of reactors, and in particular to a laboratory reactor for preparing a transformer oil desulfurization adsorbent and application thereof. Background Art

[0002] Sulfur compounds such as mercaptans and thiophenes in comprehensive transformer oil can cause corrosion of metal parts of equipment. Traditional adsorption desulfurization technology uses activated carbon and other carriers to carry metal ions such as Cu 2+ 、Ce3 + 、Ag + However, existing reactors have the following problems: 1) Insufficient high temperature tolerance: the reduction reaction needs to be carried out at 500-600°C, and conventional reactor materials are prone to deformation or oxidation; 2) Insufficient inert gas protection: oxygen infiltration during operation causes metal ion oxidation failure; 3) Difficulty in loading and unloading of adsorbents: the adsorbent is prone to sintering after high temperature reaction and is difficult to disassemble and regenerate. Summary of the invention

[0003] In order to solve the above-mentioned technical problems, the present invention provides a laboratory reactor for preparing a transformer oil desulfurization adsorbent and application thereof.

[0004] The technical solution adopted by the present invention is:

[0005] A laboratory reactor for preparing a desulfurization adsorbent for transformer oil, comprising a reactor body arranged in a muffle furnace, the reactor body comprising a shell and refractory steel pipes symmetrically arranged on both sides of the shell, a first air inlet is provided on the shell, the air inlet is provided with a valve, the valve is connected to a first air inlet pipe through a copper sleeve, and the first air inlet pipe is connected to a reducing gas cylinder; a steel cover is detachably connected to the bottom of the shell; each of the refractory steel pipes is detachably connected to a heat-resistant cover, a second air inlet and an air outlet connected to the heat-resistant covers are respectively provided in the middle of the two heat-resistant covers, the second air inlet is connected to a second air inlet pipe through a copper sleeve, and the second air inlet pipe is connected to an inert gas cylinder; handles are respectively provided on both sides of the heat-resistant cover.

[0006] Furthermore, an annular gas distribution pipe connected to the second air inlet is arranged inside the shell, and a tube wall of the annular gas distribution pipe is evenly provided with a plurality of through holes.

[0007] Furthermore, the fire-resistant steel pipe is made of silicon carbide composite material, which has a temperature resistance of up to 1200°C.

[0008] Furthermore, the temperature-resistant cover is connected to the fire-resistant steel pipe via flange bolts.

[0009] Furthermore, a graphite gasket is provided between the temperature-resistant cover and the fire-resistant steel pipe.

[0010] Furthermore, each of the temperature-resistant covers is rotatably connected to a side wall of the muffle furnace.

[0011] Furthermore, the muffle furnace is provided with a square opening, which has a built-in temperature sensor.

[0012] Furthermore, a ring is provided at the connection between the shell and each of the fire-resistant steel pipes, and the ring is integrally formed with the shell.

[0013] Furthermore, the heat-resistant cover has a water-cooling interlayer built in, and a safety valve is provided on the heat-resistant cover.

[0014] Another technical solution adopted by the present invention is:

[0015] An application of a laboratory reactor for preparing a transformer oil desulfurization adsorbent is characterized in that it specifically comprises the following steps:

[0016] 1) Remove the heat-resistant cover, soak the activated carbon in copper sulfate and cerium nitrate, and then put it into the shell;

[0017] 2) Install the temperature-resistant cover and deliver the inert gas into the shell through the inert gas cylinder, the second air inlet pipe, the second air inlet, and the refractory steel pipe in sequence to prevent the oxygen in the shell from being oxidized;

[0018] 3) Rotate the kettle as a whole and connect it to the muffle furnace, and heat it to 500-600℃;

[0019] 4) delivering the reducing gas into the shell through the reducing gas cylinder, the first air inlet pipe, and the first air inlet in sequence;

[0020] 5) Shake the kettle body by the handle to make the raw materials in the shell fully contact and react, and finally the copper ions and cerium ions in the shell are reduced and adsorbed on the activated carbon to form a transformer oil desulfurization adsorbent;

[0021] 6) After the kettle body is cooled, remove the steel cover and take out the prepared transformer oil desulfurization adsorbent.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] 1) sending reducing gas into the shell through the first air inlet to reduce copper ions and cerium ions in the shell to prepare a transformer oil desulfurization adsorbent;

[0024] 2) Inert gas is sent into the shell through the second air inlet, thereby protecting the shell from air, so that the transformer oil desulfurization adsorbent is not affected by oxygen during the preparation process;

[0025] 3) The water-cooled interlayer is set up to achieve rapid cooling through external circulating coolant;

[0026] 4) The annular gas distribution pipe and the multiple through holes arranged on the pipe wall form a uniform air curtain barrier, reduce the consumption of inert gas, and improve the efficiency of protecting the side walls and bottom walls of the shell;

[0027] 5) Use refractory steel pipes made of silicon carbide composite materials to achieve high temperature resistance;

[0028] 6) The graphite gasket is used to improve the sealing and reduce the leakage of inert gas;

[0029] 7) A temperature sensor is provided to monitor the temperature of the reactor in real time to ensure that the reduction reaction is carried out at 500-600°C. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments:

[0031] Figure 1 It is a schematic diagram of the overall structure of the kettle body and the muffle furnace in the present invention;

[0032] Figure 2 It is a front view of the kettle body of the present invention;

[0033] Figure 3 It is a side view of the kettle body in the present invention.

[0034] In the figure: 1, muffle furnace; 101, square mouth; 2, kettle body; 3, shell; 4, refractory steel pipe; 5, first air inlet; 6, valve; 7, copper sleeve; 8, temperature-resistant cover; 9, second air inlet; 10, air outlet; 11, ring. DETAILED DESCRIPTION

[0035] Example 1

[0036] like Figures 1 to 3 As shown, a laboratory reactor for preparing a desulfurization adsorbent for transformer oil comprises a reactor body 2 arranged in a muffle furnace 1, the reactor body 2 comprises a shell 3 and refractory steel pipes 4 symmetrically arranged on both sides of the shell 3, a first air inlet 5 is provided on the shell 3, a valve 6 is provided on the air inlet, the valve 6 is connected to the first air inlet pipe through a copper sleeve 7, and the first air inlet pipe is connected to a reducing gas cylinder; a steel cover is detachably connected to the bottom of the shell 3; each refractory steel pipe 4 is detachably connected to a heat-resistant cover 8, a second air inlet 9 and an air outlet 10 connected to the heat-resistant cover 8 are respectively provided in the middle of the two heat-resistant covers 8, the second air inlet 9 is connected to the second air inlet pipe through the copper sleeve 7, and the second air inlet pipe is connected to the inert gas cylinder; handles are respectively provided on both sides of the heat-resistant cover 8.

[0037] In a preferred implementation manner of this embodiment, an annular gas distribution pipe connected to the second air inlet 9 is arranged inside the shell 3, and a plurality of through holes are evenly opened on the tube wall of the annular gas distribution pipe to form a uniform air curtain barrier, thereby reducing the consumption of inert gas and improving the efficiency of protecting the side walls and bottom walls of the shell 3.

[0038] In a preferred implementation manner of this embodiment, the refractory steel pipe 4 is made of silicon carbide composite material, which has a temperature resistance of up to 1200° C., achieving high temperature resistance.

[0039] In the preferred implementation manner of this embodiment, the heat-resistant cover 8 is connected to the fire-resistant steel pipe 4 by flange bolts, which is convenient for disassembly and connection.

[0040] In a preferred implementation manner of this embodiment, a graphite gasket is provided between the temperature-resistant cover 8 and the fire-resistant steel pipe 4 to improve the sealing performance and reduce the leakage of the inert gas.

[0041] In a preferred implementation manner of this embodiment, each temperature-resistant cover 8 is rotatably connected to the side wall of the muffle furnace 1 to ensure uniform mixing and contact of the materials and improve the reaction efficiency.

[0042] In a preferred implementation manner of this embodiment, the muffle furnace 1 is provided with a square opening 101, which has a built-in temperature sensor to monitor the temperature of the reactor in real time to ensure that the reduction reaction is carried out at 500-600°C.

[0043] In a preferred implementation manner of this embodiment, a ring 11 is provided at the connection between the shell 3 and each refractory steel tube 4. The ring 11 is integrally formed with the shell 3. The two rings 11 and the first air inlet 5 form a triangular support to prevent the kettle body 2 from shaking.

[0044] In a preferred implementation manner of this embodiment, the heat-resistant cover 8 has a water-cooling interlayer built in, and a safety valve is provided on the heat-resistant cover 8. The safety valve is provided to prevent the water-cooling interlayer from bursting due to water vapor generated by sudden temperature rise. When water vapor is generated, the safety valve is opened to exhaust.

[0045] Example 2

[0046] An application of a laboratory reactor for preparing a transformer oil desulfurization adsorbent is characterized in that it specifically comprises the following steps:

[0047] 1) Remove the heat-resistant cover 8, soak the activated carbon in copper sulfate and cerium nitrate, and then install it into the housing 3;

[0048] 2) Install the temperature-resistant cover 8, and deliver the inert gas into the shell 3 through the inert gas cylinder, the second air inlet pipe, the second air inlet 9, and the fire-resistant steel pipe 4 in sequence to prevent the oxygen in the shell 3 from being oxidized;

[0049] 3) Rotate the kettle body 2 as a whole and connect it to the muffle furnace 1, and heat it to 500-600°C;

[0050] 4) The reducing gas is sequentially delivered into the housing 3 through the reducing gas cylinder, the first air inlet pipe, and the first air inlet port 5;

[0051] 5) Shake the kettle body 2 by the handle to make the raw materials in the shell 3 fully contact and react, and finally the copper ions and cerium ions in the shell 3 are reduced and adsorbed on the activated carbon to form a transformer oil desulfurization adsorbent;

[0052] 6) After the kettle body 2 is cooled, the steel cover is removed and the prepared transformer oil desulfurization adsorbent is taken out.

[0053] The reactor of the present invention is resistant to high temperatures and prevents the reactor material from being deformed or oxidized; it is fully protected by inert gas to prevent oxygen from penetrating and oxidizing; it prevents the adsorbent from sintering after high-temperature reaction and facilitates the loading and unloading of the adsorbent; the application of the reactor of the present invention is used to prepare a high-efficiency, sintering-free, and oxidation-free transformer oil desulfurization adsorbent.

[0054] The transformer oil desulfurization adsorbent prepared by the laboratory reactor of the present invention is used to conduct a sulfur corrosion test on a transformer oil sample of a hydropower plant. According to the ASTM standard, the sulfur corrosion degree of the copper sheet is reduced after the adsorption and soaking treatment.

[0055] The embodiments described above are merely descriptions of preferred implementation modes of the present invention and are not intended to limit the scope of the present invention. Without departing from the principles and essence of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should all fall within the scope of protection determined by the claims of the present invention.

Claims

1. A laboratory reactor for preparing a transformer oil desulfurization adsorbent, comprising a reactor body (2) arranged in a muffle furnace (1), characterized in that: The kettle body (2) comprises a shell (3) and fire-resistant steel pipes (4) symmetrically arranged on both sides of the shell (3); a first air inlet (5) is provided on the shell (3); a valve (6) is provided on the air inlet; the valve (6) is connected to a first air inlet pipe through a copper sleeve (7); the first air inlet pipe is connected to a reducing gas cylinder; a steel cover is detachably connected to the bottom of the shell (3); Each of the fire-resistant steel pipes (4) is detachably connected to a heat-resistant cover (8); a second air inlet (9) and an air outlet (10) connected to the heat-resistant cover (8) are respectively provided in the middle of the two heat-resistant covers (8); the second air inlet (9) is connected to a second air inlet pipe through a copper sleeve (7); the second air inlet pipe is connected to an inert gas cylinder; handles are respectively provided on both sides of the heat-resistant cover (8).

2. The laboratory reactor for preparing a transformer oil desulfurization adsorbent according to claim 1, characterized in that: An annular gas distribution pipe connected to the second air inlet (9) is arranged inside the shell (3), and a plurality of through holes are evenly arranged on the pipe wall of the annular gas distribution pipe.

3. The laboratory reactor for preparing a transformer oil desulfurization adsorbent according to claim 1, characterized in that: The fire-resistant steel pipe (4) is made of a silicon carbide composite material with a temperature resistance of up to 1200°C.

4. The laboratory reactor for preparing a transformer oil desulfurization adsorbent according to claim 1, characterized in that: The temperature-resistant cover (8) is connected to the fire-resistant steel pipe (4) via flange bolts.

5. The laboratory reactor for preparing a transformer oil desulfurization adsorbent according to claim 1, characterized in that: A graphite gasket is provided between the temperature-resistant cover (8) and the fire-resistant steel pipe (4).

6. The laboratory reactor for preparing a transformer oil desulfurization adsorbent according to claim 1, characterized in that: Each of the temperature-resistant covers (8) is rotatably connected to the side wall of the muffle furnace (1).

7. The laboratory reactor for preparing a transformer oil desulfurization adsorbent according to claim 1, characterized in that: The muffle furnace (1) is provided with a square opening (101) which has a built-in temperature sensor.

8. The laboratory reactor for preparing a transformer oil desulfurization adsorbent according to claim 1, characterized in that: A circular ring (11) is provided at the connection between the shell (3) and each of the fire-resistant steel pipes (4); the circular ring (11) and the shell (3) are integrally formed.

9. The laboratory reactor for preparing a transformer oil desulfurization adsorbent according to claim 1, characterized in that: The heat-resistant cover (8) has a water-cooling interlayer built in, and a safety valve is provided on the heat-resistant cover (8).

10. Use of a laboratory reactor for preparing a transformer oil desulfurization adsorbent according to any one of claims 1 to 9, characterized in that: The specific steps include: 1) Disassemble the heat-resistant cover (8), soak the activated carbon in copper sulfate and cerium nitrate, and then install it into the housing (3); 2) Install the temperature-resistant cover (8), and deliver the inert gas into the shell (3) through the inert gas cylinder, the second air inlet pipe, the second air inlet (9), and the fire-resistant steel pipe (4) in sequence to prevent the oxygen in the shell (3) from being oxidized; 3) Rotate the kettle body (2) as a whole and connect it to the muffle furnace (1), and heat it to 500-600° C.; 4) delivering the reducing gas into the housing (3) in sequence through the reducing gas cylinder, the first gas inlet pipe, and the first gas inlet port (5); 5) Shaking the kettle body (2) by a handle to allow the raw materials in the shell (3) to fully contact and react, and finally the copper ions and cerium ions in the shell (3) are reduced and adsorbed on the activated carbon to form a transformer oil desulfurization adsorbent; 6) After the kettle body (2) is cooled, the steel cover is removed and the prepared transformer oil desulfurization adsorbent is taken out.

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