CN114425171A - Method for preparing microsphere particles by spray drying and method for preparing catalytic cracking catalyst - Google Patents
Method for preparing microsphere particles by spray drying and method for preparing catalytic cracking catalyst Download PDFInfo
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- CN114425171A CN114425171A CN202011185292.2A CN202011185292A CN114425171A CN 114425171 A CN114425171 A CN 114425171A CN 202011185292 A CN202011185292 A CN 202011185292A CN 114425171 A CN114425171 A CN 114425171A
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- 238000001694 spray drying Methods 0.000 title claims abstract description 89
- 239000002245 particle Substances 0.000 title claims abstract description 55
- 239000003054 catalyst Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000004523 catalytic cracking Methods 0.000 title claims abstract description 27
- 239000004005 microsphere Substances 0.000 title claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 50
- 239000002002 slurry Substances 0.000 claims abstract description 49
- 239000012071 phase Substances 0.000 claims abstract description 44
- 239000007790 solid phase Substances 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- 239000002808 molecular sieve Substances 0.000 claims description 8
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- 239000005995 Aluminium silicate Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 235000012211 aluminium silicate Nutrition 0.000 claims description 5
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 5
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical class C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 claims 2
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 37
- 239000000463 material Substances 0.000 description 30
- 238000009826 distribution Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000084 colloidal system Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229940095686 granule product Drugs 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003075 superhydrophobic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/16—Evaporating by spraying
- B01D1/18—Evaporating by spraying to obtain dry solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D45/00—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces
- B01D45/12—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by centrifugal forces
- B01D45/16—Separating dispersed particles from gases or vapours by gravity, inertia, or centrifugal forces by centrifugal forces generated by the winding course of the gas stream, the centrifugal forces being generated solely or partly by mechanical means, e.g. fixed swirl vanes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0027—Powdering
- B01J37/0045—Drying a slurry, e.g. spray drying
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The spray drying method for preparing microsphere particles and the catalytic cracking catalyst comprises the steps that the adopted spray drying tower comprises an upper half cone (3), a vertical cylinder (4) and a lower cone (8) from top to bottom; a slurry feeding hole (1) is formed in the upper-section semi-cone, and a top main air inlet (2) is formed in the top of the upper-section semi-cone; the side surface of the vertical cylinder body is provided with a side gas phase inlet (12), the interior of the lower cone is provided with a gas-solid separator (6), a gas phase outlet of the gas-solid separator is led out from the side surface of the lower cone, and a solid phase outlet of the gas-solid separator is opened at the bottom of the lower cone. The method provided by the invention has the advantages of high product yield, reduction of catalyst adhesion and wall sticking in the preparation process, uniform particle size of the prepared catalyst and good particle size concentration.
Description
Technical Field
The invention relates to a method for preparing microspherical particles by spray drying, in particular to a method for preparing a catalyst in the field of petrochemical industry.
Background
The main body of the conventional spray drying process is a spray drying tower, liquid (or slurry phase) materials which are uniformly mixed are atomized into small droplets by an atomizer of the spray drying tower, the materials are dried by utilizing the instantaneous contact of hot air in the tower, most of the dried materials are gradually deposited in a conical space at the bottom of the spray drying tower, and then the materials are discharged mainly through a discharge hole at the bottom. Because the existing spray drying tower is generally provided with two outlets and no internal member is arranged in the tower, the side outlet is mainly a gas phase outlet, and meanwhile, airflow can carry a part of materials to be separated from the outlet on the side surface of the tower body and then enter a cyclone separator for separation and recovery; most of the materials are discharged from an outlet at the bottom of the tower.
From the production reality, because the existing spray drying tower mostly adopts a side air outlet design, and has no any internal component, the phenomenon of uneven flow field distribution is easy to occur, so that the problems of wall adhesion, adhesion among particles and the like are caused, meanwhile, the uneven distribution of the flow velocity field can also cause a side outlet to carry a large amount of fine powder, even a part of larger particles are discharged, equipment such as a cyclone separator, a fine fraction classifier and the like needs to be arranged subsequently, the flow is longer, the problems of large fine powder classification treatment capacity and the like exist, and the problem of wider particle size distribution range of the particles can also be caused.
CN 201813815U has provided a spray drying prevents caking equipment, including spray drying tower and gas injection apparatus, the lower part gas circuit of gas injection apparatus and spray drying tower is connected, and gas injection apparatus can connect on the inverted cone jar body apart from the high department of discharge gate third, and this utility model discloses simple structure can prevent the material caking when carrying out spray drying to the material, improves the ejection of compact speed of material. It may be at certain degree to the material caking have the effect, but can't solve the gaseous phase and carry the many scheduling problems of granule.
203853015U discloses a spray drying tower, including flue gas inlet section and barrel that communicate with each other be provided with a plurality of baffle along vertical direction on the inner wall of barrel. The baffle is even to be set up on the inner wall of barrel, through the setting of baffle can reduce the inside flue gas flow field distribution unevenness of spray drying tower, improves the turbulence degree, and then improves the spray drying tower to the desorption efficiency of acid gas, reduces absorbent consumption so that the power consumption, but not be used for the spray drying tower of production granule product.
CN203916110U discloses a catalyst spray drying tower, which is mainly characterized in that an anti-sticking cover is arranged at a hot air outlet on the side surface of a lower cone, so that the accumulation of the catalyst can be effectively avoided, and a plurality of hot air distribution plates with round holes are arranged to distribute high-temperature air, so as to achieve the purpose of uniform flow field in the drying tower, thereby resulting in that the structure of the spray drying tower is relatively complex and the wall sticking of solid particles is easily caused.
Disclosure of Invention
The invention aims to solve the technical problems of large amount of gas-phase entrained particles, wall adhesion, complex flow and the like in the prior art, and provides a method for preparing microspherical particles by spray drying.
The second technical problem to be solved by the present invention is to provide a preparation method of a catalytic cracking catalyst.
The invention provides a method for preparing microsphere particles by spray drying, slurry raw materials enter a spray drying tower to be in contact with hot air main air for drying, the other strand of hot air enters tangentially from the side surface to form an air curtain to prevent from sticking to the wall, after the spray dried particles and the hot air are separated by an air-solid separator, products are extracted from the bottom of the spray drying tower, and the hot air carrying a small amount of fine powder is discharged from a gas phase outlet; the spray drying tower comprises an upper half cone 3, a vertical cylinder 4 and a lower cone 8 from top to bottom; a slurry feeding hole 1 is formed in the upper-section semi-cone, and a top main air inlet 2 is formed in the top of the upper-section semi-cone; the side surface of the vertical cylinder body is provided with a side gas phase inlet 12, the lower section cone is internally provided with a built-in gas-solid separator 6, a gas phase outlet of the gas-solid separator is led out from the side surface of the lower section cone, and a solid phase outlet of the gas-solid separator is opened at the bottom of the lower section cone.
The invention provides a preparation method of a catalytic cracking catalyst, which adopts the method for preparing microspheres by spray drying, wherein the slurry raw materials are kaolin: molecular sieve: aluminum sol: liquid acid: pseudo-boehmite is prepared from (0.5-5): (0.5-4): (0.1-3): (0.01-0.15): 1, and then mixing the mixture with water to obtain slurry; the solid-to-liquid ratio of the slurry raw material is 0.25-0.55; the feeding flow of the slurry raw material is 1.0m3/h～20.0m3H, the slurry feeding pressure is 7-13 MPa; the hot air is air.
Compared with the prior art, the method for preparing the microsphere particles by spray drying has the beneficial effects that:
in the adopted spray drying tower, a layer of air film is formed on the wall surface of the cylinder body through the built-in rotational flow baffle and the lateral air inlet, so that the phenomenon that materials are adhered to the wall can be greatly reduced; because the hot air main air adopts top vertical feeding and all the structures are centrosymmetric, the flow field in the drying equipment is more uniform, the drying speed of the material tends to be consistent, and the product quality is favorably improved; the built-in gas-solid separator can effectively separate gas and solid phases without arranging a subsequent cyclone separator, thereby simplifying the flow, reducing the energy consumption, reducing the abrasion and saving the occupied area.
The preparation method of the catalytic cracking catalyst provided by the invention has the beneficial effects that:
because the whole tower is in a central symmetrical structure, the flow field in the spray drying equipment is uniform, the drying rate of the catalyst tends to be consistent, the quality of the catalyst product can be improved, and the particle size distribution is more concentrated; the anti-sticking design reduces the amount of sticking and results in higher yields. The cyclone separator is not needed after the built-in gas-solid separator is adopted, so that the equipment investment and the maintenance cost are saved, the energy consumption is reduced, and the economic benefit is remarkable.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing microspheroidal particles by spray drying provided by the invention.
3 fig. 3 2 3 is 3 a 3 cross 3- 3 sectional 3 view 3 of 3 the 3 spray 3 drying 3 tower 3 of 3 fig. 3 1 3 at 3 a 3 location 3 a 3- 3 a 3. 3
Fig. 3 is a top view of a cyclone in a spray drying tower.
Fig. 4 is a schematic flow chart of the preparation of the catalytic cracking catalyst by spray drying in comparative example 1.
Description of reference numerals:
1-slurry feed inlet, 2-main air inlet, 3-upper section semi-cone, 4-vertical cylinder, 5-cyclone baffle, 6-gas-solid separator, 7-gas phase outlet, 8-lower section cone, 9-solid phase outlet, 10-fixed lug, 11-gas-solid separator inlet, 12-side gas phase inlet, 13-fine powder recoverer and 14-cyclone separator.
Detailed Description
The following describes the embodiments of the present invention in detail.
The invention provides a method for preparing microsphere particles by spray drying, slurry raw materials enter a spray drying tower to be in contact with hot air main air for drying, the other strand of hot air enters tangentially from the side surface to form an air curtain to prevent from sticking to the wall, after the spray dried particles and the hot air are separated by an air-solid separator, products are extracted from the bottom of the spray drying tower, and the hot air carrying a small amount of fine powder is discharged from a gas phase outlet; the spray drying tower comprises an upper half cone 3, a vertical cylinder 4 and a lower cone 8 from top to bottom; a slurry feeding hole 1 is formed in the upper-section semi-cone, and a top main air inlet 2 is formed in the top of the upper-section semi-cone; the side surface of the vertical cylinder body is provided with a side gas phase inlet 12, the lower section cone is internally provided with a built-in gas-solid separator 6, a gas phase outlet of the gas-solid separator is led out from the side surface of the lower section cone, and a solid phase outlet of the gas-solid separator is opened at the bottom of the lower section cone.
Optionally, the height ratio of the upper half cone, the vertical cylinder and the lower cone is 1-3: 4-8: 1-3; the side gas phase inlet is arranged at the position of 10% -70% of the vertical cylinder from bottom to top.
Optionally, the included angle between the generatrix of the upper half cone and the horizontal plane is 15-75 degrees, and the included angle between the vertical cylinder and the side wall of the lower half cone is 15-75 degrees.
Optionally, a cylindrical cyclone baffle 5 is arranged on the inner side of the side gas phase inlet, a side gas phase inlet 12 tangent to the inner wall of the vertical cylinder is arranged between the cyclone baffle and the inner wall of the vertical cylinder, the height of the cyclone baffle is 2% -30% of the height of the vertical cylinder, and the minimum distance of an annular gap formed between the cyclone baffle and the side wall of the vertical cylinder is 1mm-20 mm.
Preferably, the height of the rotational flow baffle is 5% -20% of the height of the vertical cylinder, and the minimum distance of an annular gap formed between the rotational flow baffle and the side wall of the vertical cylinder is 2mm-20 mm.
Optionally, in an axial cross section, the swirl baffle is parallel to the vertical barrel sidewall.
Optionally, the cyclone baffle consists of an upper straight cylinder section and a bottom expanding section, and the bottom expanding section is fixedly connected with the side wall of the vertical cylinder through a support lug.
Optionally, an included angle between the upper straight cylinder section and the lower expanding section of the cyclone baffle is 90-160 degrees; preferably from 100 to 150.
The gas-solid separator is a cyclone separator, the cyclone separator consists of a cyclone separator shell, a material flow inlet on the side surface of the shell, a gas phase outlet arranged at the top of the shell and a solid phase outlet at the bottom of the shell, and the lower part of the shell is of an inverted cone structure.
The cyclone separator is preferably cylindrical at the upper part, and the material flow inlet is tangential to the side wall of the cyclone separator.
Optionally, two or more cyclone separators are arranged in the lower cone of the spray drying tower, and the plurality of cyclone separators are arranged in axial central symmetry.
The inner wall of the spray drying tower and the surfaces of the inner wall and the outer wall of the gas-solid separator are coated with super-hydrophobic coatings.
Optionally, the diameter of the spray drying tower is 800-12000 mm, and the total height of the spray drying tower is 1500-40000 mm; 1-20 sprayers are arranged at the slurry feed port; the diameter of the main air inlet is 1-3m, and the diameter of the gas phase outlet is 1-2.5 m.
The invention provides a preparation method of a catalytic cracking catalyst, which adopts the spray drying method for preparing microspheres, wherein the slurry raw material isKaolin: molecular sieve: aluminum sol: liquid acid: the pseudo-boehmite is (0.5-5): (0.5-4): (0.1-3): (0.01-0.15): 1, and then mixing the mixture with water to obtain slurry; the solid-liquid ratio of the slurry raw material is 25-55 wt%; the feeding flow of the slurry raw material is 1.0m3/h～20.0m3H, the slurry feeding pressure is 7-13 MPa; the hot air is air.
Preferably, the slurry feed rate is 5.0m3/h～15.0m3H; the feeding pressure of the slurry is 8-11 MPa.
Preferably, the feed temperature is 25-50 ℃; the solid content is 20-40 wt%. More preferably, the feed temperature is 20-50 ℃; the solid content is 25-35 wt%;
optionally, the flow rate of the hot air introduced into the spray drying tower ranges from 30000 m to 90000m3The temperature of hot air introduced into the spray drying tower is 350-600 ℃; the temperature of a hot air outlet is 120-200 ℃, the flow ratio of main air to side-introduced hot air is 0.7-0.9: 0.1-0.3.
Preferably, the flow range of the hot air introduced into the spray drying tower is 50000-70000 m3H; the temperature of hot air introduced into the spray drying tower is 430-550 ℃; the temperature of the hot air outlet is 120-160 ℃.
Preferably, the powder raw material may be at least one selected from kaolin, pseudo-boehmite, molecular sieve and diatomite, and the liquid raw material may include liquid and/or colloid, for example, at least one selected from molecular sieve slurry, alumina sol, inorganic acid solution and deionized water; preferably, the slurry feed rate is 5.0m3/h～15.0m3/h；
Optionally, the preparation method of the catalytic cracking catalyst provided by the invention further comprises the following steps: the hot air which is led out from the gas phase outlet and carries a small amount of fine powder is led into a fine powder recoverer to recycle the fine powder; and (3) roasting a spray-dried product discharged from the solid phase outlet at the temperature of 450-550 ℃ to obtain the catalytic cracking catalyst. The spray drying tower is used for contacting the uniformly mixed liquid or slurry phase material with hot air to perform heat exchange, so that water in the material is evaporated, water vapor enters the air, and the material is dried. The adopted spray drying tower comprises an upper half cone, a vertical cylinder and a lower cone. The hot air main air enters from a top main air inlet arranged at the top of the upper half cone and is uniformly distributed in the tower through a hot air distributor. The slurry raw material is introduced from a slurry feed inlet in the upper half cone and is sprayed into the tower from a pressure material nozzle through a feed pipe to contact with hot air, wherein the pressure material nozzle can be one or more than one, and the spray cone angle is between 30 and 90 degrees. The slurry raw material is dried by contacting with hot air main air. And the other strand of lateral hot air enters from the lateral gas phase inlet, preferably, the air inlet direction of the lateral gas phase inlet is tangent to the inner wall of the vertical cylinder, and an air curtain is formed in the spray drying tower to prevent the sprayed slurry material from sticking to the wall. A gas-solid separator is arranged in the lower section cone of the spray drying tower, the gas-solid separator is provided with a material flow inlet, a gas phase outlet and a solid phase outlet, spray-dried particles and hot air tangentially enter the gas-solid separator, the effect of grading the particles is achieved through the centrifugal force, and a microsphere particle product is collected from the bottom of the spray drying tower through the solid phase outlet of the gas-solid separator; and the hot air carrying a small amount of fine powder is discharged from a gas phase outlet of the gas-solid separator.
The spray drying tower provided by the invention is internally provided with the gas-solid separator, so that the particle classification in the tower is further enhanced, and the separation purpose is realized. Thus, the subsequent cyclone separator can be saved and the fine powder directly enters a subsequent separation unit (such as a fine powder recoverer), thereby simplifying the process flow. The material flow inlet of the gas-solid separator is a tangential inlet or a rotational flow inlet or has an inclination angle of 1-80 degrees, and the material flow inlet can be one or a plurality of centrosymmetric inlets. The number of the built-in gas-solid separators is one or more, the gas-solid separators are arranged in axial central symmetry mode, gas phase outlets at the tops of all the gas-solid separators are collected and then led out from the side face of the lower cone, and all solid phase particles enter the bottom of the lower cone.
Preferably, a cyclone baffle is arranged inside the vertical cylinder of the spray drying tower, and the side gas phase inlet is arranged between the vertical cylinder and the cyclone baffle. In a preferred embodiment, the cyclone baffle comprises an upper straight cylinder section and a bottom expanding section, and the cyclone baffle and the vertical cylinder body of the spray drying tower are fixedly connected through a support lug. The included angle between the straight cylinder section and the diameter expanding section of the rotational flow baffle is 90-160 degrees, preferably 100-150 degrees.
The ratio of the height of the straight cylinder section of the rotational flow baffle to the height of the vertical cylinder is 2-30%, preferably 5-20%. The rotational flow baffle is horizontally arranged in the spray drying tower or spirally arranged, and spirally rises at an included angle of not more than 15 degrees. The proportion of the annular space area between the rotational flow baffle and the vertical cylinder to the total cross section of the whole cylinder is 0.02-0.4, preferably 0.05-0.2.
Preferably, the inner diameter of the spray drying tower is 0.8-1.2 m, and the height is 1.5-40 m.
The preparation method of the catalytic cracking catalyst provided by the invention has the advantages that the slurry raw material contains kaolin, a molecular sieve, alumina sol and liquid acid.
The following further describes the embodiments of the present invention with reference to the drawings. It should be noted that the implementation process is only used for illustrating the invention and is not limited to the invention. Various changes and modifications can be made by one skilled in the art without departing from the spirit and scope of the invention, and the technical solution used should also fall within the scope of the invention.
FIG. 1 is a schematic flow chart of a method for preparing microspheroidal particles by spray drying according to the present invention. As shown in the attached figure 1, the spray drying tower comprises an upper half cone 3, a vertical cylinder 4 and a lower half cone 8 from top to bottom, wherein a slurry feeding port 1 is arranged in the upper half cone, a spray head is arranged at the slurry feeding port, and a top main air inlet 2-1 is arranged at the top of the upper half cone; the vertical cylinder section is provided with a rotational flow baffle 5, and the rotational flow baffle and the vertical cylinder are connected and fixed through a support lug. The upper part of the rotational flow baffle is a straight cylinder section, the lower part of the rotational flow baffle is an expanding section, and an included angle beta between the straight cylinder section and the expanding section is 90-160 degrees, preferably 100-150 degrees. A side gas phase inlet 12 is arranged in an annular space between the side surface of the vertical cylinder and the cyclone baffle 5, a gas-solid separator 6 is arranged in the lower cone 8, a gas phase outlet 7 of the gas-solid separator 6 is led out from the side surface of the lower cone, and a solid phase outlet 9 of the gas-solid separator is opened at the bottom of the lower cone.
3 FIG. 3 2 3 is 3 a 3 cross 3- 3 sectional 3 view 3 of 3 the 3 spray 3 drying 3 tower 3 of 3 FIG. 3 1 3 at 3 the 3 A 3- 3 A 3 position 3. 3 As shown in figure 2, hot air enters the annular space between the side surface of the vertical cylinder 4 and the cyclone baffle 5 through a side gas phase inlet.
Fig. 3 is a top view of a cyclone in a spray drying tower. As shown in the attached figure 3, hot air entrained with materials enters from an inlet 11 of the gas-solid separator 6, and hot air is discharged from a gas phase outlet 7 after cyclone separation.
When the spray drying tower is in a working state, hot air is introduced from the main air inlet, the slurry raw material enters the atomizer of the spray drying tower through the slurry feeding hole 1 and is atomized into fog drops, and the fog drops are contacted with the hot air to carry out heat exchange, so that moisture in the material is evaporated, water vapor enters the air, and the material is dried. Another strand of hot air is introduced from the side air supply outlet 12, and swirls upwards along the wall surface of the vertical cylinder under the action of the swirling baffle 5, so that a layer of air film is formed on the wall surface, and meanwhile, a small amount of air is supplied downwards to form the air film on the lower conical section part, so that the problem of wall sticking of materials can be effectively reduced. A small amount of liquid drops or solid particles remained in the annular space between the rotational flow baffle and the vertical cylinder body flow out from the gap between the adjacent fixed support lugs, so that the accumulation of materials is avoided. After the cyclone air supply reaches the top, the movement direction is changed due to the influence of the inclination angle of the upper half cone, and the cyclone air supply and the drying main air flow downwards in parallel, so that the drying and dehydration of the materials are completed in the vertical cylinder of the drying equipment. The mixed materials after the drying process enter the gas-solid separator together through the tangential inlet of the gas-solid separator. The gas-solid separator is arranged in a lower cone of the spray drying equipment, 1-8 inlets of the gas-solid separator can be arranged, the effect of grading particles is achieved in the gas-solid separator through the action of centrifugal force, the hot air carries smaller particles to be discharged from a side gas phase outlet 7, and the larger particles are discharged from a bottom solid phase outlet 9. The spray drying equipment is provided with the built-in gas-solid separator, so that the flow field distribution in the drying equipment can be effectively controlled while the classification of internal particles is realized, a relatively uniform flow field distribution state can be formed in the equipment, and the problems of particle wall adhesion, large gas-phase entrained particle quantity, wide particle size distribution range, poor sphericity of catalyst particles, adhesion and the like can be effectively avoided.
The following examples and comparative examples further illustrate the preparation and effectiveness of the catalytic cracking catalyst provided by the present invention.
In the examples and comparative examples, the percentages referred to are percentages by weight.
Example 1
A catalytic cracking catalyst was prepared using the scheme shown in FIG. 1.
The preparation method of the slurry raw material adopts the traditional 2-grade 10m3A pot-type stirred tank reactor is used for preparing cracking catalyst colloid, which comprises 1400kg of kaolin (product of Suzhou Kaolin Co., Ltd., causticity 22%, the same below), 900kg of pseudo-boehmite powder (product of Shandong Branch of China aluminum industries, Ltd., causticity 38%, the same below), and SOY-2 molecular sieve (product of Zilu catalyst plant, rare earth-containing USY type molecular sieve, RE2O33860kg of slurry with the content of 2.0 percent, the same below), 1850kg of alumina sol (a product produced by a Qilu catalyst factory and with the content of alumina of 21 percent, the same below) and water are put into 600kg of a first-stage stirring and mixing kettle, the colloid is transferred into a second-stage stirring and mixing kettle after stirring and mixing for 3 hours, 53.7kg of 36 percent hydrochloric acid is added, and after stirring for 1 hour, 8600kg of carrier colloid is prepared, the solid content of the colloid is 35 percent, and the catalyst slurry raw material is obtained.
The spray drying tower comprises an upper section semi-cone 3, a vertical cylinder 4 and a lower section cone 8. The column is about 25 meters in total height and 9 meters in diameter. The height of the upper half cone is 5m, the height of the vertical cylinder is 12.5m, the height of the lower half cone is 8m, the included angles are 70 degrees and 80 degrees respectively, a rotational flow baffle is arranged in the vertical cylinder, the height of the rotational flow baffle is 1.25m, the included angle between the rotational flow baffle and the diameter expansion section is 120 degrees, the number of the lateral air inlets is 4, the number of the bottom gas-solid separators is 1, and the number of the volute inlets is 4.
Conveying catalyst slurry to be introduced from a spray head of a slurry feeding hole 1 of the upper-section semi-cone by a high-pressure pump for spraying, and drying fog drops in contact with hot air introduced from a top main air inlet 2 to form microsphere particles; the other hot air is introduced from a lateral air supply outlet 12 between the rotational flow baffle 5 and the vertical cylinder; a built-in gas-solid separator 6 is arranged in the lower cone 8, gas phase obtained by separation of the gas-solid separator is led out from a gas phase outlet 7 at the side surface of the lower cone, and the microsphere particle product is collected by a solid phase outlet 9 at the bottom.
The flow rate of the slurry feeding liquid is 10m3The flow rate of hot air is 60000m3H is used as the reference value. The inlet temperature of the hot air is 550 ℃ and the outlet temperature is 80 ℃. Obtaining the catalytic cracking catalyst A, and analyzing the particle size distribution and the yield of the catalytic cracking catalyst A. The results are shown in Table 1.
The examples of the invention used RIPP 30-90 to determine the catalyst sieve data (i.e., the weight fraction of catalyst in different particle size ranges) and the average particle size. See "analytical methods of petrochemical industry (RIPP test methods)," Yanggui ", ed, science publishers, 1990.
The yield calculation method comprises the following steps: (finished dry basis/raw material dry basis) 100%.
The dust collector 12 adopts a cloth bag, the gas phase reaches the emission standard, and the fine powder is further recycled.
Example 2
Example 2 the same raw materials and experimental methods as in example 1 were used, except that no swirl baffle 5 was provided in the spray drying tower. The tower is about 9 meters in height and 2.6 meters in diameter. The inlet temperature of the hot air is 500 ℃ and the outlet temperature is 70 ℃. Obtaining the catalytic cracking catalyst B. The particle size distribution and yield of the catalytic cracking catalyst B were analyzed. The results are shown in Table 1.
Comparative example 1
Comparative example 1 the same starting material as in example 1 was used. The flow of preparing the catalytic cracking catalyst by spray drying is shown in figure 4. As shown in fig. 4, the spray drying tower comprises an upper half cone, a vertical cylinder and a lower cone. The tower is about 24 meters in height and 7.5 meters in diameter. The spray drying tower is not provided with any internal components, a cyclone separator 14 is arranged behind a gas phase outlet 7 of the spray drying tower, a gas phase outlet of the cyclone separator is communicated with a dust remover 13, and a solid phase outlet of the cyclone separator 14 is used for extracting catalytic cracking catalyst products. The flow rate of the slurry feeding liquid is 10m3The flow range of the hot air is 60000/h. The inlet temperature of the hot air is 550 ℃ and the outlet temperature is 80 ℃. The other parameters are the same, and the catalytic cracking catalyst is preparedC. The particle size distribution, yield and wall-sticking amount of the catalytic cracking catalyst C were analyzed. The results are shown in Table 1. As can be seen from table 1, the catalyst product prepared by the catalytic cracking catalyst preparation method of the present invention has significantly improved particle concentration and improved catalyst product yield, because the yield is significantly improved, i.e., the amount of wall sticking on the spray drying tower is significantly reduced.
TABLE 1
| Example 1 | Example 2 | Comparative example 1 | |
| Catalytic cracking catalyst | A | B | C |
| 0μm～20μm，％ | 0.69 | 0.98 | 2.1 |
| 0μm～40μm，％ | 15.9 | 15.14. | 15.8 |
| 0μm～80μm，％ | 58.9 | 56.1 | 53.8 |
| 0μm～105μm，％ | 76.1 | 73.9 | 72.7 |
| 0μm～149μm，％ | 94.5 | 92.9 | 90.8 |
| Average particle diameter, μm | 67.5 | 69.8 | 74.7 |
| Yield and content of | 0.992 | 0.987 | 0.981 |
Claims (13)
1. A method for preparing microsphere particles by spray drying is characterized in that slurry raw materials enter a spray drying tower to be in contact with hot air main air for drying, the other hot air enters from the side surface tangentially to form an air curtain to prevent from sticking to the wall, after the spray dried particles and the hot air are separated by an air-solid separator, products are extracted from the bottom of the spray drying tower, and the hot air carrying a small amount of fine powder is discharged from a gas phase outlet; the spray drying tower comprises an upper half cone (3), a vertical cylinder (4) and a lower cone (8) from top to bottom; a slurry feeding hole (1) is formed in the upper-section semi-cone, and a main air inlet (2) is formed in the top of the upper-section semi-cone; the side surface of the vertical cylinder body is provided with a side gas phase inlet (12), the interior of the lower cone is provided with a gas-solid separator (6), a gas phase outlet of the gas-solid separator is led out from the side surface of the lower cone, and a solid phase outlet of the gas-solid separator is opened at the bottom of the lower cone.
2. The method for preparing microspheroidal particles by spray drying of claim 1 wherein the ratio of the height of said upper cone, vertical cylinder and lower cone is from 1 to 3: 4-8: 1-3; the side gas phase inlet is arranged at the position of 10% -70% of the vertical cylinder from bottom to top.
3. The method for preparing microspheroidal particles by spray drying as claimed in claim 1 wherein the included angle between the generatrix of said upper cone and the horizontal plane is in the range of 15 ° to 75 ° and the included angle between the vertical cylinder and the side wall of the lower cone is in the range of 15 ° to 75 °.
4. The spray drying method for preparing microspheroidal particles according to claim 1, 2 or 3 wherein said side gas inlet is internally provided with a cylindrical cyclone baffle (5), a side gas inlet (12) tangential to the inner wall of the vertical cylinder is provided between said cyclone baffle and the inner wall of the vertical cylinder, the height of said cyclone baffle is 2-30% of the height of the vertical cylinder, and the minimum distance between said cyclone baffle and the side wall of the vertical cylinder to form an annular gap is 1-20 mm;
preferably, the height of the rotational flow baffle is 5% -20% of the height of the vertical cylinder, and the minimum distance of an annular gap formed between the rotational flow baffle and the side wall of the vertical cylinder is 2mm-20 mm.
5. The method of spray drying microspheroidal particles of claim 4 wherein said swirl baffle is parallel to the vertical barrel sidewall in axial cross-section.
6. The spray drying method for preparing microspheroidal particles of claim 4 wherein said cyclone baffle is comprised of an upper cylindrical section and a bottom expanded diameter section, said bottom expanded diameter section being fixedly connected to said vertical cylindrical sidewall by means of lugs.
7. The spray drying method for preparing microspheroidal particles of claim 6 wherein the angle between the upper straight section and the lower expanded diameter section of said cyclone baffle is 90-160 °; preferably from 100 to 150.
8. A method for preparing microspheroidal particles by spray drying according to any of claims 1 to 7 wherein said gas-solid separator is a cyclone separator, said cyclone separator comprising a cyclone housing, a stream inlet on the side of the housing, a gas phase outlet at the top of the housing and a solid phase outlet at the bottom of the housing, said lower portion of the housing having an inverted conical configuration.
9. The method for preparing microspheroidal particles by spray drying of claim 8 wherein said lower cone is provided with two or more cyclones, and wherein said cyclones are arranged in axial symmetry.
10. A method for preparing microspheroidal particles by spray drying according to any of claims 1 to 7 wherein said spray drying tower has a diameter of 800 to 12000mm and a total tower height of 1500 to 40000 mm; 1-20 sprayers are arranged at the slurry feed port; the diameter of the main air inlet is 1-3m, and the diameter of the gas phase outlet is 1-2.5 m.
11. A method for preparing a catalytic cracking catalyst, which is characterized in that the method for preparing microspheres by spray drying according to any one of claims 1 to 10 is adopted, wherein the slurry raw material is kaolin: molecular sieve: aluminum sol: liquid acid: the pseudo-boehmite is (0.5-5): (0.5-4): (0.1-3): (0.01-0.15): 1, and then mixing the mixture with water to obtain slurry; the solid-to-liquid ratio of the slurry raw material is 0.25-0.55; the feeding flow of the slurry raw material is 1.0m3/h～20.0m3H, the slurry feeding pressure is 7-13 MPa; the hot air is air;
preferably, the slurry feed rate is 5.0m3/h～15.0m3/h；
Preferably, the slurry feed pressure is between 8 and 11 MPa.
12. The method for preparing a catalytic cracking catalyst according to claim 11, wherein the flow rate of the hot air introduced into the spray drying tower is in the range of 30000 to 90000m3The temperature of hot air introduced into the spray drying tower is 350-600 ℃; the temperature of a hot air outlet is 120-200 ℃, the flow ratio of main air to side-introduced hot air is 0.7-0.9: 0.1-0.3;
preferably, the flow range of the hot air introduced into the spray drying tower is 50000-70000 m 3/h;
preferably, the temperature of the hot air introduced into the spray drying tower is 430-550 ℃; the temperature of the hot air outlet is 120-160 ℃.
13. The catalytic cracking catalyst preparation method according to claim 11 or 12, further comprising: the hot air which is led out from the gas phase outlet and carries a small amount of fine powder is led into a fine powder recoverer to recycle the fine powder; and (3) roasting a spray-dried product discharged from the solid phase outlet at the temperature of 450-550 ℃ to obtain the catalytic cracking catalyst.
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