CN114210274A - Sulfur trioxide gas generating device with determined concentration and generating method thereof - Google Patents

Sulfur trioxide gas generating device with determined concentration and generating method thereof Download PDF

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CN114210274A
CN114210274A CN202111449968.9A CN202111449968A CN114210274A CN 114210274 A CN114210274 A CN 114210274A CN 202111449968 A CN202111449968 A CN 202111449968A CN 114210274 A CN114210274 A CN 114210274A
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gas
fluidized bed
concentration
sulfur trioxide
inlet pipe
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鄢烈祥
王辉
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Shandong Baiyou Intelligent Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1809—Controlling processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1818—Feeding of the fluidising gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1836—Heating and cooling the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1872—Details of the fluidised bed reactor
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/69—Sulfur trioxide; Sulfuric acid
    • C01B17/74—Preparation
    • C01B17/76—Preparation by contact processes
    • C01B17/77—Fluidised-bed processes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/69—Sulfur trioxide; Sulfuric acid
    • C01B17/74—Preparation
    • C01B17/76—Preparation by contact processes
    • C01B17/80—Apparatus

Abstract

The invention discloses a sulfur trioxide gas generating device with determined concentration, which comprises a reactor shell and SO2The device comprises a gas supply device, an oxidant gas supply device, a gas valve, a first gas flowmeter, a second gas flowmeter, a first gas inlet pipe, a second gas inlet pipe, a gas distribution plate, a catalyst particle bed layer, a gas-solid separation device, a heating furnace, a diluent gas pipeline and a generated gas pipeline; the first air inlet pipe and the second air inlet pipe are vertically arranged in parallel, the upper ends of the first air inlet pipe and the second air inlet pipe are communicated and then are introduced into a reactor shell positioned in the heating furnace, and the gas-solid separation device is arranged above the catalyst particle bed layer; the generated gas pipeline is communicated with the upper end of the reactor shell for dilutionThe gas pipeline is communicated with the generated gas pipeline; the fluidized bed reactor of the device is vertically arranged; a corresponding generation method is also disclosed; ensures that the sulfur trioxide generation reaction can reach an equilibrium state at a higher speed, and improves the generation precision of sulfur trioxide gas.

Description

Sulfur trioxide gas generating device with determined concentration and generating method thereof
Technical Field
The invention belongs to the field of gas generation, and particularly relates to a sulfur trioxide gas generation device with a determined concentration and a generation method thereof.
Background
As the sulfide contained in fossil fuel (coal, petroleum and the like) is converted into sulfur dioxide (SO) in the combustion process2) A gas. Part of SO2The gas is further oxidized and converted into sulfur trioxide (SO) along with the reduction of the temperature of the tail flue and under the action of catalysts such as metal oxide, fly ash and SCR denitration catalyst on the pipe wall3) A gas. SO (SO)3The gas has active chemical reaction property and strong hydrophilicity, and can react with water vapor (H) in the smoke2O) to sulfuric acid (H)2SO4) Not only aggravate the corrosion of the tail flue, but also the ammonia (NH) escaping after the denitration reaction3) Combine to form viscous solid ammonium bisulfate (NH)4HSO4) Resulting in blockage of the air preheater and the tail flue. The sulfuric acid in the flue gas has low dew point temperature, is easy to condense to form submicron particles after entering a wet desulphurization device, and is difficult to be absorbed by the desulphurization serous fluid, so that the flue gas is discharged into the atmosphere to cause serious pollution. SO as to accurately measure SO in the flue gas3The concentration of the gas is very important, which is not only beneficial to SO in the flue gas3Implementation of desorption techniques, detecting SO3And for accurately evaluating SO of the SCR catalyst2To SO3The conversion index is of great significance, and the SO is reduced as much as possible for optimizing the formula of the catalyst3Provides guidance for generation of (1).
SO in common flue gas3The gas detection method comprises the control condensation method and the like described in the American ASTM D3226-73T standard and the Chinese national standard GB/T21508. No matter what SO is used3Gas detection apparatus, all require SO of determined concentration3The gas assists in measurement calibration and accuracy verification of the detection device. Due to SO3The stable SO is difficult to buy under the room temperature condition due to the active chemical property and easily-condensed substance3The gas source generally needs to generate SO with determined concentration in real time through an experimental generation method3A gas. Common methods include the ozone method [1 ]]Sulfuric acid heating method [2]Carrying with nitrogen [3]And the like. But all have SO3The control precision of the gas concentration is not high.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to solve the problem of the sulfur trioxide gas generation device SO of the prior art3The control precision of the gas concentration is not high, and the speed of the catalytic reaction is slow.
To achieve the above object, the present invention relates to: a sulfur trioxide gas generating device with determined concentration comprises a reactor shell and SO2The device comprises a gas supply device, an oxidant gas supply device, a gas valve, a first gas flowmeter, a second gas flowmeter, a first gas inlet pipe, a second gas inlet pipe, a gas distribution plate, a catalyst particle bed layer, a gas-solid separation device, a heating furnace, a diluent gas pipeline and a generated gas pipeline;
the first air inlet pipe and the second air inlet pipe are vertically arranged in parallel, the upper ends of the first air inlet pipe and the second air inlet pipe are communicated and then are introduced into a reactor shell positioned in the heating furnace, the gas distribution plate is arranged at the middle lower part of the reactor shell, the catalyst particle bed layer is arranged on the upper end surface of the gas distribution plate, and the gas-solid separation device is arranged above the catalyst particle bed layer; the generated gas pipeline is communicated with the upper end of the reactor shell, and the diluent gas pipeline is communicated with the generated gas pipeline;
SO2the gas supply device can supply SO with known concentration2The gas valve and the first gas flowmeter are used for controlling and controlling the gas flow entering the first gas inlet pipe; the gas valve and the second gas flowmeter are used for controlling the flow of gas entering the second gas inlet pipe; the heating furnace is used for heating the shell of the fluidized bed reactor and the diluent gas pipeline to ensure that the temperature in the reaction section of the fluidized bed is suitable for SO2The gas reacts with oxygen to form SO3Gas, and ensuring temperature of released gas and reaction to form SO3The gas temperature is close to avoid SO3Condensing the gas; a gas generation pipeline for generating SO3Gas discharge, dilution gas pipeline conveying dilution gas, dilution gas and SO3Mixing the gases to obtain SO with the required determined concentration3A gas.
Further, the active substance of the catalyst particle bed layer comprises one or a mixture of several of compounds such as vanadium pentoxide and ferric oxide.
Further, the temperature in the fluidized bed reaction section is 150-400 ℃.
Further, the standard oxidant gas is air or pure oxygen.
Furthermore, the gas distribution plate is made of porous materials, and the pore diameter of the gas distribution plate is smaller than the particle diameter of the catalyst particle bed layer.
The invention also provides a generating method of the sulfur trioxide gas generating device with determined concentration, which comprises the following steps:
step 1: first the required SO is determined3Concentration n of gas0Sum flow rate V0；
Step 2: determining an operating parameter of the fluidized bed reactor;
and step 3: generating SO with determined concentration through sulfur trioxide gas generating device3A gas.
Further, the method for determining the operating parameters of the fluidized bed reactor comprises the following steps:
step (1) calculating according to formula 1 and formula 2 to obtain SO required by an outlet of the fluidized bed reactor3Concentration n of gas1Sum flow rate V1And the flow rate V of the dilution gas2；Gas flow V1Controlling the temperature to be 0.5-2L/min according to the process requirement of the fluidized bed reactor;
V0＝V1+V2 (1)。
n1＝n0·V0/V1 (2)。
step (2) according to reaction 1
Figure BDA0003385559730000031
The required stoichiometric equivalence ratio is calculated according to formula 3 to obtain SO at the inlet of the fluidized bed reactor2Gas concentration n3Sum flow rate V3；SO of inlet2Gas concentration n3Determined according to the standard gas concentration of the purchase, and n3≥n1；
To ensure SO2Is sufficiently oxidized, the concentration n of the oxidizing agent4Much greater SO2Gas concentration n3Therefore, the change of the molar amount of the oxidizing agent due to the reaction 1 is extremely small, and the gas flow rate V of the oxidizing agent4Calculating according to the formula 4;
when SO is in the inlet2The gas itself also contains a sufficient amount of O2And O is2Is far greater than SO2Concentration of (3), SO required for export3Concentration n of gas1Equal to SO of inlet2Gas concentration n3At the time of the gas flow rate V of the oxidizing agent4Zero can be taken; at this time V3＝V1，n3＝n1；
n3·V3＝n1·V1 (3)。
V4＝V1-V3 (4)。
According to the design requirement of the fluidized bed reactor, catalyst particles are selected as bed materials of the fluidized bed, and the initial bubbling speed of the catalyst particles is equal to the initial fluidizing speed, so that when the gas speed in the fluidized bed reaches the initial fluidizing speed, the bubbling phenomenon occurs in a bed layer, the gas-solid phase coupling is uniform, and the reaction rate and the conversion rate of the reaction 1 are improved;
the gas flow velocity in the fluidized bed in the step (4) is higher and is in a turbulent flow region, the kinetic energy loss is dominant, and the viscous loss is negligible, so the critical fluidization velocity umfThe calculation is according to equation 5;
Figure BDA0003385559730000041
wherein: dpIs the particle diameter, ppIs the catalyst particle density, pgIs the gas density, g is the acceleration of gravity;
step (5) calculating according to Geldart formula 6Minimum bubbling velocity u of fluidized bed material particlesmb；
Figure BDA0003385559730000042
Wherein: mu is the dynamic viscosity of the mixed gas in the fluidized bed;
step (6) calculating the terminal velocity u of the fluidized bed material particles according to the formula 7t；
Figure BDA0003385559730000051
In the step (7), a bubbling bed process is adopted in a fluidized bed reactor, bed material catalyst particles of the fluidized bed have medium granularity, the apparent density is 1100-4000kg/m3, and belong to typical B-type particles, and the initial bubbling speed of the particles is equal to the initial fluidizing speed, so that the bubbling phenomenon occurs in the bed layer after the gas velocity reaches the initial fluidizing speed; when a bubbling fluidized bed process is used, the gas flow rate u should be greater than the minimum bubbling velocity u of the particlesmbTherefore, the diameter D of the reaction section of the fluidized bed reactor is calculated according to the formula 8; the height H of the reaction section of the fluidized bed reactor is generally equal to 3-5 times of D;
Figure BDA0003385559730000052
further, if the fluidized bed reactor employs a circulating fluidized bed process, the gas flow rate u should be less than the terminal velocity u of the particlest，Calculating according to the formula 9 to obtain the diameter D of the reaction section of the fluidized bed reactor; taking the height H of the reaction section of the fluidized bed reactor as 3-5 times of the diameter D of the reaction section;
Figure BDA0003385559730000053
further, the particle size range of the catalyst particles in the step (3) is selected to be between 0.1 and 0.6 mm.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects:
(1) the invention relates to a sulfur trioxide gas generating device with determined concentration and a generating method thereof, wherein a fluidized bed reactor is used as a carrier of a catalyst and a place for sulfur trioxide generation reaction. The solid-phase coupling of gas in the fluidized bed reactor is violent, and the catalyst particles can be selected from fine particle solids with larger specific surface area, so that the generation reaction of sulfur trioxide can reach an equilibrium state at a higher speed, and the generation precision of sulfur trioxide gas is improved.
(2) According to the device and the method for generating the sulfur trioxide gas with the determined concentration, which are disclosed by the invention, the fluidized bed reactor is vertically arranged, catalyst particles can be uniformly distributed on the whole quartz sieve plate, gas escaping from the side wall is reduced, the introduced sulfur dioxide gas can be ensured to fully react on the surface of the catalyst particles, the concentration precision of the generated sulfur trioxide gas is consistent with that of the introduced sulfur dioxide gas (generally, purchased high-precision standard gas), and the generation precision of the sulfur trioxide gas is improved.
Drawings
FIG. 1 is a block diagram of a preferred embodiment of the invention (in the form of a bubbling fluidized bed);
FIG. 2 is a block diagram of another preferred embodiment of the present invention (in the form of a circulating fluidized bed);
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention is further illustrated with reference to the following figures and examples:
a sulfur trioxide gas generating device with determined concentration comprises a reactor shell 1 and SO2Gas (es)The device comprises a supply device 2, an oxidant gas supply device 3, a gas valve 4, a gas valve 5, a first gas flowmeter 6, a second gas flowmeter 7, a first gas inlet pipe 8, a second gas inlet pipe 9, a gas distribution plate 10, a catalyst particle bed layer 11, a gas-solid separation device 12, a heating furnace 13, a diluent gas pipeline 14 and a generated gas pipeline 15;
the first air inlet pipe 8 and the second air inlet pipe 9 are vertically arranged in parallel, the upper ends of the first air inlet pipe and the second air inlet pipe are communicated and then are introduced into a reactor shell 1 in a heating furnace 13, the gas distribution plate 10 is arranged at the middle lower part of the reactor shell 1, the gas distribution plate 10 is made of porous materials, the pore diameter of the gas distribution plate is smaller than the particle diameter of a catalyst particle bed layer, the catalyst particle bed layer 11 is arranged on the upper end face of the gas distribution plate 10, and the gas-solid separation device 12 is arranged above the catalyst particle bed layer 11; the device is used for separating gas and catalyst particles in the flue gas, and ensures that the generated SO3 gas does not contain the catalyst particles; the generated gas pipeline 15 is communicated with the upper end of the reactor shell 1, and the diluent gas pipeline 14 is communicated with the generated gas pipeline 15;
SO2the gas supply device 2 can supply SO with known concentration2The oxidant gas supply device 3 can supply oxidant standard gas with known concentration (the oxidant standard gas is air or pure oxygen), and the gas valve 4 and the first gas flowmeter 6 are used for controlling and controlling the gas flow entering the first gas inlet pipe 8; the gas valve 5 and the second gas flowmeter 7 are used for controlling the flow of gas entering the second gas inlet pipe 9; the furnace 13 is used to heat the fluidized bed reactor housing 1 and the diluent gas duct 14 to ensure that the temperature in the reaction zone of the fluidized bed is suitable for SO2The gas reacts with oxygen to form SO3Gas, and ensuring temperature of released gas and reaction to form SO3The gas temperature is close to avoid SO3Condensing the gas; a generated gas pipeline 15 for generating SO3The gas is discharged and the diluent gas pipe 14 delivers diluent gas, diluent gas and SO3Mixing the gases to obtain SO with the required determined concentration3A gas.
The active substance of the catalyst particle bed 11 comprises one or a mixture of several of compounds such as vanadium pentoxide and ferric oxide. After the gas is input into the gas distribution plate 10, the catalyst particles in the catalyst particle bed 11 are in a bubbling fluidization or fast fluidization motion state, and simultaneously, the reaction 1 occurs on the surfaces of the catalyst particles.
The temperature in the fluidized bed reaction section is 150-400 ℃, and the fluidized bed reaction section refers to a flowing area of catalyst particles between a gas distribution plate and a gas-solid separation device.
The generating method of the sulfur trioxide gas generating device with the determined concentration comprises the following steps:
step 1: first the required SO is determined3Concentration n of gas0Sum flow rate V0；
Step 2: determining an operating parameter of the fluidized bed reactor;
the method for determining the operating parameters of the fluidized bed reactor comprises the following steps:
step (1) calculating according to formula 1 and formula 2 to obtain SO required by an outlet of the fluidized bed reactor3Concentration n of gas1Sum flow rate V1And the flow rate V of the dilution gas2；Gas flow V1Controlling the temperature to be 0.5-2L/min according to the process requirement of the fluidized bed reactor;
V0＝V1+V2 (1)。
(V0 and n0 are described in step 1, for the required SO3Concentration n of gas0Sum flow rate V0)
n1＝n0·V0/V1 (2)。
Step (2) according to reaction 1
Figure BDA0003385559730000081
The required stoichiometric equivalence ratio is calculated according to formula 3 to obtain SO at the inlet of the fluidized bed reactor2Gas concentration n3Sum flow rate V3；SO of inlet2Gas concentration n3Determined according to the standard gas concentration of the purchase, and n3≥n1；
To ensure SO2Is sufficiently oxidized, the concentration n of the oxidizing agent4Much greater SO2Gas concentration n3Therefore, the change of the molar amount of the oxidizing agent due to the reaction 1 is extremely small, and the gas flow rate V of the oxidizing agent4Calculating according to the formula 4;
when SO is in the inlet2The gas itself also contains a sufficient amount of O2And O is2Is far greater than SO2Concentration of (3), SO required for export3Concentration n of gas1Equal to SO of inlet2Gas concentration n3At the time of the gas flow rate V of the oxidizing agent4Zero can be taken; at this time V3＝V1，n3＝n1；
n3·V3＝n1·V1 (3)。
V4＝V1-V3 (4)。
According to the design requirement of the fluidized bed reactor, selecting catalyst particles with the particle size range of 0.1-0.6mm as bed materials of the fluidized bed, wherein the initial bubbling speed of the catalyst particles is equal to the initial fluidizing speed, so that the bubbling phenomenon occurs in the bed layer when the gas speed in the fluidized bed reaches the initial fluidizing speed, the gas-solid phase coupling is uniform, and the reaction rate and the conversion rate of the reaction 1 are improved;
the gas flow velocity in the fluidized bed in the step (4) is higher and is in a turbulent flow region, the kinetic energy loss is dominant, and the viscous loss is negligible, so the critical fluidization velocity umfThe calculation is according to equation 5;
Figure BDA0003385559730000091
wherein: dpIs the particle diameter, ppIs the catalyst particle density, pgIs the gas density, g is the acceleration of gravity;
step (5) calculating the minimum bubbling speed u of fluidized bed material particles according to Geldart formula 6mb；
Figure BDA0003385559730000092
Wherein: mu is the dynamic viscosity of the mixed gas in the fluidized bed;
step (6) calculating the terminal velocity u of the fluidized bed material particles according to the formula 7t；
Figure BDA0003385559730000093
In the step (7), a bubbling bed process is adopted in a fluidized bed reactor, bed material catalyst particles of the fluidized bed have medium granularity, the apparent density is 1100-4000kg/m3, and belong to typical B-type particles, and the initial bubbling speed of the particles is equal to the initial fluidizing speed, so that the bubbling phenomenon occurs in the bed layer after the gas velocity reaches the initial fluidizing speed; when a bubbling fluidized bed process is used, the gas flow rate u should be greater than the minimum bubbling velocity u of the particlesmbTherefore, the diameter D of the reaction section of the fluidized bed reactor is calculated according to the formula 8; the height H of the reaction section of the fluidized bed reactor is generally equal to 3-5 times of D;
Figure BDA0003385559730000094
if the fluidized bed reactor is a circulating fluidized bed process, the gas flow rate u should be less than the terminal velocity u of the particlest，Calculating according to the formula 9 to obtain the diameter D of the reaction section of the fluidized bed reactor; taking the height H of the reaction section of the fluidized bed reactor as 3-5 times of the diameter D of the reaction section;
Figure BDA0003385559730000101
and step 3: generating SO with determined concentration through sulfur trioxide gas generating device3A gas.
In the following, with reference to the examples, flue gas having a sulfur trioxide gas concentration of 0.005% vol (i.e. 50ppm) and a flow rate of 1L/min was produced by the apparatus of the present invention.
Example 1
1) First, the SO of the desired gas is determined3Concentration n00.005% + -0.0001% (i.e. 50ppm + -1 ppm), flow rate V02L/min. The diluent gas is V21L/min of nitrogen.
2) The heating temperature of the heating furnace was determined to be 300 ℃.
3) The gas generated by the fluidized bed reactor is calculated according to the formula 1 and the formula 2: SO (SO)3Concentration n of gas00.01% and flow V1＝1L/min
4) Knowing the SO of the inlet based on the standard gas purchased2Gas concentration n30.02% (precision within + -0.0004%, i.e. + -. 4 ppm), O of the inlet oxidant2Concentration n4Calculated as 21% from equations 3 and 4 to obtain inlet SO2Gas flow of V30.5L/min, gas flow of inlet oxidant V4＝0.5L/min。
5) Selecting vanadium pentoxide particles with the average particle size of 0.3mm as a catalyst particle bed layer, and calculating according to formula 5 to obtain a critical fluidization velocity umf＝0.5m/s。
6) Calculating the minimum bubbling velocity u of fluidized bed material particles according to equation 6mb＝1.4m/s
7) Calculating the terminal velocity u of the fluidized bed material particles according to equation 7t＝6.3m/s
8) The diameter D of the reaction zone of the bubbling fluidized bed reactor is calculated according to the formula 8 and is less than 316mm, and D is 300mm, and H is 900 mm. The gas-solid separation device of the bubbling fluidized bed reactor can be made of porous medium materials.
9) The diameter D of the reaction zone of the circulating fluidized bed reactor is calculated according to the formula 9 and is more than 149mm, and D is 150mm, and H is 600 mm. The gas-solid separation device of the circulating fluidized bed reactor can be realized by adopting a cyclone separator.
10) The inlet SO is controlled by a gas valve 4 and a gas valve 52The gas flow is 0.5L/min, and the inlet is controlled by a gas valve 6 and a gas valve 7The flow rate of the oxidant gas was 0.5L/min.
11)SO2The gas and the oxidant react in the fluidized bed reactor to generate SO3Gas with concentration of 0.01% and flow rate of 1L/min. Mixing the generated gas with 1L/min nitrogen in a heating furnace to obtain the required determined SO3Concentration n00.0049%, gas flow of 2L/min, error sum not exceeding 2%.

Claims (9)

1. The device for generating the sulfur trioxide gas with determined concentration is characterized by comprising a reactor shell (1) and SO2The device comprises a gas supply device (2), an oxidant gas supply device (3), a gas valve (4), a gas valve (5), a first gas flowmeter (6), a second gas flowmeter (7), a first gas inlet pipe (8), a second gas inlet pipe (9), a gas distribution plate (10), a catalyst particle bed layer (11), a gas-solid separation device (12), a heating furnace (13), a diluent gas pipeline (14) and a generated gas pipeline (15);
the first air inlet pipe (8) and the second air inlet pipe (9) are vertically arranged in parallel, the upper ends of the first air inlet pipe and the second air inlet pipe are communicated and then are introduced into a reactor shell (1) in a heating furnace (13), the gas distribution plate (10) is arranged at the middle lower part of the reactor shell (1), the catalyst particle bed layer (11) is arranged on the upper end surface of the gas distribution plate (10), and the gas-solid separation device (12) is arranged above the catalyst particle bed layer (11); the generated gas pipeline (15) is communicated with the upper end of the reactor shell (1), and the diluent gas pipeline (14) is communicated with the generated gas pipeline (15);
SO2the gas supply device (2) can supply SO with known concentration2The standard gas, the oxidant gas supply device (3) can supply the oxidant standard gas with known concentration, and the gas valve (4) and the first gas flowmeter (6) are used for controlling and controlling the gas flow entering the first gas inlet pipe (8); the gas valve (5) and the second gas flowmeter (7) are used for controlling the flow of gas entering the second gas inlet pipe (9); the heating furnace 13 is used for heating the fluidized bed reactor shell 1 and the diluent gas pipeline (14); a generated gas pipeline (15) is used for generating SO3The gas is discharged, and a diluent gas pipe (14) conveys diluent gas, diluent gas and SO3Mixing the gases to obtain SO with the required determined concentration3A gas.
2. The sulfur trioxide gas generation device of a determined concentration of claim 1, characterized in that: the active substance of the catalyst particle bed layer (11) comprises one or a mixture of more of compounds such as vanadium pentoxide, ferric oxide and the like.
3. The sulfur trioxide gas generation device of a determined concentration of claim 1, characterized in that: the temperature in the fluidized bed reaction section is 150-400 ℃.
4. The sulfur trioxide gas generation device of a determined concentration of claim 1, characterized in that: the oxidant standard gas is air or pure oxygen.
5. The sulfur trioxide gas generation device of a determined concentration of claim 1, characterized in that: the gas distribution plate (10) is made of porous materials, and the pore diameter of the gas distribution plate is smaller than the particle diameter of the catalyst particle bed layer.
6. The method for generating a determined concentration of sulfur trioxide gas generating apparatus according to claim 1, characterized in that: the method comprises the following steps:
step 1: first the required SO is determined3Concentration n of gas0Sum flow rate V0；
Step 2: determining an operating parameter of the fluidized bed reactor;
and step 3: generating SO with determined concentration through sulfur trioxide gas generating device3A gas.
7. The generation method of a sulfur trioxide gas generation device of a certain concentration according to claim 6, characterized in that: the method for determining the operating parameters of the fluidized bed reactor comprises the following steps:
step (1) calculating according to formula 1 and formula 2 to obtain the fluidized bed reactionSO required for the outlet of the reactor3Concentration n of gas1Sum flow rate V1And the flow rate V of the dilution gas2(ii) a Gas flow V1Controlling the temperature to be 0.5-2L/min according to the process requirement of the fluidized bed reactor;
V0＝V1+V2 (1)；
n1＝n0·V0/V1 (2)；
step (2) calculating according to the stoichiometric equivalence ratio required by the reaction 1 and the formula 3 to obtain SO at the inlet of the fluidized bed reactor2Gas concentration n3Sum flow rate V3(ii) a SO of inlet2Gas concentration n3Determined according to the standard gas concentration of the purchase, and n3≥n1；
To ensure SO2Is sufficiently oxidized, the concentration n of the oxidizing agent4Much greater SO2Gas concentration n3Therefore, the change of the molar amount of the oxidizing agent due to the reaction 1 is extremely small, and the gas flow rate V of the oxidizing agent4Calculating according to the formula 4;
when SO is in the inlet2The gas itself also contains a sufficient amount of O2And O is2Is far greater than SO2Concentration of (3), SO required for export3Concentration n of gas1Equal to SO of inlet2Gas concentration n3At the time of the gas flow rate V of the oxidizing agent4Zero can be taken; at this time V3＝V1，n3＝n1；
n3·V3＝n1·V1 (3)；
V4＝V1-V3 (4)；
According to the design requirement of the fluidized bed reactor, catalyst particles are selected as bed materials of the fluidized bed, and the initial bubbling speed of the catalyst particles is equal to the initial fluidizing speed, so that when the gas speed in the fluidized bed reaches the initial fluidizing speed, the bubbling phenomenon occurs in a bed layer, the gas-solid phase coupling is uniform, and the reaction rate and the conversion rate of the reaction 1 are improved;
the gas flow rate in the fluidized bed in the step (4) is higher,in the turbulent region, kinetic energy loss is dominant and viscous loss is negligible, so the critical fluidization velocity umfThe calculation is according to equation 5;
Figure FDA0003385559720000031
wherein: dpIs the particle diameter, ppIs the catalyst particle density, pgIs the gas density, g is the acceleration of gravity;
step (5) calculating the minimum bubbling speed u of fluidized bed material particles according to Geldart formula 6mb；
Figure FDA0003385559720000032
Wherein: mu is the dynamic viscosity of the mixed gas in the fluidized bed;
step (6) calculating the terminal velocity u of the fluidized bed material particles according to the formula 7t；
Figure FDA0003385559720000041
In the step (7), a bubbling bed process is adopted in a fluidized bed reactor, bed material catalyst particles of the fluidized bed have medium granularity, the apparent density is 1100-4000kg/m3, and belong to typical B-type particles, and the initial bubbling speed of the particles is equal to the initial fluidizing speed, so that the bubbling phenomenon occurs in the bed layer after the gas velocity reaches the initial fluidizing speed; when a bubbling fluidized bed process is used, the gas flow rate u should be greater than the minimum bubbling velocity u of the particlesmbTherefore, the diameter D of the reaction section of the fluidized bed reactor is calculated according to the formula 8; the height H of the reaction section of the fluidized bed reactor is generally equal to 3-5 times of D;
Figure FDA0003385559720000042
8. the generation method of a determined concentration of sulfur trioxide gas generation means according to claim 7, characterized in that: if the fluidized bed reactor is a circulating fluidized bed process, the gas flow rate u should be less than the terminal velocity u of the particlest，Calculating according to the formula 9 to obtain the diameter D of the reaction section of the fluidized bed reactor; taking the height H of the reaction section of the fluidized bed reactor as 3-5 times of the diameter D of the reaction section;
Figure FDA0003385559720000043
9. the generation method of a determined concentration of sulfur trioxide gas generation means according to claim 7, characterized in that: the particle size range of the catalyst particles in the step (3) is selected to be between 0.1 and 0.6 mm.
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Publication number Priority date Publication date Assignee Title
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