CN110898448A - Spray drying equipment and application thereof, and preparation method of catalytic cracking catalyst - Google Patents

Spray drying equipment and application thereof, and preparation method of catalytic cracking catalyst Download PDF

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Publication number
CN110898448A
CN110898448A CN201811085955.6A CN201811085955A CN110898448A CN 110898448 A CN110898448 A CN 110898448A CN 201811085955 A CN201811085955 A CN 201811085955A CN 110898448 A CN110898448 A CN 110898448A
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China
Prior art keywords
spray drying
spray
air inlet
pipe
tower body
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Pending
Application number
CN201811085955.6A
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Chinese (zh)
Inventor
周岩
杨凌
秦娅
苏周全
陈玉华
张志良
叶金应
王福功
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
Sinopec Catalyst Co
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
Sinopec Catalyst Co
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Priority to CN201811085955.6A priority Critical patent/CN110898448A/en
Publication of CN110898448A publication Critical patent/CN110898448A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/16Evaporating by spraying
    • B01D1/18Evaporating by spraying to obtain dry solids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/16Evaporating by spraying
    • B01D1/20Sprayers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00Catalysts comprising molecular sieves
    • B01J29/04Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/08Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
    • B01J29/085Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y containing rare earth elements, titanium, zirconium, hafnium, zinc, cadmium, mercury, gallium, indium, thallium, tin or lead
    • B01J29/088Y-type faujasite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/50Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • B01J35/51Spheres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Catalysts (AREA)
  • Drying Of Solid Materials (AREA)

Abstract

The application relates to the field of catalyst preparation and discloses spray drying equipment. Spray drying equipment includes air inlet room (2), spray chamber (8), tower body and discharging pipe (7) that communicate in proper order along vertical direction, be provided with air-supply line (1) on the air inlet room, be provided with inlet pipe (3) on spray chamber (8), just the one end of inlet pipe is connected in the outside, and the other end is provided with nozzle (4), the tower body includes vertical section (5) and toper section (6), wherein, the discharging pipe connect in the bottom of toper section. This application is through only setting up an export on the tower body at the spray drying tower, and gaseous commodity circulation and material granule take and flow to decurrent mode, and this kind of design makes material and gas through directly under, can not take place the bias current, and velocity field distribution is even to high temperature gas distributes more evenly, and catalyst product sphericity is high, can effectively reduce simultaneously because of the different adhesion of particle humidity or be close to the wall phenomenon that glues that takes place.

Description

Spray drying equipment and application thereof, and preparation method of catalytic cracking catalyst
Technical Field
The application relates to the field of catalyst preparation, in particular to a preparation method of a catalytic cracking catalyst in the field of petrochemical industry, spray drying equipment of spherical particle products and application of the spray drying equipment.
Background
The catalyst is a substance which can change the chemical reaction rate (increase or decrease) of a reactant in a chemical reaction without changing chemical equilibrium, and the mass and chemical properties of the catalyst are not changed before and after the chemical reaction. Especially in the field of petrochemical industry, catalytic cracking (FCC) catalysts are indispensable substances.
The catalyst is prepared by a series of processes, including drying the gelled catalyst. The conventional spray drying process is mainly completed by a spray drying tower, and comprises the following steps: liquid (or slurry phase) materials which are uniformly mixed are atomized into small liquid drops through an atomizer of a spray drying tower, hot air in the tower is utilized to carry out instantaneous contact so as to dry the materials, most of dried solid materials are gradually deposited in a space formed by a conical section at the bottom of the spray drying tower, then the materials are discharged through a discharge hole at the bottom of the conical section, gas is discharged through an exhaust port arranged on the side surface of a tower body of the drying tower, and in the process of discharging the gas, the gas flow can entrain a part of the materials to be discharged from an outlet on the side surface of the tower body and then enters a cyclone separator for separation and recovery.
However, in the actual production process, when the existing spray drying equipment dries the catalyst materials, some materials are adhered to the wall, the material particles are adhered to each other, and the sphericity of the spray-dried product is not good and the particle size distribution range of the particles is wide.
Therefore, there is a need to provide a spray drying apparatus which does not stick to the wall and the material, and has good sphericity of the catalyst product and small particle size distribution range.
Disclosure of Invention
The application aims to provide the spray drying equipment which has the advantages that the material is not adhered to the wall and the wall, the catalyst product is good in sphericity and small in particle size distribution range.
The inventor of the application discovers through deep research that because the air outlet is designed on the side face of the tower body of the existing spray drying tower, the flow field in the tower is easy to have a bias flow phenomenon, the uneven distribution of the flow field in the tower body leads to the uneven distribution of the temperature field of the high-temperature airflow, and some materials are insufficiently dried and stick to the wall, so that the adhesion phenomenon is generated among material particles, and the collision among the particles and the like lead to the poor sphericity of the catalyst, and the amount of fine powder is increased, so that the particle size distribution range is wider.
In order to realize above-mentioned purpose, this application provides a spray drying equipment on the one hand, spray drying equipment includes air inlet room, spray chamber, tower body and the discharging pipe that feeds through in proper order along vertical direction, be provided with the air-supply line on the air inlet room, be provided with the inlet pipe on the spray chamber, just the one end of inlet pipe is connected in the outside, and the other end is provided with the nozzle, the tower body includes vertical section and toper section, wherein, the discharging pipe connect in the bottom of toper section.
Preferably, the tapping pipe is an elbow pipe.
Preferably, the bending section of the tapping pipe has a curvature of 60 to 180 degrees.
Preferably, the tower body is cylindrical and the conical section is conical.
Preferably, the axis of the conical section is collinear with the axis of the tower body.
Preferably, an air inlet chamber is further arranged above the spray chamber, the air inlet pipe is arranged on the wall of the air inlet chamber, and a gas distributor is arranged in the air inlet chamber.
Preferably, the air inlet pipe is arranged on the side wall of the air inlet chamber.
Another aspect of the present application provides a use of the spray drying apparatus provided herein for preparing a catalytic cracking catalyst.
Yet another aspect of the present application provides a method for preparing a catalytic cracking catalyst, comprising a raw material metering step, a gelling reaction step, a filtration washing step, a spray drying step, a pulping step, a filtration step, an exchange step, a washing step, and a flash drying step, wherein the spray drying step is performed in the spray drying apparatus provided herein.
Preferably, the method further comprises the step of separating the gas-solid mixture after the spray drying step and before the slurrying step.
According to the technical scheme, only one outlet is arranged on the tower body of the spray drying equipment, and gas-phase material flow and material particles flow downwards, so that the material and the gas are directly communicated, bias flow cannot occur, the velocity field is uniformly distributed, and the high-temperature gas is uniformly distributed, so that on one hand, the conditions that the sphericity of the catalyst is poor and fine powder is increased due to particle collision and the like can be avoided, the phenomena of catalyst material abnormity and the like are inhibited, and the sphericity of the catalyst product is high; on the other hand, the particles are distributed more uniformly and are concentrated in the center of the tower body, the running track, the residence time and the evaporation rate of the particles tend to be consistent, the wall sticking phenomenon caused by different particle humidity adhesion or approach to the wall surface can be effectively reduced, and the operation effect of drying of the spray drying equipment is integrally improved.
Drawings
Fig. 1 is a schematic structural view of a spray drying apparatus according to a preferred embodiment provided herein.
Description of the reference numerals
1 air inlet pipe and 2 air inlet chamber
3 feeding pipe 4 nozzle
5 vertical segment 6 conical segment
7 discharge pipe 8 spray chamber
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In the following description, the term "vertical direction" refers to a direction perpendicular to the horizontal plane when the spray drying apparatus is laid flat on the horizontal plane, and may also refer to a direction of the geometric central axis of the tower body of the drying apparatus.
Hereinafter, the spray drying apparatus of the present application will be described in detail with reference to fig. 1.
As shown in fig. 1, the present application provides a spray drying apparatus. The spray drying equipment comprises an air inlet chamber 2, a spray chamber 8, a tower body (comprising a vertical section 5 and a hammer-shaped section 6) and a discharge pipe 7 which are sequentially communicated along the vertical direction.
Regarding the air inlet chamber 2, an air inlet pipe 1 is provided on the air inlet chamber 2 to introduce air into the interior of the drying apparatusHot air (preferably heated air, but not limited thereto) is introduced to dry the material, thereby obtaining a catalyst product. The spray drying equipment preferably controls the flow of hot air to be 50000-70000 m3The temperature of the inlet of the hot air is controlled to be 400-700 ℃. As for the position of the air inlet duct 1, it may be disposed at any position of the air inlet compartment 2, for example, the ceiling wall, but generally the tower body of the spray drying apparatus is very high in height in the vertical direction, and in order to reduce the height of the spray drying tower in the vertical direction, as a preferred embodiment, the air inlet duct 1 is disposed on the side wall of the air inlet compartment 2. On the basis, in this application, preferably, can also be provided with the gas distributor in the air inlet chamber 2, the steam that gets into through air-supply line 1 passes through the gas distributor, can flow into the tower body inside more evenly to make the catalyst material in the tower body be heated evenly.
Regarding the spray chamber, a feed pipe 3 is provided on the spray chamber 8, and one end of the feed pipe 3 is connected to the outside and the other end is provided with a nozzle 4 which is a pressure type material nozzle. In the present application, the flow rate of the feed liquid fed from the feed pipe 3 is preferably controlled to 5.0m3/h~15.0m3H; the nozzle may be one, but preferably a plurality of nozzles, the spray cone angle of the nozzle preferably being in the range of 30 to 90 degrees, so that the material can be dispersed and the drying efficiency is improved.
As for the tower body, the tower body of the spray drying device of the present application includes a vertical section 5 and a tapered section 6, and the material sprayed through the spray nozzle is sufficiently dried in the vertical section 5 and the dried material is gradually deposited on the tapered section 6. In the present application, it is preferable that the inner diameter of the vertical section 5 is 800-10000 mm, the height is 1500-30000 mm, and the shape of the vertical section 5 is cylindrical, and the shape of the tapered section 6 is conical, which is beneficial for the material to be heated equally at each position in the circumferential direction with the same radius, but the present application is not limited thereto, and the vertical section 5 may be a square column, and the tapered section 6 may be a square cone. More preferably, the axis of the vertical section 5 and the axis of the conical section 6 are collinear, that is, the geometric centerlines of the vertical section 5 and the conical section 6 are aligned, which design provides the most uniform distribution of the wavefield.
In the spray drying apparatus of the present application, a discharge pipe 7 is connected to the bottom end of the conical section 6. The discharge pipe 7 of the present application is preferably an elbow pipe, and the elbow pipe form is selected for the discharge pipe 7 because the tower body of a typical spray drying apparatus is very high in height in the vertical direction, and in order to reduce the height of the spray drying tower in the vertical direction, the discharge pipe is in the elbow pipe form. In addition, the bending degree of the bending section of the elbow is preferably in the range of 60-180 degrees, more preferably 60-90 degrees, and even more preferably 90 degrees, wherein the bending degree refers to the included angle between the bending part and the vertical part of the elbow. When the bending degree of the bending section of the bent pipe exceeds 90 degrees, the reduction of the height of the drying tower is not facilitated, so that the space utilization rate is reduced, and when the bending degree of the bending section of the bent pipe is less than 60 degrees, the smooth discharge of materials can be influenced. In the present application, the hot air outlet temperature of the outlet pipe 7 is preferably controlled to 80 to 200 ℃.
The operation of the spray drying apparatus of the present application is as follows: hot air is introduced into the tower body through the air inlet pipe 1, and the hot air is uniformly dispersed in the tower body under the action of the air distributor; uniformly mixed liquid (or slurry phase) materials are sprayed in the spray chamber 2 through the feeding pipe 3 and the nozzle 4, the materials are atomized into small droplets through the nozzle 4, and simultaneously the small droplets are instantaneously contacted with hot air in the vertical section 5 of the tower body to carry out heat exchange, so that moisture in the materials is evaporated, water vapor enters air, and the materials are dried; the dried material is accumulated in the conical section 6 and is discharged out of the tower body through a discharge pipe 7.
In the prior spray drying tower, because the side surface and the bottom are provided with two outlets, the flow field in the tower is easy to have a bias phenomenon, and the problems of poor sphericity, adhesion and the like of catalyst particles occur. This application only sets up an export (promptly, discharging pipe 7) through on the tower body at the spray drying tower, and gas phase commodity circulation and material granule take and flow to mode down, and the air current increases through the velocity of flow when the toper section, and the material after will drying passes through discharging pipe 7 and takes out, gets into next separation element and separates. The design ensures that the materials and the gas are directly communicated without bias flow, the velocity field distribution is uniform, and the high-temperature gas distribution is uniform, so that on one hand, the conditions of poor sphericity and fine powder increase of the catalyst, which are generated by particle collision and the like, can be avoided, the phenomena of special-shaped catalyst materials and the like are inhibited, and the sphericity of the catalyst product is high; on the other hand, the particles are distributed more uniformly and are concentrated in the center of the tower body, the running track, the residence time and the evaporation rate of the particles tend to be consistent, the wall sticking phenomenon caused by different particle humidity adhesion or approach to the wall surface can be effectively reduced, and the operation effect of drying of the spray drying equipment is integrally improved.
The foregoing is a particular result of the spray drying apparatus provided herein and its attendant advantages.
Based on this, the present application further provides a use of the spray drying apparatus provided in the present application as described above for preparing a catalytic cracking catalyst.
In addition, the application further provides a preparation method of the catalytic cracking catalyst. The method comprises the steps of raw material metering, gelling reaction, filtering and washing, spray drying, pulping, filtering, exchanging, washing and flash drying. Wherein the spray drying step is carried out in the spray drying apparatus provided herein.
The material dried by the spray drying apparatus provided herein is discharged with hot gas, and therefore, preferably, the method further comprises a step of separating the gas-solid mixture after the spray drying step and before the beating step to separate the gas-phase objects from the particulate material.
The present application will be described in detail below by way of examples.
In the following examples, the molecular sieve is a product produced by the Zilu catalyst plant, and is a rare earth-containing USY type molecular sieve, RE2O3(rare earth oxide) content was 2.0 wt%; the alumina sol is a product produced by a Qilu catalyst factory, and the content of alumina is 21 percent by weight; kaolin, a product of Suzhou Kaolin corporation, burned to 22% by weight; the pseudo-boehmite is a product of Shandong division of China aluminum industry Co., Ltd, and is reduced by 38 wt%.
Example 1
Adding water into a reaction kettle, adding 32 wt% of uniformly dispersed molecular sieve slurry (the adding amount is 25%), adding alumina sol (the adding amount is 15%), stirring for 15 minutes, adding kaolin (the adding amount is 35%), pulping for 1 hour, adding pseudo-boehmite (the adding amount is 25%), stirring for 0.5 hour, adding 37 wt% of concentrated hydrochloric acid (the adding amount is 100L), acidifying for 1 hour to obtain catalyst slurry, conveying the catalyst slurry into spray drying equipment provided by the application for spraying by a high-pressure pump, drying under the drying conditions that the inlet temperature of hot air is controlled to be 550 ℃ and the outlet temperature is 100 ℃ to obtain a catalyst A, and analyzing the particle size distribution and the sphericity of the catalyst A.
Comparative example 1
Catalyst B was prepared according to the procedure of example 1, except that, in the spray-drying apparatus used, one outlet (two outlets in total) was provided at each of the side and bottom of the column body, and the remaining parameters were the same, and catalyst B was obtained.
A comparison of the particle size and sphericity of catalyst A and catalyst B is shown in Table 1 below.
Figure BDA0001803125420000071
Referring to Table 1, the catalyst A obtained by example 1 had a particle size distribution of 92.48% between 20 μm and 149 μm and a sphericity of 0.928, while the catalyst B obtained by comparative example 1 had a particle size distribution of 91.09% between 20 μm and 149 μm and a sphericity of 0.904. It can be seen that with the spray drying apparatus of the present application, a catalyst product with a high sphericity and a more uniform particle distribution can be obtained.
The preferred embodiments of the present application have been described above in detail, but the present application is not limited thereto. Within the scope of the technical idea of the present application, many simple modifications may be made to the technical solution of the present application, including combinations of various technical features in any other suitable manner, and these simple modifications and combinations should also be considered as the content disclosed in the present application, and all fall within the scope of the present application.

Claims (10)

1. The utility model provides a spray drying equipment, its characterized in that, spray drying equipment includes air inlet room (2), spray chamber (8), tower body and discharging pipe (7) that communicate in proper order along vertical direction, be provided with air-supply line (1) on air inlet room (2), be provided with inlet pipe (3) on spray chamber (8), just the one end of inlet pipe (3) is connected in the outside, and the other end is provided with nozzle (4), the tower body includes vertical section (5) and toper section (6), wherein, discharging pipe (7) connect in the bottom of toper section (6).
2. A spray drying device according to claim 1, characterized in that the discharge pipe (7) is an elbow pipe.
3. A spray drying device according to claim 2, characterized in that the bending of the outlet pipe (7) is 60-180 degrees.
4. A spray drying device according to claim 1, wherein the vertical section (5) is cylindrical and the conical section (6) is conical.
5. A spray drying apparatus according to claim 4, characterized in that the axis of the vertical section (5) is collinear with the axis of the conical section (6).
6. A spray drying device according to claim 1, characterized in that a gas distributor is arranged in the air inlet chamber (2).
7. A spray drying device according to claim 6, characterized in that the air inlet duct (1) is arranged on a side wall of the air inlet chamber (2).
8. Use of a spray drying apparatus as claimed in any one of claims 1 to 7 for the preparation of a catalytic cracking catalyst.
9. A method for preparing a catalytic cracking catalyst, comprising a raw material metering step, a gelling reaction step, a filtration washing step, a spray drying step, a pulping step, a filtration step, an exchange step, a washing step, and a flash drying step, wherein the spray drying step is performed in the spray drying apparatus of any one of claims 1 to 7.
10. The method for preparing a catalytic cracking catalyst according to claim 9, wherein the method further comprises a step of separating a gas-solid mixture after the spray-drying step and before the slurrying step.
CN201811085955.6A 2018-09-18 2018-09-18 Spray drying equipment and application thereof, and preparation method of catalytic cracking catalyst Pending CN110898448A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002166160A (en) * 2000-12-01 2002-06-11 Asahi Kasei Corp System for automatically synthesizing catalyst precursor and system for automatically synthesizing catalyst
CN102183132A (en) * 2011-03-09 2011-09-14 上海化工研究院 Centrifugal spray drying device for catalysts for preparing olefins from formaldehyde
CN103706133A (en) * 2012-10-09 2014-04-09 天津泰士康工贸有限公司 Drying-spraying system for catalytic cracking catalyst
CN205730414U (en) * 2016-05-11 2016-11-30 成都尼达罗农业科技有限公司 A kind of production Water soluble fertilizer spray drying tower
CN206526528U (en) * 2017-02-10 2017-09-29 中国石油化工股份有限公司 A kind of press spray drying tower
CN206910831U (en) * 2017-07-12 2018-01-23 大连第一有机化工有限公司 A kind of catalyst spray drying tower

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002166160A (en) * 2000-12-01 2002-06-11 Asahi Kasei Corp System for automatically synthesizing catalyst precursor and system for automatically synthesizing catalyst
CN102183132A (en) * 2011-03-09 2011-09-14 上海化工研究院 Centrifugal spray drying device for catalysts for preparing olefins from formaldehyde
CN103706133A (en) * 2012-10-09 2014-04-09 天津泰士康工贸有限公司 Drying-spraying system for catalytic cracking catalyst
CN205730414U (en) * 2016-05-11 2016-11-30 成都尼达罗农业科技有限公司 A kind of production Water soluble fertilizer spray drying tower
CN206526528U (en) * 2017-02-10 2017-09-29 中国石油化工股份有限公司 A kind of press spray drying tower
CN206910831U (en) * 2017-07-12 2018-01-23 大连第一有机化工有限公司 A kind of catalyst spray drying tower

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Application publication date: 20200324