WO2025007635A1 - 一种氨吸收效果改善的腈的制造方法 - Google Patents

一种氨吸收效果改善的腈的制造方法 Download PDF

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Publication number
WO2025007635A1
WO2025007635A1 PCT/CN2024/091569 CN2024091569W WO2025007635A1 WO 2025007635 A1 WO2025007635 A1 WO 2025007635A1 CN 2024091569 W CN2024091569 W CN 2024091569W WO 2025007635 A1 WO2025007635 A1 WO 2025007635A1
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Prior art keywords
spray
microns
spraying
gas
liquid
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PCT/CN2024/091569
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English (en)
French (fr)
Inventor
赵乐
吴粮华
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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Priority claimed from CN202310819780.1A external-priority patent/CN119259292A/zh
Priority claimed from CN202310819805.8A external-priority patent/CN119258755A/zh
Priority claimed from CN202310819830.6A external-priority patent/CN119258756A/zh
Priority claimed from CN202310819832.5A external-priority patent/CN119258757A/zh
Application filed by China Petroleum and Chemical Corp, Sinopec Shanghai Research Institute of Petrochemical Technology filed Critical China Petroleum and Chemical Corp
Priority to KR1020267003868A priority Critical patent/KR20260033592A/ko
Publication of WO2025007635A1 publication Critical patent/WO2025007635A1/zh
Anticipated expiration legal-status Critical
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/54—Nitrogen compounds
    • B01D53/58—Ammonia
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/77—Liquid phase processes
    • B01D53/78—Liquid phase processes with gas-liquid contact

Definitions

  • the present invention relates to the technical field of gas absorption, and more particularly to a method for producing nitrile with improved ammonia absorption effect.
  • the raw gas ammonia is generally excessive, that is, the molar ratio of ammonia to the raw gas hydrocarbon is greater than 1, such as in the ammoxidation of propylene, the ammonia ratio (ammonia to propylene molar ratio) is 1.10-1.35, and in the ammoxidation of aromatic hydrocarbons, the ammonia ratio (ammonia to aromatic hydrocarbon molar ratio) is 4-8, therefore, the reactor outlet tail gas must contain unreacted ammonia.
  • Patent CN105425849 removes the remaining ammonia by adjusting the amount of added acid according to the pH value of the effluent from the absorber;
  • Patent CN1199940 improves the gas-liquid two-phase mass transfer and heat transfer effect by adding internal components at the bottom of the absorber, which is essentially to solve the problem of uniform distribution of the ammonia-containing gas phase.
  • ammonia penetration will inevitably occur in the absorber, that is, a small amount of ammonia will still escape, resulting in product loss or environmental pollution in the subsequent refining and separation units.
  • the ammonia content in the absorbed tail gas increases significantly compared with the initial stage of operation.
  • the spray liquid is pumped to the nozzle by a pump. Since the spray liquid has a very high pressure, the spray liquid enters the nozzle cavity from the tangential inlet and obtains a rotational motion. After passing through the nozzle with a special structure, the spray liquid is ejected from the nozzle at a high speed and split into countless small droplets. Most of the droplets are affected by their own gravity and the centrifugal force of the rotational motion and move to the bottom of the tower. These droplets are in reverse contact with the gas from the bottom up. At the same time, there are also a small number of droplets that will be entrained by the gas and move to the top of the tower.
  • the area of the spray device in the tower is filled with countless small droplets.
  • the droplets can produce strong attenuation for both visible light and infrared signals.
  • the extinction coefficient of the droplets in the tower By measuring the extinction coefficient of the droplets in the tower by infrared spectral radiation method or forward scattering method, the size, quantity, and distribution of the droplets can be comprehensively evaluated. Normally, the larger the droplets, the smaller the number of droplets, the smaller the light absorption, the higher the light transmittance, and the smaller the extinction coefficient, and vice versa.
  • the inventors of the present invention have found that this problem can be solved by setting the extinction coefficient of the absorbing atmosphere within a specific numerical range.
  • the present invention has been completed based on this finding.
  • the present invention relates to the following aspects.
  • a method for producing a nitrile comprising the steps of causing ammoxidation of a hydrocarbon feedstock to produce a reaction product containing nitrile (referred to as a reaction step), and introducing the reaction product into an absorber through a gas inlet and spraying a spray liquid on the reaction product in the absorber through a spray device to cool the reaction product and form an absorption atmosphere (referred to as a cooling step), wherein the extinction coefficient of the absorption atmosphere is 0.004-0.02m -1 (preferably 0.006-0.018m -1 ) when measured at a vertical distance of 3000mm above the gas inlet.
  • the average diameter D32 of the droplets of the absorption atmosphere is 400-2600 microns (preferably 600-2400 microns) when measured at a vertical distance of 3000 mm above the gas inlet, and/or the droplet particle size distribution D10 of the absorption atmosphere is 150-1500 microns, D50 is 700-3000 microns, and D90 is 1400-3600 microns (preferably D10 is 250-1400 microns, D50 is 800-2800 microns, and D90 is 1600-3500 microns) when measured at a vertical distance of 3000 mm above the gas inlet.
  • the extinction coefficient of the absorbing atmosphere is 0.001-0.004 m -1 (preferably 0.0015-0.0035 m -1 ) when measured at a vertical distance of 8500 mm above the gas inlet, and/or the average droplet diameter D 32 of the absorbing atmosphere is 200-1400 microns (preferably 400-1000 microns) when measured at a vertical distance of 8500 mm above the gas inlet.
  • the droplet size distribution D10 of the absorption atmosphere is 100-1000 microns, D50 is 300-1800 microns, and D90 is 500-2200 microns (preferably D10 is 200-600 microns, D50 is 400-1400 microns, and D90 is 600-1800 microns).
  • the spraying device comprises a spray liquid inlet, a first spray pipe fluidically connected to the spray liquid inlet, a plurality of (e.g., 10-26, preferably 12-22) second spray pipes fluidically connected to the first spray pipe and extending perpendicularly to the first spray pipe on both sides thereof, a plurality of (e.g., 4-26, preferably 6-22) third spray pipes fluidically connected to the second spray pipe and extending perpendicularly to the second spray pipe on both sides thereof, and a nozzle located at the end of the third spray pipe and fluidically connected thereto.
  • a spray liquid inlet e.g., 10-26, preferably 12-22
  • second spray pipes fluidically connected to the first spray pipe and extending perpendicularly to the first spray pipe on both sides thereof
  • a plurality of (e.g., 4-26, preferably 6-22) third spray pipes fluidically connected to the second spray pipe and extending perpendicularly to the second spray pipe on both sides thereof
  • a nozzle located at the end
  • the straight-line distance M between the end of any third spray pipe on one second spray pipe and the end of any third spray pipe on another adjacent second spray pipe is not less than 320 mm (preferably not less than 350 mm), and/or, the nozzles are the same or different from each other, and the spray liquid spraying amount is independently 0.5-7.5 t/h (preferably 0.9-6.5 t/h), and/or, the nozzles are the same or different from each other, and the spray liquid spraying amount at the nozzle outlet is
  • the pressures are each independently 0.03-0.85MPaG (preferably 0.04-0.65MPaG), and/or the spray liquid input pressure at the spray liquid inlet is controlled at 0.06-1.00MPaG (preferably 0.12-0.90MPaG, more preferably 0.18-0.80MPaG), and/or the difference (absolute value) in the spray liquid input pressures of any two spray liquid inlets of the spraying devices is less than
  • the vertical distance between the gas inlet and the spray liquid inlet of the spraying device (when there are multiple spraying devices, it refers to the spraying device closest to the gas inlet) is 800-6000mm (preferably 1000-5000mm), and/or the inner diameter of the gas inlet is 800-1900mm (preferably 900-1700mm), and/or the linear velocity of the reaction product in the absorption device is 0.6-1.5m/s (preferably 0.7-1.3m/s), and/or the mass flow ratio of the spray liquid to the reaction product is 15-25:1.
  • the angle between the projections of the spray liquid inlets of any two odd-numbered spray devices on the cross section is 0°
  • the angle between the projections of the spray liquid inlets of any two even-numbered spray devices on the cross section is 0°
  • the angle between the projections of the spray liquid inlets of any odd-numbered spray device and any even-numbered spray device on the cross section is 180°.
  • the nozzle comprises a nozzle inlet, a rotation chamber and a nozzle outlet, wherein the rotation chamber is constructed so that the spray liquid entering from the nozzle inlet leaves the nozzle outlet in a rotating manner after passing through the rotation chamber.
  • the inner diameter of the first spray pipe is 160-480 mm (preferably 200-450 mm) and the length is 4500-11500 mm (preferably 4800-10500 mm)
  • the multiple second spray pipes are the same or different from each other
  • the inner diameters are each independently 30-150 mm (preferably 40-120 mm) and the lengths are each independently 1200-5750 mm (preferably 1800-5250 mm)
  • the multiple third spray pipes are the same or different from each other
  • the inner diameters are each independently 10-60 mm (preferably 15-50 mm) and the lengths are each independently 160-325 mm (preferably 175-300 mm).
  • the inner diameter (referring to the nozzle outlet) is independently 3-20 mm (preferably 6-14 mm)
  • the diameter of the rotating chamber is independently 10.0-55.0 mm (preferably 13.0-45.0 mm)
  • the spraying angle is independently 65-120° (preferably 70-100°).
  • the horizontal spacing between two adjacent second spray pipes is 640-1300 (preferably 700-1200 mm), and/or, on the same second spray pipe, the horizontal spacing between two adjacent third spray pipes is 320-650 mm (preferably 350-600 mm).
  • the hydrocarbon feedstock is propylene
  • the molar ratio of propylene/ammonia/air in terms of molecular oxygen
  • the reaction temperature is 420-440°C
  • the reaction pressure is 0.03-0.14 MPa
  • the catalyst weight hourly space velocity is 0.06-0.15 h -1
  • the hydrocarbon feedstock is isobutylene
  • the molar ratio of isobutylene/ammonia/air (calculated as molecular oxygen) is 1:1.3-1.6:2.2-2.8
  • the reaction temperature is 395-420°C
  • the reaction pressure (gauge pressure) is 0.03-0.14 MPa
  • the catalyst weight hourly space velocity is 0.08-0.17 h -1 .
  • the spraying liquid causes the temperature of the reaction product to be cooled from 195-235°C to 81-86°C, and/or, in the cooling step, the spraying liquid causes the ammonia content of the reaction product to be reduced to below 150 ppm.
  • the ammonia content in the absorbed exhaust gas does not increase significantly compared with the initial operation period, so a good ammonia absorption effect can be maintained for a long period of time and ammonia escape can be reduced.
  • the total acid consumption can still be maintained at a low level with a small increase (such as below 3%).
  • ammonia is evenly distributed in the absorption tower, which is beneficial to ammonia absorption.
  • the gas-liquid contact is sufficient, the ammonia absorption effect is good, and the amount of acid used can be reduced.
  • FIG. 1 is a schematic front view of an ammonia absorption tower in the prior art.
  • FIG. 2 is a schematic front view of an ammonia absorption tower in the prior art.
  • 3a and 3b are schematic front views of the ammonia absorption tower of the present invention.
  • FIGS. 4A and 4B are schematic front views of an ammonia absorption tower according to the present invention.
  • FIG. 5 is a schematic top view of the spraying device of the present invention.
  • 6A and 6B are schematic top views of the spraying device of the present invention.
  • FIG. 7 is a schematic top view of the spraying device of the present invention.
  • 8A and 8B are schematic top views of comparative spraying devices.
  • 9A and 9B are schematic top and front views of a nozzle in the prior art.
  • 10A and 10B are a schematic top view and a detailed top view of a spray device in the prior art.
  • Fig. 11A is a schematic diagram of the top view/front view of the two rotation modes of the nozzle of the present invention.
  • Fig. 11B is a schematic diagram of the top view of the spraying device.
  • Figure 11C is a detail view of a top view schematic diagram of a spraying device of the present invention.
  • Figure 11D is a detail view of a top view schematic diagram of another spraying device of the present invention.
  • Figure 11E is a detail view of a top view schematic diagram of another spraying device of the present invention.
  • Ammonia absorption tower 2 Ammonia absorber internals demister 3: Spraying device for internal components of ammonia absorption tower, 3a-3f are spraying devices 4: Gas distributor for internal components of ammonia absorber 5: Spraying device for internal components of ammonia absorption tower, 5a-5b is the spraying device 6: Upper circulation pump 7: Lower circulation pump 8: Ammonia-containing gas feed 9: Gas phase discharge from ammonia absorption tower 10: Rehydration in the upper part 11: Discharge of wastewater from the lower section 12: Discharge of ammonium salt solution from the upper section 13: Lower circulating fluid 14: Upper circulating fluid 15: Acid solution 16: Circulating fluid 17: Circulation pump 18: Spraying device inlet 19: Spraying device first spray pipe 20a, 20b: Second spray pipe of the spraying device 21: The third spray pipe of the spray device 22: Spraying device atomizing nozzle 23: Gas distributor P1, P2, P3, P4, P5, P6: Inlet pressure of spray liquid of the spray
  • the extinction coefficient is measured by forward near-infrared scattering spectroscopy.
  • a near-infrared LED light source is used to irradiate a sampling volume of about 100 ml, and the scattered light intensity I( ⁇ ) in the forward 25°-45° range is measured.
  • the method for measuring the average droplet diameter D 32 is based on laser imaging to measure the plane droplet particle size, and obtain the 2D spatially resolved Shad average particle size D 32 from the droplet image information.
  • the plane global droplet particle size measurement requires the simultaneous recording of the laser induced fluorescence signal LIF and the Mie scattering signal MIE image of the measured droplet object.
  • the 2D Shad average particle size is calculated by the ratio of these two image signals.
  • the LIf image represents the volume of the droplet, and the MIE light is basically proportional to the total amount of the droplet.
  • the method for measuring droplet size distribution is the same as the method for measuring droplet average diameter D 32 , which is based on laser imaging to obtain 2D spatially resolved particle size distributions D 10 , D 50 , D 90 , etc. from droplet image information.
  • the present invention relates to a method for producing nitrile, in particular, a method for producing (meth)acrylonitrile.
  • the method for manufacturing the nitrile comprises a step (referred to as a reaction step) of making a hydrocarbon feedstock undergo an ammoxidation reaction to manufacture a reaction product comprising the nitrile, and introducing the reaction product into an absorber through a gas inlet and spraying a spray liquid to the reaction product in the absorber through a spray device to cool the reaction product and form an absorption atmosphere (referred to as a cooling step).
  • the absorber is also generally referred to as an ammonia absorber or a quench tower.
  • the extinction coefficient of the absorption atmosphere is 0.004-0.02m -1 (preferably 0.006-0.018m -1 ).
  • the inventors of the present invention have found that since the droplets produce strong attenuation of both visible light and infrared signals, by measuring the attenuation of light and calculating its extinction coefficient, it can be used to comprehensively evaluate the dispersion effect of the liquid after being ejected at high speed through the nozzle.
  • a small extinction coefficient means that the droplet size is large and the number is small, and the total surface area of these droplets is relatively small. Due to the insufficient area in contact with the gas ammonia, the ammonia absorption efficiency decreases, resulting in more ammonia penetration. On the contrary, a large extinction coefficient means that the droplet size is small and the number is large. These droplets with too small a size are carried upward by the gas and are easily taken out of the tower. In the ammonia absorption tower, the ammonium salts contained in the droplets will be carried by the gas to the subsequent process, which will increase the environmental burden. This is also something that should be avoided as much as possible.
  • the average diameter D32 of the droplets of the absorption atmosphere is 400-2600 microns (preferably 600-2400 microns).
  • the inventors of the present invention have found that the moment the liquid is ejected from the nozzle, the liquid film is torn into small droplets. When the small droplets collide with other droplets during the falling process, there are separation, aggregation, and fragmentation.
  • the average particle size of the droplets can be measured by optical methods.
  • the average particle size of the droplets is When it is larger than 2600mm, on the one hand, due to the effect of gravity, the faster the droplets move downward, the shorter the residence time of the droplets in the tower is, which may lead to a decrease in absorption efficiency due to insufficient contact time with the gas.
  • the surface area of a large-diameter droplet is smaller than the surface area of two small-diameter droplets, that is, compared with two small droplets, a large-diameter droplet has less chance to contact the gas, which will also lead to a decrease in absorption efficiency.
  • the upward lifting force of the gas on the droplets overcomes the gravity of the droplets themselves, so the droplets are more easily entrained, and more power is also required, such as the inlet pressure of the spraying device, so that the liquid is torn less when it is sprayed through the nozzle.
  • the droplet size distribution of the absorption atmosphere is D10 of 150-1500 microns, D50 of 700-3000 microns, and D90 of 1400-3600 microns (preferably D10 of 250-1400 microns, D50 of 800-2800 microns, and D90 of 1600-3500 microns).
  • the inventors of the present invention have found that after the liquid is sprayed from the nozzle, it will be torn into countless small droplets of different particle sizes. At the same time, there is a situation in which the particle size of two droplets may become larger due to aggregation or smaller due to fragmentation or remain unchanged during separation during the collision process.
  • the circulating liquid contains an acid-containing liquid, and the absorption atmosphere is an ammonia-containing gas.
  • the acid in the droplets absorbs ammonia in the gas phase to form ammonium salts that exist in the droplets. If the droplet D10 and/or D50 and/or D90 are small, it means that the droplet D32 is small.
  • the droplets containing ammonium salts are easily entrained by the gas and escape from the tower, which brings new problems to the subsequent processing. For example, if the circulating liquid contains sulfuric acid, SO2-containing gas is generated in the incineration of wastewater, and if the circulating liquid contains phosphoric acid, P2O5 is generated. These are not environmentally friendly and should be avoided as much as possible.
  • the extinction coefficient of the absorption atmosphere is 0.001-0.004 m -1 (preferably 0.0015-0.0035 m -1 ).
  • the inventors of the present invention found that the measurement position is located above the spray device of the absorption tower, and the droplets in this area are entrained by the gas. Compared with the droplet particle size at the aforementioned measurement position, the droplet particle size in this area is relatively small, and the gas entrainment amount is also within a controllable range.
  • the extinction coefficient of the absorbing atmosphere is lower than 0.001m -1 , it means that the droplet size in the spraying device area is too large, and the upward thrust of the gas is less than its gravity, resulting in a small amount of droplet entrainment. The droplet size in the spraying device area is too large, and the gas-liquid contact is insufficient, which easily leads to the penetration of the absorbing atmosphere (such as ammonia).
  • the extinction coefficient is greater than 0.004m -1 , under the condition of normal droplet size, it means that the number of droplets entrained by the gas is large, and there is a possibility that the gas passes through the tower at a high speed. Due to insufficient residence time of the gas in the tower, the absorption is incomplete and the efficiency is low, causing the penetration of the absorbing atmosphere (such as ammonia).
  • the average diameter D 32 of the droplets of the absorption atmosphere is 200-1400 microns (preferably 400-1000 microns). More preferably, when measured at a vertical distance of 8500 mm above the gas inlet, the droplet size distribution of the absorption atmosphere is D 10 of 100-1000 microns, D 50 of 300-1800 microns, and D 90 of 500-2200 microns (preferably D 10 of 200-600 microns, D 50 of 400-1400 microns, and D 90 of 600-1800 microns).
  • the inventors of the present invention have found that the average droplet diameter D 32 and droplet particle size distribution measured at the measurement position are closely related to the average droplet diameter D 32 and droplet particle size distribution in the spray device area.
  • the average droplet diameter D 32 in the spray device area is large, and the average droplet diameter D 32 in this area is also relatively large.
  • the droplet particle size distribution is also the same.
  • the average droplet diameter and droplet particle size distribution are lower than the lower limit, it means that the droplets in the spray device area are small and the droplets are easily entrained; on the contrary, when the average droplet diameter and droplet particle size distribution are higher than the upper limit, the droplets in the spray device area are large, the gas-liquid contact is insufficient, and the absorption efficiency is reduced.
  • the spray device includes a spray liquid inlet, a first spray pipe fluidically connected to the spray liquid inlet, a plurality of (e.g., 10-26, preferably 12-22) second spray pipes fluidically connected to the first spray pipe and extending perpendicularly to the first spray pipe on both sides thereof, a plurality of (e.g., 4-26, preferably 6-22) third spray pipes fluidically connected to the second spray pipe and extending perpendicularly to the second spray pipe on both sides thereof, and a nozzle located at the end of the third spray pipe and fluidically connected to it.
  • a plurality of (e.g., 10-26, preferably 12-22) second spray pipes fluidically connected to the first spray pipe and extending perpendicularly to the first spray pipe on both sides thereof
  • a plurality of (e.g., 4-26, preferably 6-22) third spray pipes fluidically connected to the second spray pipe and extending perpendicularly to the second spray pipe on both sides thereof
  • a nozzle located at the end of the third
  • connection method between the spray pipes and between the third spray pipe and the nozzle has no specific limitation on the connection method between the spray pipes and between the third spray pipe and the nozzle, and conventional connection methods in the art can be used.
  • conventional connection methods in the art can be used.
  • fixed connection or detachable connection can be used, preferably threaded connection, or other detachable connection methods, which are not specifically limited.
  • the spraying liquid is water or an acidic aqueous solution.
  • the ammonia-containing gas contacts the acidic aqueous solution as the spraying liquid from bottom to top in reverse from top to bottom, and the acidic H+ contained in the aqueous solution reacts with ammonia to remove the ammonia.
  • the acidic aqueous solution is an aqueous solution of an acidic substance.
  • the acidic substance may be an inorganic acid, such as hydrochloric acid, sulfuric acid, phosphoric acid; may also be an organic acid, such as acrylic acid, acetic acid; may also be an acidic salt, such as ammonium sulfate, without specific limitation.
  • the spraying liquid contacts the reaction product in a countercurrent manner.
  • the spray liquid input pressure at the spray liquid inlet is controlled at 0.06-1.00 MPaG (preferably 0.12-0.90 MPaG, more preferably 0.18-0.80 MPaG).
  • the inventors of the present invention have found that the circulating liquid enters the spray device from the spray device inlet, passes through the first spray pipe, the second spray pipe, the third spray pipe, and is transported to the absorption tower through the nozzle at the end of the third spray pipe.
  • the larger the droplet size the weaker the droplet absorption of light, and the lower the extinction efficiency.
  • the droplet size is inversely proportional to the pressure.
  • the droplet size is constantly increasing along the direction of circulating fluid travel.
  • the droplet size D32 formed at the atomizing nozzle far from the spray inlet fluid travel direction is larger than the droplet size D32 formed at the atomizing nozzle near the spray inlet fluid travel direction. This also leads to the ammonia absorption efficiency far from the spray inlet fluid travel direction is lower than the ammonia absorption efficiency near the spray inlet fluid travel direction.
  • the spray liquid input pressure at the spray liquid inlet is controlled within the aforementioned specified range to meet the sufficient pressure of the far nozzle, meet the average droplet particle size and particle size distribution requirements required by the device, and ensure the atomization effect.
  • the polymer with a certain viscosity produced during the reaction and the ammonium salt mixed in the circulating liquid adhere to the wall of the spray pipe, resulting in a continuous increase in the resistance of the pipe.
  • the increase in the resistance of the pipe is more obvious, and the pressure of the distal nozzle is further reduced, resulting in a larger droplet size at the distal nozzle, and the droplet size distribution becomes wider and more uneven, and the atomization effect is worse.
  • the spray liquid input pressure at the spray liquid inlet within the aforementioned specified range, even after a long period of continuous operation, sufficient pressure at the distal nozzle can be met to ensure the atomization effect.
  • the plurality of second spraying pipes extend substantially in parallel along a horizontal direction perpendicular to the first spraying pipe toward opposite sides thereof.
  • the plurality of third spraying pipes extend substantially in parallel along a horizontal direction perpendicular to the second spraying pipe toward opposite sides thereof.
  • the inner diameter of the first spray pipe is 160-480 mm (preferably 200-450 mm), and the length is 4500-11500 mm (preferably 4800-10500 mm).
  • the plurality of second spray pipes are the same as or different from each other, and each has an inner diameter independently of 30-150 mm (preferably 40-120 mm) and a length independently of 1200-5750 mm (preferably 1800-5250 mm).
  • the plurality of third spray pipes are the same or different from each other, and the inner diameters are independently 10-60 mm (preferably 15-50 mm), and the lengths are independently 160-325 mm (preferably Choose 175-300mm).
  • the nozzle comprises a nozzle inlet, a rotating chamber and a nozzle outlet, wherein the rotating chamber is configured so that the spray liquid entering from the nozzle inlet leaves the nozzle outlet in a rotating manner after passing through the rotating chamber.
  • the rotating chamber can adopt any structure known in the art, as long as the spray liquid can leave the nozzle outlet in a rotating manner after passing through the rotating chamber, and there is no particular limitation.
  • the nozzles are the same or different from each other, the inner diameter (referring to the nozzle outlet) is independently 3-20mm (preferably 6-14mm), the diameter of the rotating chamber is independently 10.0-55.0mm (preferably 13.0-45.0mm), and the spraying angle is independently 65-120° (preferably 70-100°).
  • the rotating chamber can adopt any structure known in the art, as long as the spray liquid can leave the nozzle outlet in a rotating manner after passing through the rotating chamber, and there is no special limitation.
  • the horizontal interval between two adjacent second spray pipes is 640-1300 mm (preferably 700-1200 mm).
  • the horizontal distance between two adjacent third spraying pipes is 320-650 mm (preferably 350-600 mm).
  • the straight-line distance M between the end of any third spray pipe on one second spray pipe and the end of any third spray pipe on another adjacent second spray pipe is not less than 320 mm, preferably not less than 350 mm.
  • the inventor of the present invention found that in order to improve the absorption efficiency of ammonia, generally, at any position on the cross section of the tower, there are at least two or more conical liquid surfaces formed with the nozzle as the center overlapping and covering, including the tower wall.
  • the distance between the ends of the two spray pipes is too large, it is difficult to meet the overlap of the liquid surfaces sprayed by more than two nozzles at any position of the tower wall due to the limitation of the nozzle structure. In other words, the number of droplets in the tower is reduced, which is manifested as a decrease in the absorption rate of the droplets to light and a decrease in the extinction ability, thereby increasing the probability of ammonia escaping from the "gap". If the distance between the ends of the two spray pipes is too small, in order to ensure the atomization quality of the spray liquid, the circulating liquid volume in the ammonia absorption tower will inevitably increase, that is, the energy consumption of the pump will increase. In addition, as shown in FIG. 6A and FIG. 6B , if the upper and lower multi-layer spraying devices are overlapped in upper and lower projections, only the upper spraying device and the spraying liquid inlets facing each other can be seen.
  • the nozzles are the same as or different from each other, and the spraying liquid spraying amount is independently 0.5-7.5 t/h (preferably 0.9-6.5 t/h).
  • the nozzles are the same or different from each other, and the spraying pressure of the spray liquid at the nozzle outlet is independently 0.03-0.85MPaG (preferably 0.04-0.65MPaG).
  • pressure is one of the main factors that prompt the liquid to form droplets.
  • the size of the droplet particle size will increase as the pressure decreases.
  • small atomized droplets are generally considered to have better mass transfer and heat transfer efficiency.
  • the smaller the droplets the narrower the particle size distribution, the greater the absorption of light, and the stronger the extinction energy.
  • the viscous polymer produced during the operation of the device also adheres to the inner cavity of the nozzle, increasing the resistance of the nozzle and causing the pressure at the nozzle outlet to decrease.
  • dirt adheres to the inner cavity of the nozzle, changing the movement behavior of the spraying liquid in the nozzle, especially increasing the instability of the atomization of the distal nozzle, and this instability will become more prominent as the running time of the device increases.
  • the present invention by controlling the spraying pressure of the spray liquid at the nozzle outlet within the aforementioned specified range, even after a long period of continuous operation, the atomization of the distal nozzle can be ensured to be stable and the atomization effect can be guaranteed.
  • the spraying liquid contacts the reaction product in a countercurrent manner.
  • the mass flow ratio of the spraying liquid to the reaction product is 15-25:1.
  • the cooling step is carried out in the absorption device, and a plurality of (such as 2-10, preferably 4-8) spraying devices are layered inside the absorption device along the central axis direction of the absorption device at a predetermined vertical spacing.
  • a plurality of (such as 2-10, preferably 4-8) spraying devices are layered inside the absorption device along the central axis direction of the absorption device at a predetermined vertical spacing.
  • the projections of at least one (preferably all) of the first spray pipe, the second spray pipe and the third spray pipe of one of the multiple spray devices and another of the multiple spray devices on the cross section substantially overlap. That is, the projections of the nozzles (cone centers) of each layer on the cross section overlap, so that ammonia is evenly distributed in the gas rest channel.
  • the one spraying device and the other spraying device The projections of all nozzles on the cross section basically overlap.
  • the inventors of the present invention have found that the multiple spraying devices in the absorption device are both relatively independent individuals and an organic whole.
  • the circulating liquid is transported to the nozzles of each spraying device through the first spraying pipe, the second spraying pipe, and the third spraying pipe of each spraying device, and a hollow conical liquid surface is formed with the nozzle as the center.
  • the gas contacts the circulating liquid in reverse. The gas can only contact the conical liquid surface formed by the upper spraying device after passing through the conical liquid surface formed by the lower spraying device.
  • the hollow conical liquid surfaces of the upper and lower spraying devices can be regarded as a gas rising channel. Since each section is required to have an independent liquid phase circulation spraying device, the rising gas channel has a certain height.
  • the projections of at least one (preferably all) of the first spray pipe, the second spray pipe and the third spray pipe on the cross section basically overlap, that is, the projections of the nozzles (cone centers) of each layer on the cross section overlap, so that ammonia is evenly distributed in the gas channel, the fusion with the droplets is more complete, and the extinction efficiency is more consistent. If the projections of the upper layer of nozzles and the lower layer of nozzles on the cross section do not overlap, since the hollow cone liquid levels of the upper and lower layers are not in the same position, the gas channel of the rising gas is changed.
  • the vertical spacing between two adjacent spray devices is 650-1350mm, preferably 750-1200mm.
  • the inventor of the present invention has found that if the projections of the upper layer of nozzles and the lower layer of nozzles on the cross section do not overlap, since the upper and lower hollow conical liquid surfaces are not in the same position, the gas channel of the rising gas is changed, and some channels become “wider” while some channels become “narrower".
  • the “widening” of the channel also means that the amount of droplets in the channel decreases, and the extinction capacity decreases. On the contrary, the "narrowing" of the channel increases the extinction capacity.
  • the rising gas passes through the gas channels at different heights, due to the different gas residence times in the channel, there is a problem of uneven gas distribution in the channel. That is, when the ammonia-containing gas passes through the hollow conical liquid surface, acid is left in some areas of the liquid surface, while ammonia penetrates in another part of the liquid surface due to insufficient acid, thereby reducing the ammonia absorption effect.
  • the inventor of the present invention has also found that if the projections of the upper layer of nozzles and the lower layer of nozzles on the cross section do not overlap, the spray liquids sprayed by the upper layer of nozzles and the lower layer of nozzles will have more collisions.
  • the projections of the upper layer of nozzles and the lower layer of nozzles on the cross section do not overlap, the droplets produced by the upper layer of nozzles and the droplets produced by the lower layer of nozzles will have more collisions.
  • the droplets are more likely to aggregate and form larger droplets.
  • the number of droplets is relatively reduced, which is manifested in a decrease in extinction efficiency, which is not conducive to the absorption of ammonia.
  • each spraying device flows along the first spraying pipe to the second spraying pipe to the third spraying pipe until the nozzle.
  • the pressure along the way is continuously reduced by the resistance of the pipe wall.
  • the pressure at the nozzle far from the spraying liquid inlet is lower than the pressure at the nozzle near the spraying liquid inlet. Since the pressure at the farthest nozzle is relatively the lowest, the average particle size of the droplets here is relatively large, the droplet particle size distribution is wider, the droplet absorption efficiency of light is the lowest, and the atomization effect is also the worst, resulting in insufficient gas-liquid contact at the farthest nozzle, which is easy to cause ammonia to escape.
  • the pipe wall resistance is further increased, the droplet absorption efficiency of light is further reduced, that is, the extinction efficiency is further reduced, and the atomization effect at the far nozzle becomes worse, causing more ammonia to escape.
  • the spray liquid inlets of the multi-layer spray devices are on the same side, since the distal nozzles of the spray devices of each layer are on the same side, the gas-liquid contact in this area is the weakest, and ammonia in the gas phase can more easily escape from the ammonia absorption tower from this area.
  • the angle between the projections of the spray liquid inlet of the one spray device and the other spray device on the cross section is 180°.
  • the distal nozzle of the spray device is sufficient to atomize the spray liquid into droplets of suitable size.
  • the escaped ammonia is captured by the spray liquid at the proximal nozzle of the upper layer of the spray device and undergoes a neutralization reaction to generate corresponding salts, the average droplet diameter and droplet size distribution of the upper and lower opposite spray device inlet end position areas are similar, that is, the extinction efficiency is similar.
  • multiple layers of spraying devices are arranged in the ammonia absorption tower, such as 3 layers, 4 layers, 5 layers or more layers, and the projected angle between the spraying liquid inlet of the upper (or second) layer of spraying device and the spraying liquid inlet of the lower (or second) layer of spraying device on the cross section is 180°, which can absorb ammonia to a greater extent, thereby reducing the escape of ammonia and also reducing the consumption of acid to a greater extent.
  • two nozzles whose projections substantially coincide with each other have the same spray diameter.
  • the angle between the projections of the spray liquid inlets of any two odd-numbered spray devices on the cross section is 0°, and the angle between the projections of the spray liquid inlets of any two even-numbered spray devices on the cross section is 0°.
  • the angle between the projections of the spraying liquid inlet of any odd-numbered spraying device and any even-numbered spraying device on the cross section is 180°.
  • two nozzles whose projections are substantially overlapped have the same spray liquid rotation direction.
  • the inventor of the present invention has found that when the spray liquids sprayed from the nozzles whose projections overlap with each other collide downward, the droplet states of the nozzles are different. Relatively speaking, the two nozzles whose projections overlap with each other and whose rotation directions are opposite are more likely to break the droplets into several small droplets than the two nozzles whose rotation directions are the same, thereby enhancing the absorption rate of light and the extinction efficiency. However, if the droplets are too small, they are easily entrained by the gas and escape.
  • two adjacent (preferably all) nozzles located on the same side of the second spray pipe are constructed so that the spray liquid is sprayed in the same rotation direction.
  • the inventor of the present invention found that the spray liquid enters the rotating tower from the tangential direction of the nozzle, and forms a hollow cone with the nozzle outlet as the vertex after passing through the nozzle outlet.
  • the nozzle outlets of two adjacent nozzles are required to be equidistantly distributed in the cross section of the tower, that is, the spray liquid enters the nozzle in the same tangential direction.
  • the spray liquid on the same side of the second spray pipe is sprayed in the same rotation direction, and the spray liquid on the opposite sides of the second spray pipe is sprayed in the opposite rotation direction.
  • the spray liquid sprayed from the nozzle on the same second spray pipe intersects and collides, more droplets remain in the same state of light absorption and still maintain the original state and move downward along the original direction of movement.
  • all nozzles on the opposite sides of two second spray pipes adjacent to each other are constructed so that the spray liquid is sprayed in opposite rotation directions.
  • the so-called “adjacent to each other” refers to being on the same side of the first spray pipe and adjacent to each other
  • the so-called “opposite sides” refers to the respective sides of one second spray pipe and the other second spray pipe facing each other, as shown in FIG11C.
  • At least one (preferably all) of the nozzles located on one side of the second spray pipe are configured so that the spray liquid is sprayed in a rotation direction A, and at least one (preferably all) of the nozzles located on the other side of the second spray pipe are configured so that the spray liquid is sprayed in a rotation direction A.
  • the nozzle is constructed so that the spray liquid is sprayed in a rotation direction B, wherein the rotation direction A is opposite to the rotation direction B.
  • the rotation direction A is clockwise, and the rotation direction B is counterclockwise.
  • the number of nozzles spraying the spray liquid in the rotation direction A is equal to or substantially equal to the number of nozzles spraying the spray liquid in the rotation direction B.
  • the premise of uniform spraying is that the nozzles are evenly distributed in the tower, and usually preferably in an axisymmetric distribution. Therefore, the inventors of the present invention found that the rotation directions of the nozzles appear in pairs in axisymmetric manner. If the rotation directions of the paired nozzles are all in the same direction, it means that the rotation directions of all nozzles are the same, which easily causes the spray liquid sprayed from two adjacent nozzles to rotate and descend. The droplet collision becomes larger, the extinction efficiency becomes weaker, and the ammonia absorption efficiency is reduced due to the reduction of the total effective contact area with the gas ammonia.
  • two adjacent (preferably all) nozzles located on the same side of the second spray pipe are configured so that the spray liquid is sprayed in opposite rotation directions.
  • the third spray pipe is perpendicular to the second spray pipe and extends horizontally parallel to both sides thereof, and all nozzles on the same horizontal parallel extension line of the second spray pipe are configured so that the spray liquid is sprayed in the same rotation direction. As shown in Figure 11E.
  • one nozzle located in the second spray pipe is configured to spray the spray liquid in a rotation direction A, and at least another nozzle adjacent to one side is configured to spray the spray liquid in a rotation direction B.
  • At least one (preferably all) nozzles located on the other side of the second spray pipe are configured to spray the spray liquid in a rotation direction A, wherein the rotation direction A is opposite to the rotation direction B.
  • the nozzle includes a nozzle inlet, a nozzle cavity and a nozzle outlet, wherein the cavity has a special structure so that the spray liquid entering from the nozzle inlet forms droplets after passing through the cavity and leaving the nozzle outlet.
  • the cavity can adopt any structure known in the art, as long as it can make the spray liquid leave the nozzle outlet and form droplets, and there is no special limitation.
  • the spray liquid enters the cavity from above the nozzle, and forms a solid cone with the nozzle outlet as the vertex after passing through the nozzle outlet.
  • two adjacent nozzles are equidistantly distributed in the cross section of the tower, and the projections of the nozzles of multiple spraying devices basically overlap.
  • the spray liquid sprayed from the two adjacent nozzles After colliding during their respective downward processes, the droplets can still maintain their original state and move downward.
  • the vertical spacing between two adjacent spraying devices is 650-1350mm (preferably 750-1200mm).
  • the inventor of the present invention found that when the vertical spacing between two adjacent spraying devices is less than 650mm, for an ammonia absorption tower with the same number of spraying devices, due to the insufficient contact time between the rising ammonia-containing gas and the descending circulating liquid, the gas-liquid fusion becomes poor, the extinction efficiency is reduced, and part of the ammonia in the gas phase directly passes through the hollow cone liquid surface formed by the circulating liquid, resulting in poor ammonia absorption efficiency.
  • the difference (absolute value) of the spray liquid input pressure at the spray liquid inlet of any two of the spray devices is less than 0.024MPa (preferably less than 0.018MPa, more preferably less than 0.012MPa).
  • the inventors of the present invention have found that the size of the droplets of the circulating liquid after atomization is closely related to the pressure of the nozzle. Too much or too little pressure is not conducive to the operation of the device. The nozzle pressure starts from the spray liquid input pressure at the spray liquid inlet. In theory, it is hoped that the spray liquid input pressure at the spray liquid inlet is the same.
  • the multi-layer spray devices are arranged up and down, there is a pressure drop loss when the circulating pump transports the circulating liquid to each layer of the spray device. Therefore, the difference in the spray liquid input pressure at the spray liquid inlet of any two spray devices is as low as possible, so that all nozzles of the uppermost and lowermost spray devices can meet the optimal pressure conditions, and the average droplet diameter and droplet size distribution on the longitudinal section of the device are similar, that is, the longitudinal extinction efficiency of the device is also the same.
  • the inner diameter of the absorption device is 4.5-11.5 m (preferably 4.8-10.5 m).
  • the absorption device further comprises a shell and a gas inlet.
  • the spraying device is arranged inside the shell of the absorption device.
  • the reaction product is input into the absorption device from the gas inlet.
  • the gas inlet is located below the spraying device along the central axis direction of the absorption device.
  • the vertical distance between the gas inlet and the spray liquid inlet of the spraying device (when there are multiple spraying devices, it refers to the spraying device closest to the gas inlet) is The distance is 800-6000mm (preferably 1000-5000mm).
  • the inventors of the present invention found that the gas enters the tower from the inlet along the semicircular inlet pipe that bends downward toward the bottom of the tower, and then moves from bottom to top. Relatively speaking, the gas concentration is highest at the inlet pipe. While the gas is going up, due to the difference in gas concentration, the gas diffuses to the surrounding area, and finally the gas concentration on the cross section of the tower reaches uniformity.
  • the vertical distance is less than 800mm, the gas concentration is prone to insufficient diffusion, uneven concentrations, and uneven gas-liquid separation, which affects the uneven extinction efficiency and easily causes incomplete local ammonia absorption and excessive local acid.
  • the vertical distance is too large, on the one hand, the tangent height of the ammonia absorption tower is too high, increasing equipment investment.
  • the two colliding droplets separate, aggregate, and break, and when aggregation occurs, larger droplets are formed; when fragmentation occurs, smaller droplets are formed. The longer the droplet spray distance, the easier it is to aggregate or break up, and the droplet size distribution becomes wider, which may reduce the extinction efficiency, which is not conducive to the absorption of ammonia.
  • the inner diameter of the gas inlet is 800-1900 mm (preferably 900-1700 mm).
  • the linear velocity of the gas inside the shell is 0.6-1.5m/s (preferably 0.7-1.3m/s).
  • the inventors of the present invention have found that the operating speed inside the shell affects the gas diffusion speed. The greater the operating speed inside the shell, the stronger the turbulence effect, the more entrained droplets, the higher the extinction efficiency, and the diffusion of the gas. Therefore, the diffusion distance is also shorter.
  • the speed inside the shell is lower than 0.6, relatively speaking, it takes a long time for the gas to diffuse uniformly, that is, the distance from the inlet to the first layer of the spraying device increases.
  • no mechanical components that can substantially affect the flow of the gas such as mechanical components that disturb the flow of the gas, especially baffles, trays, fillers, etc. are provided.
  • the inventors of the present invention have found that although the gaseous ammonia can be evenly dispersed on the cross section before contacting the first layer of spray liquid by adding internal components, no matter what type of mechanical components are used, the system pressure of the device will increase, which will eventually be reflected in the increase of reaction pressure and the reduction of the yield of the target product.
  • the vertical distance from the first layer of spray devices to the inlet is 800-6000mm, preferably 1000-5000mm, which can meet the high efficiency of the previous reaction stage, the extinction efficiency of the tower, and the absorption efficiency of ammonia, which is more economical for the entire device.
  • the hydrocarbon feedstock is propylene
  • the molar ratio of propylene/ammonia/air in terms of molecular oxygen
  • the reaction temperature is 420-440°C
  • the reaction pressure gauge pressure
  • the catalyst weight hourly space velocity is 0.06-0.15 h -1
  • the hydrocarbon feedstock is isobutylene
  • the molar ratio of isobutylene/ammonia/air in terms of molecular oxygen
  • the reaction temperature is 395-420°C
  • the reaction pressure (gauge pressure) is 0.03-0.14 MPa
  • the catalyst weight hourly space velocity is 0.08-0.17 h -1 .
  • the composition of the reaction product is generally C 1-4 nitriles (such as acrylonitrile, etc.) accounting for about 10-20wt%, C 1-4 oxygen-containing compounds (such as acrolein, etc.) accounting for about 0.1-5wt%, O 2 accounting for about 0.1-5wt%, ammonia accounting for about 0.1-2wt%, and other impurities are the remainder, relative to the total weight of the reaction product is 100wt%.
  • the temperature of the reaction product is generally 195-235°C
  • the pressure is generally 0.03-0.14MPaG. According to the present invention, for this specific reaction product, the above-mentioned technical effects of the manufacturing method of the present invention are particularly excellent.
  • the spraying liquid cools the temperature of the reaction product from 195-235° C. to 81-86° C.
  • the spraying liquid reduces the ammonia content of the reaction product to below 150 ppm.
  • the reaction gas with a temperature of 225 and the unreacted ammonia enter the ammonia absorption tower 1 from the ammonia-containing gas feed port 8, and the circulating liquid is extracted from the bottom of the tower and sent to the multi-layer spraying device 3a-spraying device 3f through the circulating pump 17.
  • the spraying devices 3a-3f are arranged in sequence from top to bottom in the tower, wherein the spraying devices 3a ⁇ 3c ⁇ 3e are on the same side, and the spraying devices 3b ⁇ 3d ⁇ 3f are on the opposite side to the spraying devices 3a ⁇ 3c ⁇ 3e.
  • the vertical distance between the ammonia-containing gas feed port 8 and the spraying device 3f is The distance is 1800mm; the spray liquid input pressures of the spray liquid inlet of the spray device 3a ⁇ 3c ⁇ 3e are 0.327MPaG, 0.330MPaG, and 0.334MpaG, respectively; the spray liquid input pressures of the spray liquid inlet of the spray device 3a ⁇ 3c ⁇ 3e are 0.327MPaG, 0.330MPaG, and 0.334MpaG, respectively; sulfuric acid is added to the circulating pump outlet pipeline from the acid solution port 15, and the circulating liquid passes through the spray device 3 and enters from the inlet 18 of the spray device 3, along the flow The circulating liquid is sprayed from the nozzle 22 to form an acid mist liquid layer in the ammonia absorption tower, absorbing the gas ammonia from the gas feed port 8, and the tail gas is discharged from the ammonia absorption tower from the gas phase discharge port 9.
  • the tail gas temperature at the top of the tower is 84°C.
  • the reaction gas with a temperature of 225° C. and unreacted ammonia enter the ammonia absorption tower 1 from the ammonia-containing gas feed port 8, the circulating liquid is extracted from the bottom of the tower and sent to the spraying device 3a-spraying device 3f through the circulating pump 17, wherein the spraying device 3a ⁇ 3c ⁇ 3e is on the same side, and the spraying device 3b ⁇ 3d ⁇ 3f is on the opposite side to the spraying device 3a ⁇ 3c ⁇ 3e, the acid-containing liquid is added to the circulating pump outlet pipeline from the acid solution port 15, the circulating liquid passes through the spraying device 3, enters from the inlet 18 of the spraying device 3, and passes through the first spraying pipe 19, the second spraying pipe 20a (20b), and the third spraying pipe 21 along the fluid direction to the atomizing nozzle 22, and the atomizing nozzle rotates to the left: rotates to the right at a ratio of 1:1.
  • the circulating liquid sprayed from the nozzle 22 forms an acid mist liquid layer in the ammonia absorption tower, absorbs the gas ammonia from the gas feed port 8, and the tail gas is discharged from the ammonia absorption tower from the gas phase discharge port 9.
  • the tail gas temperature at the top of the tower is 84°C.
  • the projections of the ends of the third spray pipes of the spray devices 3a-3f on the cross section of the tower overlap, as shown in Figure 6A.
  • the schematic diagram of the nozzle (nozzle) structure of the spray device and the top view of the spray device are shown in Figures 11C and 11B.
  • the residual ammonia concentration in the tail gas can be measured by off-line analysis, specifically, a certain volume (V) of gas is taken from the top of the ammonia absorber, the gas is absorbed by a certain amount of water, the amount of ammonia in the water is analyzed, and converted to the volume of gas phase ammonia (v), and the residual ammonia concentration in the tail gas is calculated as v/V.
  • the acid consumption is measured by the acid meter entering the ammonia absorber.
  • the ammonia absorption tower adopts the two-stage structure of Figure 3b.
  • the inner diameter of the absorption tower is 7200mm.
  • the linear velocity of the reaction gas in the tower is 1.1m/s.
  • the acid added to the circulating liquid is sulfuric acid.
  • the acid-containing circulating liquid is sent to the absorption tower through the upper circulation pump through 4 spraying devices.
  • the fluid directions in the first spraying pipes of the spraying devices 3a and 3c and 3b and 3d are opposite, that is, the projection angle of two adjacent spraying liquid inlets is 180°.
  • the top view of the spraying device is shown in Figure 11B, and the top view of the spraying device is shown in Figure 11C.
  • the spray liquid input pressures at the spray liquid inlets of the spray devices 3a(b) and 3c(d) are 0.440MPaG and 0.446MPaG respectively
  • the spray liquid discharge pressure is 0.051MPaG
  • the interval between two adjacent spray devices is 1200mm
  • each spray device has 16 second spray pipes
  • the second spray pipes are provided with 11 to 18 third spray pipes.
  • the third spray end projections of the spray devices overlap and rotate in the same direction, all the nozzles on the same side of the second spray pipe rotate in the same direction, the nozzles on the opposite sides of the second spray pipe rotate in opposite directions, and all the nozzles on the opposite sides of the two adjacent second spray pipes rotate in opposite directions, and the number of nozzles with the same rotation chamber direction is 480 and 480 respectively.
  • the inner diameter of the first spray pipe of the spray device is 250mm, and the length of the first spray pipe is 7000mm; the spacing of the second spray pipe of the spray device is 820mm, the inner diameter of the second spray pipe is 100mm, and the length of the second spray pipe is 2100mm-3450mm; the spacing of the third spray pipe of the spray device is 410mm, the inner diameter of the third spray pipe is 40mm, and the length of the third spray pipe is 205mm; the spray device has a total of 960 nozzles, and the distance between the ends of two adjacent third spray pipes is 580mm as shown in Figure 6B; the nozzle outlet diameter is 11.5mm, the nozzle rotation chamber diameter is 40mm, and the nozzle spray angle is 75°.
  • the vertical distance from the gas feed port 8 to the spray device 3d is 4000mm, and the inner diameter of the feed port is 1300mm.
  • the reaction product gas entering from the feed port contains about 0.71wt% ammonia, 13.2wt% acrylonitrile, and the rest are impurities such as O2 , acrolein, and nitrogen. Its temperature is 225°C, and the pressure is 0.06MPaG.
  • the spray liquid spraying amount of each nozzle is 4.8t/h, and the weight ratio of the spray liquid to the reaction product gas entering from the gas inlet is 20.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 41ppm. After the device has been in operation for 24 months, the residual ammonia concentration of the tail gas from the reaction outlet is 52ppm; the acid consumption of the device in operation for 24 months/the acid consumption of the device in operation for 1 month is 1.02.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.011 m -1 , the average diameter of the droplets D 32 is 1130 microns, and the droplet size distribution is D 10 of 625 microns, D 50 of 1328 microns, and D 90 of 2195 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0021 m -1 , the average diameter of the droplets D 32 is 462 microns, and the droplet size distribution is D 10 of 406 microns, D 50 of 593 microns, and D 90 of 894 microns.
  • the ammonia absorption tower adopts the one-stage structure of FIG. 4B .
  • the inner diameter of the absorption tower is 7200 mm.
  • No gas distributor 23 is provided in the tower.
  • the linear velocity of the reaction gas in the tower is 1.1 m/s.
  • the acid added to the circulating liquid is sulfuric acid.
  • the acid-containing circulating liquid is delivered to the absorption tower through a circulating pump through 6 spraying devices, of which the spraying device
  • the directions of the fluids in the first spray pipes of 3a, 3c, 3e and 3b, 3d, 3f are opposite, that is, the projection angle of two adjacent spray liquid inlets is 180°.
  • the top view of the spray device is shown in FIG11B, and the top view of the spray device is shown in FIG11C.
  • the spray liquid input pressures of the spray liquid inlets of the spray devices 3a (b), 3c (d) and 3e (f) are 0.425 MPaG, 0.430 MPaG, and 0.435 MPaG, respectively, and the spray liquid spray pressures are 0.055 MPaG, respectively.
  • the vertical spacing between two adjacent spray devices is 880 mm.
  • Each spray device has 14 second spray pipes, and the second spray pipes are provided with 6 to 14 third spray pipes.
  • the projections of the third spraying ends of the spraying devices overlap and have the same rotation direction, all nozzles on the same side of the second spray pipe have the same rotation chamber direction, the nozzles on opposite sides of the second spray pipe have opposite rotation chamber directions, and all nozzles on the opposite sides of two adjacent second spray pipes have opposite rotation directions, and the number of nozzles with the same rotation chamber direction are 456 and 456 respectively.
  • the inner diameter of the first spray pipe of the spray device is 200mm, and the length of the first spray pipe is 7000mm; the spacing of the second spray pipes of the spray device is 1000mm, the inner diameter of the second spray pipe is 100mm, and the length is 1850mm-3450mm; the spacing of the third spray pipes of the spray device is 500mm, the inner diameter of the third spray pipe is 40mm, and the length is 250mm.
  • the projection of the third spray end of the spray device overlaps, and the distance between the ends of two adjacent third spray pipes as shown in Figure 6A is 500mm; the spray device has a total of 912 nozzles, the nozzle outlet diameter of the spray device is 11.7mm, the nozzle rotation chamber diameter is 36mm, and the spray angle is 80°.
  • the vertical distance from the gas feed port 8 to the spray device 3f is 1500mm
  • the vertical distance from the gas feed port 8 to the spray device 3d is 4000mm
  • the inner diameter of the feed port is 1200mm.
  • the reaction product gas entering from the feed port contains about 0.71wt% ammonia, 13.2wt% acrylonitrile, and the rest are impurities such as O2 , acrolein, and nitrogen. Its temperature is 225°C, and the pressure is 0.06MPaG.
  • the spray liquid spraying amount of each nozzle is 5.1t/h, and the weight ratio of the spray liquid to the reaction product gas entering from the gas inlet is 20.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 27ppm. After the device has been in operation for 24 months, the residual ammonia concentration of the tail gas from the reaction outlet is 34ppm; the acid consumption of the device in operation for 24 months/the acid consumption of the device in operation for 1 month is 1.01.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0128 m -1 , the average diameter of the droplets D 32 is 1054 microns, and the droplet size distribution is D 10 of 832 microns, D 50 of 1242 microns, and D 90 of 1956 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0019 m -1 , the average diameter of the droplets D 32 is 412 microns, and the droplet size distribution is D 10 of 386 microns, D 50 of 574 microns, and D 90 of 878 microns.
  • Example 2 The same as Example 2, the only difference is that the spray liquid input pressures at the spray liquid inlets of the spray devices 3a (b), 3c (d) and 3e (f) are 0.152 MPaG, 0.160 MPaG, and 0.168 MPaG, respectively, and the spray liquid spray pressures are 0.04 MPaG, respectively.
  • the nozzle outlet diameter of the spray device is 11.9 mm.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 72 ppm. After the device has been in operation for 24 months, the residual ammonia concentration of the tail gas from the reaction outlet is 98 ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0058 m -1 , the average diameter of the droplets D 32 is 2226 microns, and the droplet size distribution is D 10 of 1298 microns, D 50 of 2384 microns, and D 90 of 3203 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0013 m -1 , the average diameter of the droplets D 32 is 542 microns, and the droplet size distribution is D 10 of 427 microns, D 50 of 671 microns, and D 90 of 914 microns.
  • Example 2 The same as Example 2, the only difference is that the spray liquid input pressures at the spray liquid inlets of the spray devices 3a (b), 3c (d) and 3e (f) are 0.838 MPaG, 0.844 MPaG, and 0.85 MPaG, respectively, and the spray liquid spraying pressures are 0.42 MPaG, respectively.
  • the nozzle outlet diameter of the spray device is 12.1 mm.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 84 ppm. After the device has been in operation for 24 months, the residual ammonia concentration of the tail gas from the reaction outlet is 92 ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.018 m -1 , the average diameter of the droplets D 32 is 726 microns, and the droplet size distribution is D 10 of 422 microns, D 50 of 989 microns, and D 90 of 1803 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0035 m -1 , the average diameter of the droplets D 32 is 321 microns, and the droplet size distribution is D 10 of 267 microns, D 50 of 389 microns, and D 90 of 543 microns.
  • Example 2 The same as Example 2, the only difference is that the spray liquid input pressures at the spray liquid inlets of the spray devices 3a (b), 3c (d) and 3e (f) are 0.950 MPaG, 0.954 MPaG, and 0.959 MPaG, respectively, and the spray liquid spray pressures are 0.42 MPaG, respectively.
  • the nozzle outlet diameter of the spray device is 11.1 mm.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 105 ppm. After the device has been in operation for 24 months, the residual ammonia concentration of the tail gas from the reaction outlet is 116 ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.01925 m -1 , the average diameter of the droplets D 32 is 432 microns, and the droplet size distribution is D 10 of 392 microns, D 50 of 750 microns, and D 90 of 1439 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0038 m -1 , the average diameter of the droplets D 32 is 280 microns, and the droplet size distribution is D 10 of 159 microns, D 50 of 345 microns, and D 90 of 511 microns.
  • Example 2 The same as Example 2, the only difference is that the spray liquid input pressures at the spray liquid inlets of the spray devices 3a (b), 3c (d) and 3e (f) are 0.098 MPaG, 0.103 MPaG, and 0.108 MPaG, respectively, and the spray liquid spray pressures are 0.04 MPaG, respectively.
  • the nozzle outlet diameter of the spray device is 12.3 mm.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 132 ppm. After the device has been in operation for 24 months, the residual ammonia concentration of the tail gas from the reaction outlet is 181 ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0042 m -1 , the average diameter of the droplets D 32 is 2426 microns, and the droplet size distribution is D 10 of 1398 microns, D 50 of 2434 microns, and D 90 of 3390 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0012 m -1 , the average diameter of the droplets D 32 is 692 microns, and the droplet size distribution is D 10 of 547 microns, D 50 of 682 microns, and D 90 of 950 microns.
  • Example 2 The same as Example 2, except that the vertical spacing between two adjacent spraying devices is 1200 mm, and the distance between the ends of two adjacent third spraying pipes as shown in FIG6B is 707 mm.
  • the nozzle outlet diameter of the spraying device is 11.8 mm, and the spraying liquid spraying amount of each nozzle is 5.8 t/h.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 68 ppm.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 96 ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.005 m -1 , the average droplet diameter D 32 is 1623 ⁇ m, and the droplet size distribution is D 10 of 1189 ⁇ m, D 50 of 2148 ⁇ m, and D 90 of 2415 ⁇ m.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0021 m -1 , and the average droplet diameter is The D 32 was 432 ⁇ m, and the droplet size distribution was D 10 was 387 ⁇ m, D 50 was 601 ⁇ m, and D 90 was 914 ⁇ m.
  • each spraying device has 18 second spraying pipes, the second spraying pipes are provided with 7 to 20 third spraying pipes, the spacing between the second spraying pipes of the spraying device is 670mm, the inner diameter of the second spraying pipe is 80mm, and the end distance between two adjacent third spraying pipes as shown in Figure 6A is 335mm.
  • the spraying device has a total of 2000 nozzles, the nozzle outlet diameter of the spraying device is 11.3mm, the nozzle rotation chamber diameter is 30mm, the spraying angle is 65°, and the spraying liquid spraying amount of each nozzle is 2.64t/h.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 86ppm, and the residual ammonia concentration of the tail gas from the reaction outlet is 105ppm after the device has been in operation for 24 months.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0078 m -1 , the average diameter of the droplets D 32 is 1814 microns, and the droplet size distribution is D 10 of 1075 microns, D 50 of 2184 microns, and D 90 of 2851 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0015 m -1 , the average diameter of the droplets D 32 is 460 microns, and the droplet size distribution is D 10 of 437 microns, D 50 of 651 microns, and D 90 of 893 microns.
  • Example 2 The same as Example 2, except that the spray liquid input pressures of the spray liquid inlets of the spray devices 3a (b), 3c (d) and 3e (f) are 0.376 MPaG, 0.380 MPaG, and 0.385 MPaG, respectively; the spray liquid spray pressures are 0.045 MPaG, respectively, the vertical spacing between two adjacent spray devices is 550 mm, and the distance between the ends of two adjacent third spray pipes as shown in FIG6B is 707 mm.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 120 ppm
  • the residual ammonia concentration of the tail gas from the reaction outlet is 162 ppm after the device has been in operation for 24 months.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0042 m -1 , the average diameter of the droplets D 32 is 2154 microns, and the droplet size distribution is D 10 of 1096 microns, D 50 of 2628 microns, and D 90 of 2865 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0011 m -1 , the average diameter of the droplets D 32 is 367 microns, and the droplet size distribution is D 10 of 316 microns, D 50 of 484 microns, and D 90 of 616 microns. rice.
  • each spraying device has 24 second spraying pipes, and the second spraying pipes are provided with 9 to 24 third spraying pipes.
  • the spacing between the second spraying pipes of the spraying device is 580mm
  • the inner diameter of the second spraying pipe is 80mm
  • the distance between the ends of two adjacent third spraying pipes as shown in Figure 6A is 290mm.
  • the spraying device has a total of 2640 nozzles, the nozzle outlet diameter of the spraying device is 9.1mm, the nozzle rotation chamber diameter is 30mm, the spraying angle is 65°, and the spraying liquid spraying amount of each nozzle is 2.0t/h.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 146ppm
  • the residual ammonia concentration of the tail gas from the reaction outlet is 185ppm after the device has been in operation for 24 months.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0059 m -1 , the average diameter of the droplets D 32 is 1934 microns, and the droplet size distribution is D 10 of 1738 microns, D 50 of 2128 microns, and D 90 of 2665 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0013 m -1 , the average diameter of the droplets D 32 is 347 microns, and the droplet size distribution is D 10 of 284 microns, D 50 of 482 microns, and D 90 of 615 microns.
  • Example 2 The same as Example 2, except that the spray liquid output of each nozzle is 8.5t/h, the weight ratio of the spray liquid to the reaction product gas entering from the gas inlet is 32; the device has been in operation for 1 month, and the residual ammonia concentration of the tail gas at the reaction outlet is 85ppm, the device has been in operation for 24 months, and the residual ammonia concentration of the tail gas at the reaction outlet is 99ppm, and the acid consumption of the device in operation for 24 months/the acid consumption of the device in operation for 1 month is 1.03.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0016 m -1 , the average diameter of the droplets D 32 is 1712 microns, and the droplet size distribution is D 10 of 1138 microns, D 50 of 2324 microns, and D 90 of 2765 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0014 m -1 , the average diameter of the droplets D 32 is 787 microns, and the droplet size distribution is D 10 of 556 microns, D 50 of 832 microns, and D 90 of 1042 microns.
  • Example 2 The same as Example 2, except that the spray liquid output of each nozzle is 1.5 t/h, and the weight ratio of the spray liquid to the reaction product gas entering from the gas inlet is 11; the device has been in operation for 1 month, and the residual ammonia concentration of the tail gas at the reaction outlet is 145 ppm, the device has been in operation for 24 months, and the residual ammonia concentration of the tail gas at the reaction outlet is 178 ppm, and the acid consumption of the device in 24 months of operation/the acid consumption of the device in 1 month of operation is 1.05.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.005 m -1 , the average diameter of the droplets D 32 is 469 microns, and the droplet size distribution is D 10 of 409 microns, D 50 of 772 microns, and D 90 of 1091 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0012 m -1 , the average diameter of the droplets D 32 is 348 microns, and the droplet size distribution is D 10 of 159 microns, D 50 of 393 microns, and D 90 of 604 microns.
  • Example 2 It is the same as Example 2, except that the inlets of the spray devices 3a-3f are arranged at different positions of the equipment, the projections of the first spray pipes of the spray devices 3a-3f overlap on the cross section, and the projections of the second spray pipe, the third spray pipe and the nozzle on the cross section do not overlap.
  • the residual ammonia concentration of the exhaust gas at the reaction outlet is 137ppm
  • the residual ammonia concentration of the exhaust gas at the reaction outlet is 148ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0063 m -1 , the average diameter of the droplets D 32 is 1852 microns, and the droplet size distribution is D 10 of 1593 microns, D 50 of 1882 microns, and D 90 of 2191 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.001 m -1 , the average diameter of the droplets D 32 is 430 microns, and the droplet size distribution is D 10 of 392 microns, D 50 of 575 microns, and D 90 of 783 microns.
  • Example 2 The same as Example 2, the difference is that the nozzle diameter on the 1st to 11th second spray pipes of the first spray pipe along the fluid direction is 36 mm, and the nozzle diameter on the 12th to 14th second spray pipes of the first spray pipe is 32 mm; after the device has been in operation for 1 month, the residual ammonia concentration in the exhaust gas from the reaction outlet is 63 ppm, and after the device has been in operation for 24 months, the residual ammonia concentration in the exhaust gas from the reaction outlet is 99 ppm.
  • the extinction coefficient of the absorbing atmosphere is 0.0127 m -1
  • the average diameter D 32 of the droplets is 824 microns
  • the droplet size distribution is D 10
  • the D 10 of the absorbing atmosphere was 375 microns
  • the D 50 was 586 microns
  • the D 90 was 880 microns.
  • Example 2 The same as Example 2, the only difference is that the vertical spacing between two adjacent spraying devices is 1250 mm, the residual ammonia concentration of the tail gas from the reaction outlet is 77 ppm at the initial operation of the device, the residual ammonia concentration of the tail gas from the reaction outlet is 85 ppm after the device has been in operation for 24 months, and the acid consumption of the device in 24 months of operation/the acid consumption of the device in 1 month of operation is 1.04.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0094 m -1 , the average diameter of the droplets D 32 is 1408 microns, and the droplet size distribution is D 10 of 1009 microns, D 50 of 2083 microns, and D 90 of 2362 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0016 m -1 , the average diameter of the droplets D 32 is 469 microns, and the droplet size distribution is D 10 of 372 microns, D 50 of 579 microns, and D 90 of 880 microns.
  • Example 2 The same as Example 2, the only difference is that the vertical spacing between two adjacent spraying devices is 720 mm, the residual ammonia concentration of the tail gas from the reaction outlet is 111 ppm at the initial operation of the device, the residual ammonia concentration of the tail gas from the reaction outlet is 129 ppm after the device has been in operation for 24 months, and the acid consumption of the device in operation for 24 months/the acid consumption of the device in operation for 1 month is 1.07.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0143 m -1 , the average diameter of the droplets D 32 is 935 microns, and the droplet size distribution is D 10 of 616 microns, D 50 of 1323 microns, and D 90 of 1950 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0015 m -1 , the average diameter of the droplets D 32 is 420 microns, and the droplet size distribution is D 10 of 389 microns, D 50 of 480 microns, and D 90 of 632 microns.
  • Example 2 The same as Example 2, the only difference is that the vertical spacing between two adjacent spraying devices is 1650mm, the residual ammonia concentration of the tail gas from the reaction outlet is 177ppm at the initial operation of the device, the residual ammonia concentration of the tail gas from the reaction outlet is 195ppm after the device has been in operation for 24 months, and the acid consumption of the device in operation for 24 months/the acid consumption of the device in operation for 1 month is 1.05.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0053 m -1 , the average diameter of the droplets D 32 is 2215 microns, and the droplet size distribution is D 10 of 1295 microns, D 50 of 2489 microns, and D 90 of 3125 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 10350 mm above the gas inlet (located above the spraying device), the extinction coefficient of the absorbing atmosphere is 0.0011 m -1 , the average diameter of the droplets D 32 is 580 microns, and the droplet size distribution is D 10 of 319 microns, D 50 of 645 microns, and D 90 of 711 microns.
  • Example 2 The same as Example 2, the only difference is that the vertical spacing between two adjacent spraying devices is 550 mm, the device is operated for 1 month, the residual ammonia concentration of the reaction outlet exhaust gas is 129 ppm, the device is operated for 24 months, the residual ammonia concentration of the reaction outlet exhaust gas is 145 ppm, and the acid consumption of the device operating for 24 months/the acid consumption of the device operating for 1 month is 1.04.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0187 m -1 , the average diameter of the droplets D 32 is 895 microns, and the droplet size distribution is D 10 of 566 microns, D 50 of 1129 microns, and D 90 of 1921 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0011 m -1 , the average diameter of the droplets D 32 is 350 microns, and the droplet size distribution is D 10 of 219 microns, D 50 of 445 microns, and D 90 of 511 microns.
  • Example 2 The same as Example 2, the only difference is that the spray liquid input pressures at the spray liquid inlets of spray devices 3a (b), 3c (d) and 3e (f) are 0.405 MPaG, 0.421 MPaG, and 0.435 MPaG, respectively.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 65 ppm.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 89 ppm.
  • the extinction coefficient of the absorbing atmosphere is 0.0135 m -1
  • the average diameter D 32 of the droplets is 992 microns
  • the droplet size distribution is D 10
  • the D 10 of the absorbing atmosphere was 366 microns
  • the D 50 was 580 microns
  • the D 90 was 808 microns.
  • Example 2 The same as Example 2, the only difference is that the spray liquid input pressures of the spray liquid inlets of the spray devices 3a (b), 3c (d) and 3e (f) are 0.327 MPaG, 0.352 MPaG, and 0.376 MPaG, respectively.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 112 ppm.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 145 ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0094 m -1 , the average diameter of the droplets D 32 is 1432 microns, and the droplet size distribution is D 10 of 1032 microns, D 50 of 1789 microns, and D 90 of 2647 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0012 m -1 , the average diameter of the droplets D 32 is 497 microns, and the droplet size distribution is D 10 of 452 microns, D 50 of 620 microns, and D 90 of 913 microns.
  • Example 2 The same as Example 1, the only difference is that the vertical distance from the gas inlet to the spraying device 3f is 6000mm, the residual ammonia concentration of the tail gas from the reaction outlet at the initial operation of the device is 77ppm, and the device has been in operation for 24 months, and the residual ammonia concentration of the tail gas from the reaction outlet is 85ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0093 m -1 , the average diameter of the droplets D 32 is 1132 microns, and the droplet size distribution is D 10 of 932 microns, D 50 of 1248 microns, and D 90 of 2101 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 13500 mm above the gas inlet (above the spraying device), the extinction coefficient of the absorbing atmosphere is 0.0016 m -1 , the average diameter of the droplets D 32 is 372 microns, and the droplet size distribution is D 10 of 416 microns, D 50 of 491 microns, and D 90 of 638 microns.
  • Example 2 Same as Example 2, except that the vertical distance from the gas inlet to the spraying device 3f is 8000mm. At the beginning of the operation of the device, the residual ammonia concentration of the tail gas from the reaction outlet was 90ppm. After the device was operated for 24 months, the residual ammonia concentration of the tail gas from the reaction outlet was 106ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0062 m -1 , the average diameter of the droplets D 32 is 1520 microns, and the droplet size distribution is D 10 of 1249 microns, D 50 of 1742 microns, and D 90 of 2345 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 16000 mm above the gas inlet (above the spraying device), the extinction coefficient of the absorbing atmosphere is 0.0015 m -1 , the average diameter of the droplets D 32 is 326 microns, and the droplet size distribution is D 10 of 291 microns, D 50 of 485 microns, and D 90 of 794 microns.
  • Example 2 The same as Example 2, the only difference is that the vertical distance from the gas inlet to the spraying device 3f is 900mm, the residual ammonia concentration of the tail gas from the reaction outlet at the initial operation of the device is 125ppm, and the device has been in operation for 24 months, and the residual ammonia concentration of the tail gas from the reaction outlet is 142ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0055 m -1 , the average diameter of the droplets D 32 is 1220 microns, and the droplet size distribution is D 10 of 749 microns, D 50 of 1468 microns, and D 90 of 2845 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0016 m -1 , the average diameter of the droplets D 32 is 486 microns, and the droplet size distribution is D 10 of 419 microns, D 50 of 685 microns, and D 90 of 898 microns.
  • Example 2 The same as Example 2, the only difference is that the vertical distance from the gas inlet to the spraying device 3f is 500mm. At the initial stage of the device operation, the residual ammonia concentration of the tail gas from the reaction outlet is 182ppm. After the device has been in operation for 24 months, the residual ammonia concentration of the tail gas from the reaction outlet is 219ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0043 m -1 , the average droplet diameter D 32 is 1143 ⁇ m, and the droplet size distribution is D 10 of 648 ⁇ m, D 50 of 2163 ⁇ m, and D 90 of 3556 ⁇ m.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0018 m -1 , and the average droplet diameter is D 32 was 402 ⁇ m, and the droplet size distribution was D 10 was 284 ⁇ m, D 50 was 575 ⁇ m, and D 90 was 969 ⁇ m.
  • Example 2 The same as Example 2, the only difference is that a gas distributor 23 is provided in the tower. As shown in FIG4B , the residual ammonia concentration of the tail gas from the reaction outlet is 35 ppm. After the gas distribution internal components are added, the pressure of the ammonia absorption tower kettle increases by 10 KPa, resulting in an increase in the reaction pressure of the ammonia absorption tower front system by 10 KPa, and the yield of the target product nitrile decreases by 1.5%.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0127 m -1 , the average diameter of the droplets D 32 is 1068 microns, and the droplet size distribution is D 10 of 790 microns, D 50 of 1222 microns, and D 90 of 1960 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.002 m -1 , the average diameter of the droplets D 32 is 398 microns, and the droplet size distribution is D 10 of 376 microns, D 50 of 572 microns, and D 90 of 864 microns.
  • Example 2 The same as Example 2, the only difference is that the linear velocity of the reaction gas in the tower is 0.6 m/s, and the spraying amount of each nozzle is 2.8 t/h.
  • the residual ammonia concentration of the tail gas from the reaction outlet at the initial operation of the device is 82 ppm. After the device has been in operation for 24 months, the residual ammonia concentration of the tail gas from the reaction outlet is 99 ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.009 m -1 , the average diameter of the droplets D 32 is 1254 microns, and the droplet size distribution is D 10 of 895 microns, D 50 of 1405 microns, and D 90 of 2084 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0016 m -1 , the average diameter of the droplets D 32 is 486 microns, and the droplet size distribution is D 10 of 385 microns, D 50 of 568 microns, and D 90 of 880 microns.
  • Example 2 The same as Example 2, the only difference is that the linear velocity of the reaction gas in the tower is 1.4m/s, the spraying liquid spraying amount of each nozzle is 5.1t/h, the weight ratio of the spraying liquid to the reaction product gas entering from the gas inlet is 17, the residual ammonia concentration of the tail gas from the reaction outlet at the initial operation of the device is 132ppm, and the device After 24 months of operation, the residual ammonia concentration in the tail gas from the reaction outlet was 154 ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0191 m -1 , the average droplet diameter D 32 is 954 microns, and the droplet size distribution is D 10 of 595 microns, D 50 of 1389 microns, and D 90 of 2052 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0029 m -1 , the average droplet diameter D 32 is 390 microns, and the droplet size distribution is D 10 of 336 microns, D 50 of 564 microns, and D 90 of 882 microns.
  • Example 2 The same as Example 2, the only difference is that the linear velocity of the reaction gas in the tower is 0.4m/s, and the spraying amount of each nozzle is 2.0t/h.
  • the residual ammonia concentration of the tail gas from the reaction outlet at the initial operation of the device is 173ppm, and the residual ammonia concentration of the tail gas from the reaction outlet is 195ppm after the device has been in operation for 24 months.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.006 m -1 , the average diameter of the droplets D 32 is 1350 microns, and the droplet size distribution is D 10 of 985 microns, D 50 of 1549 microns, and D 90 of 2256 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.001 m -1 , the average diameter of the droplets D 32 is 416 microns, and the droplet size distribution is D 10 of 385 microns, D 50 of 581 microns, and D 90 of 872 microns.
  • the present invention is the same as Example 2, except that the linear velocity of the reaction gas in the tower is 1.9 m/s, the spray liquid output of each nozzle is 6.2 t/h, the weight ratio of the spray liquid to the reaction product gas entering from the gas inlet is 15, and the residual ammonia concentration of the tail gas from the reaction outlet at the initial operation of the device is 182 ppm. After the device has been in operation for 24 months, the residual ammonia concentration of the tail gas from the reaction outlet is 199 ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.02 m -1 , the average diameter of the droplets D 32 is 890 microns, and the droplet size distribution is D 10 of 522 microns, D 50 of 1234 microns, and D 90 of 2043 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0039 m -1 , the average diameter of the droplets D 32 is 361 microns, and the droplet size distribution is D 10 of 306 microns, D 50 of 514 microns, and D 90 of 847 microns.
  • Example 2 The same as Example 2, the only difference is that the ammonia absorption tower adopts the one-stage structure of Figure 4A, and the fluid directions in the first spray pipes of the spray devices 3a, 3b, 3c and 3d, 3e, 3f are opposite, that is, the spray inlet projections of the upper three layers of spray devices 3a, 3b, 3c are basically overlapped, and the spray inlet projections of the lower three layers of spray devices 3d, 3e, 3f are also basically overlapped, and the angle between the upper three layers and the lower three layers of spray inlet projections is 180°.
  • the residual ammonia concentration of the reaction outlet tail gas was 42ppm, and the residual ammonia concentration of the reaction outlet tail gas was 61ppm after the device was operated for 24 months, and the acid consumption of the device for 24 months/the acid consumption of the device for 1 month was 1.03.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0118 m -1 , the average diameter of the droplets D 32 is 934 microns, and the droplet size distribution is D 10 of 698 microns, D 50 of 1367 microns, and D 90 of 2182 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0019 m -1 , the average diameter of the droplets D 32 is 417 microns, and the droplet size distribution is D 10 of 392 microns, D 50 of 584 microns, and D 90 of 898 microns.
  • Example 2 The same as Example 2, the only difference is that the projections of the first spray pipes of the spray devices 3a, 3c, 3e and 3b, 3d, 3f on the cross section overlap, while the projections of the second spray pipe, the third spray pipe and the nozzle on the cross section do not overlap.
  • the residual ammonia concentration in the exhaust gas at the reaction outlet is 78ppm
  • the residual ammonia concentration in the exhaust gas at the reaction outlet is 95ppm
  • the acid consumption of the device in operation for 24 months/the acid consumption of the device in operation for 1 month is 1.05.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0103 m -1 , the average diameter of the droplets D 32 is 1146 microns, and the droplet size distribution is D 10 of 790 microns, D 50 of 1742 microns, and D 90 of 1956 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.002 m -1 , the average diameter of the droplets D 32 is 442 microns, and the droplet size distribution is D 10 of 401 microns, D 50 of 612 microns, and D 90 of 934 microns.
  • Example 2 The same as Example 2, except that the nozzle rotation chambers on the opposite sides of the 8 second spray pipes on each spray device are in opposite directions, and the nozzle rotation chambers on the opposite sides of the other 8 second spray pipes are in the same direction.
  • the residual ammonia concentration of the reaction outlet tail gas was 90ppm
  • the device was operated for 24 months
  • the residual ammonia concentration of the reaction outlet tail gas was 105ppm.
  • the acid consumption of the device for 24 months of operation/the acid consumption of the device for 1 month of operation was 1.04.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0103 m -1 , the average diameter of the droplets D 32 is 1231 microns, and the droplet size distribution is D 10 of 778 microns, D 50 of 1692 microns, and D 90 of 1923 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0018 m -1 , the average diameter of the droplets D 32 is 449 microns, and the droplet size distribution is D 10 of 420 microns, D 50 of 643 microns, and D 90 of 946 microns.
  • Example 2 It is the same as Example 2, except that the projections of the third spraying ends of the spraying devices overlap and the nozzles of adjacent spraying devices with overlapping projections rotate in opposite directions.
  • the residual ammonia concentration of the exhaust gas at the reaction outlet is 85 ppm.
  • the residual ammonia concentration of the exhaust gas at the reaction outlet is 110 ppm.
  • the acid consumption after the device has been in operation for 24 months/the acid consumption after the device has been in operation for 1 month is 1.05.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0100 m -1 , the average diameter of the droplets D 32 is 1327 microns, and the droplet size distribution is D 10 of 808 microns, D 50 of 1700 microns, and D 90 of 1906 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0018 m -1 , the average diameter of the droplets D 32 is 452 microns, and the droplet size distribution is D 10 of 424 microns, D 50 of 656 microns, and D 90 of 989 microns.
  • Example 2 The same as Example 2, the only difference is that the two adjacent nozzles on one side of the second spray pipe of the spray device rotate in opposite directions, and all the nozzles on the same horizontal parallel extension line of the second spray pipe rotate in the same direction.
  • the top view of the spray device is shown in Figure 11B, and the top view of the spray device is shown in Figure 11E.
  • the residual ammonia concentration of the reaction outlet tail gas was 106ppm.
  • the residual ammonia concentration of the reaction outlet tail gas was 125ppm.
  • the acid consumption/device operation after 24 months of operation The acid consumption in one month is 1.05.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0074 m -1 , the average diameter of the droplets D 32 is 1291 microns, and the droplet size distribution is D 10 of 728 microns, D 50 of 1702 microns, and D 90 of 2011 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.00145 m -1 , the average diameter of the droplets D 32 is 519 microns, and the droplet size distribution is D 10 of 436 microns, D 50 of 672 microns, and D 90 of 1046 microns.
  • Example 2 The same as in Example 2, except that all nozzles on the opposite sides of two adjacent second spray pipes of the spray device have the same rotation direction of spray liquid, and the nozzles on both sides of the same second spray pipe have opposite rotation directions of spray liquid.
  • the residual ammonia concentration of the tail gas at the reaction outlet was 108 ppm
  • the residual ammonia concentration of the tail gas at the reaction outlet was 121 ppm.
  • the acid consumption of the device for 24 months of operation/the acid consumption of the device for 1 month of operation was 1.04.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0072 m -1 , the average diameter of the droplets D 32 is 1345 microns, and the droplet size distribution is D 10 of 723 microns, D 50 of 1726 microns, and D 90 of 2071 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.00143 m -1 , the average diameter of the droplets D 32 is 503 microns, and the droplet size distribution is D 10 of 438 microns, D 50 of 699 microns, and D 90 of 1167 microns.
  • Example 2 The same as Example 2, the only difference is that the two adjacent nozzles on one side of the second spray pipe of the spray device rotate in opposite directions, and the nozzles on opposite sides of the same second spray pipe rotate in opposite directions.
  • the residual ammonia concentration of the reaction outlet tail gas was 125ppm
  • the residual ammonia concentration of the reaction outlet tail gas was 148ppm.
  • the acid consumption of the device for 24 months of operation/the acid consumption of the device for 1 month of operation was 1.05.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0064 m -1 , the average droplet diameter D 32 is 1446 ⁇ m, and the droplet size distribution is D 10 of 723 ⁇ m, D 50 of 1825 ⁇ m, and D 90 of 2270 ⁇ m.
  • the extinction coefficient of the absorbing atmosphere is 0.00141 m -1
  • the average droplet diameter D 32 is 513 ⁇ m
  • the droplet size distribution is D 10 of 420 ⁇ m, D 50 of 739 ⁇ m, and D 90 of 1190 ⁇ m.
  • Example 2 The same as Example 1, except that the rotation chamber directions of all nozzles of the spraying device are all the same, the device has been in operation for 1 month, and the residual ammonia concentration of the tail gas at the reaction outlet is 129ppm, the device has been in operation for 24 months, and the residual ammonia concentration of the tail gas at the reaction outlet is 149ppm, and the acid consumption of the device in operation for 24 months/the acid consumption of the device in operation for 1 month is 1.06.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0052 m -1 , the average diameter of the droplets D 32 is 1586 microns, and the droplet size distribution is D 10 of 723 microns, D 50 of 1825 microns, and D 90 of 2331 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0012 m -1 , the average diameter of the droplets D 32 is 545 microns, and the droplet size distribution is D 10 of 430 microns, D 50 of 780 microns, and D 90 of 1254 microns.
  • Example 2 The same as Example 2, except that the distance between adjacent third spray pipes is 300 mm, and the distance between the ends of two adjacent third spray pipes as shown in Figure 6A is 300 mm.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 76 ppm.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0051 m -1 , the average diameter of the droplets D 32 is 1620 microns, and the droplet size distribution is D 10 of 1182 microns, D 50 of 2145 microns, and D 90 of 2405 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0022 m -1 , the average diameter of the droplets D 32 is 430 microns, and the droplet size distribution is D 10 of 382 microns, D 50 of 604 microns, and D 90 of 924 microns.
  • Example 2 The same as Example 2, except that the distance between the ends of two adjacent third spray pipes as shown in Figure 6A is 340 mm.
  • the residual ammonia concentration of the tail gas from the reaction outlet is 105 ppm.
  • the absorption atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the absorption atmosphere
  • the extinction coefficient of the absorption atmosphere is 0.0079 m -1
  • the average droplet diameter D 32 is 1821 microns
  • the droplet size distribution is D 10 is 1077 microns
  • D 50 is 2180 microns
  • D 90 is 2855 microns.
  • the extinction coefficient of the absorption atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorption atmosphere is 0.00156 m -1
  • the average droplet diameter D 32 is 461 microns
  • the droplet size distribution is D 10 is 427 microns
  • D 50 is 654 microns
  • D 90 is 883 microns.
  • Example 2 The same as Example 2, except that the nozzle outlet diameter on the 1st to 11th second spray pipes of the first spray pipe along the fluid direction is 11.7 mm, and the nozzle outlet diameter on the 12th to 14th second spray pipes of the first spray pipe is 11.9 mm; after the device has been in operation for 1 month, the residual ammonia concentration in the tail gas at the reaction outlet is 85 ppm, and after the device has been in operation for 24 months, the residual ammonia concentration in the tail gas at the reaction outlet is 99 ppm, and the acid consumption of the device in operation for 24 months/the acid consumption of the device in operation for 1 month is 1.03.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.00161 m -1 , the average droplet diameter D 32 is 1722 microns, and the droplet size distribution is D 10 of 1128 microns, D 50 of 2310 microns, and D 90 of 2785 microns.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0014 m -1 , the average droplet diameter D 32 is 777 microns, and the droplet size distribution is D 10 of 536 microns, D 50 of 841 microns, and D 90 of 998 microns.
  • Example 2 The same as Example 1, except that the ammonia absorption tower adopts the two-stage structure of Figure 1, the spray liquid input pressures of the spray liquid inlets of the spray devices 3a, 3b, 3c, and 3d are 0.04MPaG, 0.044MPaG, 0.046MPaG, and 0.051MPaG, respectively, the spray liquid spraying pressure is 0.02MPaG, the nozzle outlet diameter is 14.2mm, and the initial operation of the device, the residual ammonia concentration of the tail gas from the reaction outlet is 400ppm, and the device has been in operation for 24 months, and the residual ammonia concentration of the tail gas from the reaction outlet is 529ppm.
  • the spray liquid input pressures of the spray liquid inlets of the spray devices 3a, 3b, 3c, and 3d are 0.04MPaG, 0.044MPaG, 0.046MPaG, and 0.051MPaG, respectively, the spray liquid spraying pressure is 0.02MPaG, the nozzle outlet diameter is 14.2mm, and the initial
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0033 m -1 , the average droplet diameter D 32 is 2976 ⁇ m, and the droplet size distribution is D 10 of 1298 ⁇ m, D 50 of 3174 ⁇ m, and D 90 of 3990 ⁇ m.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0008 m -1 , the average droplet diameter D 32 is 742 ⁇ m, and the droplet size distribution is D 10 of 523 ⁇ m, D 50 of 882 ⁇ m, and D 90 of 1050 ⁇ m.
  • Micrometer when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere is 0.0033 m -1 , the average droplet diameter D 32 is 2976 ⁇ m, and the droplet size distribution is
  • Example 2 The same as Example 2, except that the ammonia absorber adopts the one-stage structure of Figure 2, spray devices 3a, 3b, 3c, 3d, 3e and 3f, the spray liquid input pressure at the spray liquid inlet is 1.202MPaG, 1.205MPaG, 1.209MPaG, 1.214MPaG, 1.217MPaG, 1.220MPaG, respectively, the spray liquid spray pressure is 0.076MPaG, the initial operation of the device, the residual ammonia concentration of the tail gas from the reaction outlet is 85ppm, the device has been in operation for 24 months, and the residual ammonia concentration of the tail gas from the reaction outlet is 96ppm, but 1.5% of ammonium sulfate is detected in the tail gas condensate at the outlet of the ammonia absorber.
  • the spray liquid input pressure at the spray liquid inlet is 1.202MPaG, 1.205MPaG, 1.209MPaG, 1.214MPaG, 1.217MPaG, 1.220MPaG,
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere was 0.0263 m -1 , the average droplet diameter D 32 was 369 ⁇ m, and the droplet size distribution was D 10 of 232 ⁇ m, D 50 of 550 ⁇ m, and D 90 of 1239 ⁇ m.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere was 0.0052 m -1 , the average droplet diameter D 32 was 231 ⁇ m, and the droplet size distribution was D 10 of 149 ⁇ m, D 50 of 315 ⁇ m, and D 90 of 436 ⁇ m.
  • Example 1 The same as Example 1, the only difference is that the spray inlet 18 of the spray devices 3a, 3c and 3b, 3d is on the same side of the ammonia absorption tower, that is, the direction of the fluid in the first spray pipe is the same, the spray inlet projections of the spray devices 3a, 3b, 3c and 3d basically overlap, (as shown in Figure 1), and the projections of the nozzles at the end of the third spray pipes of the spray devices 3a, 3c and 3b, 3d on the cross section overlap (as shown in Figure 5).
  • the residual ammonia concentration of the reaction outlet tail gas was 85ppm
  • the device was operated for 24 months
  • the residual ammonia concentration of the reaction outlet tail gas was 253ppm
  • the acid consumption of the device in 24 months of operation/the acid consumption of the device in 1 month of operation was 1.13.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere was 0.0038 m -1 , the average droplet diameter D 32 was 1386 ⁇ m, and the droplet size distribution was D 10 of 523 ⁇ m, D 50 of 1725 ⁇ m, and D 90 of 2831 ⁇ m.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere was 0.0008 m -1 , the average droplet diameter D 32 was 545 ⁇ m, and the droplet size distribution was D 10 of 130 ⁇ m, D 50 of 680 ⁇ m, and D 90 of 1454 ⁇ m.
  • Example 2 The same as Example 2, the only difference is that the spray inlet 18 of the spraying devices 3a, 3c, 3e and 3b, 3d, 3f is on the same side of the ammonia absorption tower, that is, the direction of the fluid in the first spray pipe is the same, the spray inlet projections of the spraying devices 3a, 3b, 3c, 3d, 3e, 3f basically overlap, (as shown in Figure 2), and the projections of the nozzles at the end of the third spray pipes of the spraying devices 3a, 3c and 3b, 3d on the cross section overlap (as shown in Figure 5).
  • the device was operated for 1 month, and the residual ammonia concentration of the reaction outlet tail gas was 73ppm.
  • the device was operated for 24 months, and the residual ammonia concentration of the reaction outlet tail gas was 223ppm.
  • the acid consumption of the device for 24 months of operation/the acid consumption of the device for 1 month of operation was 1.13.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere was 0.0039 m -1 , the average droplet diameter D 32 was 1356 ⁇ m, and the droplet size distribution was D 10 of 521 ⁇ m, D 50 of 1856 ⁇ m, and D 90 of 2913 ⁇ m.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere was 0.0008 m -1 , the average droplet diameter D 32 was 536 ⁇ m, and the droplet size distribution was D 10 of 137 ⁇ m, D 50 of 649 ⁇ m, and D 90 of 1450 ⁇ m.
  • Example 2 The same as Example 2, the only difference is that the spray inlet 18 of the spray devices 3a, 3c, 3e and 3b, 3d, 3f is projected at 30° on the cross section, that is, the fluid direction of the corresponding first spray pipe of the spray device is 30°, and the projection of the end of the third spray pipe of the spray device does not overlap, as shown in Figure 8B.
  • the residual ammonia concentration of the reaction outlet tail gas was 130ppm
  • the device was operated for 24 months
  • the residual ammonia concentration of the reaction outlet tail gas was 343ppm
  • the acid consumption of the device in 24 months of operation/the acid consumption of the device in 1 month of operation was 1.15.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere was 0.0034 m -1 , the average droplet diameter D 32 was 1672 ⁇ m, and the droplet size distribution was D 10 of 540 ⁇ m, D 50 of 1738 ⁇ m, and D 90 of 3213 ⁇ m.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere was 0.0008 m -1 , the average droplet diameter D 32 was 436 ⁇ m, and the droplet size distribution was D 10 of 189 ⁇ m, D 50 of 649 ⁇ m, and D 90 of 1550 ⁇ m.
  • the difference is only in the spraying devices 3a, 3c, 3e and 3b, 3d, 3f.
  • the projection of the spray inlet 18 on the cross section is 90°, that is, the fluid direction of the corresponding first spray pipe of the spray device is 90°, and the projection of the end of the third spray pipe of the spray device does not overlap.
  • the residual ammonia concentration of the tail gas at the reaction outlet is 110ppm.
  • the residual ammonia concentration of the tail gas at the reaction outlet is 293ppm.
  • the acid consumption of the device running for 24 months/the acid consumption of the device running for 1 month is 1.10.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere was 0.0035 m -1 , the average droplet diameter D 32 was 1582 ⁇ m, and the droplet size distribution was D 10 of 640 ⁇ m, D 50 of 1714 ⁇ m, and D 90 of 3138 ⁇ m.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere was 0.0009 m -1 , the average droplet diameter D 32 was 461 ⁇ m, and the droplet size distribution was D 10 of 259 ⁇ m, D 50 of 618 ⁇ m, and D 90 of 1489 ⁇ m.
  • Example 2 The same as Example 2, the only difference is that the spray inlet 18 of the spray devices 3a, 3c, 3e and 3b, 3d, 3f is projected at 120° on the cross section, that is, the fluid direction of the corresponding first spray pipe of the spray device is 90°, and the projection of the end of the third spray pipe of the spray device does not overlap, as shown in Figure 8B.
  • the residual ammonia concentration of the reaction outlet tail gas was 132ppm
  • the device was operated for 24 months
  • the residual ammonia concentration of the reaction outlet tail gas was 353ppm
  • the acid consumption of the device for 24 months of operation/the acid consumption of the device for 1 month of operation was 1.15.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 3000 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere was 0.0032 m -1 , the average droplet diameter D 32 was 2522 ⁇ m, and the droplet size distribution was D 10 of 678 ⁇ m, D 50 of 2924 ⁇ m, and D 90 of 3738 ⁇ m.
  • the extinction coefficient of the absorbing atmosphere when measured at a vertical distance of 8500 mm above the gas inlet, the extinction coefficient of the absorbing atmosphere was 0.0006 m -1 , the average droplet diameter D 32 was 491 ⁇ m, and the droplet size distribution was D 10 of 259 ⁇ m, D 50 of 876 ⁇ m, and D 90 of 1573 ⁇ m.

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Abstract

一种改善氨吸收效果的腈的制造方法，包括反应步骤：使烃原料发生氨氧化反应而制造包含腈的反应产物，和冷却步骤：通过气体入口将反应产物引入吸收装置并在吸收装置中通过喷洒装置向反应产物喷洒喷洒液以冷却反应产物并形成吸收气氛，其中在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.004-0.02m -1。该方法可以使喷洒液雾化，增加与氨的接触面积，改善氨吸收效果。

Description

一种氨吸收效果改善的腈的制造方法 技术领域
本发明涉及气体吸收技术领域，更具体涉及一种氨吸收效果改善的腈的制造方法。
背景技术
氨化或氨氧化法生成相应地腈类的工艺路线，为使得烃类等原料气尽量转化，一般原料气氨均为过量，即氨与原料气烃类摩尔比大于1，如丙烯氨氧化中，氨比(氨与丙烯摩尔比)为1.10-1.35，芳烃氨氧化中，氨比(氨与芳烃摩尔比)为4-8，因此，反应器出口尾气中一定含有未反应的氨。一方面如丙烯腈生产工艺中，反应气体中丙烯腈等在碱性条件下易发生聚合，另一方面即便有少量未反应氨的逃逸也容易造成对环境的污染，因此，在氨化或氨氧化工艺中，都需要利用吸收装置(一般称为氨吸收塔或急冷塔)用酸或水将气相中的未反应氨去除，这个过程是十分必要的。
随着生产技术的发展，生产负荷也不断提高，装置大型化、规模化是未来发展的趋势，装置负荷越高，相对而言，包括吸收装置在内的设备也同步越大。已知的是，在吸收装置中，循环液(喷洒液)经喷洒装置散布于吸收装置内，与含氨气体逆向接触而吸收，达到去除气相中的剩余氨的目的。
专利CN105425849通过对吸收装置流出物中PH值，调整添加酸的量来去除剩余氨；专利CN1199940通过在吸收装置底部增加内构件的方式，改善气液两相传质传热效果，其实质是解决含氨气相均匀分布的问题。但是，吸收装置仍然不可避免的会发生氨穿透情况，即仍存在少量氨的逃逸，在后续精制分离单元中导致产品损失或造成对环境的污染。
现有技术的氨吸收方法，在吸收装置长周期运行之后，吸收尾气中的氨含量与运行初期相比明显增加。
发明内容
在氨吸收塔内，喷洒液由泵输送至喷嘴，由于喷洒液具有很高的压力，喷洒液由切线入口进入喷嘴空腔，获得旋转运动，通过特殊结构的喷嘴后，喷洒液从喷嘴高速喷出，分裂成无数个小雾滴。大部分的雾滴受自身重力和旋转运动离心力影响，向塔下方运动，这部分雾滴与从下而上的气体逆向接触，同时也存在很少一部分雾滴会被气体夹带向塔上方运行。塔内，设置有多层喷洒装置，每个喷洒装置上又含有几十甚至上百个喷嘴均匀分布在截面上，在装置操作运行时，在气流的加权作用下，塔内喷洒装置的区域范围，充满了无数个小液滴。而液滴对可见光和红外信号均可产生较强的衰减，通过红外光谱辐射法或前向散射法测量塔内液滴的消光系数，可以对雾滴粒径大小、数量、分布等进行综合评估。通常情况，雾滴大，雾滴数量小，对光的吸收小，光的透射率高，消光系数小，反之就大。
本发明的发明人发现，通过将吸收气氛的消光系数设置在特定的数值范围之内，就可以解决该问题。本发明基于该发现而完成。
具体而言，本发明涉及以下方面的内容。
1.一种腈的制造方法，包括使烃原料发生氨氧化反应而制造包含腈的反应产物的步骤(称为反应步骤)、和通过气体入口将所述反应产物引入吸收装置并在所述吸收装置中通过喷洒装置向所述反应产物喷洒喷洒液以冷却所述反应产物并形成吸收气氛的步骤(称为冷却步骤)，其中在所述气体入口上方垂直距离为3000mm处测量时，所述吸收气氛的消光系数为0.004-0.02m-1(优选0.006-0.018m-1)。
2.前述或后述任一方面所述的制造方法，其中在所述气体入口上方垂直距离为3000mm处测量时，所述吸收气氛的液滴平均直径D32为400-2600微米(优选600-2400微米)，和/或，在所述气体入口上方垂直距离为3000mm处测量时，所述吸收气氛的液滴粒径分布D10为150-1500微米,D50为700-3000微米，D90为1400-3600微米(优选D10为250-1400微米,D50为800-2800微米，D90为1600-3500微米)。
3.前述或后述任一方面所述的制造方法，其中在所述气体入口上方垂直距离为8500mm处测量时，所述吸收气氛的消光系数为0.001-0.004m-1(优选0.0015-0.0035m-1)，和/或，在所述气体入口上方垂直距离为8500mm处测量时，所述吸收气氛的液滴平均直径D32为200-1400微米(优选400-1000微 米)，和/或，在所述气体入口上方垂直距离为8500mm处测量时，所述吸收气氛的液滴粒径分布D10为100-1000微米,D50为300-1800微米，D90为500-2200微米(优选D10为200-600微米,D50为400-1400微米，D90为600-1800微米)。
4.前述或后述任一方面所述的制造方法，其中所述喷洒装置包括喷洒液入口、与所述喷洒液入口流体连通的第一喷洒管、与所述第一喷洒管流体连通且垂直于所述第一喷洒管向其两侧延伸的多个(比如10-26个，优选12-22个)第二喷洒管、与所述第二喷洒管流体连通且垂直于所述第二喷洒管向其两侧延伸的多个(比如4-26个，优选6-22个)第三喷洒管、以及位于所述第三喷洒管末端且与其流体连通的喷嘴。
5.前述或后述任一方面所述的制造方法，其中在相邻的两个第二喷洒管上，一个第二喷洒管上的任意一个第三喷洒管的末端与另一个相邻第二喷洒管上的任意一个第三喷洒管的末端的直线距离M不小于320mm(优选不小于350mm)，和/或，所述喷嘴彼此相同或不同，喷洒液喷出量各自独立地为0.5-7.5t/h(优选0.9-6.5t/h)，和/或，所述喷嘴彼此相同或不同，喷嘴出口的喷洒液喷出压力各自独立地为0.03-0.85MPaG(优选0.04-0.65MPaG)，和/或，将所述喷洒液入口的喷洒液输入压力控制在0.06-1.00MPaG(优选为0.12-0.90MPaG，更优选为0.18-0.80MPaG)，和/或，任意两个所述喷洒装置的喷洒液入口的喷洒液输入压力的差异(绝对值)小于0.024MPa(优选小于0.018MPa，更优选小于0.012MPa)。
6.前述或后述任一方面所述的制造方法，其中多个(比如2-10个，优选4-8个)所述喷洒装置以预定的垂直间距沿着所述吸收装置的中心轴线方向分层设置在所述吸收装置内部，和/或，相邻两个所述喷洒装置的垂直间距(按喷洒装置的喷洒液入口的垂直间距计)为650-1350mm(优选750-1200mm)。
7.前述或后述任一方面所述的制造方法，其中在垂直于所述吸收装置的中心轴线方向横切所述吸收装置而获得横截面时，所述多个喷洒装置中的一个与所述多个喷洒装置中的另一个的选自第一喷洒管、第二喷洒管和第三喷洒管中的至少一个(优选全部)在所述横截面上的投影基本上重合。
8.前述或后述任一方面所述的制造方法，其中所述一个喷洒装置与所述另一个喷洒装置的全部喷嘴在所述横截面上的投影基本上重合，和/或，投影基本上重合的两个喷嘴具有相同的喷洒直径，和/或，投影基本上重合的两个 喷嘴具有相同的喷洒液旋转方向。
9.前述或后述任一方面所述的制造方法，其中所述气体入口与所述喷洒装置(在存在多个时，指的是距离所述气体入口最近的所述喷洒装置)的喷洒液入口的垂直距离为800-6000mm(优选1000-5000mm)，和/或，所述气体入口的内径为800-1900mm(优选900-1700mm)，和/或，所述反应产物在所述吸收装置内的线速度为0.6-1.5m/s(优选0.7-1.3m/s)，和/或，所述喷洒液与所述反应产物的质量流量比为15-25:1。
10.前述或后述任一方面所述的制造方法，其中在所述气体入口与所述喷洒装置(在存在多个时，指的是距离所述气体入口最近的所述喷洒装置)之间的吸收装置内部空间，不设置能够实质性影响所述气体流动的机械构件。
11.前述或后述任一方面所述的制造方法，其中所述一个喷洒装置与所述另一个喷洒装置的喷洒液入口在所述横截面上的投影之间的夹角为180°。
12.前述或后述任一方面所述的吸收装置，其中在全部所述喷洒装置中，任意两个奇数编号的所述喷洒装置的喷洒液入口在所述横截面上的投影之间的夹角为0°，任意两个偶数编号的所述喷洒装置的喷洒液入口在所述横截面上的投影之间的夹角为0°，并且任一奇数编号的所述喷洒装置与任一偶数编号的所述喷洒装置的喷洒液入口在所述横截面上的投影之间的夹角为180°。
13.前述或后述任一方面所述的吸收装置，其中所述喷嘴包括喷嘴入口、旋转室和喷嘴出口，其中所述旋转室被构造为使得从所述喷嘴入口进入的喷洒液在经过所述旋转室之后以旋转方式离开所述喷嘴出口。
14.前述或后述任一方面所述的吸收装置，其中在至少一个(优选全部)所述第二喷洒管上，位于所述第二喷洒管的相同一侧的相邻两个(优选全部)喷嘴被构造为使得喷洒液以相同的旋转方向喷出。
15.前述或后述任一方面所述的吸收装置，其中并排相邻的两个所述第二喷洒管的相向一侧的全部喷嘴被构造为使得喷洒液以相反的旋转方向喷出。
16.前述或后述任一方面所述的吸收装置，其中在至少一个(优选全部)所述第二喷洒管上，位于所述第二喷洒管的一侧的至少一个(优选全部)喷嘴被构造为使得喷洒液以旋转方向A喷出，位于所述第二喷洒管的相对另一侧的至少一个(优选全部)喷嘴被构造为使得喷洒液以旋转方向B喷出，其 中所述旋转方向A与所述旋转方向B相反。
17.前述或后述任一方面所述的吸收装置，其中在所述喷洒装置的全部喷嘴中，以所述旋转方向A喷出喷洒液的喷嘴的数量与以所述旋转方向B喷出喷洒液的喷嘴的数量相等或基本上相等。
18.前述或后述任一方面所述的制造方法，其中所述多个第二喷洒管垂直于所述第一喷洒管向其相对两侧沿水平方向基本上平行延伸，和/或，所述多个第三喷洒管垂直于所述第二喷洒管向其相对两侧沿水平方向基本上平行延伸。
19.前述或后述任一方面所述的制造方法，其中所述第一喷洒管的内径为160-480mm(优选200-450mm)，长度为4500-11500mm(优选4800-10500mm)，和/或，所述多个第二喷洒管彼此相同或不同，内径各自独立地为30-150mm(优选40-120mm)，长度各自独立地为1200-5750mm(优选1800-5250mm)，和/或，所述多个第三喷洒管彼此相同或不同，内径各自独立地为10-60mm(优选15-50mm)，长度各自独立地为160-325mm(优选175-300mm)。
20.前述或后述任一方面所述的制造方法，其中所述喷嘴彼此相同或不同，内径(指的是喷嘴出口)各自独立地为3-20mm(优选6-14mm)，旋转室的直径各自独立地为10.0-55.0mm(优选为13.0-45.0mm)，喷洒角度各自独立地为65-120°(优选70-100°)。
21.前述或后述任一方面所述的制造方法，其中在所述第一喷洒管上，相邻两个第二喷洒管的水平间距为640-1300(优选700-1200mm)，和/或，在同一个所述第二喷洒管上，相邻两个第三喷洒管的水平间距为320-650mm(优选350-600mm)。
22.前述或后述任一方面所述的制造方法，其中在所述冷却步骤中，所述喷洒液与所述反应产物以逆流方式接触。
23.前述或后述任一方面所述的制造方法，其中所述吸收装置的内径为4.5-11.5m(优选4.8-10.5m)。
24.前述或后述任一方面所述的制造方法，其中所述气体入口沿着所述吸收装置的中心轴线方向位于所述喷洒装置的下方。
25.前述或后述任一方面所述的制造方法，其中在所述反应步骤中，所述烃原料是丙烯，丙烯/氨气/空气(以分子氧计)的摩尔比为1：1.1-1.3： 1.8-2.0，反应温度为420-440℃，反应压力(表压)为0.03-0.14MPa，催化剂重时空速为0.06-0.15h-1，或者，所述烃原料是异丁烯，异丁烯/氨气/空气(以分子氧计)的摩尔比为1：1.3-1.6：2.2-2.8，反应温度为395-420℃，反应压力(表压)为0.03-0.14MPa，催化剂重时空速为0.08-0.17h-1。
26.前述或后述任一方面所述的制造方法，其中在所述冷却步骤中，所述喷洒液使得所述反应产物的温度从195-235℃冷却至81-86℃，和/或，在所述冷却步骤中，所述喷洒液使得所述反应产物的氨含量降低至150ppm以下。
27.前述或后述任一方面所述的吸收装置，其中所述旋转方向A是顺时针方向，所述旋转方向B是逆时针方向。
技术效果
根据本发明，即使长周期运行(比如连续运行18个月甚至更长时间)，吸收尾气中的氨含量与运行初期相比也不明显增加，可以长周期维持良好的氨吸收效果，减少氨的逃逸。
根据本发明，即使长周期运行(比如连续运行18个月甚至更长时间)，酸的总消耗依然可以维持较低的水平，增加幅度较小(比如在3％以下)。
根据本发明，氨气在吸收塔内分布均匀，有利于氨吸收。
根据本发明，气液接触充分，氨吸收效果佳，可以降低酸的使用量。
附图说明
图1是现有技术的氨吸收塔正视示意图。
图2是现有技术的氨吸收塔正视示意图。
图3a、图3b是本发明的氨吸收塔正视示意图。
图4A、图4B是本发明的氨吸收塔正视示意图。
图5是本发明的喷洒装置俯视示意图。
图6A、图6B是本发明的喷洒装置俯视示意图。
图7是本发明的喷洒装置俯视示意图。
图8A、图8B是对比例喷洒装置俯视示意图。
图9A、图9B是现有技术的喷嘴俯视和正视示意图。
图10A、图10B是现有技术的喷洒装置俯视示意图和俯视细节图。
图11A是本发明喷嘴两种旋转方式俯视/正视示意图。图11B是喷洒装置俯视示意图。
图11C是本发明一种喷洒装置俯视示意图的细节图。图11D是本发明另一种喷洒装置俯视示意图的细节图。图11E是本发明另一种喷洒装置俯视示意图的细节图。
附图标记说明：
1：氨吸收塔
2：氨吸收塔内构件除沫器
3：氨吸收塔内构件喷洒装置，3a-3f为喷洒装置
4：氨吸收塔内构件气体分布器
5：氨吸收塔内构件喷洒装置，5a-5b为喷洒装置
6：上段循环泵
7：下段循环泵
8：含氨气体进料
9：氨吸收塔气相出料
10：上段补水
11：下段废水出料
12：上段含铵盐溶液出料
13：下段循环液
14：上段循环液
15：含酸溶液
16：循环液
17：循环泵
18：喷洒装置入口
19：喷洒装置第一喷洒管
20a、20b：喷洒装置第二喷洒管
21：喷洒装置第三喷洒管
22：喷洒装置雾化喷嘴
23:气体分布器
P1、P2、P3、P4、P5、P6：喷洒装置喷洒液的入口压力。
具体实施方式
下面对本发明的具体实施方式进行详细说明，但是需要指出的是，本发明的保护范围并不受这些具体实施方式的限制，而是由附录的权利要求书来确定。
本说明书提到的所有出版物、专利申请、专利和其它参考文献全都引于此供参考。除非另有定义，本说明书所用的所有技术和科学术语都具有本领域技术人员常规理解的含义。在有冲突的情况下，以本说明书的定义为准。
当本说明书以词头“本领域技术人员公知”、“现有技术”或其类似用语来导出材料、物质、方法、步骤、装置或部件等时，该词头导出的对象涵盖本申请提出时本领域常规使用的那些，但也包括目前还不常用，却将变成本领域公认为适用于类似目的的那些。
在本说明书的上下文中，所谓基本上，指的是偏离不超过10％，优选不超过5％或2％。
在本说明书的上下文中，消光系数的测量方法是前向近红外散射光谱法，在可见光范围的强辐射区，采用近红外的LED光源照射至约100ml取样体积上，测量前向25°-45°范围内的散射光强I(θ)，进而计算出消光系数σ,计算式为σ＝I(θ)/k,其中，k为散射消光比，可由高精度的透射仪进行标定。
在本说明书的上下文中，液滴平均直径D32的测量方法是基于激光成像测量平面液滴粒径，从雾滴图像信息中获得2D空间分辩的沙德平均粒径D32，平面全局液滴粒径测量需同时记录被测液滴对象的激光诱导荧光信号LIF，和米式散射信号MIE图像，2维的沙德平均粒径通过这两个图像信号的比值求出。LIf图像代表液滴的体积，MIE光基本上与液滴总量成正比，
D32＝液滴体积总和/液滴面积总和＝LIf信号/MIE信号。
在本说明书的上下文中，液滴粒径分布的测量方法是同液滴平均直径D32测量方法一样，基于激光成像测液滴粒度分布，从雾滴图像信息中获得2D空间分辩的各个粒径分布D10、D50、D90等。
在没有明确指明的情况下，本说明书内所提到的所有百分数、份数、比率等都是以重量为基准的，而且压力是表压。
在本说明书的上下文中，本发明的任何两个或多个实施方式都可以任意组合，由此而形成的技术方案属于本说明书原始公开内容的一部分，同时也落入本发明的保护范围。
在本说明书的上下文中，所有没有提到的技术细节等，直接适用本领域已知的相关信息。
根据本发明的一个实施方式，涉及一种腈的制造方法，特别是(甲基)丙烯腈的制造方法。
根据本发明的一个实施方式，所述腈的制造方法包括使烃原料发生氨氧化反应而制造包含腈的反应产物的步骤(称为反应步骤)、和通过气体入口将所述反应产物引入吸收装置并在所述吸收装置中通过喷洒装置向所述反应产物喷洒喷洒液以冷却所述反应产物并形成吸收气氛的步骤(称为冷却步骤)。在本领域中，所述吸收装置一般也称为氨吸收塔或急冷塔。
根据本发明，在所述气体入口上方垂直距离为3000mm处测量时，所述吸收气氛的消光系数为0.004-0.02m-1(优选0.006-0.018m-1)。本发明的发明人发现，由于液滴对可见光和红外信号均产生较强的衰减，通过测量光的衰减情况，计算出其消光系数的，可用来综合评价液体经喷嘴高速喷出后分散效果。对于等量的液体经喷嘴后被打散成若干个小液滴，通常情况，液滴粒径越大，液滴数量相对越小，对光的吸收小，光的透射率高，消光系数小，反之就大。消光系数小，意味着液滴粒径大、数量少，这些液滴表面积总量相对就小，由于与气体氨接触的面积不足，导致氨吸收效率下降，造成更多的氨穿透。反之，消光系数大，意味着液滴粒径小、数量多，而这些过小粒径的液滴被气体夹带往上运动，容易被带离出塔，在氨吸收塔内，液滴中含有的铵盐随气体至后序流程中，会增加环保负担，这也是要尽可能避免的。
根据本发明的一个优选实施方式，在所述气体入口上方垂直距离为3000mm处测量时，所述吸收气氛的液滴平均直径D32为400-2600微米(优选600-2400微米)。本发明的发明人发现，液体从喷嘴喷出的一瞬间，液膜被撕裂成小液滴，小液滴在下落过程中，与其他液滴发生碰撞时，存在分离、聚合、破碎等情况，通过光学法可以测量液滴的平均粒径。当液滴的平均粒径 大于2600mm时，一方面由于重力作用，液滴向下速度越快，液滴在塔内停留时间明显缩短，容易因与气体接触时间不足导致吸收效率下降，另一方面，相同体积的两液滴，一个大粒径的液滴的表面积小于分裂成两个小粒径液滴的表面积，也即相对于两小液滴，一个大粒径的液滴获得更少的与气体接触的机会，也同样会导致吸收效率的降低。而在液滴平均粒径小于400mm时，由于气体向上对液滴的托举力克服了液滴自身的重力，液滴更容易被夹带，同时也需要更多的动力，如喷洒装置的入口压力，在液体经过喷嘴喷出时被撕裂的更小。
根据本发明的一个优选实施方式，在所述气体入口上方垂直距离为3000mm处测量时，所述吸收气氛的液滴粒径分布为D10为150-1500微米,D50为700-3000微米，D90为1400-3600微米(优选D10为250-1400微米,D50为800-2800微米，D90为1600-3500微米)。本发明的发明人发现，液体从喷嘴喷出后会被撕裂成无数个不同粒径的小液滴，同时存在着两液滴在碰撞过程中，粒径可能发生因聚合变大或因破碎变小或分离不变的情况。在具体实施方案中，循环液中为含酸的液体，吸收气氛为含氨气体，液滴中的酸吸收气相中氨后形成铵盐存在于液滴，若液滴D10和/或D50和/或D90较小，也就意味着液滴D32较小，含铵盐的液滴易被气体夹带逃离塔器，给后序工艺中处理带来新的问题，如循环液中含硫酸，在废水焚烧的产生的含SO2气体，如循环液中含磷酸，则产生P2O5，这些都是对环境不友好的，应尽量避免。
根据本发明的一个进一步优选的实施方式，在所述气体入口上方垂直距离为8500mm处测量时，所述吸收气氛的消光系数为0.001-0.004m-1(优选0.0015-0.0035m-1)。本发明的发明人发现，测量位置位于吸收塔喷洒装置的上方，该区域的液滴为被气体夹带所致，与前述测量位置的液滴粒径相比，该区域液滴粒径相对较小，且气体夹带量也在可控的范围内。而吸收气氛在消光系数低于0.001m-1时，说明喷洒装置区域的液滴粒径偏大，气体对其向上的推力小于其重力，导致液滴的夹带量偏小，而喷洒装置区域液滴粒径偏大，气液接触不充分，容易导致吸收气氛(如：氨)的穿透；在消光系数大于0.004m-1时，在液滴粒径正常的情况下，说明气体夹带的液滴数量较多，存在气体通过塔器速度较大的可能，气体因在塔器内停留时间不足，导致吸收不完全，效率低，造成吸收气氛(如：氨)的穿透。
根据本发明的一个优选实施方式，在所述气体入口上方垂直距离为8500mm处测量时，所述吸收气氛的液滴平均直径D32为200-1400微米(优选400-1000微米)。更为优选的是，在所述气体入口上方垂直距离为8500mm处测量时，所述吸收气氛的液滴粒径分布为D10为100-1000微米,D50为300-1800微米，D90为500-2200微米(优选D10为200-600微米,D50为400-1400微米，D90为600-1800微米)。本发明的发明人发现，测量位置所测的液滴平均直径D32和液滴粒径分布与喷洒装置区域的液滴平均直径D32和液滴粒径分布息息相关，通常喷洒装置区域的液滴平均直径D32大，该区域的液滴平均直径D32也相对会大，同样，液滴粒径分布情况也是如此。当液滴平均直径和液滴粒径分布低于下限时，说明喷洒装置区域的液滴偏小，液滴易被夹带；反之当液滴平均直径和液滴粒径分布高于上限时，喷洒装置区域的液滴偏大，气液接触不足，降低吸收效率。
根据本发明的一个实施方式，所述喷洒装置包括喷洒液入口、与所述喷洒液入口流体连通的第一喷洒管、与所述第一喷洒管流体连通且垂直于所述第一喷洒管向其两侧延伸的多个(比如10-26个，优选12-22个)第二喷洒管、与所述第二喷洒管流体连通且垂直于所述第二喷洒管向其两侧延伸的多个(比如4-26个，优选6-22个)第三喷洒管、以及位于所述第三喷洒管末端且与其流体连通的喷嘴。
本发明对于各喷洒管之间以及第三喷洒管与喷嘴的连接方式等没有具体限定，可以采用本领域的常规连接方式。比如，可以采用固定式连接，也可以采用可拆式连接，优选采用螺纹连接，或其它可拆式连接方式，没有具体限定。
根据本发明的一个实施方式，所述喷洒液是水或酸性水溶液。优选的情况下，含氨气体从下往上与作为喷洒液的酸性水溶液从上往下逆向接触，水溶液中所含的酸性H+与氨发生中和反应而将氨除去。在此，所述酸性水溶液是酸性物质的水溶液。作为所述酸性物质，可以为无机酸，如盐酸、硫酸、磷酸；也可以为有机酸，如丙烯酸、醋酸；也可以为酸性的盐，如硫酸铵，没有具体的限定。
根据本发明的一个实施方式，在所述冷却步骤中，所述喷洒液与所述反应产物以逆流方式接触。
根据本发明的一个实施方式，在所述冷却步骤中，将所述喷洒液入口的喷洒液输入压力控制在0.06-1.00MPaG(优选为0.12-0.90MPaG，更优选为0.18-0.80MPaG)。本发明的发明人发现，循环液从喷洒装置入口进入喷洒装置，经第一喷洒管、第二喷洒管、第三喷洒管，通过第三喷洒管末端的喷嘴输送至吸收塔内。通常情况，雾滴粒度越大，液滴对光的吸收越弱，消光效率也会降低，而雾滴粒径与压力成反比，由于沿流体行进方向压力逐渐降低，因此，雾滴粒度沿循环液流体行进方向是不断地增大的，离喷淋入口流体行进方向远端雾化喷嘴处所形成的雾滴大小D32大于离喷淋入口流体行进方向近端雾化喷嘴处所形成的雾滴大小D32，这也就导致了离喷淋入口流体行进方向远端处的氨吸收效率低于离喷淋入口流体行进方向近端处的氨吸收效率。喷洒液入口的喷洒液输入压力控制在前述规定范围，才能满足远端喷嘴足够的压力，满足装置所需的雾滴平均粒径以及粒径分布的要求，保证雾化效果。另外，随着装置长时间运行，反应过程中产生的具有一定粘性的聚合物、混夹着循环液中的铵盐附着在喷洒管管壁上，导致管程的阻力不断增加，特别是装置运行18个月以后，管程阻力增速更为明显，远端喷嘴压力进一步降低，导致远端喷嘴雾滴粒度更大，且雾滴粒径分布变得更宽，更不均匀，雾化效果更差。根据本发明，通过将喷洒液入口的喷洒液输入压力控制在前述规定范围，即使经过长周期连续运行，也可以满足远端喷嘴足够的压力，保证雾化效果。
根据本发明的一个实施方式，所述多个第二喷洒管垂直于所述第一喷洒管向其相对两侧沿水平方向基本上平行延伸。
根据本发明的一个实施方式，所述多个第三喷洒管垂直于所述第二喷洒管向其相对两侧沿水平方向基本上平行延伸。
根据本发明的一个实施方式，所述第一喷洒管的内径为160-480mm(优选200-450mm)，长度为4500-11500mm(优选4800-10500mm)。
根据本发明的一个实施方式，所述多个第二喷洒管彼此相同或不同，内径各自独立地为30-150mm(优选40-120mm)，长度各自独立地为1200-5750mm(优选1800-5250mm)。
根据本发明的一个实施方式，所述多个第三喷洒管彼此相同或不同，内径各自独立地为10-60mm(优选15-50mm)，长度各自独立地为160-325mm(优 选175-300mm)。
根据本发明的一个实施方式，所述喷嘴包括喷嘴入口、旋转室和喷嘴出口，其中所述旋转室被构造为使得从所述喷嘴入口进入的喷洒液在经过所述旋转室之后以旋转方式离开所述喷嘴出口。根据本发明，所述旋转室可以采用本领域已知的任何结构的旋转室，只要可以使所述喷洒液在经过所述旋转室之后以旋转方式离开所述喷嘴出口即可，并没有特别的限定。
根据本发明的一个实施方式，所述喷嘴彼此相同或不同，内径(指的是喷嘴出口)各自独立地为3-20mm(优选6-14mm)，旋转室的直径各自独立地为10.0-55.0mm(优选为13.0-45.0mm)，喷洒角度各自独立地为65-120°(优选70-100°)。根据本发明，所述旋转室可以采用本领域已知的任何结构的旋转室，只要可以使所述喷洒液在经过所述旋转室之后以旋转方式离开所述喷嘴出口即可，并没有特别的限定。
根据本发明的一个实施方式，在所述第一喷洒管上，相邻两个第二喷洒管的水平间距为640-1300(优选700-1200mm)。
根据本发明的一个实施方式，在同一个所述第二喷洒管上，相邻两个第三喷洒管的水平间距为320-650mm(优选350-600mm)。
根据本发明的一个实施方式，在相邻的两个第二喷洒管上，一个第二喷洒管上的任意一个第三喷洒管的末端与另一个相邻第二喷洒管上的任意一个第三喷洒管的末端的直线距离M(如图6A、图6B所示意)不小于320mm，优选不小于350mm。本发明的发明人发现，为了提高氨的吸收效率，一般塔内横截面上任一位置均有至少两个以上以喷嘴为中心所形成的锥形液面重叠覆盖，包括塔壁处也是如此，若两个喷洒管末端的距离过大，受喷嘴结构限制，塔壁任意位置很难满足两个以上喷嘴喷洒出的液面重叠，换言之，即塔液滴的数量少了，表现为液滴对光的吸收率降低，消光能力降弱，这样就增加了氨从“空隙”处逃逸的机率。若两个喷洒管末端距离过小，为了保证喷洒液的雾化质量，势必会在氨吸收塔内增加循环液量，即增加泵的能耗。另外，如图6A和图6B所示意，如果上下多层喷洒装置上下投影重合，则只能看到上层喷洒装置和相互对置的喷洒液入口。
根据本发明的一个实施方式，所述喷嘴彼此相同或不同，喷洒液喷出量各自独立地为0.5-7.5t/h(优选0.9-6.5t/h)。
根据本发明的一个优选实施方式，所述喷嘴彼此相同或不同，喷嘴出口的喷洒液喷出压力各自独立地为0.03-0.85MPaG(优选0.04-0.65MPaG)。本发明的发明人发现，对于氨吸收塔的雾化喷嘴而言，压力是促使液体形成雾滴的主要因素之一，在一定的压力范围内，雾滴粒径的大小随着压力的下降会增大，相对于大的雾化液滴，通常认为小的雾化液滴具有更好的传质传热效率，通常情况液滴越小，粒度分布越“窄”，对光的吸收越大，消光能越强。当喷嘴出口的喷洒液喷出压力小于0.03MPaG时，酸性循环液经喷洒装置后雾化效果差，液滴粒径大，即与氨的接触不够充分；当喷嘴出口的喷洒液喷出压力大于0.85MPaG时，虽然酸性循环液经喷洒装置后雾化效果好，但由于液滴粒径太小，液体容易被气体夹带出氨吸收塔，而液体中溶解的铵盐对后序工艺带来不必要的麻烦。另外，随着装置长时间运行，装置运行过程中产生的粘性聚合物也同样粘附在喷嘴内腔中，增加喷嘴的阻力，导致喷嘴出口处压力降低，比如装置连续运行18个月以后，喷嘴内腔附着污垢，改变了喷洒液在喷嘴的运动行为，特别的，增加远端喷嘴雾化情况的不稳定性，而这个不稳定性随着装置运行时间的延长将变得越发突出。根据本发明，通过将喷嘴出口的喷洒液喷出压力控制在前述规定范围，即使经过长周期连续运行，也能够确保远端喷嘴的雾化情况稳定，保证雾化效果。
根据本发明的一个实施方式，在所述冷却步骤中，所述喷洒液与所述反应产物以逆流方式接触。
根据本发明的一个实施方式，在所述冷却步骤中，所述喷洒液与所述反应产物的质量流量比15-25:1。
根据本发明的一个实施方式，所述冷却步骤在吸收装置中进行，并且多个(比如2-10个，优选4-8个)所述喷洒装置以预定的垂直间距沿着所述吸收装置的中心轴线方向分层设置在所述吸收装置内部。
根据本发明的一个实施方式，在垂直于所述吸收装置的中心轴线方向横切所述吸收装置而获得横截面时，所述多个喷洒装置中的一个与所述多个喷洒装置中的另一个的选自第一喷洒管、第二喷洒管和第三喷洒管中的至少一个(优选全部)在所述横截面上的投影基本上重合。即各个层的喷嘴(圆锥中心)在横截面上的投影重合，如此，氨在气休通道分布也是均匀的。
根据本发明的一个实施方式，所述一个喷洒装置与所述另一个喷洒装置 的全部喷嘴在所述横截面上的投影基本上重合。本发明的发明人发现，吸收装置中的多个喷洒装置即是相对独立的个体又是有机整体。循环液通过各个喷洒装置的第一喷洒管、第二喷洒管、第三喷洒管输送到各个喷洒装置的喷嘴，并以喷嘴为中心，形成空心的圆锥液面，气体与循环液体逆向接触，气体穿过下一层喷洒装置形成的圆锥液面才能与上一层喷洒装置形成的圆锥液面相接触，在气体穿过圆锥液面的瞬间，气体中的氨与液体中的酸发生中和反应，随着含氨气体穿过多个喷洒装置的多个空心圆锥液面，最终被循环液中的酸完全中和。上下两层喷洒装置的空心圆锥液面之间可视为气体上升通道，由于要求每段有独立的液相循环喷洒装置，因此上升气体通道有一定的高度。第一喷洒管、第二喷洒管和第三喷洒管中的至少一个(优选全部)在所述横截面上的投影基本重合，即各个层的喷嘴(圆锥中心)在横截面上的投影重合，如此，氨在气休通道分布也是均匀的，与液滴的融合也更充分，消光效率也更为一致。若上一层喷嘴与下一层喷嘴在横截面上的投影不重合，由于上下两层的空心圆锥液面不在同一位置，上升气体的气体通道被改变，上升气体通过气体通道后，由于不同通道上的消光效率不同，在气体通道之间容易存在着气体分布不均的问题，降低氨吸收效果。根据本发明的一个实施例，相邻两个所述喷洒装置的垂直间距(按喷洒装置的喷洒液入口的垂直间距计)为650-1350mm，优选750-1200mm。
本发明的发明人发现，若上一层喷嘴与下一层喷嘴在横截面上的投影不重合，由于上下两层的空心圆锥液面不在同一位置，上升气体的气体通道被改变，有部分通道变“宽”，同时也有部分通道变“窄”，通道变“宽”也意味着其间液滴量的变少，消光能力降低，反之，通道变“窄”，消光能力增加，上升气体通过不同高度的气体通道后，由于在通道内气体停留时间不同，容易存在着通道内气体分布不均的问题。也即，含氨气体在经过空心圆锥液面时，导致液面部分区域酸有剩余,而另一部分液面因酸不足导致氨穿透的情况，从而降低氨吸收效果。
本发明的发明人还发现，若上一层喷嘴与下一层喷嘴在横截面上的投影不重合，上一层喷嘴与下一层喷嘴喷出的喷洒液增加更多的碰撞。两液滴在碰撞时，存在分离、聚合、破碎等情况，本发明人发现上一层喷嘴与下一层喷嘴在横截面上的投影不重合时，上一层喷嘴产生的液滴与下一层喷嘴产生的 液滴在碰撞过程中，更容易聚合，形成更大的液滴，同时液滴的数量也相对减少，表现在消光效率的下降，这不利于氨的吸收的。
本发明的发明人进一步发现，各喷洒装置的循环液沿第一喷洒管至第二喷洒管至第三喷洒管直至喷嘴，流体在流动过程中，受管壁阻力影响，沿程压力不断下降，离喷洒液入口远端喷嘴处的压力低于离喷洒液入口近端处喷嘴的压力，由于最远端喷嘴处压力相对最低，相对来说，此处的液滴平均粒径偏大，液滴粒度分布更为宽泛，液滴对光的吸收效率最低，雾化效果也最差，导致最远端喷嘴处，气液接触不充分，容易造成氨的逃逸。随着装置运行周期的延长，如装置连续运行18个月，甚至是更长时间，管线内固体杂质以及粘度较大的重组分粘附在管壁上，管壁阻力进一步增大，液滴对光吸收效率进一步降低，即消光效率进一步降低，远端喷嘴处雾化效果变得更差，造成更多氨的逃逸。若是多层喷洒装置的喷洒液入口在同一侧，由于各层喷洒装置远端喷嘴在同一侧，此区域的气液接触最为薄弱，气相中的氨更容易从此区域逃逸出氨吸收塔。
基于这些发现，根据本发明的一个实施方式，所述一个喷洒装置与所述另一个喷洒装置的喷洒液入口在所述横截面上的投影之间的夹角为180°。在装置运行初期，由于喷洒装置管线内相对较干净，喷洒装置远端喷嘴足以将喷洒液雾化成合适尺寸的液滴，而在装置连续运行18个月甚至更长时间后，虽然一个喷洒装置最远端喷嘴处，由于喷嘴雾化效果变差，因气液接触不佳导致的氨逃逸情况，但是逃逸的氨被上一层的喷洒装置的近端喷嘴处的喷洒液捕捉并发生中和反应生成相应的盐类，上下对置的喷洒装置入口端位置区域的液滴平均粒径和液滴粒度分布相近，也即为消光效率相近。通常氨吸收塔内设置多层喷洒装置，如3层、4层、5层或更多层，上一(或二)层喷洒装置与下一(或二)层喷洒装置喷洒液入口在所述横截面上投影夹角为180°，能更大程度吸收氨，从而减少氨的逃逸，也能更大程度的降低酸的消耗。
根据本发明的一个实施方式，投影基本上重合的两个喷嘴具有相同的喷洒直径。
根据本发明的一个实施方式，在全部所述喷洒装置中，任意两个奇数编号的所述喷洒装置的喷洒液入口在所述横截面上的投影之间的夹角为0°，任意两个偶数编号的所述喷洒装置的喷洒液入口在所述横截面上的投影之间 的夹角为0°，并且任一奇数编号的所述喷洒装置与任一偶数编号的所述喷洒装置的喷洒液入口在所述横截面上的投影之间的夹角为180°。本发明的发明人发现，如此设置，就可以尽可能满足气相中的氨在气体通道中的均匀分布。
根据本发明的一个实施方式，投影基本上重合的两个喷嘴具有相同的喷洒液旋转方向。本发明的发明人发现，由于两个喷洒装置投影重合的喷嘴喷出的喷洒液下行碰撞时，喷嘴各自的液滴状态是不同的，相对而言，投影重合旋转方向相反的两个喷嘴比旋转方向相同的两个喷嘴更容易使液滴破裂形成若干个小液滴，对光的吸收率增强，消光效率增大，而液滴过小，则容易被气体夹带逃离。
根据本发明的一个实施方式，在至少一个(优选全部)所述第二喷洒管上，位于所述第二喷洒管的相同一侧的相邻两个(优选全部)喷嘴被构造为使得喷洒液以相同的旋转方向喷出。本发明的发明人发现，喷洒液从喷嘴的切线方向进入旋转窒，经喷嘴出口后形成以喷嘴出口为顶点的空心圆锥，为了满足喷洒液在塔内均匀性，要求相邻两个喷嘴的喷嘴出口在塔内截面是等距分布的，即喷洒液以相同的切线方向进入喷嘴，因此在第二喷洒管相同一侧的喷洒液以相同的旋转方向喷出，而在第二喷洒管相反两侧的喷洒液以相反的旋转方向喷出。如此，同一个第二喷洒管上喷嘴喷出的喷洒液在交汇碰撞后，满足更多的液滴对光吸收状态不变，仍保持原有状态沿原运动方向下行。
根据本发明的一个实施方式，并排相邻的两个所述第二喷洒管的相向一侧的全部喷嘴被构造为使得喷洒液以相反的旋转方向喷出。在此，所谓“并排相邻”指的是处于所述第一喷洒管的同一侧且相互邻近，而所谓“各自相向一侧”则指的是一个所述第二喷洒管与另一个所述第二喷洒管相互朝向的各自一侧，如图11C所示。并排相邻的第二喷洒管所相邻的两个喷嘴喷出的喷洒液在各自下行过程碰撞后，液滴仍可维持原状态运动下行，液滴不易聚合变大，也不易破裂为更为细小的液滴。
根据本发明的一个实施方式，在至少一个(优选全部)所述第二喷洒管上，位于所述第二喷洒管的一侧的至少一个(优选全部)喷嘴被构造为使得喷洒液以旋转方向A喷出，位于所述第二喷洒管的相对另一侧的至少一个(优 选全部)喷嘴被构造为使得喷洒液以旋转方向B喷出，其中所述旋转方向A与所述旋转方向B相反。
根据本发明的一个实施方式，所述旋转方向A是顺时针方向，所述旋转方向B是逆时针方向。
根据本发明的一个实施方式，在所述喷洒装置的全部喷嘴中，以所述旋转方向A喷出喷洒液的喷嘴的数量与以所述旋转方向B喷出喷洒液的喷嘴的数量相等或基本上相等。前述可知，喷洒均匀的前提是喷嘴在塔内分布均匀，通常优先为轴对称分布方式。因此，本发明的发明人发现，喷嘴的旋转方向以轴对称成对出现，若成对的喷嘴旋转方向均为同一方向，也就意味着所有喷嘴的旋转方向是相同的，容易造成两个相邻喷嘴喷出的喷洒液在旋转并下行过程中，液滴碰撞变大，消光效率变弱，由于与气体氨总有效接触面积变小，导致氨吸收效率降低。
根据本发明的一个实施方式，在至少一个(优选全部)所述第二喷洒管上，位于所述第二喷洒管的相同一侧的相邻两个(优选全部)喷嘴被构造为使得喷洒液以相反的旋转方向喷出。第三喷洒管垂直于所述第二喷洒管并向其两侧沿水平方向平行延伸的，在第二喷洒管同一水平方向平行延伸线上的全部喷嘴被构造为使得喷洒液以相同的旋转方向喷出。如图11E所示。
根据本发明的一个实施方式，在至少一个(优选全部)所述第二喷洒管上，位于所述第二喷洒管的一个喷嘴被构造为使得喷洒液以旋转方向A喷出，一侧相邻的至少另一个喷嘴被构造为使得喷洒液以旋转方向B喷出。位于所述第二喷洒管的相对另一侧的至少一个(优选全部)喷嘴被构造为使得喷洒液以旋转方向A喷出，其中所述旋转方向A与所述旋转方向B相反。
根据一个实施方式，喷嘴包括喷嘴入口、喷嘴腔体和喷嘴出口，其中所述腔体具有特殊结构使得从所述喷嘴入口进入的喷洒液在经过所述的腔体离开所述喷嘴出口形成雾滴。如图9所示。所述腔体可以采用本领域已知的任何结构，只要可以使所述喷洒液离开所述喷嘴出口形成雾滴即可，并没有特别的限定。
根据一个实施方式，喷洒液从喷嘴的上方进入腔体，经喷嘴出口后形成以喷嘴出口为顶点的实心圆锥，通常，相邻两个喷嘴在塔内截面是等距分布的，且多个喷洒装置的喷嘴的投影基本重合，相邻的两个喷嘴喷出的喷洒液 在各自下行过程碰撞后，液滴仍可维持原状态运动下行。
根据本发明的一个实施方式，相邻两个所述喷洒装置的垂直间距(按喷洒装置的喷洒液入口的垂直间距计)为650-1350mm(优选750-1200mm)。本发明的发明人发现，当相邻两个喷洒装置的垂直间距小于650mm时，对于具有相同数量喷洒装置的氨吸收塔，由于上升的含氨气体与下行的循环液接触时间不足，气液融合变差，消光效率降低，气相中部分氨直接穿过循环液形成的空心圆锥液面，导致氨吸收效率变差，虽然可以通过增加喷洒装置数量的方式满足足够的气液接触时间，达到气相中的氨完全吸收，但会增加循环液总量，增加泵的能耗，显然是不经济的。当相邻两个喷洒装置的垂直间距大于1350mm时，在相同喷洒装置的情况下，会塔的高度增加，即设备投资费用增多，除此以外也会增加维检修难度。
根据本发明的一个实施方式，任意两个所述喷洒装置的喷洒液入口的喷洒液输入压力的差异(绝对值)小于0.024MPa(优选小于0.018MPa，更优选小于0.012MPa)。本发明的发明人发现，循环液雾化后液滴的大小与喷嘴所处的压力大小息息相关，压力过大或过小均对装置运行不利，而喷嘴压力起始于喷洒液入口的喷洒液输入压力，理论上希望喷洒液入口的喷洒液输入压力相同，但实际情况，由于多层喷洒装置为上下布置，循环泵在将循环液输送至各层喷洒装置时，存在压降的损失。因此，任意两个喷洒装置的喷洒液入口的喷洒液输入压力差尽可能低，才能最上和最下的喷洒装置的所有喷嘴均满足最佳压力条件，满足装置纵向截面上液滴平均粒径和液滴粒度分布相近，也即装置纵向的消光效率也是一样的。
根据本发明的一个实施方式，所述吸收装置的内径为4.5-11.5m(优选4.8-10.5m)。
根据本发明的一个实施方式，所述吸收装置还包括壳体和气体入口。根据本发明，所述喷洒装置设置在所述吸收装置的所述壳体的内部。另外，所述反应产物从所述气体入口输入所述吸收装置中。
根据本发明的一个实施方式，所述气体入口沿着所述吸收装置的中心轴线方向位于所述喷洒装置的下方。
根据本发明的一个实施方式，所述气体入口与所述喷洒装置(在存在多个时，指的是距离所述气体入口最近的所述喷洒装置)的喷洒液入口的垂直 距离为800-6000mm(优选1000-5000mm)。本发明的发明人发现，气体从入口沿向塔底下弯的半圆入口管进入塔内，再由下往上行进。相对而言，入口管处气体浓度最高，在气体往上的同时，由于气体浓度的不同，气体向周边扩散，最终塔截面上气体浓度达到均匀。若是垂直距离小于800mm,气体浓度容易扩散不充分，浓度高低不一，气液隔合不均匀，影响到消光效率的不均匀，容易造成局部氨吸收不完全以及局部酸过量的情况；若是垂直距离过大，一方面氨吸收塔切线高度过高，增加设备投资。另一方面，喷洒液在旋转下落过程中，两碰撞的液滴存在分离、聚合、破碎等行为，而在聚合发生时，形成更大的液滴；在破碎发生时，就形成更小的液滴。液滴喷出距离越长，越易发生聚合或破碎，液滴粒度分布变为更“宽”，存在消光效率下降的可能，这也是不利于氨的吸收的。
根据本发明的一个实施方式，所述气体入口的内径为800-1900mm(优选900-1700mm)。
根据本发明的一个实施方式，所述气体在所述壳体内部的线速度为0.6-1.5m/s(优选0.7-1.3m/s)。本发明的发明人发现，壳体内的操作速度影响到气体扩散速度，壳体内操作速度越大，湍流作用越强，夹带的液滴越多，消光效率相对也越高，也有利于气体的扩散，因此，扩散距离也越短。当壳体内速度低于0.6时，相对而言，气体扩散至均匀所而的时间长，也即入口至第一层喷洒装置的距离增加。但是当壳体内部的线速度高于1.5m/s，由于喷洒装置喷洒液的液滴通常都成雾滴状，这些雾滴易被气体夹带，壳体内速度越大，雾沫夹带现象越严重，导致更多含铵盐的雾滴被气体带离出氨吸收塔。
根据本发明的一个实施方式，在所述气体入口与所述喷洒装置(在存在多个时，指的是距离所述气体入口最近的所述喷洒装置)之间的吸收装置内部空间，不设置能够实质性影响所述气体流动的机械构件，比如扰动所述气体流动的机械构件，特别是折流板、托盘、填料等。本发明的发明人发现，虽然可以通过增加内构件的方式使得气相氨在与第一层喷淋液接触前的截面上分散均匀，但无论何种型式的机械构件均会增加装置的系统压力，最终体现在反应压力的增加，降低目标产物的收率。液滴尺寸越小，液滴与气体氨接触表面越大，吸收效果越好，反之，氨吸收效果越差。而气体相对容易扩散，即便在第一层喷淋位置处气相氨未完全分散均匀，消光效率略差，但气相氨 在上升过程中继续扩散，也会被后几层喷淋装置的喷洒液捕捉吸收。因此，在此增加构件，虽然满足气相氨快速分散均匀的目的，但第一层喷淋装置至入口垂直距离800-6000mm，优选1000-5000mm，即可满足前序反应段的高效反应，又可满足本塔消光效率，满足氨的吸收效率，对整个装置经济性更高。
根据本发明的一个实施方式，在所述反应步骤中，所述烃原料是丙烯，丙烯/氨气/空气(以分子氧计)的摩尔比为1：1.1-1.3：1.8-2.0，反应温度为420-440℃，反应压力(表压)为0.03-0.14MPa，催化剂重时空速为0.06-0.15h-1，或者，所述烃原料是异丁烯，异丁烯/氨气/空气(以分子氧计)的摩尔比为1：1.3-1.6：2.2-2.8，反应温度为395-420℃，反应压力(表压)为0.03-0.14MPa，催化剂重时空速为0.08-0.17h-1。
根据本发明的一个实施方式，取决于所述反应步骤的不同，所述反应产物的组成一般为C1-4腈类(比如丙烯腈等)约占10-20wt％，C1-4含氧化合物(比如丙烯醛等)约占0.1-5wt％，O2约占0.1-5wt％，氨约占0.1-2wt％，其他杂质是余量，相对于所述反应产物的总重量为100wt％计。在经过初步冷却之后，所述反应产物的温度一般为195-235℃，压力一般为0.03-0.14MPaG。根据本发明，针对该特定的反应产物，本发明的制造方法的前述技术效果特别优异。
根据本发明的一个实施方式，在所述冷却步骤中，所述喷洒液使得所述反应产物的温度从195-235℃冷却至81-86℃。另外，优选的是，所述喷洒液使得所述反应产物的氨含量降低至150ppm以下。
下面结合附图，以举例说明的方式对本发明的一个具体实施方式进行详细描述。
举例而言，如图4A所示，根据本发明，温度为225反应气体以及未反应的氨从含氨气体进料口8进入氨吸收塔1内，循环液从塔底抽出经循环泵17送至多层喷洒装置3a-喷洒装置3f，喷洒装置3a-3f在塔内由上而下依次布置，其中喷洒装置3a\3c\3e为同一侧，喷洒装置3b\3d\3f为与喷洒装置3a\3c\3e对置侧，含氨气体进料口8与喷洒装置3f的垂直距离为1800mm；喷洒装置3a\3c\3e喷洒液入口的喷洒液输入压力分别为0.327MPaG、0.330MPaG、0.334MpaG，喷洒装置3a\3c\3e喷洒液入口的喷洒液输入压力分别为0.327MPaG、0.330MPaG、0.334MpaG；硫酸从含酸溶液口15加入至循环泵出口管线上，循环液通过喷洒装置3，从喷洒装置3的入口18进入，沿流 体方向经第一喷洒管19、第二喷洒管20a(20b)、第三喷洒管21至雾化喷嘴22，从喷嘴22喷出循环液在氨吸收塔内形成酸雾液层，吸收来自气体进料口8中的气体氨，尾气从气相出料口9排出氨吸收塔。塔顶尾气温度为84℃。喷洒装置3a-3f第三喷洒管末端在塔横截面的投影重合，如图5所示。
进一步举例而言，如图4B所示，根据本发明，温度为225℃反应气体以及未反应的氨从含氨气体进料口8进入氨吸收塔1内，循环液从塔底抽出经循环泵17送至喷洒装置3a-喷洒装置3f，其中喷洒装置3a\3c\3e为同一侧，喷洒装置3b\3d\3f为与喷洒装置3a\3c\3e对置侧，含酸液体从含酸溶液口15加入至循环泵出口管线上，循环液通过喷洒装置3，从喷洒装置3的入口18进入，沿流体方向经第一喷洒管19、第二喷洒管20a(20b)、第三喷洒管21至雾化喷嘴22，雾化喷嘴向左旋转：向右旋转为1:1。从喷嘴22喷出循环液在氨吸收塔内形成酸雾液层，吸收来自气体进料口8中的气体氨，尾气从气相出料口9排出氨吸收塔。塔顶尾气温度为84℃。喷洒装置3a-3f第三喷洒管末端在塔横截面的投影重合，如图6A所示。喷洒装置的喷嘴(喷嘴)结构示意图以及喷洒装置俯视图如图11C、图11B所示。
实施例
以下采用实施例进一步详细地说明本发明，但本发明并不限于这些实施例。
在以下的实施例和对比例中，尾气残留氨浓度可以通过离线分析进行测量，具体是在氨吸收塔顶部采取一定体积(V)气体，气体通过一定量的水吸收，分析水中氨量，折算为气相氨体积(v)，尾气残留氨浓度计算式为v/V。另外，酸耗通过进氨吸收塔酸计量表进行测量。
实施例1
氨吸收塔采用图3b的二段式结构形式，吸收塔内径为7200mm，塔内未设有气体分布器23，反应气体在塔内的线速度为1.1m/s，循环液中添加的酸为硫酸，含酸的循环液经上段循环泵通过4个喷洒装置送至吸收塔内，其中喷洒装置3a、3c与3b、3d的第一喷洒管内流体方向相反，即相邻两个喷洒液入口投影夹角为180°。喷洒装置俯视如图11B、喷洒装置俯视细节图如图11C 示意图所示，喷洒装置3a(b)与3c(d)喷洒液入口的喷洒液输入压力分别为0.440MPaG和0.446MPaG，喷洒液喷出压力为0.051MPaG，相邻的两个喷洒装置间隔为1200mm，每个喷洒装置各有16个第二喷洒管，第二喷洒管设置有11至18个第三喷洒管。喷洒装置的第三喷洒末端投影重合且旋转方向相同，第二喷洒管的相同一侧的全部喷嘴旋转室方向相同，第二喷洒管相反两侧的喷嘴旋转室方向相反，且并排相邻的两个第二喷洒管的相向一侧全部喷嘴旋转方向相反，且旋转室方向相同的喷嘴各为480个和480个。喷洒装置的第一喷洒管内径为250mm，第一喷洒管长度为7000mm；喷洒装置的第二喷洒管间距均为820mm，第二喷洒管内径为100mm，第二喷洒管长度为2100mm-3450mm；喷洒装置的第三喷洒管间距均为410mm，第三喷洒管内径40mm，第三喷洒管长度为205mm；喷洒装置共有960个喷嘴，相邻两个第三喷洒管如图6B所示末端距离580mm；喷嘴出口直径为11.5mm，喷嘴旋转室直径为40mm，喷嘴的喷洒角度为75°。气体进料口8至喷洒装置3d的垂直距离为4000mm，进料口内径为1300mm。从进料口进入的反应产物气体约含氨0.71wt％，丙烯腈13.2wt％，其余是O2、丙烯醛、氮气等杂质，其温度为225℃，压力为0.06MPaG，每个喷嘴的喷洒液喷出量为4.8t/h，喷洒液与从气体入口进入的反应产物气体的重量比为20。装置运行初期，从反应出口处尾气残留氨浓度为41ppm，装置运行24个月，从反应出口处尾气残留氨浓度为52ppm；装置运行24个月酸耗/装置运行1个月酸耗为1.02。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.011m-1，液滴平均直径D32为1130微米，液滴粒径分布为D10为625微米，D50为1328微米，D90为2195微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0021m-1，液滴平均直径D32为462微米，液滴粒径分布为D10为406微米，D50为593微米，D90为894微米。
实施例2
氨吸收塔采用图4B的一段式结构形式，吸收塔内径为7200mm，塔内未设有气体分布器23，反应气体在塔内的线速度为1.1m/s，循环液中添加的酸为硫酸，含酸的循环液经循环泵通过6个喷洒装置送至吸收塔内，其中喷洒装 置3a、3c、3e与3b、3d、3f的第一喷洒管内流体方向相反，即相邻两个喷洒液入口投影夹角为180°。喷洒装置俯视如图11B、喷洒装置俯视细节图如图11C示意图所示。喷洒装置3a(b)、3c(d)与3e(f)喷洒液入口的喷洒液输入压力分别为0.425MPaG、0.430MPaG、0.435MpaG，喷洒液喷出压力分别为0.055MPaG，相邻两个喷洒装置的垂直间距为880mm，每个喷洒装置各有14个第二喷洒管，第二喷洒管设置有6至14个第三喷洒管。喷洒装置的第三喷洒末端投影重合且旋转方向相同，第二喷洒管的相同一侧的全部喷嘴旋转室方向相同，第二喷洒管相反两侧的喷嘴旋转室方向相反，且并排相邻的两个第二喷洒管的相向一侧全部喷嘴旋转方向相反，且旋转室方向相同的喷嘴各为456个和456个。喷洒装置的第一喷洒管内径为200mm，第一喷洒管长度为7000mm；喷洒装置的第二喷洒管间距均为1000mm，第二喷洒管内径为100mm，长度为1850mm-3450mm；喷洒装置的第三喷洒管间距均为500mm，第三喷洒管内径40mm，长度为250mm，喷洒装置的第三喷洒末端投影重合，相邻两个第三喷洒管如图6A所示的末端距离为500mm；喷洒装置共有912个喷嘴，喷洒装置的喷嘴出口直径11.7mm，喷嘴旋转室直径36mm，喷洒角度为80°。气体进料口8至喷洒装置3f的垂直距离为1500mm，气体进料口8至喷洒装置3d的垂直距离为4000mm，进料口内径为1200mm。从进料口进入的反应产物气体约含氨0.71wt％，丙烯腈13.2wt％，其余是O2、丙烯醛、氮气等杂质，其温度为225℃，压力为0.06MPaG，每个喷嘴的喷洒液喷出量为5.1t/h，喷洒液与从气体入口进入的反应产物气体的重量比为20。装置运行初期，从反应出口处尾气残留氨浓度为27ppm，装置运行24个月，从反应出口处尾气残留氨浓度为34ppm；装置运行24个月酸耗/装置运行1个月酸耗为1.01。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0128m-1，液滴平均直径D32为1054微米，液滴粒径分布为D10为832微米，D50为1242微米，D90为1956微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0019m-1，液滴平均直径D32为412微米，液滴粒径分布为D10为386微米，D50为574微米，D90为878微米。
实施例3
与实施例2相同，区别仅在于喷洒装置3a(b)、3c(d)与3e(f)喷洒液入口的喷洒液输入压力分别为0.152MPaG、0.160MPaG、0.168MpaG，喷洒液喷出压力分别为0.04MPaG，喷洒装置的喷嘴出口直径11.9mm，装置运行初期，从反应出口处尾气残留氨浓度为72ppm，装置运行24个月，从反应出口处尾气残留氨浓度为98ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0058m-1，液滴平均直径D32为2226微米，液滴粒径分布为D10为1298微米，D50为2384微米，D90为3203微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0013m-1，液滴平均直径D32为542微米，液滴粒径分布为D10为427微米，D50为671微米，D90为914微米。
实施例4
与实施例2相同，区别仅在于喷洒装置3a(b)、3c(d)与3e(f)喷洒液入口的喷洒液输入压力分别为0.838MPaG、0.844MPaG、0.85MpaG，喷洒液喷出压力分别为0.42MPaG，喷洒装置的喷嘴出口直径12.1mm，装置运行初期，从反应出口处尾气残留氨浓度为84ppm，装置运行24个月，从反应出口处尾气残留氨浓度为92ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.018m-1，液滴平均直径D32为726微米，液滴粒径分布为D10为422微米，D50为989微米，D90为1803微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0035m-1，液滴平均直径D32为321微米，液滴粒径分布为D10为267微米，D50为389微米，D90为543微米。
实施例5
与实施例2相同，区别仅在于喷洒装置3a(b)、3c(d)与3e(f)喷洒液入口的喷洒液输入压力分别为0.950MPaG、0.954MPaG、0.959MpaG，喷洒液喷出压力分别为0.42MPaG，喷洒装置的喷嘴出口直径11.1mm，装置运行初期，从反应出口处尾气残留氨浓度为105ppm，装置运行24个月，从反应出口处尾气残留氨浓度为116ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.01925m-1，液滴平均直径D32为432微米，液滴粒径分布为D10为392微米，D50为750微米，D90为1439微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0038m-1，液滴平均直径D32为280微米，液滴粒径分布为D10为159微米，D50为345微米，D90为511微米。
实施例6
与实施例2相同，区别仅在于喷洒装置3a(b)、3c(d)与3e(f)喷洒液入口的喷洒液输入压力分别为0.098MPaG、0.103MPaG、0.108MpaG，喷洒液喷出压力分别为0.04MPaG，喷洒装置的喷嘴出口直径12.3mm，装置运行初期，从反应出口处尾气残留氨浓度为132ppm，装置运行24个月，从反应出口处尾气残留氨浓度为181ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0042m-1，液滴平均直径D32为2426微米，液滴粒径分布为D10为1398微米，D50为2434微米，D90为3390微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0012m-1，液滴平均直径D32为692微米，液滴粒径分布为D10为547微米，D50为682微米，D90为950微米。
实施例7
与实施例2相同，区别在于相邻两个喷洒装置的垂直间距为1200mm，相邻两个第三喷洒管如图6B所示的末端距离为707mm。喷洒装置的喷嘴出口直径11.8mm，每个喷嘴的喷洒液喷出量为5.8t/h，装置运行初期，从反应出口处尾气残留氨浓度为68ppm，装置运行24个月，从反应出口处尾气残留氨浓度为96ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.005m-1，液滴平均直径D32为1623微米，液滴粒径分布为D10为1189微米，D50为2148微米，D90为2415微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0021m-1，液滴平均直径 D32为432微米，液滴粒径分布为D10为387微米，D50为601微米，D90为914微米。
实施例8
与实施例2相同，区别在于相邻两个喷洒装置的垂直间距为1200mm，每个喷洒装置各有18个第二喷洒管，第二喷洒管设置有7至20个第三喷洒管，喷洒装置的第二喷洒管间距均为670mm，第二喷洒管内径为80mm，相邻两个第三喷洒管如图6A所示的末端距离335mm。喷洒装置共有2000个喷嘴，喷洒装置的喷嘴出口直径11.3mm，喷嘴旋转室直径30mm，喷洒角度为65°，每个喷嘴的喷洒液喷出量为2.64t/h。装置运行初期，从反应出口处尾气残留氨浓度为86ppm，装置运行24个月，从反应出口处尾气残留氨浓度为105ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0078m-1，液滴平均直径D32为1814微米，液滴粒径分布为D10为1075微米，D50为2184微米，D90为2851微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0015m-1，液滴平均直径D32为460微米，液滴粒径分布为D10为437微米，D50为651微米，D90为893微米。
实施例9
与实施例2相同，区别在于喷洒装置3a(b)、3c(d)与3e(f)喷洒液入口的喷洒液输入压力分别为0.376MPaG、0.380MPaG、0.385MpaG；喷洒液喷出压力分别为0.045MPaG，相邻两个喷洒装置的垂直间距为550mm，相邻两个第三喷洒管如图6B所示的末端距离707mm。装置运行初期，从反应出口处尾气残留氨浓度为120ppm，装置运行24个月，从反应出口处尾气残留氨浓度为162ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0042m-1，液滴平均直径D32为2154微米，液滴粒径分布为D10为1096微米，D50为2628微米，D90为2865微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0011m-1，液滴平均直径D32为367微米，液滴粒径分布为D10为316微米，D50为484微米，D90为616微 米。
实施例10
与实施例2相同，区别在于相邻两个喷洒装置的垂直间距为1200mm，每个喷洒装置各有24个第二喷洒管，第二喷洒管设置有9至24个第三喷洒管，喷洒装置的第二喷洒管间距均为580mm，第二喷洒管内径为80mm，相邻两个第三喷洒管如图6A所示的末端距离290mm。喷洒装置共有2640个喷嘴，喷洒装置的喷嘴出口直径9.1mm，喷嘴旋转室直径30mm，喷洒角度为65°，每个喷嘴的喷洒液喷出量为2.0t/h。装置运行初期，从反应出口处尾气残留氨浓度为146ppm，装置运行24个月，从反应出口处尾气残留氨浓度为185ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0059m-1，液滴平均直径D32为1934微米，液滴粒径分布为D10为1738微米，D50为2128微米，D90为2665微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0013m-1，液滴平均直径D32为347微米，液滴粒径分布为D10为284微米，D50为482微米，D90为615微米。
实施例11
与实施例2相同，区别在于每个喷嘴的喷洒液喷出量为8.5t/h，喷洒液与从气体入口进入的反应产物气体的重量比为32；装置运行1个月，从反应出口处尾气残留氨浓度为85ppm，装置运行24个月，反应出口尾气的残留氨浓度为99ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.03。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0016m-1，液滴平均直径D32为1712微米，液滴粒径分布为D10为1138微米，D50为2324微米，D90为2765微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0014m-1，液滴平均直径D32为787微米，液滴粒径分布为D10为556微米，D50为832微米，D90为1042微米。
实施例12
与实施例2相同，区别在于每个喷嘴的喷洒液喷出量为1.5t/h，喷洒液与从气体入口进入的反应产物气体的重量比为11；装置运行1个月，从反应出口处尾气残留氨浓度为145ppm，装置运行24个月，反应出口尾气的残留氨浓度为178ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.05。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.005m-1，液滴平均直径D32为469微米，液滴粒径分布为D10为409微米，D50为772微米，D90为1091微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0012m-1，液滴平均直径D32为348微米，液滴粒径分布为D10为159微米，D50为393微米，D90为604微米。
实施例13
与实施例2相同，区别仅在于喷洒装置3a-3f入口分别布置在设备不同方位，喷洒装置3a-3f的第一喷洒管在截面上投影重合，第二喷洒管、第三喷洒管以及喷嘴在截面上的投影不重合，装置运行1个月，反应出口尾气的残留氨浓度为137ppm，装置运行24个月，反应出口尾气的残留氨浓度为148ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0063m-1，液滴平均直径D32为1852微米，液滴粒径分布为D10为1593微米，D50为1882微米，D90为2191微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.001m-1，液滴平均直径D32为430微米，液滴粒径分布为D10为392微米，D50为575微米，D90为783微米。
实施例14
与实施例2相同，区别在于沿流体方向第一喷洒管的第1至11个第二喷洒管上的喷嘴直径36，第一喷洒管的第12至14个第二喷洒管上的喷嘴直径为32mm；装置运行1个月，从反应出口处尾气残留氨浓度为63ppm，装置运行24个月，反应出口尾气的残留氨浓度为99ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0127m-1，液滴平均直径D32为824微米，液滴粒径分布为D10 为598微米，D50为1198微米，D90为1976微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0018m-1，液滴平均直径D32为411微米，液滴粒径分布为D10为375微米，D50为586微米，D90为880微米。
实施例15
与实施例2相同，区别仅在于区别在于相邻两个喷洒装置的垂直间距为1250mm，装置运行初期从反应出口对尾气残留氨浓度为77ppm，装置运行24个月，从反应出口处尾气残留氨浓度为85ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.04。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0094m-1，液滴平均直径D32为1408微米，液滴粒径分布为D10为1009微米，D50为2083微米，D90为2362微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0016m-1，液滴平均直径D32为469微米，液滴粒径分布为D10为372微米，D50为579微米，D90为880微米。
实施例16
与实施例2相同，区别仅在于区别在于相邻两个喷洒装置的垂直间距为720mm，装置运行初期从反应出口对尾气残留氨浓度为111ppm，装置运行24个月，从反应出口处尾气残留氨浓度为129ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.07。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0143m-1，液滴平均直径D32为935微米，液滴粒径分布为D10为616微米，D50为1323微米，D90为1950微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0015m-1，液滴平均直径D32为420微米，液滴粒径分布为D10为389微米，D50为480微米，D90为632微米。
实施例17
与实施例2相同，区别仅在于区别在于相邻两个喷洒装置的垂直间距为1650mm，装置运行初期从反应出口对尾气残留氨浓度为177ppm，装置运行24个月，从反应出口处尾气残留氨浓度为195ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.05。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0053m-1，液滴平均直径D32为2215微米，液滴粒径分布为D10为1295微米，D50为2489微米，D90为3125微米。另外，在气体入口上方垂直距离为10350mm处测量时(位于喷洒装置上方)，吸收气氛的消光系数为0.0011m-1，液滴平均直径D32为580微米，液滴粒径分布为D10为319微米，D50为645微米，D90为711微米。
实施例18
与实施例2相同，区别仅在于相邻两个喷洒装置的垂直间距为550mm,装置运行1个月，反应出口尾气的残留氨浓度为129ppm，装置运行24个月，反应出口尾气的残留氨浓度为145ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.04。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0187m-1，液滴平均直径D32为895微米，液滴粒径分布为D10为566微米，D50为1129微米，D90为1921微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0011m-1，液滴平均直径D32为350微米，液滴粒径分布为D10为219微米，D50为445微米，D90为511微米。
实施例19
与实施例2相同，区别仅在于喷洒装置3a(b)、3c(d)与3e(f)喷洒液入口的喷洒液输入压力分别为0.405MPaG、0.421MpaG，0.435MpaG，装置运行初期，从反应出口处尾气残留氨浓度为65ppm，装置运行24个月，从反应出口处尾气残留氨浓度为89ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0135m-1，液滴平均直径D32为992微米，液滴粒径分布为D10 为735微米，D50为1112微米，D90为1601微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0025m-1，液滴平均直径D32为402微米，液滴粒径分布为D10为366微米，D50为580微米，D90为808微米。
实施例20
与实施例2相同，区别仅在于喷洒装置3a(b)、3c(d)与3e(f)喷洒液入口的喷洒液输入压力分别为0.327MPaG、0.352MpaG，0.376MpaG，，装置运行初期，从反应出口处尾气残留氨浓度为112ppm，装置运行24个月，从反应出口处尾气残留氨浓度为145ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0094m-1，液滴平均直径D32为1432微米，液滴粒径分布为D10为1032微米，D50为1789微米，D90为2647微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0012m-1，液滴平均直径D32为497微米，液滴粒径分布为D10为452微米，D50为620微米，D90为913微米。
实施例21
与实施例1相同，区别仅在于气体入口至喷洒装置3f的垂直距离为6000mm，装置运行初期从反应出口对尾气残留氨浓度为77ppm，装置运行24个月，从反应出口处尾气残留氨浓度为85ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0093m-1，液滴平均直径D32为1132微米，液滴粒径分布为D10为932微米，D50为1248微米，D90为2101微米。另外，在气体入口上方垂直距离为13500mm处测量时(喷洒装置上方)，吸收气氛的消光系数为0.0016m- 1，液滴平均直径D32为372微米，液滴粒径分布为D10为416微米，D50为491微米，D90为638微米。
实施例22
与实施例2相同，区别仅在于气体入口至喷洒装置3f的垂直距离为 8000mm，装置运行初期从反应出口对尾气残留氨浓度为90ppm，装置运行24个月，从反应出口处尾气残留氨浓度为106ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0062m-1，液滴平均直径D32为1520微米，液滴粒径分布为D10为1249微米，D50为1742微米，D90为2345微米。另外，在气体入口上方垂直距离为16000mm处测量时(喷洒装置上方)，吸收气氛的消光系数为0.0015m- 1，液滴平均直径D32为326微米，液滴粒径分布为D10为291微米，D50为485微米，D90为794微米。
但由于塔设备总高度增高，设备投资费用增加，同时，也提高了装置的检修难度。
实施例23
与实施例2相同，区别仅在于气体入口至喷洒装置3f的垂直距离为900mm，装置运行初期从反应出口对尾气残留氨浓度为125ppm，装置运行24个月，从反应出口处尾气残留氨浓度为142ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0055m-1，液滴平均直径D32为1220微米，液滴粒径分布为D10为749微米，D50为1468微米，D90为2845微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0016m-1，液滴平均直径D32为486微米，液滴粒径分布为D10为419微米，D50为685微米，D90为898微米。
实施例24
与实施例2相同，区别仅在于气体入口至喷洒装置3f的垂直距离为500mm，装置运行初期从反应出口对尾气残留氨浓度为182ppm，装置运行24个月，从反应出口处尾气残留氨浓度为219ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0043m-1，液滴平均直径D32为1143微米，液滴粒径分布为D10为648微米，D50为2163微米，D90为3556微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0018m-1，液滴平均直径 D32为402微米，液滴粒径分布为D10为284微米，D50为575微米，D90为969微米。
实施例25
与实施例2相同，区别仅在于塔内设有气体分布器23，如图4B所示从反应出口对尾气残留氨浓度为35ppm，增设气体分配内构件后，氨吸收塔塔釜压力增加10KPa，致使氨吸收塔前置系统的反应压力增加了10KPa，目标产物腈的收率下降了1.5％。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0127m-1，液滴平均直径D32为1068微米，液滴粒径分布为D10为790微米，D50为1222微米，D90为1960微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.002m-1，液滴平均直径D32为398微米，液滴粒径分布为D10为376微米，D50为572微米，D90为864微米。
实施例26
与实施例2相同，区别仅在于反应气体在塔内的线速度为0.6m/s，每个喷嘴的喷洒液喷出量为2.8t/h。装置运行初期从反应出口对尾气残留氨浓度为82ppm，装置运行24个月，从反应出口处尾气残留氨浓度为99ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.009m-1，液滴平均直径D32为1254微米，液滴粒径分布为D10为895微米，D50为1405微米，D90为2084微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0016m-1，液滴平均直径D32为486微米，液滴粒径分布为D10为385微米，D50为568微米，D90为880微米。
实施例27
与实施例2相同，区别仅在于反应气体在塔内的线速度为1.4m/s，每个喷嘴的喷洒液喷出量为为5.1t/h，喷洒液与从气体入口进入的反应产物气体的重量比为17，装置运行初期从反应出口对尾气残留氨浓度为132ppm，装置 运行24个月，从反应出口处尾气残留氨浓度为154ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0191m-1，液滴平均直径D32为954微米，液滴粒径分布为D10为595微米，D50为1389微米，D90为2052微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0029m-1，液滴平均直径D32为390微米，液滴粒径分布为D10为336微米，D50为564微米，D90为882微米。
实施例28
与实施例2相同，区别仅在于反应气体在塔内的线速度为0.4m/s，每个喷嘴的喷洒液喷出量为2.0t/h。装置运行初期从反应出口对尾气残留氨浓度为173ppm，装置运行24个月，从反应出口处尾气残留氨浓度为195ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.006m-1，液滴平均直径D32为1350微米，液滴粒径分布为D10为985微米，D50为1549微米，D90为2256微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.001m-1，液滴平均直径D32为416微米，液滴粒径分布为D10为385微米，D50为581微米，D90为872微米。
实施例29
与实施例2相同，区别仅在于反应气体在塔内的线速度为1.9m/s，每个喷嘴的喷洒液喷出量为6.2t/h，喷洒液与从气体入口进入的反应产物气体的重量比为15，装置运行初期从反应出口对尾气残留氨浓度为182ppm，装置运行24个月，从反应出口处尾气残留氨浓度为199ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.02m-1，液滴平均直径D32为890微米，液滴粒径分布为D10为522微米，D50为1234微米，D90为2043微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0039m-1，液滴平均直径D32为361微米，液滴粒径分布为D10为306微米，D50为514微米，D90为847微米。
实施例30
与实施例2相同，区别仅在于氨吸收塔采用图4A的一段式结构形式，喷洒装置3a、3b、3c与3d、3e、3f的第一喷洒管内流体方向相反，即上三层喷洒装置3a、3b、3c喷洒入口投影基本重合，下三层喷洒装置3d、3e、3f喷洒入口投影也基本重合，而上三层与下三层喷洒入口投影夹角为180°。装置运行1个月，反应出口尾气的残留氨浓度为42ppm，装置运行24个月，反应出口尾气的残留氨浓度为61ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.03。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0118m-1，液滴平均直径D32为934微米，液滴粒径分布为D10为698微米，D50为1367微米，D90为2182微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0019m-1，液滴平均直径D32为417微米，液滴粒径分布为D10为392微米，D50为584微米，D90为898微米。
实施例31
与实施例2相同，区别仅在于喷洒装置3a、3c、3e与3b、3d、3f的第一喷洒管在截面上投影重合，而第二喷洒管、第三喷洒管以及喷嘴在截面上的投影不重合，如图7所示，装置运行1个月，反应出口尾气的残留氨浓度为78ppm，装置运行24个月，反应出口尾气的残留氨浓度为95ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.05。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0103m-1，液滴平均直径D32为1146微米，液滴粒径分布为D10为790微米，D50为1742微米，D90为1956微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.002m-1，液滴平均直径D32为442微米，液滴粒径分布为D10为401微米，D50为612微米，D90为934微米。
实施例32
与实施例2相同，区别在于每个喷洒装置上8个第二喷洒管相反两侧的喷嘴旋转室方向相反，另外8个第二喷洒管相反两侧的喷嘴旋转室方向相同。装置运行1个月，反应出口尾气的残留氨浓度为90ppm，装置运行24个月，反应出口尾气的残留氨浓度为105ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.04。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0103m-1，液滴平均直径D32为1231微米，液滴粒径分布为D10为778微米，D50为1692微米，D90为1923微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0018m-1，液滴平均直径D32为449微米，液滴粒径分布为D10为420微米，D50为643微米，D90为946微米。
实施例33
与实施例2相同，区别仅在于喷洒装置的第三喷洒末端投影重合且相邻的喷洒装置的投影重合的喷嘴旋转方向相反，装置运行1个月，反应出口尾气的残留氨浓度为85ppm，装置运行24个月，反应出口尾气的残留氨浓度为110ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.05。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0100m-1，液滴平均直径D32为1327微米，液滴粒径分布为D10为808微米，D50为1700微米，D90为1906微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0018m-1，液滴平均直径D32为452微米，液滴粒径分布为D10为424微米，D50为656微米，D90为989微米。
实施例34
与实施例2相同，区别仅在于喷洒装置第二喷洒管一侧的相邻的两个喷嘴旋转方向相反，且在第二喷洒管同一水平方向平行延伸线上的全部喷嘴旋转方向相同。喷洒装置俯视如图11B、喷洒装置俯视细节图如图11E示意图所示。装置运行1个月，反应出口尾气的残留氨浓度为106ppm，装置运行24个月，反应出口尾气的残留氨浓度为125ppm，装置运行24个月酸耗/装置运行 1个月酸耗为1.05。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0074m-1，液滴平均直径D32为1291微米，液滴粒径分布为D10为728微米，D50为1702微米，D90为2011微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.00145m-1，液滴平均直径D32为519微米，液滴粒径分布为D10为436微米，D50为672微米，D90为1046微米。
实施例35
与实施例2相同，区别喷洒装置相邻的两个第二喷洒管的相向一侧的全部喷嘴喷洒液的旋转方向相同，同一个第二喷洒管两侧的喷嘴喷洒液旋转方向相反。装置运行1个月，反应出口尾气的残留氨浓度为108ppm，装置运行24个月，反应出口尾气的残留氨浓度为121ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.04。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0072m-1，液滴平均直径D32为1345微米，液滴粒径分布为D10为723微米，D50为1726微米，D90为2071微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.00143m-1，液滴平均直径D32为503微米，液滴粒径分布为D10为438微米，D50为699微米，D90为1167微米。
实施例36
与实施例2相同，区别仅在于喷洒装置第二喷洒管一侧的相邻的两个喷嘴旋转方向相反，且同一第二喷洒管相反两侧的喷嘴旋转方向相反。装置运行1个月，反应出口尾气的残留氨浓度为125ppm，装置运行24个月，反应出口尾气的残留氨浓度为148ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.05。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0064m-1，液滴平均直径D32为1446微米，液滴粒径分布为D10为723微米，D50为1825微米，D90为2270微米。另外，在气体入口上方垂直 距离为8500mm处测量时，吸收气氛的消光系数为0.00141m-1，液滴平均直径D32为513微米，液滴粒径分布为D10为420微米，D50为739微米，D90为1190微米。
实施例37
与实施例1相同，区别在于喷洒装置的全部喷嘴的旋转室方向全部相同，装置运行1个月，从反应出口处尾气残留氨浓度为129ppm，装置运行24个月，反应出口尾气的残留氨浓度为149ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.06。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0052m-1，液滴平均直径D32为1586微米，液滴粒径分布为D10为723微米，D50为1825微米，D90为2331微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0012m-1，液滴平均直径D32为545微米，液滴粒径分布为D10为430微米，D50为780微米，D90为1254微米。
实施例38
与实施例2相同，区别在于相邻第三喷洒管间距为300mm，相邻两个第三喷洒管如囷6A所示的末端距离300mm。从反应出口处尾气残留氨浓度为76ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0051m-1，液滴平均直径D32为1620微米，液滴粒径分布为D10为1182微米，D50为2145微米，D90为2405微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0022m-1，液滴平均直径D32为430微米，液滴粒径分布为D10为382微米，D50为604微米，D90为924微米。
实施例39
与实施例2相同，区别在于相邻两个第三喷洒管如图6A所示的末端距离340mm。从反应出口处尾气残留氨浓度为105ppm。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛 的消光系数为0.0079m-1，液滴平均直径D32为1821微米，液滴粒径分布为D10为1077微米，D50为2180微米，D90为2855微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.00156m-1，液滴平均直径D32为461微米，液滴粒径分布为D10为427微米，D50为654微米，D90为883微米。
实施例40
与实施例2相同，区别在于沿流体方向第一喷洒管的第1至11个第二喷洒管上的喷嘴出口直径为11.7mm，第一喷洒管的第12至14个第二喷洒管上的喷嘴出口直径为11.9mm；装置运行1个月，从反应出口处尾气残留氨浓度为85ppm，装置运行24个月，反应出口尾气的残留氨浓度为99ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.03。
在本实施例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.00161m-1，液滴平均直径D32为1722微米，液滴粒径分布为D10为1128微米，D50为2310微米，D90为2785微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0014m-1，液滴平均直径D32为777微米，液滴粒径分布为D10为536微米，D50为841微米，D90为998微米。
对比例1
与实施例1相同，区别在于氨吸收塔采用图1的二段式结构形式，喷洒装置3a、3b、3c、3d喷洒液入口的喷洒液输入压力分别为0.04MPaG、0.044MPaG、0.046MPaG，0.051MPaG，喷洒液喷出压力为0.02MPaG，喷嘴出口直径为14.2mm，装置运行初期，从反应出口处尾气残留氨浓度为400ppm，装置运行24个月，从反应出口处尾气残留氨浓度为529ppm。
在本对比例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0033m-1，液滴平均直径D32为2976微米，液滴粒径分布为D10为1298微米，D50为3174微米，D90为3990微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0008m-1，液滴平均直径D32为742微米，液滴粒径分布为D10为523微米，D50为882微米，D90为1050 微米。
对比例2
与实施例2相同，区别在于氨吸收塔采用图2的一段式结构形式，喷洒装置3a、3b、3c、3d、3e与3f，喷洒液入口的喷洒液输入压力分别为1.202MPaG、1.205MPaG、1.209MPaG，1.214MPaG、1.217MPaG、1.220MPaG，喷洒液喷出压力为0.076MPaG，装置运行初期，从反应出口处尾气残留氨浓度为85ppm，装置运行24个月，从反应出口处尾气残留氨浓度为96ppm，但是在氨吸收塔出口尾气冷凝液中检测出1.5％的硫酸铵。
在本对比例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0263m-1，液滴平均直径D32为369微米，液滴粒径分布为D10为232微米，D50为550微米，D90为1239微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0052m-1，液滴平均直径D32为231微米，液滴粒径分布为D10为149微米，D50为315微米，D90为436微米。
对比例3
与实施例1相同，区别仅在于喷洒装置3a、3c与3b、3d的喷洒入口18在氨吸收塔同一侧，即第一喷洒管内流体方向相同，喷洒装置3a、3b、3c和3d喷洒入口投影基本重合，(如图1所示)，且喷洒装置3a、3c与3b、3d的第三喷洒管末端喷嘴在截面上的投影重合(如图5所示)。装置运行1个月，反应出口尾气的残留氨浓度为85ppm，装置运行24个月，反应出口尾气的残留氨浓度为253ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.13。
在本对比例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0038m-1，液滴平均直径D32为1386微米，液滴粒径分布为D10为523微米，D50为1725微米，D90为2831微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0008m-1，液滴平均直径D32为545微米，液滴粒径分布为D10为130微米，D50为680微米，D90为1454微米。
对比例4
与实施例2相同，区别仅在于喷洒装置3a、3c、3e与3b、3d、3f喷洒入口18在氨吸收塔同一侧，即第一喷洒管内流体方向相同，喷洒装置3a、3b、3c、3d、3e、3f喷洒入口投影基本重合，(如图2所示)，且喷洒装置3a、3c与3b、3d的第三喷洒管末端喷嘴在截面上的投影重合(如图5所示)。装置运行1个月，反应出口尾气的残留氨浓度为73ppm，装置运行24个月，反应出口尾气的残留氨浓度为223ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.13。
在本对比例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0039m-1，液滴平均直径D32为1356微米，液滴粒径分布为D10为521微米，D50为1856微米，D90为2913微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0008m-1，液滴平均直径D32为536微米，液滴粒径分布为D10为137微米，D50为649微米，D90为1450微米。
对比例5
与实施例2相同，区别仅在于喷洒装置3a、3c、3e与3b、3d、3f的喷洒入口18在截面上投影成30°，即喷洒装置相应的第一喷洒管流体方向成30°，喷洒装置的第三喷洒管末端投影不重合，如图8B所示。装置运行1个月，反应出口尾气的残留氨浓度为130ppm，装置运行24个月，反应出口尾气的残留氨浓度为343ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.15。
在本对比例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0034m-1，液滴平均直径D32为1672微米，液滴粒径分布为D10为540微米，D50为1738微米，D90为3213微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0008m-1，液滴平均直径D32为436微米，液滴粒径分布为D10为189微米，D50为649微米，D90为1550微米。
对比例6
与实施例2相同，区别仅在于喷洒装置3a、3c、3e与3b、3d、3f的喷 洒入口18在截面上投影成90°，即喷洒装置相应的第一喷洒管流体方向成90°，喷洒装置的第三喷洒管末端投影不重合。装置运行1个月，反应出口尾气的残留氨浓度为110ppm，装置运行24个月，反应出口尾气的残留氨浓度为293ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.10。
在本对比例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0035m-1，液滴平均直径D32为1582微米，液滴粒径分布为D10为640微米，D50为1714微米，D90为3138微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0009m-1，液滴平均直径D32为461微米，液滴粒径分布为D10为259微米，D50为618微米，D90为1489微米。
对比例7
与实施例2相同，区别仅在于喷洒装置3a、3c、3e与3b、3d、3f的喷洒入口18在截面上投影成120°，即喷洒装置相应的第一喷洒管流体方向成90°，喷洒装置的第三喷洒管末端投影不重合，如图8B所示。装置运行1个月，反应出口尾气的残留氨浓度为132ppm，装置运行24个月，反应出口尾气的残留氨浓度为353ppm，装置运行24个月酸耗/装置运行1个月酸耗为1.15。
在本对比例中，在气体入口上方垂直距离为3000mm处测量时，吸收气氛的消光系数为0.0032m-1，液滴平均直径D32为2522微米，液滴粒径分布为D10为678微米，D50为2924微米，D90为3738微米。另外，在气体入口上方垂直距离为8500mm处测量时，吸收气氛的消光系数为0.0006m-1，液滴平均直径D32为491微米，液滴粒径分布为D10为259微米，D50为876微米，D90为1573微米。

Claims (17)

  1. 一种腈的制造方法，包括使烃原料发生氨氧化反应而制造包含腈的反应产物的步骤(称为反应步骤)、和通过气体入口将所述反应产物引入吸收装置并在所述吸收装置中通过喷洒装置向所述反应产物喷洒喷洒液以冷却所述反应产物并形成吸收气氛的步骤(称为冷却步骤)，其中在所述气体入口上方垂直距离为3000mm处测量时，所述吸收气氛的消光系数为0.004-0.02m-1(优选0.006-0.018m-1)。
  2. 权利要求1所述的制造方法，其中在所述气体入口上方垂直距离为3000mm处测量时，所述吸收气氛的液滴平均直径D32为400-2600微米(优选600-2400微米)，和/或，在所述气体入口上方垂直距离为3000mm处测量时，所述吸收气氛的液滴粒径分布为D10为150-1500微米,D50为700-3000微米，D90为1400-3600微米(优选D10为250-1400微米,D50为800-2800微米，D90为1600-3500微米)。
  3. 权利要求1所述的制造方法，其中在所述气体入口上方垂直距离为8500mm处测量时，所述吸收气氛的消光系数为0.001-0.004m-1(优选0.0015-0.0035m-1)，和/或，在所述气体入口上方垂直距离为8500mm处测量时，所述吸收气氛的液滴平均直径D32为200-1400微米(优选400-1000微米)，和/或，在所述气体入口上方垂直距离为8500mm处测量时，所述吸收气氛的液滴粒径分布为D10为100-1000微米,D50为300-1800微米，D90为500-2200微米(优选D10为200-600微米,D50为400-1400微米，D90为600-1800微米)。
  4. 权利要求1所述的制造方法，其中所述喷洒装置包括喷洒液入口、与所述喷洒液入口流体连通的第一喷洒管、与所述第一喷洒管流体连通且垂直于所述第一喷洒管向其两侧延伸的多个第二喷洒管、与所述第二喷洒管流体连通且垂直于所述第二喷洒管向其两侧延伸的多个第三喷洒管、以及位于所述第三喷洒管末端且与其流体连通的喷嘴。
  5. 权利要求4所述的制造方法，其中在相邻的两个第二喷洒管上，一个第二喷洒管上的任意一个第三喷洒管的末端与另一个相邻第二喷洒管上的任意一个第三喷洒管的末端的直线距离M不小于320mm(优选不小于350mm)，和/或，所述喷嘴彼此相同或不同，喷洒液喷出量各自独立地为0.5-7.5t/h (优选0.9-6.5t/h)，和/或，所述喷嘴彼此相同或不同，喷嘴出口的喷洒液喷出压力各自独立地为0.03-0.85MPaG(优选0.04-0.65MPaG)，和/或，将所述喷洒液入口的喷洒液输入压力控制在0.06-1.00MPaG(优选为0.12-0.90MPaG，更优选为0.18-0.80MPaG)，和/或，任意两个所述喷洒装置的喷洒液入口的喷洒液输入压力的差异(绝对值)小于0.024MPa(优选小于0.018MPa，更优选小于0.012MPa)。
  6. 权利要求1所述的制造方法，其中多个(比如2-10个，优选4-8个)所述喷洒装置以预定的垂直间距沿着所述吸收装置的中心轴线方向分层设置在所述吸收装置内部，和/或，相邻两个所述喷洒装置的垂直间距(按喷洒装置的喷洒液入口的垂直间距计)为650-1350mm(优选750-1200mm)。
  7. 权利要求4所述的制造方法，其中在垂直于所述吸收装置的中心轴线方向横切所述吸收装置而获得横截面时，所述多个喷洒装置中的一个与所述多个喷洒装置中的另一个的选自第一喷洒管、第二喷洒管和第三喷洒管中的至少一个(优选全部)在所述横截面上的投影基本上重合。
  8. 权利要求7所述的制造方法，其中所述一个喷洒装置与所述另一个喷洒装置的全部喷嘴在所述横截面上的投影基本上重合，和/或，投影基本上重合的两个喷嘴具有相同的喷洒直径，和/或，投影基本上重合的两个喷嘴具有相同的喷洒液旋转方向。
  9. 权利要求1所述的制造方法，其中所述气体入口与所述喷洒装置(在存在多个时，指的是距离所述气体入口最近的所述喷洒装置)的喷洒液入口的垂直距离为800-6000mm(优选1000-5000mm)，和/或，所述气体入口的内径为800-1900mm(优选900-1700mm)，和/或，所述反应产物在所述吸收装置内的线速度为0.6-1.5m/s(优选0.7-1.3m/s)，和/或，所述喷洒液与所述反应产物的质量流量比为15-25:1。
  10. 权利要求1所述的制造方法，其中在所述气体入口与所述喷洒装置(在存在多个时，指的是距离所述气体入口最近的所述喷洒装置)之间的吸收装置内部空间，不设置能够实质性影响所述气体流动的机械构件。
  11. 权利要求7所述的制造方法，其中所述一个喷洒装置与所述另一个喷洒装置的喷洒液入口在所述横截面上的投影之间的夹角为180°。
  12. 权利要求11所述的吸收装置，其中在全部所述喷洒装置中，任意两 个奇数编号的所述喷洒装置的喷洒液入口在所述横截面上的投影之间的夹角为0°，任意两个偶数编号的所述喷洒装置的喷洒液入口在所述横截面上的投影之间的夹角为0°，并且任一奇数编号的所述喷洒装置与任一偶数编号的所述喷洒装置的喷洒液入口在所述横截面上的投影之间的夹角为180°。
  13. 权利要求11所述的吸收装置，其中所述喷嘴包括喷嘴入口、旋转室和喷嘴出口，其中所述旋转室被构造为使得从所述喷嘴入口进入的喷洒液在经过所述旋转室之后以旋转方式离开所述喷嘴出口。
  14. 权利要求11所述的吸收装置，其中在至少一个(优选全部)所述第二喷洒管上，位于所述第二喷洒管的相同一侧的相邻两个(优选全部)喷嘴被构造为使得喷洒液以相同的旋转方向喷出。
  15. 权利要求14所述的吸收装置，其中并排相邻的两个所述第二喷洒管的相向一侧的全部喷嘴被构造为使得喷洒液以相反的旋转方向喷出。
  16. 权利要求14所述的吸收装置，其中在至少一个(优选全部)所述第二喷洒管上，位于所述第二喷洒管的一侧的至少一个(优选全部)喷嘴被构造为使得喷洒液以旋转方向A喷出，位于所述第二喷洒管的相对另一侧的至少一个(优选全部)喷嘴被构造为使得喷洒液以旋转方向B喷出，其中所述旋转方向A与所述旋转方向B相反。
  17. 权利要求16所述的吸收装置，其中在所述喷洒装置的全部喷嘴中，以所述旋转方向A喷出喷洒液的喷嘴的数量与以所述旋转方向B喷出喷洒液的喷嘴的数量相等或基本上相等。
PCT/CN2024/091569 2023-07-05 2024-05-08 一种氨吸收效果改善的腈的制造方法 Ceased WO2025007635A1 (zh)

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