CN111139107A - Regeneration method of molecular sieve of synthesis gas cooling box and gas distributor - Google Patents
Regeneration method of molecular sieve of synthesis gas cooling box and gas distributor Download PDFInfo
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- CN111139107A CN111139107A CN202010021248.1A CN202010021248A CN111139107A CN 111139107 A CN111139107 A CN 111139107A CN 202010021248 A CN202010021248 A CN 202010021248A CN 111139107 A CN111139107 A CN 111139107A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/32—Purifying combustible gases containing carbon monoxide with selectively adsorptive solids, e.g. active carbon
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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
- B01D53/02—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 by adsorption, e.g. preparative gas chromatography
- B01D53/04—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 by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/106—Silica or silicates
- B01D2253/108—Zeolites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
Abstract
The invention provides a gas distribution plate, which comprises a support ring, a support beam and a distribution plate main body, wherein the support ring and the support beam are connected to form a support framework for supporting the gas distribution plate main body; the number of the supporting beams is n, one end of each supporting beam is connected with the inner edge of the supporting ring, and the other ends of the supporting beams are connected with each other, so that the supporting beams and the supporting rings form a conical surface; the distribution plate main body comprises m layers of distribution plates, each layer of distribution plate is an annular plate consisting of n fan-ring plates with uniform size, the annular plates are connected with the supporting beams, and the distribution plates are distributed in a step shape along the conical surface. The gas distribution plate is beneficial to uniform distribution of gas. Based on the gas distribution plate, the invention also provides a molecular sieve regeneration method, which uses the gas distribution plate of the invention to improve the molecular sieve regeneration rate and effect by using low-temperature plasma and simultaneously prevent the hydrogen-rich gas from generating side reaction under high temperature and high pressure.
Description
Technical Field
The invention belongs to the technical field of synthesis gas separation, and relates to a synthesis gas cooling box molecular sieve regeneration gas method and a matched regeneration gas distributor.
Background
The synthesis gas generated by coal gasification is purified by a low-temperature methanol washing system and then sent into a cold box (153 ℃) to separate hydrogen and carbon monoxide. Because the synthesis gas carries trace methanol, the synthesis gas directly enters the cold box to cause icing and blockage, and therefore, a molecular sieve for adsorbing the methanol is arranged at the upstream of the cold box and is generally used for one-time operation and one-time standby operation. The single molecular sieve needs to be cut out for regeneration after being saturated in adsorption, hot nitrogen is used for regeneration in the traditional process, methanol adsorbed on the molecular sieve is desorbed, and the methanol is sent to a torch along with the nitrogen for treatment. Because the molecular sieve is frequently desorbed, the process not only causes a large amount of consumption of nitrogen, but also wastes desorbed methanol and carbon monoxide, so that part of enterprises in the industry adopt a cold box hydrogen-rich gas as a regeneration medium. The hydrogen-rich gas in the cold box contains hydrogen and CO, and is used for molecular sieve regeneration at high temperature and high pressure, so that Fischer-Tropsch side reaction is easy to occur, alkane is generated to cause molecular sieve failure, and potential safety hazards exist.
Disclosure of Invention
The invention aims to improve the regeneration rate and effect of the molecular sieve by utilizing the high activity of low-temperature plasma, and simultaneously prevent the hydrogen-rich gas from generating side reaction at high temperature and high pressure. The hydrogen-rich gas after ionization produces great amount of active atoms to desorb the methanol adsorbed by the molecular sieve, and the hydrocracking of the active atoms can decompose the long paraffin pollutant on the molecular sieve into gaseous hydrocarbon to avoid the degradation of the adsorption performance of the molecular sieve. The hydrogen-rich gas is ionized by the plasma torch and the temperature rises, so that the steam heating can be replaced, and the process flow is simplified. Because the physical properties of the ionized hydrogen-rich gas are changed greatly, the regeneration process needs to be improved to ensure the regeneration effect of the molecular sieve, and a gas distributor which is beneficial to the uniform distribution of the gas is developed.
In order to achieve one aspect of the above object, the invention adopts the following technical scheme:
a gas distribution plate for a molecular sieve of a synthesis gas cold box, wherein the gas distribution plate comprises a support ring, a support beam and a distribution plate main body.
The support ring is of a hollow round table structure or a hollow ring structure with a narrow upper part and a wide lower part, and is connected with the support beam to form a support framework for supporting the distribution plate main body; when the support ring is in a hollow circular truncated cone structure, an included angle between the side surface of the hollow circular truncated cone and a plane P where the outer edge of the support ring is located is theta, the edge where a circle with a smaller radius is located at the upper part is an inner edge, and the edge where a circle with a larger radius is located at the lower part is an outer edge; when the support ring is a hollow ring structure, the edge where the circle with the smaller radius is located is the inner edge, and the edge where the circle with the larger radius is located is the inner edge.
The number of the supporting beams is n, n is greater than or equal to 3 and is an integer, one end of each supporting beam is connected with the inner edge of the supporting ring, the other end of each supporting beam is upwards connected with one point on a central axis bb' of a plane P which passes through the center of the outer edge of the supporting ring and is perpendicular to the outer edge of the supporting ring, and a central circular surface is formed at the connecting point, so that the supporting beams and the supporting ring form a conical surface, the included angle between each supporting beam and the plane P is theta, the theta is 15-25 degrees, and the included angles between every two adjacent supporting beams are equal.
The distribution plate main body comprises m layers of distribution plates, wherein m is more than or equal to 3 and is an integer, each layer of distribution plate is an annular plate consisting of n fan-ring plates with uniform size, the annular plate is connected with the supporting beam, each layer of distribution plate is distributed along the conical surface in a step shape, the circle centers of the distribution plates are all positioned on the central axis bb', the top layer of distribution plate and the central circular surface are positioned on the same plane, and the inner edges of the top layer of distribution plate are connected with the central circular surface; the radius of the inner circle of the K-th distribution plate is equal to that of the outer circle of the K-1-th distribution plate, the radius of the outer circle of the K-th distribution plate is equal to that of the inner circle of the K + 1-th distribution plate, and K is an integer of 1-m; each fan ring board includes the fan ring top cap that the level set up, and upper and lower baffling board of crisscross setting from top to bottom, wherein baffling board one side is connected in the outward flange department of K layer fan ring top cap and the opposite side extends down on the K th layer, baffling board one side is connected in the interior edge department of K +1 layer fan ring top cap and the opposite side extends up under the K th layer, wherein the lower baffling board one side on mth layer with the support ring is connected and the opposite side extends up, form the gap form distribution hole that is used for the gas circulation between the last baffling board on the K th layer and the lower baffling board on the K th layer.
When K is 1, the radius of the inner circle of the 1 st layer distribution plate (i.e., the top layer distribution plate, which is located at the uppermost part of the gas distribution plate) is equal to the radius R of the central circular surface0The 1 st layer of distribution plate and the central circular surface are in the same plane, the inner edge of the 1 st layer of distribution plate is connected with the central circular surface, the excircle radius of the 1 st layer of distribution plate is equal to the inner circle radius of the 2 nd layer of distribution plate, one side of the 1 st layer of upper baffle plate is connected with the outer edge of the 1 st layer of fan ring top cover (namely the arc edge with larger radius at the outer side of the fan ring) and the other side extends downwards, one side of the 1 st layer of lower baffle plate is connected with the inner edge of the 2 nd layer of fan ring top cover (namely the arc edge with smaller radius at the inner side of the fan ring; when K is m, the inner circle radius of the mth layer of distribution plate (namely, the bottom layer of distribution plate which is positioned at the lowest part of the gas distribution plate) is equal to the outer circle radius of the (m-1) th layer of distribution plate, the outer circle radius of the mth layer of distribution plate is equal to the radius of the circle with smaller radius of the support beam, one side of the upper baffle plate of the mth layer is connected to the outer edge of the top cover of the mth layer of fan ring, while the other side extends downwards, one side of the lower baffle plate of the mth layer is connected to the inner edge; when K is not equal to 1, the inner side and the outer side of the K-th distribution plate are respectively connected with a K-1-th lower baffle plate and a K-th upper baffle plate. The inner side of the support ring is connected with the mth layer of lower baffle plate.
In addition, in the present specification, the circle with the larger radius of the support ring is on a horizontal plane, i.e. the plane P, wherein the radius of the inner circle of the 1 st layer distribution plate (i.e. the top layer distribution plate) is R0The outer circle radius is R1The ring width (in this context, the ring width refers to the width of the ring of the annular plate of the distribution plate in the horizontal plane) is R1-R0(ii) a The radius of the inner circle of the 2 nd layer of distribution plate (adjacent to the 1 st layer of distribution plate and below the 1 st layer of distribution plate) is R1The outer circle radius is R2With a ring width R2-R1(ii) a Layer 3 distribution plate (i.e. with layer 2 distribution phase)Adjacent and below the 2 nd layer distribution plate) has an inner circle radius of R3The outer circle radius is R2With ring width R in the horizontal plane3-R2(ii) a The inner circle radius of the distribution plate main body positioned on the mth layer (namely, the distribution plate which is adjacent to the distribution of the (m-1) th layer, positioned below the distribution plate of the (m-1) th layer and closest to the support ring) is RmOuter radius of the outer circle Rm-1The width of the ring on the horizontal plane is Rm-Rm-1. The vertical direction extending along the top layer distribution plate, namely the 1 st layer distribution plate, is upward, and the direction extending along the bottom layer distribution plate, namely the mth layer distribution plate, is downward.
Preferably, the ring plate further comprises 2 triangular steel plates for connecting the ring plate and the support beam, the triangular steel plates are vertically arranged, one side of each triangular steel plate is connected with a linear edge of the ring top cover (namely, a linear edge connected with arc-shaped edges on the inner side and the outer side of the ring in the ring top cover), one side of each triangular steel plate is connected with the support beam, and the other side of each triangular steel plate is connected with a vertical edge of the upper baffle plate.
In one embodiment, the lower baffle is an "L" shaped plate with an included angle of 90 ° + θ.
In one embodiment, the lower edge of the upper baffle of the Kth layer and the upper edge of the lower baffle of the Kth layer are at the same horizontal height, and the height L of the upper baffle of the Kth layer1A height difference L between the K +1 th layer and the K-th layer340-60%, and the horizontal distance L between the upper baffle plate on the K-th layer and the lower baffle plate on the K-th layer2Is L340-70%, and the height L of the lower baffle plate on the K-th layer4＝L3-L1-L2×tanθ。
Wherein, for any layer of the distribution plate main body, the height L of the upper baffle plate1Height L of lower baffle plate4Horizontal distance L between upper and lower baffle plates2Height difference L between adjacent lower distribution plate bodies3Are all independent.
In one embodiment, when m is 3, the annular width of the 1 st and 3 rd layer distribution plates is less than the annular width of the 2 nd layer distribution plate, the 1 st and 3 rd layer distribution platesThe width of the ring is 50-200 mm, and the width of the ring of the 2 nd layer distribution plate is 150-250 mm; when m is 4, the ring width of the 1 st and 4 th distribution plates is smaller than that of the 2 nd and 3 rd distribution plates, the ring width of the 1 st and 4 th distribution plates is 50-200 mm, and the ring width of the 2 nd and 3 rd distribution plates is 150-250 mm; when m is 5, the ring width of the 1 st layer and the 5 th layer of distribution plate is less than that of the 2 nd, 3 rd and 4 th layers of distribution plates, the ring width of the 1 st layer and the 5 th layer of distribution plate is 50-200 mm, and the ring width of the 2 nd, 3 th and 4 th layers of distribution plates is 150-250 mm; when m is an integer greater than or equal to 6, the ring width of the 1 st, 2 nd, m-1 th and m-2 th distribution plates is less than that of the 3 rd to m-2 th distribution plates, the ring width of the 1 st and 2 nd distribution plates and the m-1 th and m-2 th distribution plates is 50-200 mm, and the ring width of the 3 rd to (m-2) th distribution plates is 150-250 mm; preferably, the radius R of the central circular surface0Is 40 mm-60 mm.
In one embodiment, the support beam and the support ring are made of steel and have the same thickness and width, wherein the thickness is 12mm to 25mm (0.5 to 1 inch) and the width is 100mm to 200mm, and the specific thickness is calculated according to the weight of the molecular sieve above. When the support ring is a hollow circular truncated cone, the width of the support ring is the width of the side surface of the hollow circular truncated cone; when the support ring is a hollow ring, the width of the support ring is the circular ring width of the hollow ring. Preferably, the gas distribution plate is made of steel, and the thickness of any one position of the gas distribution plate is the same as that of the support beam.
In one embodiment, n is 4 and m is 6.
In order to achieve another aspect of the above object, the present invention adopts the following technical solutions:
a molecular sieve tank of a molecular sieve of a synthesis gas cooling box comprises a tank body, wherein a process gas inlet valve and a process gas outlet valve are arranged on the tank body, the process gas inlet valve is positioned at the top of the tank body, the process gas outlet valve is positioned at the bottom of the tank body, a pressure relief pipeline connected with the pressure relief valve is arranged at the top of the tank body, q plasma torches are uniformly arranged on a seal head at the bottom of the tank body in an annular mode, the q plasma torches are preferably 8 plasma torches, the q plasma torches are integers larger than or equal to 3, the plasma torches are direct current plasma torches and are respectively connected with corresponding working gas pipelines, the plasma torches are preferably arranged on the tank body through flanges, and the working gas; the interior of the tank body is provided with a gas distribution plate according to any one of the preceding claims, a molecular sieve bed layer and a wire mesh, wherein the molecular sieve bed layer is positioned above the gas distribution plate, and the wire mesh is positioned at the top of the molecular sieve bed layer.
In one embodiment, the lower portion of the tank is provided with a molecular sieve discharge opening, preferably arranged obliquely downwards, such as an obliquely downwards directed flange, for discharging the molecular sieve.
In one embodiment, the hydrogen-rich gas is a mixed gas of hydrogen and carbon monoxide, preferably a mixed gas of 87% by volume of hydrogen and 13% by volume of carbon monoxide.
The invention further adopts the following technical scheme:
a method for regenerating molecular sieves using a molecular sieve tank according to the invention, wherein the method is divided into 3 stages:
the first stage is pressure relief, a process gas inlet valve and a process gas outlet valve of the molecular sieve tank are closed, the molecular sieve tank is cut into a working system, and a pressure relief valve is opened to release high-pressure gas in the tank into a PSA desorption gas compressor so that the pressure in the molecular sieve tank is reduced to 0.2-0.4 MPa;
the second stage is a regeneration stage, a hydrogen-rich gas valve on a working gas pipeline is opened, hydrogen-rich gas is introduced until the pressure in the molecular sieve tank is 0.4MPa, a plasma torch power supply is turned on, the hydrogen-rich gas is ionized by 10kV direct current, the hydrogen-rich gas is converted into low-temperature plasma at the temperature of 200-250 ℃, the low-temperature plasma is directly blown into the bottom of the molecular sieve tank, the low-temperature plasma is subjected to molecular sieve regeneration through a molecular sieve bed layer from bottom to top after being distributed through a gas distribution plate, the low-temperature plasma is discharged through a pressure relief valve and is sent into the PSA desorption gas compressor, and the regeneration process lasts 25-40min, preferably 30 min;
and the third stage is a pressurizing stage, the power supply of the plasma torch is closed, the hydrogen-rich gas is continuously introduced for 8-15min, preferably 10min for purging and cooling, the pressure relief valve is closed, the hydrogen-rich gas still enters the molecular sieve tank through the plasma torch and a corresponding pipeline so as to pressurize the molecular sieve tank, the pressurizing rate is 0.2-0.4 MPa/min, the hydrogen-rich gas valve is closed after the working pressure is reached, the introduction of the hydrogen-rich gas is stopped, a process gas inlet valve and a process gas outlet valve of the molecular sieve tank are opened, the molecular sieve tank is cut into the working system, and the working pressure is preferably 4.9-5.2 MPa, such as 5 MPa.
By adopting the technical scheme, the invention has the following positive effects:
according to the invention, the novel gas distribution plate is adopted to replace a ceramic ball as a supporting structure, so that gas flow distribution of the molecular sieve in the adsorption and regeneration processes is uniform, and the adsorption and regeneration effects are improved; in a molecular sieve tank using a traditional air distribution plate, firstly, ceramic balls with the diameter of 30mm are required to be filled on the air distribution plate as supports, the height of a ceramic ball layer is 0.5m, and then, molecular sieves are filled above the ceramic ball layer, so that the filling space of the molecular sieves is reduced; the gas distribution plate can be directly used as a molecular sieve supporting structure, the molecular sieve has no infiltration problem, and the filling amount of the molecular sieve in the molecular sieve tank is increased by 15 percent and the upper limit of the system load is increased because ceramic balls or silk screens are not required to be paved on the gas distribution plate.
On the other hand, the molecular sieve tank is easy to discharge the molecular sieve from the tank body, the side face of the molecular sieve tank is opened with a downward inclined discharge port flange when the molecular sieve is discharged, most of the molecular sieve can automatically flow out as shown in figure 1, and meanwhile, the distribution plate is high in the middle and low in the periphery, so that the molecular sieve can be discharged, and the labor cost is reduced.
In addition, in the molecular sieve regeneration method, the plasma torch is adopted to generate plasma, so that the tank body is compact and modularized in structure, the plasma torch can be simply and conveniently arranged on the tank body through the flange, and the plasma torch is of a direct current type, so that the influence of alternating current induction heating on the tank body is avoided. The invention adopts hydrogen-rich gas as working medium, which can prolong the service life of the plasma torch, ensure the plasma torch to be in the same reducing environment as the tank, and reduce the safety risk; the hydrogen-rich gas is ionized by high-voltage direct current to generate hydrogen plasma, and the temperature rise of the hydrogen plasma is synchronously realized, so that the steam heating process is omitted, and the process is simpler. Moreover, the molecular sieve regenerated by the hydrogen plasma has the following effects: (1) the hydrogen plasma has extremely high heat transfer and mass transfer capacity, and can keep the temperature of the molecular sieve bed layer uniform; (2) the hydrogen plasma contains a large amount of high-activity electrons and hydrogen atoms, so that the methanol desorption rate in the molecular sieve can be greatly improved; (3) the hydrogen plasma has the hydrocracking characteristic, can promote the cracking of long-chain alkane pollutants on the surface of the molecular sieve into gaseous hydrocarbons, and recovers the adsorption capacity of the molecular sieve, thereby realizing the regeneration purpose.
Drawings
FIG. 1 is a block diagram of a molecular sieve tank according to one embodiment of the present invention;
FIG. 2 is a diagram of a gas distribution plate according to one embodiment of the present invention;
FIG. 3 is a top view of the gas distribution plate according to FIG. 2;
FIG. 4 is a cross-sectional view along aa' of the gas distribution plate according to FIG. 2;
FIG. 5 is a partial enlarged view according to the dashed box portion of FIG. 4;
FIG. 6 is a graph of the molecular sieve of example 1 after 1 month of use;
figure 7 is a graph of the molecular sieve in comparative example 3 after 1 month of use.
Description of the symbols:
1 Process gas inlet valve
2 pressure relief pipeline
3 molecular sieve bed top wire mesh
Bed layer of 4 molecular sieve
5 gas distribution plate
6 molecular sieve discharge opening
7 working gas pipeline
8 process gas outlet valve
9 plasma torch
51 support ring
52 support beam
53 distribution plate body
531 Fan Ring coping
532 upper baffle plate
533 lower baffle
534 distribution hole
Detailed Description
Detailed description of the preferred embodimentsthe technical solution of the present invention will be further described with reference to the accompanying drawings and specific embodiments.
Example 1
As shown in fig. 1, the molecular sieve tank with a diameter of 2m and a height of 4m comprises a tank body, wherein a process gas inlet valve 1 and a process gas outlet valve 8 are arranged on the tank body, the process gas inlet valve 1 is arranged at the top of the tank body, the process gas outlet valve 8 is arranged at the bottom of the tank body, a pressure relief pipeline 2 connected with the pressure relief valve is arranged at the top of the tank body, 8 plasma torches 9 (not all shown in fig. 1) are uniformly arranged on a seal head at the bottom of the tank body in an annular shape, the plasma torches 9 are all direct current type plasma torches and are respectively connected with corresponding working gas pipelines 7, the plasma torches 9 are installed on the tank body through flanges, and the working gas is hydrogen-rich gas of hydrogen with a volume content; the gas distribution plate 5, the molecular sieve bed layer 4 and the metal wire mesh 3 are arranged in the tank body, the molecular sieve bed layer 4 is positioned above the gas distribution plate 5, and the metal wire mesh 3 is positioned at the top of the molecular sieve bed layer 4.
The gas distribution plate 5 assembled in the molecular sieve tank is shown in fig. 2 and 3, and the gas distribution plate 5 is made of steel and comprises a support ring 51, 4 support beams 52 and a distribution plate main body.
The support ring 51 is a hollow circular truncated cone structure with a narrow top and a wide bottom, the included angle between the side surface and the bottom surface (i.e. the surface where the circle with the larger radius at the bottom) of the hollow circular truncated cone is 20 degrees, and the width of the side surface is 150 mm.
One end of each of the 4 support beams 52 is connected to the support ring 51, and the other end is in a plane P passing through the center of the bottom surface of the support ring 51 and perpendicular to the bottom surface of the support ring 51A point on the axis bb' is connected with each other to form a central circular surface with a radius R0The support ring 51 and the 4 support beams 52 form a conical surface with an included angle theta of 20 degrees with the plane P, the included angle between the 4 support beams 52 is equal, the gas distribution plate is divided into four areas equally, wherein the support beam 52 has a width of 150mm and a thickness of 10mm, and the support ring 51 at the lowest part has a thickness of 10mm, so as to be mounted on the wall surface of the tank body for supporting.
The distribution plate main body is formed by 6 layers of distribution plates 53, each layer of distribution plate 53 is an annular plate consisting of 4 fan-ring plates with uniform size, each layer of distribution plate 53 is distributed in a step shape along a cone, the circle centers of all the layers of distribution plates are all arranged on a central axis bb', the 1 st layer of distribution plate and the central circular surface are arranged on the same plane, the inner edge of the 1 st layer of distribution plate is connected with the central circular surface, the excircle radius R1 of the 1 st layer of distribution plate is 100mm (the width of the ring corresponding to the 1 st layer of distribution plate is R1-R050 mm); the radius of the inner circle of the 2 nd layer of distribution plate is R1Outer radius of circle R2Is 250mm (ring width corresponding to the 2 nd layer distribution plate is R2-R1150mm), the radius of the inner circle of the 3 rd layer distribution plate is R2Outer radius of circle R3Is 450mm (the width of the ring corresponding to the 3 rd layer distribution plate is R3-R2＝200mm)，R4Is 600mm, R5Is 750mm, R6The diameter is 900mm, and the width of the circular ring of each layer of distribution plate can be calculated by analogy. Each fan ring plate of the distribution plate 53 comprises a horizontally arranged fan ring top cover 531, and upper baffle plates 532 and lower baffle plates 533 which are arranged in a vertically staggered manner, wherein one side of the upper baffle plate 532 on the 1 st layer is connected to the outer edge of the fan ring top cover 531 on the 1 st layer, while the other side extends downwards, one side of the lower baffle plate 533 on the 1 st layer is connected to the inner edge of the fan ring top cover 531 on the 2 nd layer, while the other side extends upwards; the upper baffle 532 on level 2 is connected to the outer edge of the top cover 531 of level 2 fan ring on one side and extends downward on the other side, and the lower baffle 533 on level 2 is connected to the inner edge of the top cover 531 of level 3 fan ring on one side and extends upward on the other side; successively recurrently, the upper baffle 532 of the 6 th layer is connected at one side to the outer edge of the top cover 531 of the 6 th sector ring and extends downwards at the other side, and the lower baffle 533 of the 6 th layer is connected at one side to the round edge with smaller radius of the support ring 51While the other side extends upward and slit-like distribution holes for gas communication are formed between the adjacent upper and lower baffles 532 and 533. Each layer of distribution plate 53 has a thickness of 10 mm.
The lower edge of the upper baffle 532 of each layer of distribution plate is at the same level as the upper edge of the lower baffle 533 of that layer of distribution plate. For the 1 st to 6 th distribution plates, the vertical height difference L of each distribution plate from the next distribution plate3The tangent value of the included angle theta (20 ℃) multiplied by the radius of the inner ring and the radius of the outer ring of the distribution plate and the height L of each upper baffle plate1Is L350% of the total amount of the slurry, and the horizontal distance L between the upper and lower baffle plates2Is L350% of the total. Namely, the vertical height difference L between the 1 st layer distribution plate and the second layer distribution plate3＝(R1-R0) X tan theta, height L of upper baffle 532 of layer 1 distribution plate1Height difference L between the 2 nd and 1 st distribution plates350% of the total vertical distance L between the upper baffle 532 of the 1 st layer of distribution plate and the lower baffle 533 of the 1 st layer of distribution plate2Is L350% of the total height of the lower baffle 533 of the 1 st layer of distribution plate4＝L3-L1-L2Xtan (20 DEG), and similarly, the 2 nd to 6 th layers of the distribution plate satisfy the similar relationship.
The hydrogen plasma in the molecular sieve tank desorbs methanol adsorbed by the molecular sieve, the alumina type molecular sieve with the diameter of 1.8-2.6 mm is adopted, the main component is a white sphere formed by alumina, the white sphere contains a large number of micropores, the effective aperture is 0.5nm, the supplier is UOP, and the molecular sieve has strong adsorption capacity on the methanol and can realize the removal of the methanol in the synthesis gas. During regeneration, hydrogen-rich gas forms hydrogen plasma through the plasma torch 9 and enters the molecular sieve tank, the regeneration pressure is 0.4MPa, the temperature is 240 ℃, and the flow rate of the hydrogen plasma is 0.5 t/h. The pressure drop of the gas distribution plate is 5kPa, and the pressure drop measured in the molecular sieve bed layer is 20 kPa. When the molecular sieve is regenerated, the plasma enters the molecular sieve tank from the bottom of the tank and passes through the gas distribution plate 5 through the distribution holes. The total time of single regeneration of the molecular sieve is 1 h.
When molecular sieve regeneration is performed using a molecular sieve tank system as shown in fig. 1, the following operations are performed:
and 3, closing the plasma torch 9, continuously introducing the hydrogen-rich gas to purge and cool the molecular sieve bed layer 4 for 10min, closing a pressure relief valve connected with the pressure relief pipeline 2 to improve the pressure in the tank, filling the molecular sieve with the hydrogen-rich gas at the speed of 0.3MPa/min until the pressure is the same as the pressure before the pressure reduction of the hydrogen-rich gas, closing the hydrogen-rich gas valve after the regeneration of the molecular sieve is finished, stopping introducing the hydrogen-rich gas, and entering a standby state.
After the gas distribution plate is adopted in the regeneration process of the molecular sieve in the embodiment 1, the ceramic balls do not need to be filled, and the loading of the molecular sieve can be improved by 15% under the condition of maintaining the position of the top part of the molecular sieve bed layer. After technical improvement, the molecular sieve is continuously used for 12 months, the pressure drop of the molecular sieve is always kept stable in the process, the regenerated molecular sieve is used for adsorbing methanol in the synthesis gas, and the methanol in the synthesis gas is always not detected after adsorption. When the load of the cold box is increased and the flow of the hydrogen-rich gas is increased to 125% of the design value through the molecular sieve, the synthetic gas at the outlet of the molecular sieve still does not detect methanol within reasonable operation time after the load is increased due to the reasons that the filling amount of the molecular sieve in the tank is increased after the technology is improved, the gas distribution efficiency of the gas distribution plate is improved, the regeneration effect of the molecular sieve is improved by plasma and the like. When the device is overhauled, the molecular sieve tank is opened for inspection, and the molecular sieve bed layer has no sign of being blown by airflow. After the molecular sieve is taken out and checked, the color of the originally polluted partial molecular sieve is restored to white, as shown in fig. 6, in the original regeneration process, a trace amount of Fischer-Tropsch reaction occurs when hydrogen-rich gas flows through a molecular sieve bed layer at high temperature, long-chain alkane is generated and adhered to the surface of the molecular sieve, and the molecular sieve is yellowed, and after the regeneration process is changed into hydrogen plasma, the high reaction activity of the hydrogen plasma enables the long-chain alkane adhered to the molecular sieve to be decomposed and disappear, so that the molecular sieve is restored to white.
Comparative example 1
At present, no industrial application report for the regeneration of the molecular sieve exists in the low-temperature plasma, the main research focuses on the treatment of VOC (volatile organic compounds) in the air, and the process flow is that the molecular sieve is firstly used for adsorbing target pollutants, and then the molecular sieve is subjected to oxidation treatment by using the air plasma (air is used as working gas to form an oxidizing environment). The low-temperature plasma regeneration characteristics of the ZSM-5 molecular sieve (environmental engineering report, 2017(11): 2951-.
This comparative example is different from example 1 in that the plasma generator used is composed of a coil wound around the outside of the molecular sieve tank and an electrode at the center of the tank, and the plasma generator generates low-temperature plasma by means of discharge of the internal and external electrodes, and has three problems when applied to engineering: (1) a metal shield cannot be arranged between the inner electrode and the outer electrode, otherwise, the electrodes cannot discharge, a quartz tube is adopted in the experiment of the comparative example 1, and the molecular sieve tank in the industry is generally made of carbon steel; if the outer electrode is installed on the inner wall of the tank body, the problems of short circuit and bias current exist. (2) In the experiment of the comparative example 1, the outer diameter of the quartz tube is only 25mm, the voltage required for breakdown of an inter-electrode medium is lower (6-10 kV), the diameter of a molecular sieve tank in industrial application is 2-4 m, if a plasma generation mode in the comparative example 1 is adopted, the voltage must be increased by more than 100 times, the high voltage cannot be provided on site (the highest direct current transmission voltage in China is 1000kV at present), and the potential safety hazard is very high. (3) The plasma generator in the comparative example 1 uses high-frequency alternating current, induction heating is serious, and particularly, the tank body is made of carbon steel in engineering application, so that the tank body can be over-heated (the principle is the same as that of an induction cooker).
Meanwhile, the plasma generator used in the comparative example 1 takes air as working gas, the air has strong oxidizability after being subjected to plasma treatment, the damage to the tank body and the electrode is serious, and the service life of a plasma torch taking air as working gas in general industry is only 300-500 h, so that the industrial production requirement cannot be met. Air is used as working gas, and oxidation reaction is carried out in the regeneration process to realize the removal of pollutants (benzene in comparative example 1) adsorbed by the molecular sieve; the working gas used in example 1 is rich in hydrogen, the regeneration process of the working gas mainly depends on the excitation and heating of the plasma to desorb the methanol adsorbed by the molecular sieve, and meanwhile, the hydrocracking of the hydrogen plasma can crack the long-chain alkane which is a pollutant on the surface of the molecular sieve, so the regeneration mechanism of the working gas is completely different from that of comparative example 1. In addition, the system according to example 1 is a reducing atmosphere (hydrogen, carbon monoxide) and the introduction of air presents a significant safety risk.
The method of comparative example 1 is only suitable for laboratory research, the object to be researched is the regeneration of the molecular sieve after adsorbing trace pollutants in the air, and the difference of the engineering application scene related to the method is huge. In order to solve the above problems, in example 1, a plasma torch is adopted, hydrogen-rich gas is used as a working gas, the working gas is directly ionized into plasma in the plasma torch, and the required voltage is 10kV due to the small distance between electrodes in the plasma torch; the plasma torch is a modularized product and is arranged on the tank bottom sealing head through a flange, so that the influence of the tank body on discharge is avoided; the plasma torch adopts direct current, so that the problem of induction and heat release does not exist; the hydrogen-rich gas is used as the working gas, the service life of the plasma torch can reach 5000h, and meanwhile, the safety risk brought by the oxygen is avoided.
Through the comparison between the example 1 and the comparative example 1, the research on the regeneration of the low-temperature plasma molecular sieve in the comparative example 1 does not have a technical reference relationship with the example 1, and the research in the comparative example 1 cannot be applied to the scene of the example 1.
Comparative example 2
The comparison example relates to the field of air VOC treatment, and is different from the comparison example 1 in that the adsorption of the molecular sieve and the regeneration of plasma are synchronously carried out, the molecular sieve simultaneously plays a catalytic role, and the details can be found in research on catalytic degradation of hexanal by combining the plasma with the molecular sieve catalyst (2010 Master thesis of southern China university, eastern China).
Similar to comparative example 1, the plasma working gas in this comparative example was air, high frequency alternating current was used, and a coil was wound outside the molecular sieve vessel to generate plasma. Therefore, if the method is applied to the scene described in embodiment 1 according to the technical route, a series of problems such as electrode oxidation, high voltage, safety risk and the like still exist, and there is no reference relationship with the technical scheme described in embodiment 1.
Comparative example 3
The difference between the comparative example and the example 1 is that a molecular sieve tank with the diameter of 2m and the height of 4m is not provided with a gas distribution plate, a ceramic ball layer with the thickness of 0.5m is filled below a molecular sieve bed layer, and the diameter of the ceramic ball is 30 mm. The molecular sieve type was the same as in example 1. The bed layer is regenerated by using hydrogen-rich gas containing 87% of CO and H213 percent, the regeneration process is carried out at 5MPa, the temperature is 250 ℃, and the hydrogen-rich gas flow rate is 650Nm3And h, the integral pressure drop of the ceramic ball and molecular sieve bed layer is 30 kPa. When the molecular sieve is regenerated, the hydrogen-rich gas passes through the molecular sieve bed layer from the lower end through the ceramic ball layer, and the total regeneration time is 2 hours. Opening the molecular sieve tank to the inlet valve of the PSA desorption gas compressor, and discharging the pressure in the tank to 0.3 MPa; (2) the valve for hydrogen rich gas to the molecular sieve tank was opened and the flow rate was set to 650Nm3H, simultaneously opening a steam valve of a hydrogen-rich gas preheater, and preheating the hydrogen-rich gas to 250 ℃ by using steam with the pressure of 4 MPa; (3) after the molecular sieve is regenerated for 1h by high-temperature hydrogen-rich gas, closing a steam valve of a hydrogen-rich gas preheater, and continuously introducing the hydrogen-rich gas to cool the molecular sieve until the temperature in the molecular sieve tank is reduced to below 50 ℃; (4) and closing the molecular sieve tank to an inlet valve of the PSA desorption gas compressor, pressurizing the molecular sieve tank to the same pressure as the hydrogen-rich gas by using the hydrogen-rich gas, closing a valve for leading the hydrogen-rich gas to the molecular sieve tank, and finishing the regeneration of the molecular sieve.
When the regeneration method is adopted, after the regeneration method is operated for one month, the methanol in the synthesis gas at the outlet of the molecular sieve is increased to 3ppm, so that the cold box is blocked due to icing. The molecular sieve tank is opened to observe that the molecular sieve turns yellow and black, and as shown in figure 7, the white part of the polluted molecular sieve is the normal molecular sieve, and the dark part of the polluted molecular sieve is the polluted molecular sieve. The detected pollutant is alkane, which is caused by the Fischer-Tropsch reaction of hydrogen-rich gas at high temperature and high pressure.
After the molecular sieve is replaced, the regeneration temperature is adjusted to 200 ℃, in order to achieve the regeneration effect, the regeneration time must be prolonged to 3 hours, but the alkane generation risk still exists.
In addition, when the regeneration system works normally, the ceramic balls are used as supports at the bottom of the bed layer, and in actual operation, because hydrogen-rich gas flows through the bed layer from bottom to top, the upper and lower layers of the molecular sieve-ceramic balls are easily damaged when the air flow speed is too high, the molecular sieve leaks downwards, and the ceramic balls turn upwards to the top of the molecular sieve. In the replacement embodiment 1, the distribution plate strengthens the air flow distribution, and meanwhile, the distribution plate is fixed on the tank body through bolts, so that the problem of bed layer disorder cannot occur.
The changes of the methanol content of the gas at the outlet of the molecular sieve tank in a typical adsorption period of the embodiment 1 and the comparative example 3 are respectively shown in the following table, and the embodiment 1 shows that not only the methanol removal precision is improved, but also the molecular sieve adsorption capacity is improved after the gas distribution plate is replaced and the molecular sieve regeneration method is changed. When the methanol content of the synthesis gas is analyzed, firstly, a high-pressure sampling steel cylinder is used for sampling from a sampling point of the device, the pressure is reduced to normal pressure through a pressure reducing valve, and then the gas chromatography is carried out, so that the methanol content can be obtained.
The use effects of example 1 and comparative example 3 show that: the regeneration medium is replaced by hydrogen plasma, and the high-activity plasma can improve the regeneration effect of the molecular sieve and simultaneously achieve the purposes of decomposing pollutants and recovering the activity of the molecular sieve. The novel gas distribution plate can improve the distribution effect of the gas flow during adsorption and regeneration, can reduce the pressure drop after replacing porcelain balls, improve the loading capacity of the molecular sieve and improve the maximum load of the molecular sieve.
The above embodiments are only for illustrating the invention and not for limiting the technical solutions described in the invention, and those skilled in the art should make modifications or equivalent substitutions on the invention, and all technical solutions and modifications without departing from the spirit and scope of the invention should be covered by the claims of the present invention.
Claims (10)
1. A gas distribution plate for a molecular sieve of a synthesis gas cold box is characterized by comprising a support ring, a support beam and a distribution plate main body,
the support ring is of a hollow round table structure with a narrow top and a wide bottom or a hollow ring structure, and is connected with the support beam to form a support framework for supporting the distribution plate main body;
the number of the supporting beams is n, n is greater than or equal to 3 and is an integer, one end of each supporting beam is connected with the inner edge of the supporting ring, the other end of each supporting beam is upwards connected with one point on a central axis bb' of a plane P which passes through the center of the outer edge of the supporting ring and is perpendicular to the outer edge of the supporting ring, and a central circular surface is formed at the connecting point, so that the supporting beams and the supporting ring form a conical surface, the included angle between each supporting beam and the plane P is theta, the theta is 15-25 degrees, and the included angles between every two adjacent supporting beams are equal;
the distribution plate main body comprises m layers of distribution plates, wherein m is more than or equal to 3 and is an integer, each layer of distribution plate is an annular plate consisting of n fan-ring plates with uniform size, the annular plate is connected with the supporting beam, each layer of distribution plate is distributed along the conical surface in a step shape, the circle centers of the distribution plates are all positioned on the central axis bb', the top layer of distribution plate and the central circular surface are positioned on the same plane, and the inner edges of the top layer of distribution plate are connected with the central circular surface; the radius of the inner circle of the K-th distribution plate is equal to that of the outer circle of the K-1-th distribution plate, the radius of the outer circle of the K-th distribution plate is equal to that of the inner circle of the K + 1-th distribution plate, and K is an integer of 1-m; each fan ring plate comprises a fan ring top cover arranged horizontally, an upper baffle plate and a lower baffle plate which are arranged in a vertically staggered manner, wherein one side of the upper baffle plate on the K layer is connected to the outer edge of the fan ring top cover on the K layer, the other side of the upper baffle plate on the K layer extends downwards, one side of the lower baffle plate on the K layer is connected to the inner edge of the fan ring top cover on the K +1 layer, the other side of the lower baffle plate on the K layer extends upwards, one side of the lower baffle plate on the m layer is connected with the support ring, the other side of the lower baffle plate on the m layer extends upwards, and gap-shaped distribution holes for;
preferably, the ring plate further comprises 2 triangular steel plates for connecting the ring plate and the support beam, the triangular steel plates are vertically arranged, one side of each triangular steel plate is connected with the linear edge of the ring top cover, one side of each triangular steel plate is connected with the support beam, and the other side of each triangular steel plate is connected with the vertical edge of the upper baffle plate.
2. The gas distribution plate of claim 1, wherein the lower baffle is an "L" shaped plate having an included angle of 90 ° + θ.
3. The gas distribution plate of claim 2, wherein the lower edge of the K-th upper baffle is at the same level as the upper edge of the K-th lower baffle, and the height L of the K-th upper baffle1The height difference L between the K +1 th layer and the K th layer of distribution plate340-60%, and the horizontal distance L between the upper baffle plate on the K layer and the lower baffle plate on the K layer2Is L340-70%, and the height L of the K-th lower baffle plate4＝L3-L1-L2×tanθ。
4. The gas distribution plate of claim 1, wherein when m is 3, the annular width of the 1 st and 3 rd layer distribution plates is less than the annular width of the 2 nd layer distribution plate, the annular width of the 1 st and 3 rd layer distribution plates is 50-200 mm, and the annular width of the 2 nd layer distribution plate is 150-250 mm;
when m is 4, the ring width of the 1 st layer and the 4 th layer of distribution plate is smaller than that of the 2 nd layer and the 3 rd layer of distribution plate, the ring width of the 1 st layer and the 4 th layer of distribution plate is 50-200 mm, and the ring width of the 2 nd layer and the 3 rd layer of distribution plate is 150-250 mm;
when m is 5, the ring width of the 1 st layer and the 5 th layer of distribution plate is less than that of the 2 nd, 3 rd and 4 th layers of distribution plates, the ring width of the 1 st layer and the 5 th layer of distribution plate is 50-200 mm, and the ring width of the 2 nd, 3 th and 4 th layers of distribution plates is 150-250 mm;
when m is an integer greater than or equal to 6, the ring width of the 1 st, 2 nd, m-1 th and m-2 th distribution plates is less than that of the 3 rd to m-2 th distribution plates, the ring width of the 1 st and 2 nd distribution plates and the m-1 th and m-2 th distribution plates is 50-200 mm, and the ring width of the 3 rd to (m-2) th distribution plates is 150-250 mm; preferably, the radius R of the central circular surface0Is 40 mm-60 mm.
5. The gas distribution plate according to claim 1, wherein the support beam and the support ring are made of steel and have the same thickness and width, wherein the thickness is 12mm to 25mm and the width is 100mm to 200mm, and preferably the gas distribution plate is made of steel and has the same thickness at any point as the support beam.
6. The gas distribution plate of any of claims 1 to 5, wherein n is 4 and m is 6.
7. The molecular sieve tank of the molecular sieve of the synthesis gas cooling box is characterized by comprising a tank body, wherein a process gas inlet valve positioned at the top of the tank body and a process gas outlet valve positioned at the bottom of the tank body are arranged on the tank body, a pressure relief pipeline connected with the pressure relief valve is arranged at the top of the tank body, q plasma torches are uniformly arranged on a seal head at the bottom of the tank body in an annular shape, the number of the plasma torches is preferably q, the number of the plasma torches is more than or equal to 3, the plasma torches are direct current plasma torches and are respectively connected with corresponding working gas pipelines, the plasma torches are preferably arranged on the tank body through flanges, and the working gas is hydrogen-rich gas; the interior of the tank body is provided with a gas distribution plate according to any one of the preceding claims, a molecular sieve bed layer and a wire mesh, wherein the molecular sieve bed layer is positioned above the gas distribution plate, and the wire mesh is positioned at the top of the molecular sieve bed layer.
8. The molecular sieve tank of claim 6, wherein the tank body is provided at a lower portion thereof with a molecular sieve discharge opening, preferably arranged obliquely downward, for discharging the molecular sieve.
9. The molecular sieve tank of claim 6, wherein the hydrogen-rich gas is a mixed gas of hydrogen and carbon monoxide, preferably a mixed gas of 87% by volume of hydrogen and 13% by volume of carbon monoxide.
10. A method for regenerating molecular sieves using a molecular sieve tank according to any of claims 7 to 9, characterized in that the method is divided into 3 stages:
the first stage is pressure relief, a process gas inlet valve and a process gas outlet valve of the molecular sieve tank are closed, the molecular sieve tank is cut into a working system, and a pressure relief valve is opened to release high-pressure gas in the tank into a PSA desorption gas compressor so that the pressure in the molecular sieve tank is reduced to 0.2-0.4 MPa;
the second stage is a regeneration stage, a hydrogen-rich gas valve on a working gas pipeline is opened, hydrogen-rich gas is introduced until the pressure in the molecular sieve tank is 0.4MPa, a plasma torch power supply is turned on, the hydrogen-rich gas is ionized by 10kV direct current, the hydrogen-rich gas is converted into low-temperature plasma at the temperature of 200-250 ℃, the low-temperature plasma is directly blown into the bottom of the molecular sieve tank, the low-temperature plasma is subjected to molecular sieve regeneration through a molecular sieve bed layer from bottom to top after being distributed through a gas distribution plate, the low-temperature plasma is discharged through a pressure relief valve and is sent into the PSA desorption gas compressor, and the regeneration process lasts 25-40min, preferably 30 min;
and the third stage is a pressurizing stage, the power supply of the plasma torch is closed, the hydrogen-rich gas is continuously introduced for 8-15min, preferably 10min, the pressure relief valve is closed, the hydrogen-rich gas still enters the molecular sieve tank through the plasma torch and a corresponding pipeline so as to pressurize the molecular sieve tank, the pressurizing rate is 0.2-0.4 MPa/min, after the working pressure is reached, the hydrogen-rich gas valve is closed to stop introducing the hydrogen-rich gas, the process gas inlet valve and the process gas outlet valve of the molecular sieve tank are opened, the molecular sieve tank is switched into the working system, and the working pressure is preferably 4.9-5.2 MPa, such as 5 MPa.
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