CN111111569A - Apparatus for preparing molecular sieve - Google Patents
Apparatus for preparing molecular sieve Download PDFInfo
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- CN111111569A CN111111569A CN201811279418.5A CN201811279418A CN111111569A CN 111111569 A CN111111569 A CN 111111569A CN 201811279418 A CN201811279418 A CN 201811279418A CN 111111569 A CN111111569 A CN 111111569A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/026—After-treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/20—Faujasite type, e.g. type X or Y
- C01B39/24—Type Y
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- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to the field of catalyst preparation, and discloses equipment for preparing a molecular sieve. The equipment for preparing the molecular sieve comprises a roasting furnace (A), a first gas-solid reactor (B1), a homogenizer (F), a second gas-solid reactor (B2), a gas-solid separator (C), a slurrying tank (D) and a tail gas treatment device (E), wherein the roasting furnace, the first gas-solid reactor, the homogenizer, the second gas-solid reactor and the gas-solid separator are sequentially communicated, the slurrying tank is connected with a discharging pipe of the gas-solid separator, and the tail gas treatment device is connected with an exhaust port of the gas-solid separator. Therefore, in the equipment for preparing the molecular sieve, the roasted molecular sieve solid material can react with SiCl in the process of one-time reaction, uniform mixing and re-reaction4The gas is fully reacted, so that a high-quality high-silicon molecular sieve product can be obtained.
Description
Technical Field
The invention relates to the field of catalyst preparation, in particular to equipment for preparing a molecular sieve used as a catalyst.
Background
Molecular sieves refer to a class of materials having uniform micropores with pore sizes comparable to the typical molecular size. The molecular sieve can be used as high-efficiency drying agent, selective adsorbent, catalyst, ion exchanger, etc. According to SiO2And Al2O3The molecular ratio of (A) is different, and molecular sieves with different apertures are obtained and are divided into A type, Z type, Y type and the like.
Wherein, the ratio of silicon to aluminum in the framework of the zeolite molecular sieve is closely related to the thermal stability, hydrothermal stability, chemical stability and the like of the molecular sieve. SiCl in a gas phase process is generally used4Dealuminizing and silicon supplementing by a method. Specifically, SiCl is adopted at a certain temperature4And (3) dealuminizing and replenishing silicon between the gas and the Y-type molecular sieve so as to prepare the high-silicon Y-type molecular sieve. SiCl4The method for dealuminizing and silicon supplementing has the characteristics of uniform dealuminizing, timely silicon supplementing, high crystal retention degree of a product and good thermal stability.
However, SiCl is currently being utilized4In the process of preparing the high-silicon Y-type molecular sieve by dealuminizing and silicon supplementing by the method, firstly, the Y-type molecular sieve and SiCl4The gas reacts in the fixed reactor, and the gas material and the solid material are not mixed uniformly in the cylinder, so that the molecular sieve and SiCl in the reactor are caused4The contact is insufficient, so that the molecular sieve has large mass difference, and the performance of the product and the stability of the using effect are influenced.
Therefore, it is necessary to provide a molecular sieve manufacturing apparatus with good product quality uniformity.
Disclosure of Invention
The invention aims to overcome the problem of large mass difference of molecular sieves in the prior art and provide equipment for preparing the molecular sieves.
In order to achieve the above object, in one aspect, the present invention provides an apparatus for preparing a molecular sieve, including a roasting furnace, a first gas-solid reactor, a homogenizer, a second gas-solid reactor, a gas-solid separator, a slurrying tank, and a tail gas treatment device, where the roasting furnace, the first gas-solid reactor, the homogenizer, the second gas-solid reactor, and the gas-solid separator are sequentially communicated, an inlet of the slurrying tank is connected to a discharge pipe of the gas-solid separator, and the tail gas treatment device is respectively connected to a gas outlet of the gas-solid separator and a gas outlet of the slurrying tank.
Preferably, the first gas-solid reactor comprises a material conveying chamber, a mixing chamber and a material discharging chamber, wherein the material conveying chamber is connected with a material inlet pipe and a material inlet pipe, the material discharging chamber is provided with a material discharging pipe, and the mixing chamber is a rotatable rotary drum.
Preferably, the inner wall of the rotating drum is provided with a material distribution structure.
Preferably, the material distribution structure is a paddle projecting inwardly in a radial direction of the drum.
Preferably, the length of the protruding of the pick from the inner wall of the drum is 0.05-0.10 times the diameter of the drum.
Preferably, the paddle is provided in plurality in the longitudinal direction and the radial direction of the drum, respectively.
Preferably, a material disperser is also arranged inside the inlet of the mixing chamber.
Preferably, the rotation speed of the drum is 5-25 rpm.
Preferably, the first gas-solid reactor further comprises a temperature sensor disposed inside the drum.
Through the technical scheme, in the equipment for preparing the molecular sieve, the molecular sieve is roasted in the roasting furnaceThe solid material enters a first gas-solid reactor and is reacted with SiCl4The gas-solid mixture after the gas reaction enters a homogenizer to be uniformly mixed and then enters a second gas-solid reactor, so that the molecular sieve solid material and SiCl4The gas reacts again, so that the calcined molecular sieve solid material can react with SiCl through the process of one-time reaction-uniform mixing-secondary reaction4The gas fully reacts, so that the uniformity of the molecular sieve is greatly improved, and a high-quality high-silicon molecular sieve product can be obtained.
Drawings
FIG. 1 is a flow diagram of an apparatus for preparing molecular sieves provided herein.
FIG. 2 is a schematic diagram of a gas-solids reactor for producing molecular sieves as provided herein.
Description of the reference numerals
Y molecular sieve A roasting furnace
B1 first gas-solid reactor B2 second gas-solid reactor
C gas-solid separator D slurrying jar
E tail gas treatment device F homogenizer
1 inlet pipe and 2 inlet pipes
3 material disperser 4 plectrum
5 rotary drum 6 temperature sensor
7 discharge pipe
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 addition, herein, "first," "second," "third," etc. are named merely to distinguish devices of the same or similar structure, and do not represent a sequential or primary-secondary relationship.
Hereinafter, the apparatus for preparing a molecular sieve provided herein will be described in detail with reference to fig. 1 and 2.
FIG. 1 is a flow diagram of an apparatus for preparing molecular sieves provided herein. As shown in fig. 1, the present application provides an apparatus for preparing a molecular sieve. The equipment for preparing the molecular sieve comprises a roasting furnace A, a first gas-solid reactor B1, a homogenizer F, a second gas-solid reactor B2, a gas-solid separator C, a slurrying tank D and a tail gas treatment device E. The roasting furnace A, the first gas-solid reactor B1, the homogenizer F, the second gas-solid reactor B2 and the gas-solid separator C are sequentially communicated, the inlet of the slurrying tank D is connected with the discharge pipe of the gas-solid separator C, and the tail gas treatment device is respectively connected with the exhaust port of the gas-solid separator C and the exhaust port of the slurrying tank D.
The molecular sieve Y is sent into a roasting furnace A to be roasted, the roasted molecular sieve solid material enters a first gas-solid reactor B1 and is mixed with SiCl which is introduced into a first gas-solid reactor B14After the gas is reacted, the gas-solid mixture enters a homogenizer F to be uniformly mixed, and then enters a second gas-solid reactor B2 to be reacted again, so that the molecular sieve solid material which is not reacted in the first gas-solid reactor B1 is reacted with SiCl in the second gas-solid reactor B24The gas continuously reacts, enters a gas-solid separator C after reaction, is separated into gas and solid in the gas-solid separator, the separated solid material enters a slurrying tank D to be prepared into liquid, and finally becomes a molecular sieve product, meanwhile, gases such as HCl and the like generated in the slurrying process in the slurrying tank are discharged to a tail gas treatment device E, the separated gas enters the tail gas treatment device E, and the gas entering the tail gas treatment device E is discharged to the air after being treated and reaching the standard.
In the equipment for preparing the molecular sieve, the roasted molecular sieve solid material can react with SiCl in the process of one-time reaction, uniform mixing and secondary reaction4The gas fully reacts, so that the uniformity of the molecular sieve is greatly improved, and a high-quality high-silicon molecular sieve product can be obtained.
On the basis of the above, when dividing into two partsWhen the requirement of the reaction depth of the molecular sieve is high, a second homogenizer (not shown) and a third gas-solid reactor (not shown) can be added after the second gas-solid reactor, so that the molecular sieve and SiCl are preferably mixed4The gas reacts for three times to reach the molecular sieve and SiCl4The gas is fully reacted to obtain high-quality molecular sieve products.
In the present application, the first gas-solid reactor B1 and the second gas-solid reactor B2 employ a different apparatus than the existing stationary gas-solid reactor, as follows. However, the present application is not limited thereto, and the two gas-solid reactors may both adopt the existing gas-solid reactor, or one of the two gas-solid reactors may adopt the gas-solid reactor of the preferred embodiment provided in the present application, and the other one adopts the existing gas-solid reactor. For convenience of description, the first gas-solid reactor and the second gas-solid reactor are both described below as gas-solid reactors.
Referring to fig. 2, the gas-solid reactor includes a material conveying chamber for inputting materials to be reacted into the gas-solid reactor, a mixing chamber for mixing the materials, and a material discharging chamber for discharging the reacted materials out of the reactor and inputting the materials into the gas-solid mixer C. It should be noted that the feeding chamber, the mixing chamber and the discharging chamber of the gas-solid reactor of the present application are structures in which spaces are communicated with each other, and are not structures in which the spaces are separated from each other, and therefore, the feeding chamber, the mixing chamber and the discharging chamber are named by dividing into three chambers in order to distinguish functions of the chambers. In addition, it will be explained below that, during operation of the gas-solid reactor, the feed chamber and the discharge chamber are stationary and the mixing chamber is rotating.
Specifically, a feed pipe 1 and an air inlet pipe 2 are arranged on the feed chamber, the molecular sieve enters the gas-solid reactor through the feed pipe 1, and SiCl is added4Gas enters the gas-solid reactor through a gas inlet pipe 2, wherein the molecular sieve and SiCl are respectively input through a feed pipe 1 and the gas inlet pipe 24The gas feeding structure and the gas feeding structure can be in various manners, as shown in fig. 2, a port of the feeding pipe 1 can extend into the mixing chamber, so that the molecular sieve directly enters the mixing chamber, and a port of the feeding pipe 2 is located in the feeding chamber, but the application is not limited theretoThe port of the feed pipe 1 may be provided above the feed chamber, and the port of the feed pipe may be formed in a dustpan shape or a trumpet shape to scatter the solid material into the mixing chamber. The discharge pipe 7 is provided in the discharge chamber, and the discharge structure may be various types, for example, as shown in fig. 2, the gas-solid mixture after the reaction is directly transferred to the next step through the discharge pipe 7, or may be transferred to the next step after being collected in a storage tank provided below the discharge pipe.
On this basis, the mixing chamber of the gas-solid reactor for preparing molecular sieves of the present application is a rotatable drum 5, the drum 5 can be driven by a motor, and the rotation speed of the drum 5 is preferably controlled at 5 to 25rpm, more preferably at 10 to 20rpm, still more preferably at 15 rpm. Solid molecular sieve and SiCl4When the gas reacts in the mixing chamber, the molecular sieve rotates and rolls in the interior of the rotating drum 5 along with the rotation of the rotating drum 5, so that each surface of the molecular sieve can be contacted with SiCl4Gaseous abundant contact for reaction homogeneity between them improves, can guarantee finally the performance of molecular sieve product and the stability of result of use, and rotary drum 5 itself is rotatory simultaneously, thereby the molecular sieve is difficult for the accumulation at the inner wall of rotary drum 5, thereby rotary drum 5 itself seldom takes place the scale deposit phenomenon, thereby has improved the ability of the transported substance material of the gas-solid reactor of this application.
In addition, as a preferred embodiment of the present application, a material distribution structure is provided on the inner wall of the rotating drum 5, and the material distribution structure is provided to improve the dispersibility of the material. The present application does not limit the form of the material distribution structure, and any member that can function as a dispersing member may be used, but the present application provides a more preferable material distribution structure, that is, as shown in fig. 2, the material distribution structure of the present application is a paddle 4 that protrudes inward in the radial direction of the rotating drum 5. The structure is simple, but the effect of dispersing materials is very good. Preferably, a plurality of the pulling pieces 4 are respectively arranged on the inner wall of the rotary drum 5 along the length direction and the radial direction of the rotary drum 5, and the plurality of the pulling pieces 4 are uniformly arranged, thereby improving the material and the SiCl4Mixing and reacting. The number and the angle of the poking pieces 4 can be reasonably designed according to the size of the rotary drum. Under the structure, in the process that the molecular sieve enters the rotary drum 5 and advances along the axial direction of the rotary drum 5, the molecular sieve is lifted by the stirring sheet 4 and dispersed while performing rotary motion, so that the molecular sieve moves in the radial direction of the rotary drum and then performs rotary motion, therefore, compared with a gas-solid reactor without the stirring sheet 4, the molecular sieve has high dispersion degree, and the molecular sieve and SiCl are high in dispersion degree4The gas is fully contacted, and the reaction effect is better.
With a material distribution structure in the form of a paddle 4, the paddle 4 preferably protrudes from the inner wall of the drum 5 by a length of 0.05 to 0.10 times the diameter of the drum, more preferably by 0.08 times. When the protruding length of the plectrum 4 is more than 0.10 times of the diameter of the rotary drum, the conveying of the molecular sieve along the axial direction of the rotary drum 5 is influenced, and when the protruding length of the plectrum 4 is less than 0.05 times of the diameter of the rotary drum, the dispersing effect of the plectrum 4 on the molecular sieve is general.
In the present application, it is preferable that the paddles 4 are uniformly distributed in the interior of the drum 5 in the length direction of the drum 5, and 20 paddles are provided, but the present application is not limited thereto. Further, the arrangement form and shape of the pick in the circumferential direction are also not limited, and for example, the pick may be in the form of a plurality of serrations arranged at intervals in the circumferential direction. In general, the paddles 4 are only required to disperse the material with the SiCl in the reactor4The gas is fully reacted.
As for the material of the paddle 4, a metal material is preferably used for the paddle 4, and a metal material of a corrosion-resistant material, for example, stainless steel, is more preferably used.
As shown in fig. 2, a material disperser 3 is provided inside the inlet of the mixing chamber. In particular, the material disperser 3 may be a helical bar suspended on the inner wall of the mixing chamber, the material disperser 3 acting: the molecular sieve is disturbed, thereby preventing agglomeration of the material.
In addition, in order to control the reaction temperature, the gas-solid reactor provided by the application also comprises a temperature sensor 6, and the temperature sensor 6 is arranged inside the rotary drum 5. The reaction temperature is controlled at 400-600 ℃ through the temperature sensed by the temperature sensor 6, so as to achieve the effect of monitoring the reaction temperature in real time.
Compared with the existing gas-solid reactor for preparing the molecular sieve, the gas-solid reactor for preparing the molecular sieve of the preferred embodiment of the application has the following advantages:
1) the mixing chamber of the gas-solid reactor adopts a rotary drum form, materials can be in full contact, so that the reaction uniformity is high, and the performance of a product and the stability of the using effect can be ensured finally; meanwhile, the rotary drum is rotary, and materials are not easy to accumulate on the inner wall of the rotary drum, so that the scaling phenomenon rarely occurs on the inner wall of the gas-solid reactor, and the material conveying capacity of the gas-solid reactor is improved;
2) the material distribution structure (stirring sheet) is arranged on the inner wall of the rotary drum, so that the dispersibility of the materials is improved, and the molecular sieve and SiCl are enabled to be4The gases react fully, the quality of the product can be improved finally, and SiCl is reduced4And (4) using the amount.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (9)
1. The equipment for preparing the molecular sieve is characterized by comprising a roasting furnace (A), a first gas-solid reactor (B1), a homogenizer (F), a second gas-solid reactor (B2), a gas-solid separator (C), a slurrying tank (D) and a tail gas treatment device (E), wherein the roasting furnace (A), the first gas-solid reactor (B1), the homogenizer (F), the second gas-solid reactor (B2) and the gas-solid separator (C) are sequentially communicated, an inlet of the slurrying tank (D) is connected to a discharging pipe of the gas-solid separator (C), and the tail gas treatment device is respectively connected to a gas exhaust port of the gas-solid separator (C) and a gas exhaust port of the slurrying tank (D).
2. The apparatus for preparing molecular sieves of claim 1, wherein the first gas-solid reactor (B1) comprises a feeding chamber, a mixing chamber and a discharge chamber, the feeding chamber is connected with a feeding pipe (1) and a feeding pipe (2), the discharge chamber is provided with a discharging pipe (7), and the mixing chamber is a rotatable drum (5).
3. The apparatus for the preparation of molecular sieves of claim 2, characterized in that the inner wall of the rotating drum (5) is provided with a material distribution structure.
4. The apparatus for preparing molecular sieves of claim 3, wherein said material distribution structure is a paddle protruding inwards in the radial direction of said rotating drum (5).
5. The apparatus for preparing molecular sieves of claim 4, wherein the plectrum protrudes from the inner wall of the rotating drum (5) by a length of 0.05-0.10 times the diameter of the rotating drum.
6. The apparatus for preparing a molecular sieve according to claim 4, wherein the plectrum is provided in plurality in the longitudinal direction and the radial direction of the rotary drum (5), respectively.
7. The apparatus for preparing molecular sieves of claim 2, wherein a material disperser (3) is further arranged inside the inlet of the mixing chamber.
8. The apparatus for the preparation of molecular sieves of claim 2, characterized in that the rotation speed of the rotating drum (5) is 5-25 rpm.
9. The apparatus for the preparation of molecular sieves of claim 2, wherein said first gas-solid reactor further comprises a temperature sensor (6), which temperature sensor (6) is arranged inside said drum (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811279418.5A CN111111569A (en) | 2018-10-30 | 2018-10-30 | Apparatus for preparing molecular sieve |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811279418.5A CN111111569A (en) | 2018-10-30 | 2018-10-30 | Apparatus for preparing molecular sieve |
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| CN111111569A true CN111111569A (en) | 2020-05-08 |
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| CN201811279418.5A Pending CN111111569A (en) | 2018-10-30 | 2018-10-30 | Apparatus for preparing molecular sieve |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1249428A2 (en) * | 2001-04-09 | 2002-10-16 | Chevron U.S.A. Inc. | Methods for making molecular sieves |
| CN202199339U (en) * | 2011-07-25 | 2012-04-25 | 北京世纪地和科技有限公司 | Internal rotation cylinder type gas-solid reactor in continuous operation and reaction system |
| CN203108482U (en) * | 2012-12-24 | 2013-08-07 | 广东塔牌集团股份有限公司惠州龙门分公司 | Barrel-shaped mixer |
| CN103787352A (en) * | 2012-10-26 | 2014-05-14 | 中国石油化工股份有限公司 | Method for preparing molecular sieve |
| CN103787353A (en) * | 2012-10-26 | 2014-05-14 | 中国石油化工股份有限公司 | Molecular sieve production apparatus |
| WO2015005407A1 (en) * | 2013-07-09 | 2015-01-15 | 三菱化学株式会社 | Zeolite production method |
| CN107159064A (en) * | 2017-05-19 | 2017-09-15 | 江苏和福特种气体有限公司 | A kind of horizontal gas solid reactor |
-
2018
- 2018-10-30 CN CN201811279418.5A patent/CN111111569A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1249428A2 (en) * | 2001-04-09 | 2002-10-16 | Chevron U.S.A. Inc. | Methods for making molecular sieves |
| CN202199339U (en) * | 2011-07-25 | 2012-04-25 | 北京世纪地和科技有限公司 | Internal rotation cylinder type gas-solid reactor in continuous operation and reaction system |
| CN103787352A (en) * | 2012-10-26 | 2014-05-14 | 中国石油化工股份有限公司 | Method for preparing molecular sieve |
| CN103787353A (en) * | 2012-10-26 | 2014-05-14 | 中国石油化工股份有限公司 | Molecular sieve production apparatus |
| CN203108482U (en) * | 2012-12-24 | 2013-08-07 | 广东塔牌集团股份有限公司惠州龙门分公司 | Barrel-shaped mixer |
| WO2015005407A1 (en) * | 2013-07-09 | 2015-01-15 | 三菱化学株式会社 | Zeolite production method |
| CN107159064A (en) * | 2017-05-19 | 2017-09-15 | 江苏和福特种气体有限公司 | A kind of horizontal gas solid reactor |
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Application publication date: 20200508 |