CN109915728B - SF (sulfur hexafluoride)6Full-automatic vacuum pumping and inflating trolley - Google Patents

SF (sulfur hexafluoride)6Full-automatic vacuum pumping and inflating trolley Download PDF

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CN109915728B
CN109915728B CN201811582567.9A CN201811582567A CN109915728B CN 109915728 B CN109915728 B CN 109915728B CN 201811582567 A CN201811582567 A CN 201811582567A CN 109915728 B CN109915728 B CN 109915728B
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inflation
silicon dioxide
pressure
gas
graphene oxide
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CN109915728A (en
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刘健
傅达宏
徐小峰
王绍强
李青杉
周磊
王辉
徐红标
许胜蔚
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State Grid Zhejiang Longyou County Power Supply Co ltd
State Grid Corp of China SGCC
Quzhou Power Supply Co of State Grid Zhejiang Electric Power Co Ltd
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State Grid Zhejiang Longyou County Power Supply Co ltd
State Grid Corp of China SGCC
Quzhou Power Supply Co of State Grid Zhejiang Electric Power Co Ltd
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Abstract

The invention relates to the field of full-automatic vacuumizing and inflating, in particular to SF6Full-automatic evacuation inflation cart comprises a cart body, an evacuation system and a constant pressure inflation system, wherein the cart body comprises a controller and a bearing platform, and the constant pressure inflation system comprises SF6The invention relates to an SF gas storage buffer tank, which comprises an air bottle, a stop valve, a filter, a pressure sensor, a pressure reducing valve, an electromagnetic valve and an air storage buffer tank which are communicated with each other by a charging channel, and a vacuum pumping system which comprises an absorber, a vacuum pump, a vacuum meter and the stop valve6The gas cylinder vacuumizing system and the constant-pressure inflating system are integrated on the trolley, so that the trolley is convenient to operate and carry; the pressure of the gas-using equipment can be monitored in real time during inflation, and the switch of the electromagnetic valve is operated, so that the inflation pressure can be accurately controlled; an absorber loaded with silver-loaded graphene/silicon dioxide aerogel particles is arranged at an air outlet of the vacuum pump, toxic gas molecules decomposed by SF6 gas can be absorbed, and the environment and the health of operators are protected.

Description

SF (sulfur hexafluoride)6Full-automatic vacuum pumping and inflating trolley
Technical Field
The invention relates to the field of full-automatic vacuumizing and inflating, in particular to SF6Full-automatic evacuation inflation shallow.
Background
SF6Sulfur hexafluoride is an insulating medium, the insulating strength of which is 2.33 times of air, and the arc extinguishing capacity of which is 100 times of air, so that the sulfur hexafluoride is generally used as an arc extinguishing medium for electrical equipment such as a circuit breaker, and before the electrical equipment is maintained and inflated, in order to prevent air from being mixed into the electrical equipment, the electrical equipment needs to be vacuumized to ensure SF6The purity of gas, however, most of the traditional vacuumizing and inflating devices are manual, and vacuumizing and inflating are performed only through manual control by experience of operators, so that the traditional vacuumizing and inflating device has a great potential safety hazard, wastes a great amount of manpower and material resources, reduces efficiency, and is easy to cause instability of vacuumizing and inflating due to manual control, and generates loss on equipment; and, realize simultaneously that evacuation, the function of aerifing need more equipment synergism such as gas cylinder, vacuum pump, controller, pipeline, valve, design one set and integrate in an organic whole with above-mentioned equipment, and the device of being convenient for remove can effectively improve work efficiency, reduces manpower and materials cost.
Pure SF6The gas is colorless, tasteless, odorless and non-inflammable, has stable chemical property at normal temperature, and belongs to inert gas. Under the influence of arc, corona, spark discharge and partial discharge, high temperature and other factors, SF6The gas will decompose to form some harmful low-fluoride compounds, especially some highly toxic decomposition products, such as SOF2、SO2F2And SO2Etc., which irritate the skin, eyes, mucous membranes, and if inhaled in large quantities, cause dizziness and pulmonary edema, even moreThe exhaust gas is not filtered and adsorbed by the vacuumizing inflation device in the prior art when vacuumizing, so that toxic gas decomposed by SF6 flows into the atmosphere when the equipment is used, the environment is polluted, and the health of workers is easily injured.
For example, the invention discloses a manual gas-filling and vacuum-pumping device for sulfur hexafluoride electrical equipment, which is disclosed in the Chinese patent document with the publication number CN203488991U, and comprises a joint, a pipeline and a pumping device, wherein the joint is a three-way joint, one end of the three-way joint is connected with the pumping device, and the other two ends of the three-way joint are respectively connected with SF through pipelines6However, the pumping device of the present invention is a manual pumping device, and is inconvenient to carry, wastes manpower and material resources, and is liable to cause a reduction in working efficiency.
Disclosure of Invention
The invention aims to solve the problems that most vacuumizing inflation devices are manual and inconvenient to carry in the prior art and the like, and provides SF which can be used for full-automatic vacuumizing and constant-pressure inflation and integrates all devices into a whole so as to be convenient to carry6Full-automatic evacuation inflation shallow.
The invention also solves the problem of SF during vacuum pumping6Decomposed toxic gas flows into the atmosphere, easily causes the problems of injury and the like to personnel and environment, and provides the gas-liquid separation device capable of effectively adsorbing SF6The silver of the decomposed gas carries graphene/silica aerogel particles.
In order to achieve the purpose, the invention adopts the following technical scheme:
SF (sulfur hexafluoride)6Full-automatic evacuation inflation cart, including shallow body, evacuation system and level pressure inflation system, the shallow body includes controller and bearing platform, level pressure inflation system includes SF6The gas cylinder, the stop valve, the filter, the pressure sensor, the pressure reducing valve, the electromagnetic valve and the gas storage buffer tank are communicated with each other by a charging channel, and the SF6The gas cylinder is connected with the pipeline gas inlet, the pipeline gas inlet is provided with a filter, a pressure sensor and a pressure reducing valve, and the pipeline gas outlet is provided with a pressure sensorThe vacuum pumping system comprises a vacuum pump, a vacuum meter and a stop valve, one end of the stop valve is connected with a pipeline of the inflation system, one end of the stop valve is connected with the vacuum meter, the other end of the vacuum meter is connected with the vacuum pump, an air outlet end of the vacuum pump is provided with an absorber, the vacuum pump and the gas storage buffer tank are arranged on a bearing platform, and a controller is connected with the stop valve, the solenoid valve, a pressure sensor and a vacuum pump circuit and used for controlling the opening and closing of the vacuum pumping or the inflation state.
The cart body is provided with a vacuum pumping system and a constant pressure inflation system, wherein SF in the constant pressure inflation system6The gas cylinder is connected with the gas inlet to provide a gas source, the gas inlet end is sequentially provided with a filter, a pressure sensor and a pressure reducing valve, wherein the filter is used for filtering SF6SF in gas cylinder6Impurity such as moisture in the gas, pressure sensor is used for monitoring the pressure of air inlet end, the relief pressure valve is used for reducing the pressure of air inlet end, and keep the stability of pressure, air outlet end sets up pressure sensor, gas storage buffer tank and solenoid valve, wherein, because the gas outlet is connected with electrical equipment, gas storage buffer tank can be used to buffer gas, prevent to fill in electrical equipment gas velocity of flow too big and produce the damage to electrical equipment, when aerifing, pressure sensor is used for monitoring air outlet end, electrical equipment's pressure promptly, whether reach the setting value for judging electrical equipment's pressure, when electrical equipment's pressure did not reach the setting value, the solenoid valve is automatic to be opened, fill electrical equipment's pressure to the settlement pressure.
The residual SF in the electrical equipment and in the cart ducts needs to be treated before inflation6The gas is evacuated by a vacuum-pumping system, and SF is generated by electric arc, corona, spark discharge, partial discharge, high temperature and other factors during the use of the electrical equipment6The gas will decompose to form some harmful low-fluoride compounds, especially some highly toxic decomposition products, such as SOF2、SO2F2And SO2Etc., which irritate the skin, eyes, mucous membranes, and if inhaled in large quantities, cause dizziness and pulmonary edema, even moreSo as to cause death, therefore, when the vacuum pump is vacuumized, an absorber is arranged at the air outlet end of the vacuum pump and is used for absorbing SF6Highly toxic decomposition products of gases.
The vacuum pump and the gas storage buffer tank are arranged on the bearing platform, the vacuum pump and the gas storage buffer tank are two devices with heavier vacuumizing systems and constant-pressure inflating systems, and are arranged on the bearing platform to be beneficial to the stability of the cart.
Preferably, the pressure reducing valve is provided on the controller.
Preferably, the upper part of the cart body is provided with SF6The gas cylinder limiting block is provided with a gas cylinder and SF6The gas cylinder is a semicircular notch matched with the gas cylinder in shape.
Preferably, the bottom of the cart body is provided with SF6The gas cylinder bearing block.
Preferably, the bearing block is provided with SF6The gas cylinder is provided with a matched circular notch.
SF6The gas cylinder can be placed in the SF arranged at the bottom of the cart body6The gas cylinder is arranged on the bearing block and is embedded into the round notch on the bearing block, and SF6The gas cylinder can be embedded into the semicircular notch of the limiting block, and further SF (sulfur hexafluoride) is treated6And the gas cylinder is limited.
Preferably, the cart body is provided with a handrail.
Preferably, the bottom of the two sides of the cart body is provided with rollers.
Preferably, the absorber is filled with silver-loaded graphene/silica aerogel particles.
Preferably, the preparation of the silver-loaded graphene/silica aerogel particles comprises the following steps:
(1) dispersing graphene oxide in N, N-dimethylformamide, and performing ultrasonic dispersion for 0.5-1h to obtain a graphene oxide dispersion liquid;
(2) dissolving ethyl orthosilicate in deionized water, then adding 0.1mol/L hydrochloric acid solution and ethanol, and stirring for 1-2h at 50-80 ℃ to obtain silicon dioxide sol;
(3) adding the silica sol prepared in the step (2) into N, N-dimethylformamide, then adding ethylene glycol fatty acid ester, sorbitan laurate and propylene glycol, stirring at 40-70 ℃ for 0.5-1h, uniformly mixing, adding the graphene oxide dispersion liquid prepared in the step (1), ultrasonically dispersing for 0.5-1h, adding 10-20 wt% of ammonia water until the pH value is 7-8, and stirring for 10-30min to obtain graphene oxide/silica gel particles;
(4) placing the graphene oxide/silicon dioxide gel particles in an aging solution, aging for 20-30h at 50-90 ℃, and then soaking the particles in acetone for solvent replacement;
(5) placing the aged graphene oxide/silicon dioxide aerogel particles subjected to solvent replacement in a reaction kettle, continuously introducing carbon dioxide until the pressure reaches 8-14Mpa, extracting at 40-60 ℃ for 10-15h, and cooling to room temperature to obtain graphene oxide/silicon dioxide aerogel particles;
(6) slowly dropping 5-10 wt% of ammonia water into the silver nitrate solution until the generated black precipitate completely disappears to prepare a silver-ammonia solution;
(7) immersing the graphene oxide/silicon dioxide aerogel particles in a silver-ammonia solution, uniformly stirring, reacting for 15-20h under an oil bath at the temperature of 150-180 ℃, then cooling at room temperature, washing with deionized water, and drying for 12-24h at the temperature of 60-80 ℃ to obtain the silver-loaded graphene/silicon dioxide aerogel particles.
The silicon dioxide aerogel is a light porous material with a 3D network structure, has high surface area, large pore volume and narrow pore size distribution, takes silicon dioxide aerogel particles as a carrier, is compounded with graphene oxide while preparing the silicon dioxide aerogel, and finally endows the material with SF by attaching silver6Strong adsorption capacity of gas decomposition products. In the preparation process, firstly, ethyl orthosilicate is dissolved in water and is mixed with ethanol and hydrochloric acid to obtain silicon dioxide solThe silicon oxide sol is a colloidal solution formed by that nanometer silicon dioxide particles exist in water through single spheres or a plurality of aggregates, the silicon dioxide particles are connected together through silicon-oxygen bonds, in addition, a large number of hydroxyl groups exist on the surface, when the silicon dioxide sol is placed in N, N-dimethylformamide and mixed with a graphene oxide dispersion liquid, active groups such as hydroxyl groups, carboxyl groups and the like on the surface of graphene oxide form hydrogen bonds with the hydroxyl groups on the surface of silicon dioxide, so that graphene oxide is adsorbed on the surface of silicon dioxide, the silicon dioxide sol is stirred in the presence of glycol fatty acid ester, sorbitan laurate and propylene glycol to form liquid drops in an organic solvent, then ammonia water is added, the ammonia water surrounds the surface of the liquid drops of the silicon dioxide sol and is diffused into the interior, and the silicon dioxide sol is polymerized to form gel, and obtaining graphene oxide/silicon dioxide aerogel particles, wherein the graphene oxide can be well dispersed in the silicon dioxide gel, then the graphene oxide/silicon dioxide aerogel particles are placed in an aging solution for aging, soaked in an acetone solution, and the raw materials which are not completely reacted are replaced, and then the graphene oxide/silicon dioxide aerogel particles are placed in a carbon dioxide environment and dried under specific conditions to obtain the graphene oxide/silicon dioxide aerogel particles.
After the graphene oxide/silicon dioxide aerogel particles are prepared, in order to enable the graphene oxide in the graphene oxide/silicon dioxide aerogel particles to successfully carry silver, ammonia water is used for reducing silver nitrate and graphene oxide, however, two steps are needed for respectively reducing the silver nitrate and the graphene oxide by using the ammonia water, the process is complex, and when the method is used, after silver ions in the silver nitrate are reduced to elemental silver, the carrying amount of the elemental silver on the graphene is small and the carrying amount is not uniform, therefore, firstly, the ammonia water is slowly dripped into the silver nitrate solution to prepare a silver ammonia solution, then, the silver ammonia solution is used for reacting with the graphene oxide, the silver nitrate and the graphene oxide are reduced at the same time, silver is carried on the reduced graphene oxide, and the silver-carried graphene/silicon dioxide aerogel particles are prepared.
Silver-loaded graphene/silica aerogel particle pair SF6The decomposed products of the gas have a strong adsorption effect,this is due to the silver loaded graphene surface and SOF2、SO2F2And SO2Equal SF6There is a strong interaction between the molecules of the decomposition gas, in which SO2F2The gas molecules are cracked when interacting with the surface of the silver-loaded graphene, and simultaneously, the cracked atoms are combined into SO2Gas molecules, and SO2The sulfur-oxygen bond of the gas molecule is broken in a stretching way in the interaction, and forms a silver-sulfur bond and a silver-oxygen bond with the silver on the surface of the graphene; SOF2The gas molecules are also broken when interacting with the surface of the silver-loaded graphene, fluorine atoms and silver atoms form a new silver-fluorine bond, and sulfur atoms and silver also form a new silver-sulfur bond, so that adsorption is realized.
Preferably, the concentration of the graphene oxide in the graphene oxide dispersion liquid in the step (1) is 10-20mg/100 ml.
Preferably, the mass ratio of the ethyl orthosilicate to the ethanol in the step (2) is 4-5: 1.
Preferably, the mass ratio of the glycol fatty acid ester to the sorbitan laurate in the step (3) is 1-3: 1.
The inventor conducts experiments, and finds that the mixed surfactant is more beneficial to the stability of the emulsion, when the mixed surfactant is used, when a new interface is formed in the emulsion, the speed of providing emulsifier molecules for the interface is higher than that of using a single emulsifier, and the mass ratio of the glycol fatty acid ester and the sorbitan laurate is within the proportion, so that the mixed emulsifier has a more proper hydrophilic-lipophilic balance value, and the excessive or insufficient hydrophilic-lipophilic balance value is not beneficial to the stability of the emulsion.
Preferably, the aging solution in the step (4) is a mixed solution of tetraethoxysilane and ethanol, and the mass ratio of tetraethoxysilane to ethanol is 1-9: 3.
Therefore, the invention has the following beneficial effects: (1) mixing SF6The gas cylinder vacuumizing system and the constant-pressure inflating system are integrated on the trolley, so that the trolley is convenient to operate and carry; (2) can monitor the pressure of the electrical equipment in real time during inflation, and operate the switch of the electromagnetic valve to realize real-time monitoringThe inflation pressure is accurately controlled; (3) the buffer gas storage tank can be used for buffering gas, prevents the gas flow velocity in the charging electrical equipment from being too large and causing damage to the electrical equipment (4), and an absorber loaded with silver-loaded graphene/silicon dioxide aerogel particles is arranged at the gas outlet of the vacuum pump and can absorb SF6Gas decomposed SOF2、SO2F2And SO2And the like, and protects the environment and the health of operators.
Drawings
Fig. 1 is a front view of the structure of the present invention.
Fig. 2 is a schematic diagram of the structural principle of the present invention.
Figure 3 is a side view of the structure of the present invention.
Fig. 4 is a schematic structural diagram of the limiting block of the present invention.
Fig. 5 is a schematic view of the bearing block structure of the present invention.
In the figure: shallow body 1, controller 2, bearing platform 3, stopper 4, semicircle breach 5, bearing block 9, circular notch 10, handrail 11, gyro wheel 12, air inlet 13, gas outlet 14, SF6The device comprises a gas cylinder 21, a gas storage buffer tank 22, a vacuum pump 23, a vacuum meter 24, an absorber 25, a first stop valve V1, a second stop valve V2, a third stop valve V3, a pressure reducing valve PV1, an electromagnetic valve SV1, a first pressure sensor G1, a second pressure sensor G2 and a filter F1.
Detailed Description
The invention is further described with reference to the following detailed description and accompanying drawings.
Example 1: as shown in FIGS. 1-5, an SF6Full-automatic evacuation inflation cart, including cart body 1, vacuum pumping system and level pressure inflation system, the cart body includes controller 2 and bearing platform 3, and the upper portion of cart body 1 is equipped with SF6A gas cylinder limiting block 4, the bottom of which is provided with SF6The gas cylinder bearing block 9 is provided with a SF (sulfur hexafluoride) gas cylinder on the bearing block 96A circular notch 10 matched with the shape of the gas cylinder, handrails 11 arranged on the cart body, rollers 12 arranged at the bottoms of the two sides of the cart body, and a constant pressure inflation system comprising SF6Gas cylinder 21, three stop valves, filter F1 and twoThe pressure sensors, the pressure reducing valve PV1, the electromagnetic valve SV1 and the gas storage buffer tank 22 are communicated with each other by pipelines, wherein three stop valves are a first stop valve V1, a second stop valve V2 and a third stop valve V3 respectively, and two pressure sensors are a first pressure sensor G1 and a second pressure sensor G2 respectively6The gas cylinder is connected with a pipeline gas inlet 13, a first stop valve V1 is arranged at the end of the gas inlet 13, one end of a first pressure sensor G1 is connected with a first stop valve V1, the other end of the first pressure sensor G1 is connected with a filter F1, a pipeline at the other end of the filter F1 penetrates through the controller 2 and is connected with a pressure reducing valve PV1 on the controller 2, the pipeline penetrates through the controller 2 and then is divided into two parts, one of the two parts is sequentially connected with an electromagnetic valve SV1, a gas storage buffer tank 22, a second pressure sensor G2 and a second stop valve V2, the other end of the second stop valve V2 is connected with a gas outlet 14, the other pipeline is connected with a vacuum pumping system and sequentially comprises a third stop valve V3, a vacuum meter 24, a vacuum pump 23 and an absorber 25, the absorber 25 is loaded with silver loaded graphene/silicon dioxide aerogel particles, the gas outlet of the vacuum pump 23 is connected with the absorber 25 and is communicated with, the controller 2 is electrically connected with the first stop valve V1, the second stop valve V2, the third stop valve V3, the solenoid valve SV1, the first pressure sensor G1, the second pressure sensor G2 and the vacuum pump 23, and is used for controlling the on and off of the vacuumizing or inflation state.
When the electrical equipment is maintained or inflated, the method is divided into two steps of vacuumizing and constant-pressure inflating, and SF is firstly pumped before vacuumizing6The gas cylinder 21 is embedded into the circular notch 10 of the bearing block 9, is arranged in the semicircular notch 5 of the limiting block 4, and is screwed out of the first rotating semicircle 6 and the second rotating semicircle 7 to enable the SF to be sprayed into the first rotating semicircle 76The gas cylinder 21 is limited and then SF is added6The gas cylinder 21 is connected to the gas inlet 13, where SF is supplied6The gas bottle 21 is still in a closed state, the electrical equipment is connected with the gas outlet 14, then the first stop valve V1, the second stop valve V2, the third stop valve V3 and the solenoid valve SV1 are opened through the controller, and the vacuum pump 23 starts to operate and vacuumize, at the same time, the vacuum pump 23 pumps residual gas in the vacuum system and the inflation system pipeline and gas in the electrical equipmentCompletely pumping out the silver loaded graphene/silicon dioxide aerogel particles loaded by the absorber 25, and then leading the silver loaded graphene/silicon dioxide aerogel particles to the atmosphere, wherein when the vacuum gauge 24 on the vacuum pump 23 reaches a set vacuum degree, the vacuum pump 23 automatically stops running, the third stop valve V3 is closed, and at the moment, SF is opened6After the gas cylinder 21, SF6The gas is flushed into the electrical equipment through a pipeline of a constant-pressure inflation system, the pressure reducing valve PV1 can be adjusted to adjust the pressure of the inlet gas at the moment, the first pressure sensor G1 and the second pressure sensor G2 respectively monitor the pressure of the pipelines of the gas inlet 13 and the gas outlet 14 while inflating, the electromagnetic valve SV1 is automatically closed to stop inflating after the pressure of the first pressure sensor G1 reaches a set value, and after the pressure in the pipeline is stable, because the first pressure sensor G1 is closer to SF than the pipeline where the second pressure sensor G2 is located during inflating6The gas cylinder 21, therefore, when the first pressure sensor G1 reaches the set pressure during charging, after the solenoid valve SV1 is closed, and when the pressure of the electrical equipment is stable, that is, the pressure at the gas outlet 14 is stable, the pressure of the second pressure sensor G2 is necessarily slightly lower than the set pressure, at this time, the controller automatically controls the on-off of the solenoid valve, and slowly charges the pressure of the electrical equipment to the set pressure, that is, after the pressure at the second pressure sensor G2 reaches the set value, all the valves are closed, and the whole charging process is completed.
The preparation of the silver-loaded graphene/silica aerogel particles comprises the following steps:
(1) dispersing graphene oxide in N, N-dimethylformamide, and ultrasonically dispersing for 0.5h to obtain a graphene oxide dispersion liquid with the graphene oxide concentration of 10mg/100 ml;
(2) dissolving 40g of tetraethoxysilane in 100g of deionized water, then adding 3.8g of 0.1mol/L hydrochloric acid solution and 10g of ethanol, and stirring for 2 hours at 50 ℃ to obtain silicon dioxide sol;
(3) adding 50g of the silica sol prepared in the step (2) into 150g of N, N-dimethylformamide, then adding 0.45g of ethylene glycol fatty acid ester, 0.45g of sorbitan laurate and 0.3g of propylene glycol, stirring for 1h at 40 ℃, uniformly mixing, adding 25ml of the graphene oxide dispersion liquid prepared in the step (1), ultrasonically dispersing for 0.5h, adding 10wt% of ammonia water until the pH value is 7, and stirring for 10min to obtain graphene oxide/silica gel particles;
(4) placing the graphene oxide/silicon dioxide gel particles in a mixed solution of 50g of ethyl orthosilicate and 10g of ethanol, aging at 90 ℃ for 20h, and then soaking the particles in acetone for solvent replacement;
(5) placing the aged graphene oxide/silicon dioxide aerogel particles subjected to solvent replacement in a reaction kettle, continuously introducing carbon dioxide until the pressure reaches 8Mpa, extracting at 60 ℃ for 10 hours, and cooling to room temperature to obtain graphene oxide/silicon dioxide aerogel particles;
(6) slowly dropping 5 wt% of ammonia water into 2 wt% of silver nitrate solution until the generated black precipitate completely disappears to prepare silver ammonia solution;
(7) immersing the graphene oxide/silicon dioxide aerogel particles into a silver ammonia solution, uniformly stirring, reacting for 15h under an oil bath at 180 ℃, then cooling at room temperature, washing with deionized water, and drying at 70 ℃ for 18h to obtain the silver-loaded graphene/silicon dioxide aerogel particles.
Example 2: the difference from example 1 is that the preparation of the silver-loaded graphene/silica aerogel particles comprises the following steps:
(1) dispersing graphene oxide in N, N-dimethylformamide, and ultrasonically dispersing for 0.7h to obtain a graphene oxide dispersion liquid with the graphene oxide concentration of 15mg/100 ml;
(2) dissolving 45g of tetraethoxysilane in 100g of deionized water, then adding 4.3g of 0.1mol/L hydrochloric acid solution and 10g of ethanol, and stirring at 70 ℃ for 1.5h to obtain silicon dioxide sol;
(3) adding 70g of the silica sol prepared in the step (2) into 190g of N, N-dimethylformamide, then adding 0.9g of ethylene glycol fatty acid ester, 0.3g of sorbitan laurate and 0.4g of propylene glycol, stirring at 50 ℃ for 0.8h, uniformly mixing, adding 30ml of the graphene oxide dispersion liquid prepared in the step (1), ultrasonically dispersing for 1h, adding 20wt% of ammonia water until the pH value is 8, and stirring for 30min to obtain graphene oxide/silica gel particles;
(4) placing the graphene oxide/silicon dioxide gel particles in a mixed solution of 40g of tetraethoxysilane and 10g of ethanol, aging at 50 ℃ for 20-30h, and then soaking the particles in acetone for solvent replacement;
(5) placing the aged graphene oxide/silicon dioxide aerogel particles subjected to solvent replacement in a reaction kettle, continuously introducing carbon dioxide until the pressure reaches 14Mpa, extracting at 40 ℃ for 13 hours, and cooling to room temperature to obtain graphene oxide/silicon dioxide aerogel particles;
(6) slowly dropping 7 wt% of ammonia water into 2 wt% of silver nitrate solution until the generated black precipitate completely disappears to prepare silver ammonia solution;
(7) immersing the graphene oxide/silicon dioxide aerogel particles into a silver ammonia solution, uniformly stirring, reacting for 20h under an oil bath at 150 ℃, then cooling at room temperature, washing with deionized water, and drying at 80 ℃ for 12h to obtain the silver-loaded graphene/silicon dioxide aerogel particles.
Example 3: the difference from example 1 is that the preparation of the silver-loaded graphene/silica aerogel particles comprises the following steps:
(1) dispersing graphene oxide in N, N-dimethylformamide, and ultrasonically dispersing for 1h to obtain a graphene oxide dispersion liquid with the graphene oxide concentration of 20mg/100 ml;
(2) dissolving 50g of tetraethoxysilane in 100g of deionized water, then adding 4.8g of 0.1mol/L hydrochloric acid solution and 10g of ethanol, and stirring for 1h at 80 ℃ to obtain silicon dioxide sol;
(3) adding 60g of the silica sol prepared in the step (2) into 170g of N, N-dimethylformamide, then adding 0.9g of ethylene glycol fatty acid ester, 0.5g of sorbitan laurate and 0.36g of propylene glycol, stirring at 70 ℃ for 0.5h, uniformly mixing, adding 28ml of the graphene oxide dispersion liquid prepared in the step (1), ultrasonically dispersing for 0.7h, adding 15 wt% of ammonia water until the pH value is 7.5, and stirring for 20min to obtain graphene oxide/silica gel particles;
(4) placing the graphene oxide/silicon dioxide gel particles in a mixed solution of 45g of tetraethoxysilane and 10g of ethanol, aging at 70 ℃ for 25h, and then soaking the particles in acetone for solvent replacement;
(5) placing the aged graphene oxide/silicon dioxide aerogel particles subjected to solvent replacement in a reaction kettle, continuously introducing carbon dioxide until the pressure reaches 12Mpa, extracting at 50 ℃ for 15 hours, and cooling to room temperature to obtain graphene oxide/silicon dioxide aerogel particles;
(6) slowly dropping 10wt% of ammonia water into 2 wt% of silver nitrate solution until the generated black precipitate completely disappears to prepare silver ammonia solution;
(7) immersing the graphene oxide/silicon dioxide aerogel particles into a silver ammonia solution, uniformly stirring, reacting for 18h under an oil bath at 170 ℃, then cooling at room temperature, washing with deionized water, and drying at 60 ℃ for 24h to obtain the silver-loaded graphene/silicon dioxide aerogel particles.
Comparative example 1: the difference from example 1 is that the addition amounts of the ethylene glycol fatty acid ester and sorbitan laurate are 0.3g and 0.6g, respectively, i.e., the mass ratio of the addition amounts of the ethylene glycol fatty acid ester and sorbitan laurate is 0.5: 1.
Comparative example 2: the difference from example 1 is that the addition amounts of the ethylene glycol fatty acid ester and the sorbitan laurate are 0.7g and 0.2g, respectively, i.e., the mass ratio of the addition amounts of the ethylene glycol fatty acid ester and the sorbitan laurate is 3.5: 1.
Comparative example 3: the difference from example 1 is that the graphene oxide/silica aerogel particles were not loaded with silver particles.
The adsorbing materials prepared in example 1 and different comparative examples are respectively placed in SOF at normal temperature2、SO2F2、SO2And nitrogen, wherein SOF2、SO2F2And SO2The volume of the three gas molecules was 10% of the volume of the mixed gas, and after 1 hour of adsorption, the data obtained are shown in the following table.
Figure BDA0001918263140000091
As can be seen from the data in the above table, when the mass ratio of the ethylene glycol fatty acid ester to the sorbitan laurate is too large or too small, the emulsion is easily unstable, and the particle size and porosity of the graphene oxide/silica gel particles are controlled, so that the subsequent silver loading is affected, and the final adsorption capacity is reduced in comparative example 1 and comparative examples 1 and 2.
Comparing example 1 with comparative example 3, it is understood that SF can be greatly increased after silver is loaded6Adsorption of the gas decomposition products.

Claims (8)

1. SF (sulfur hexafluoride)6Full-automatic evacuation inflation cart, its characterized in that, including cart body, evacuation system and level pressure inflation system, the cart body includes controller and bearing platform, level pressure inflation system includes SF6The gas cylinder, the first stop valve, the second stop valve, the third stop valve, the filter, the pressure sensor, the pressure reducing valve, the electromagnetic valve and the gas storage buffer tank are communicated with each other by using pipelines, and the SF is6The vacuum pumping system comprises a vacuum pump, a vacuum meter and a third stop valve, one end of the third stop valve is connected with a pipeline of an inflation system, one end of the third stop valve is connected with the vacuum meter, the other end of the vacuum meter is connected with the vacuum pump, the air outlet end of the vacuum pump is provided with an absorber, the vacuum pump and the air storage buffer tank are arranged on a bearing platform, and the controller is in circuit connection with the stop valve, the electromagnetic valve, the pressure sensor and the vacuum pump and is used for controlling the on-off of the vacuumizing or inflation state;
silver-loaded graphene/silicon dioxide aerogel particles are filled in the absorber;
the preparation method of the silver-loaded graphene/silicon dioxide aerogel particles comprises the following preparation steps:
(1) dispersing graphene oxide in N, N-dimethylformamide, and performing ultrasonic dispersion for 0.5-1h to obtain a graphene oxide dispersion liquid;
(2) dissolving ethyl orthosilicate in deionized water, then adding 0.1mol/L hydrochloric acid solution and ethanol, and stirring for 1-2h at 50-80 ℃ to obtain silicon dioxide sol;
(3) adding the silica sol prepared in the step (2) into N, N-dimethylformamide, then adding ethylene glycol fatty acid ester, sorbitan laurate and propylene glycol, stirring at 40-70 ℃ for 0.5-1h, uniformly mixing, adding the graphene oxide dispersion liquid prepared in the step (1), ultrasonically dispersing for 0.5-1h, adding 10-20 wt% of ammonia water until the pH value is 7-8, and stirring for 10-30min to obtain graphene oxide/silica gel particles;
(4) placing the graphene oxide/silicon dioxide gel particles in an aging solution, aging for 20-30h at 50-90 ℃, and then soaking the particles in acetone for solvent replacement;
(5) placing the aged graphene oxide/silicon dioxide aerogel particles subjected to solvent replacement in a reaction kettle, continuously introducing carbon dioxide until the pressure reaches 8-14Mpa, extracting at 40-60 ℃ for 10-15h, and cooling to room temperature to obtain graphene oxide/silicon dioxide aerogel particles;
(6) slowly dropping 5-10 wt% of ammonia water into the silver nitrate solution until the generated black precipitate completely disappears to prepare a silver-ammonia solution;
(7) immersing the graphene oxide/silicon dioxide aerogel particles in a silver-ammonia solution, uniformly stirring, reacting for 15-20h under an oil bath at the temperature of 150-180 ℃, then cooling at room temperature, washing with deionized water, and drying for 12-24h at the temperature of 60-80 ℃ to obtain the silver-loaded graphene/silicon dioxide aerogel particles.
2. SF according to claim 16The full-automatic vacuumizing inflation cart is characterized in that the pressure reducing valve is arranged on the controller.
3. An SF according to claim 1 or 26A full-automatic vacuum-pumping and air-inflating cart is characterized in thatWherein the upper part of the cart body is provided with SF6The gas cylinder limiting block is provided with a gas cylinder and SF6The gas cylinder is a semicircular notch matched with the gas cylinder in shape.
4. An SF according to claim 36Full-automatic evacuation inflation cart, which is characterized in that the bottom of the cart body is provided with SF6The gas cylinder bearing block.
5. An SF according to claim 46The full-automatic vacuum-pumping and air-inflating trolley is characterized in that the bearing block is provided with an SF (sulfur hexafluoride) gas-filled tube6The gas cylinder is provided with a matched circular notch.
6. An SF according to claim 1 or 26The full-automatic vacuumizing inflation trolley is characterized in that a handrail is arranged on the trolley body.
7. An SF according to claim 1 or 26The full-automatic vacuumizing and inflating trolley is characterized in that rollers are arranged at the bottoms of two sides of the trolley body.
8. The fully automatic vacuum pumping and inflation cart of SF6, of claim 1, wherein said glycol fatty acid ester and sorbitan laurate are present in step (3) in a mass ratio of 1-3: 1.
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