CN114477218A - Molecular sieve crystallization slurry cleaning equipment and cleaning method - Google Patents

Molecular sieve crystallization slurry cleaning equipment and cleaning method Download PDF

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Publication number
CN114477218A
CN114477218A CN202011171833.6A CN202011171833A CN114477218A CN 114477218 A CN114477218 A CN 114477218A CN 202011171833 A CN202011171833 A CN 202011171833A CN 114477218 A CN114477218 A CN 114477218A
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unit
molecular sieve
washing water
cleaning
waste liquid
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盛毅
乔晓俊
张林瑞
邢瑞思
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China Petroleum and Chemical Corp
Sinopec Catalyst Co
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China Petroleum and Chemical Corp
Sinopec Catalyst Co
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Priority to CN202011171833.6A priority Critical patent/CN114477218A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02Crystalline 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
    • C01B39/26Mordenite type
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D35/00Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
    • B01D35/02Filters adapted for location in special places, e.g. pipe-lines, pumps, stop-cocks
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02Crystalline 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
    • C01B39/36Pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
    • C01B39/38Type ZSM-5
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02Crystalline 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
    • C01B39/42Type ZSM-12
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02Crystalline 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
    • C01B39/46Other types characterised by their X-ray diffraction pattern and their defined composition

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  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Cleaning By Liquid Or Steam (AREA)

Abstract

The invention relates to the field of molecular sieve preparation, and discloses equipment and a method for cleaning molecular sieve crystallization slurry. The apparatus includes a main body (100), a feed unit (110), a discharge unit (120), a washing water inlet unit (200), a waste liquid discharge unit (300), a mixing and transferring unit (500), and a filtering unit (600). The cleaning method provided by the invention comprises the following steps: mixing the materials with the washing water entering from the washing water entering unit (200) under the action of the mixing and conveying unit (500), and filtering and washing the materials through the filtering unit (600). The cleaning equipment and the cleaning method provided by the invention can improve the cleaning effect, reduce the using amount of cleaning water and reduce the pollution to the environment.

Description

Molecular sieve crystallization slurry cleaning equipment and cleaning method
Technical Field
The invention relates to the field of molecular sieve preparation, in particular to a cleaning device and a cleaning method for molecular sieve crystallization slurry.
Background
Molecular sieves have been widely used in a variety of fields such as adsorption, separation, catalysis and ion exchange due to their regular and uniform pores, regularly arranged pores, close molecular size pores and adjustable modification of surface properties. The mordenite molecular sieve has excellent heat resistance, acid resistance and steam resistance, is an important petrochemical catalytic material, and shows excellent catalytic performance in hydrocarbon cracking, hydrocracking, modification, dewaxing, dimethylamine synthesis, alkane isomerization and polycyclic aromatic compound alkylation reactions. Has become an important petrochemical catalytic material.
In the preparation of the molecular sieve, metal cations are usually introduced in the gelling process, and since the introduced metal cations affect the performance of the molecular sieve, the metal cations in the crystallization slurry of the molecular sieve need to be removed after the colloid is crystallized.
At present, the traditional molecular sieve cleaning method is carried out by utilizing an open belt filter, and in the actual production, the open belt filter must ensure that materials are immersed in cleaning water in the cleaning and filtering process to achieve the cleaning effect, so that the consumption of the belt filter on the cleaning water is very large, the recovery rate of mother liquor after cleaning is very low, and the raw materials are seriously wasted. In addition, especially when the mordenite molecular sieve is prepared, because ammonia gas needs to be introduced in the production process, the open belt filter also has the problem of ammonia gas leakage in the washing process, and the open belt filter also can harm the health of operators and cause air pollution.
Therefore, a cleaning device and a cleaning method for molecular sieve crystallization slurry are needed to clean the molecular sieve with high efficiency and energy saving.
Disclosure of Invention
The invention aims to solve the problems of high water consumption for cleaning molecular sieve crystallization slurry, easy environmental pollution and the like in the prior art, and provides a molecular sieve crystallization slurry cleaning device and a cleaning method.
In order to achieve the above objects, a first aspect of the present invention provides an apparatus for cleaning a molecular sieve crystallization slurry, the apparatus comprising a main body, a feeding unit, a discharging unit, a cleaning water inlet unit, a waste liquid discharge unit, a mixing and conveying unit, and a filtering unit.
The feeding unit and the discharging unit are respectively arranged at two ends of the main body and are respectively used for enabling materials to enter and discharging the materials.
The washing water inlet unit is disposed at an upper end of the main body, and is used for allowing washing water to enter the washing apparatus.
The waste liquid discharge unit is arranged at the lower end of the main body and used for discharging waste liquid in the cleaning equipment.
The mixing and transferring unit is provided inside the main body, and includes a rotation shaft at the center, a connection member provided on the rotation shaft at a certain interval, and an impeller connected to the rotation shaft through the connection member.
The filtering unit is arranged in the main body and is perpendicular to the rotating shaft, the filtering unit and the impeller are alternately arranged, the filtering unit comprises a filtering plate, a chamber positioned in the middle of the filtering plate and a filtering medium positioned on the surface of the filtering plate, a round hole is formed in the center of the filtering plate, the rotating shaft penetrates through the round hole, an annular gap is reserved between the round hole and the rotating shaft, and one end of the chamber is connected with the waste liquid discharge unit.
Preferably, the cleaning equipment further comprises a power unit for providing power for the feeding unit to convey the materials.
Preferably, the power unit is selected from one or more of a diaphragm pump, a hydraulic power pump and a magnetic force driven pump.
Preferably, the impeller is rotated by the rotating shaft, and the material entering from the feeding unit is mixed with the washing water entering from the washing water entering unit during the rotation, and the mixed slurry of the washing water and the material is pushed to be conveyed.
Preferably, the number of the filter units is more than one, and more preferably 8-9.
Preferably, the number of the impellers is more than one, and more preferably 9-10.
Preferably, one or more washing water inlet units are provided, each washing water inlet unit includes a washing water inlet valve for controlling the inlet of washing water, and the inlet amount of washing water is controlled by adjusting the opening degree of the washing water inlet valve.
Preferably, the waste liquid discharge unit is provided with one or more waste liquid discharge valves for controlling the discharge of waste liquid, and the discharge amount of waste liquid is controlled by adjusting the opening degree of the waste liquid discharge valves.
Preferably, the discharge unit comprises a discharge valve for controlling the discharge of material.
Preferably, the filter medium is selected from a filter mesh; more preferably, the filter medium (630) is selected from a metal filter mesh and/or a ceramic filter mesh.
In a second aspect, the present invention provides a method for cleaning molecular sieve crystallization slurry, the method being performed by using the cleaning apparatus of the first aspect, the method including: the materials are mixed with the cleaning water entering from the cleaning water inlet unit under the action of the mixing and conveying unit, and the materials are filtered and cleaned through the filtering unit.
Preferably, the entry rate of the washing water is 0.5 to 5m3H; the material inlet speed is 1-10m3H; the discharge rate of the waste liquid is 1-7m3H; the discharge rate of the material is 0.5-8m3H; the rotating speed of the impeller (530) is 50-300 r/min; the pressure in the main body (100) is 0.08-0.6 MPa.
More preferably, the washing water has an entry rate of 3 to 4m3H; the entry rate of the materials is 2-3m3H; the discharge rate of the waste liquid is 3-4m3H; the discharge rate of the material is 2-3m3H; the rotating speed of the impeller is 150-200 r/min; the pressure in the main body (100) is 0.08-0.4 MPa; further preferably, the pressure inside the body (100) is 0.08-0.1 MPa.
Preferably, the molecular sieve in the molecular sieve crystallization slurry is one or more of a mordenite molecular sieve, a ZSM-5 molecular sieve, a ZSM-12 molecular sieve, a NU-87 molecular sieve and a beta zeolite molecular sieve; more preferably, the molecular sieve in the molecular sieve crystallization slurry is a mordenite molecular sieve.
Preferably, the conductivity of the material obtained after cleaning is less than 5 mS/cm; more preferably 3mS/cm or less.
By adopting the technical scheme, the cleaning equipment provided by the invention can fully mix the cleaning water and the material to be cleaned through the impeller, and transmit the mixed slurry of the cleaning water and the material to be cleaned, so that the metal cations enter the cleaning water, and the cleaning water (waste liquid) containing the metal cations is removed through the filtering unit, thereby reducing the conductivity of the material and greatly improving the cleaning effect.
Secondly, the dynamic regulation is carried out on the cleaning process by controlling the entering speed of cleaning water and materials, the discharging speed of waste liquid and materials, the rotating speed of an impeller, the pressure in a main body and the like, so that the cleaning is efficiently realized, and the using amount of the cleaning water is saved.
In addition, the cleaning equipment provided by the invention can be used for cleaning the molecular sieve crystallization slurry under a closed condition, so that leakage of harmful substances such as ammonia gas and the like is prevented, and adverse effects on operators and the environment are avoided.
Drawings
FIG. 1 is a schematic structural diagram of a molecular sieve crystallization slurry cleaning apparatus of the present invention;
FIG. 2 is a schematic view of a part of a filtering unit in the cleaning equipment for molecular sieve crystallized slurry of the present invention.
Description of the reference numerals
100: the main body 110: feed unit
120: the discharging unit 121: discharge valve
200: the washing water inlet unit 210: cleaning water inlet valve
300: waste liquid discharge unit 310: waste liquid discharge valve
500: the hybrid transmission unit 510: rotating shaft
520: the connecting member 530: impeller
600: the filtering unit 610: filter plate
620: chamber 630: filter medium
A: mixing the slurry B: waste liquid
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 present invention, it is to be understood that the terms "center, inside, outside, up, down" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or unit must have a specific orientation and a specific orientation configuration and operation, and thus, are not to be construed as limiting the present invention.
In the present invention, the use of the directional terms such as "upper and lower" in the case where no reverse explanation is made generally means that the apparatus for washing the crystallized slurry of molecular sieve is vertically up and down in the use state.
The first aspect of the present invention provides a molecular sieve crystallization slurry cleaning apparatus, as shown in fig. 1, the apparatus includes a main body 100, a feeding unit 110, a discharging unit 120, a cleaning water inlet unit 200, a waste liquid discharge unit 300, a mixing and conveying unit 500, and a filtering unit 600, wherein the feeding unit 110 and the discharging unit 120 are respectively disposed at two ends of the main body 100, and are respectively used for feeding and discharging materials; the washing water inlet unit 200 is disposed at an upper end of the main body 100, and is used to introduce washing water into the washing apparatus; the waste liquid discharge unit 300 is disposed at a lower end of the main body 100, and discharges waste liquid in the cleaning apparatus; the mixing and transferring unit 500 is provided inside the main body 100, and includes a rotating shaft 510 at the center, a coupling member 520 provided at a certain interval on the rotating shaft, and an impeller 530 coupled to the rotating shaft through the coupling member 520; the filtering unit 600 is disposed inside the main body 100, perpendicular to the rotating shaft 500, and the impeller 530 is alternately disposed, and includes a filtering plate 610, a chamber 620 disposed in the middle of the filtering plate, and a filtering medium 630 disposed on the surface of the filtering plate, the filtering plate 610 has a circular hole at the center thereof, the rotating shaft 510 is penetrated by the hole, an annular space is left between the hole and the rotating shaft 510, and one end of the chamber 620 is connected to the waste liquid discharging unit 300.
According to the present invention, the cleaning apparatus may further include a power unit (not shown) for supplying power to the feeding unit 110, which may be disposed outside the main body 100 and connected to the feeding unit 110, for allowing the material (i.e., the molecular sieve crystallized slurry) to enter the main body 100 under pressure, to be transported in the main body 100, and to perform cleaning.
The power unit may be selected from a variety of devices commonly used in the art for providing power, such as one or more of a diaphragm pump, a hydraulically powered pump, and a magnetically driven pump. Preferably, the power unit is selected from a diaphragm pump.
According to the present invention, the shape of the main body 100 of the apparatus is not particularly limited, and may be various conventional shapes satisfying the requirements of the cleaning apparatus of the present invention, and preferably, the main body 100 is cylindrical, whereby the utilization rate of the inner space of the apparatus may be improved, the arrangement of the mixing and transferring unit 500 and the filtering unit 600, etc. may be facilitated, and thus the cleaning effect may be improved.
In the invention, the feeding unit 110 for feeding the material into the main body 100 and the discharging unit 120 for discharging the material are respectively arranged at two ends of the main body, and the material is cleaned in the cleaning equipment in the process of passing through the main body 100, so that the metal cations in the molecular sieve crystallization slurry are removed.
In the present invention, the feeding unit 110 and the discharging unit 120 may be provided according to various configurations conventionally used for feeding and discharging in the art, without particular requirements. For example, valves and the like that can be opened and closed may be installed on the feeding unit 110 and the discharging unit 120, a metering unit such as a flow meter may be provided, and preferably, the discharging unit 120 includes a discharge valve 121 for controlling discharge of the material. By adjusting the opening degree of the discharge valve 121, the cleaning conditions can be changed. For example, under otherwise constant conditions, decreasing the opening of the discharge valve 121 increases the pressure in the main body 100, thereby increasing the flow rate of the discharged waste liquid, and the solids content of the material obtained after washing may be higher. Therefore, the opening degree of the discharge valve 121 can be flexibly adjusted according to actual cleaning requirements.
In the present invention, the upper end of the main body 100 is provided with a cleaning water inlet unit 200 for allowing cleaning water to enter a cleaning apparatus, and the cleaning water is mixed with the molecular sieve crystallization slurry after entering the apparatus, thereby realizing cleaning.
In the present invention, the number of the washing water inlet units 200 may be flexibly selected according to the length and volume of the main body 100, the washing requirements, and the like, and one or more washing water inlet units 200 may be provided at the upper end of the main body 100, but is not particularly limited. The washing water inlet unit 200 may include a washing water inlet valve 210 for controlling the inlet of washing water, and the amount of washing water entering the main body 100 may be controlled by adjusting the opening degree of the washing water inlet valve 210. Of course, it is a preferred embodiment of the present invention that the washing water inlet unit 200 is provided at the upper end of the main body 100, and it may be provided at other positions of the main body.
According to the present invention, after washing water is mixed with materials and washed, the materials are discharged out of the washing apparatus through the waste liquid discharge unit 300, and the waste liquid discharge unit 300 is disposed at the lower end of the main body 100, and one or more waste liquid discharge units may be disposed according to actual needs, without any particular limitation. The waste liquid discharge unit 300 may include a waste liquid discharge valve 310 for controlling the discharge of waste liquid, and the discharge amount of waste liquid may be controlled by adjusting the opening degree of the waste liquid discharge valve 310 during washing. Of course, it is a preferred embodiment of the present invention that the waste liquid discharge unit 300 is provided at the lower end of the main body 100, and it may be provided at another position of the main body.
Hereinafter, the mixing and transferring unit 500 and the filtering unit 600 will be described in detail with reference to fig. 1.
As shown in fig. 1, the mixing and transferring unit 500 is provided inside the main body 100, and includes a rotation shaft 510 at the center; a connection member 520 provided at a certain interval on the rotation shaft; and an impeller 530 connected to the rotation shaft by a connection member 520. In addition, the mixing and transferring unit 500 may further include a motor for supplying power to rotate the rotating shaft 510, thereby rotating the impeller 530.
In the present invention, the material fed from the feeding unit 100 is mixed with the washing water fed from the washing water feeding unit 200 by the rotation of the impeller 530, and the mixed slurry of the washing water and the material is also pushed to be transferred, so that the washing is smoothly performed.
In the present invention, the flow rate of the mixed slurry can be adjusted and the degree of filtration can be controlled by adjusting the rotation speed of the impeller 530.
According to the present invention, the filter unit 600 is also disposed inside the main body 100, perpendicular to the rotation shaft 500, and alternately disposed with the impeller 530, and includes: a filter plate 610; a chamber 620 located in the middle of the filter plate; and filter media 630 on the surface of the filter plate. Wherein, a circular hole is formed in the center of the filter plate 610, the rotation shaft 510 passes through the circular hole, and an annular space is left between the circular hole and the rotation shaft 510, so that the mixed slurry of the cleaning water and the material passes through, and one end of the chamber 620 is connected to the waste liquid discharge unit 300, for discharging the waste liquid out of the cleaning apparatus.
Fig. 2 is a partial schematic view of a filtering unit 600 in the molecular sieve crystallized slurry cleaning apparatus of the present invention. As shown in fig. 2, during the transportation of the mixed slurry a, the waste liquid B in the mixed slurry (the mixture of the molecular sieve crystallized slurry and the washing water) will pass through the filter medium 630 in the direction perpendicular to the filter plate 610 under the pressure, enter the chamber 620 and exit the washing apparatus through the waste liquid outlet 300, while the molecular sieve material cannot pass through the filter medium 630 due to its large particles and thus remains on the surface of the filter plate 610. Then, under the action of the pressure and the impeller 530, the material of the molecular sieve which fails to pass through the filter medium 630 gradually moves forward, passes through the subsequent filter unit 600 during the movement, is repeatedly cleaned and the waste liquid is removed, and is finally discharged from the discharging unit 120, thereby completing the cleaning.
In the present invention, the filter medium 630 may be any of various media commonly used in the art for filtration, and is not particularly limited, and for example, the filter medium may be selected from a filter mesh, and as the filter mesh, a metal filter mesh, a ceramic filter mesh, an alumina sintered filter mesh, and the like; preferably, the filter media 630 is selected from a metal filter mesh and/or a ceramic filter mesh.
According to the present invention, it is preferable that the filter units 600 and the impellers 530 are alternately arranged inside the main body 100. The number of the filter units 600 and the impellers 530 may be flexibly set according to the cleaning requirement, and preferably, the number of the filter units 600 and the impellers 530 is more than one. When the molecular sieve crystallization slurry is washed, more preferably, the number of the filter units 600 is 8 to 9, and the number of the impellers 530 is 9 to 10. The two are alternately arranged, so that an ideal cleaning effect can be achieved.
In the present invention, the main body 100, the rotary shaft 510, the connection member 520, the impeller 530, the filter unit 600, and the like may be made of corrosion-resistant materials, and may be made of, for example, stainless steel, without any particular limitation.
The second aspect of the present invention provides a method for cleaning molecular sieve crystallization slurry, the method is performed by using the cleaning apparatus provided by the first aspect of the present invention, and the method comprises: the material is mixed with the washing water introduced from the washing water introduction unit 200 by the mixing and transferring unit 500, and is filtered and washed through the filtering unit 600.
According to the present invention, after the material enters the main body 100 through the power unit from the feeding unit 110, the material is mixed with the washing water entering from the washing water entering unit 200 under the stirring action of the impeller 530 in the mixing and conveying unit 500, during the mixing process, the metal cations contained in the molecular sieve crystallized slurry enter the washing water, and under the pressure provided by the power unit, the mixed slurry of the washing water and the material is filtered through the filtering unit 600, so that the waste liquid containing the metal cations is removed. Thus, the mixed slurry is sequentially mixed with the washing water while being conveyed in the main body 100, and the cation is washed away by the filter unit, and finally the washed material is discharged from the discharging unit 120 to be washed.
According to the invention, the solid content of the mixed slurry in the washing machine can be changed by adjusting the entering speed of the washing water, and specifically, the larger the entering speed of the washing water is, the lower the solid content of the mixed slurry in the washing machine is, the better the washing effect is, but the more waste liquid is generated. Preferably, the entry rate of the washing water is 0.5 to 5m3H; more preferably, the washing water has an entry rate of 3 to 4m3/h。
According to the invention, the higher the material entering speed, the higher the cleaning efficiency, but the too high material entering speed can affect the cleaning effect. Preferably, the material has an entry rate of 1 to 10m3H; more preferably, the material has an entry rate of 2 to 3m3/h。
According to the present invention, the discharge rate of the waste liquid can be appropriately adjusted according to the amount of washing water actually generated in washing. Preferably, the discharge rate of the waste liquid is 1 to 7m3H; more preferably, the discharge rate of the waste liquid is 3 to 4m3/h。
According to the present invention, the discharging rate of the materials may be determined according to the entering rate of the materials and the entering rate of the washing water, and preferably, the discharging rate of the materials is 0.5 to 8m3H; more preferably, the discharge rate of the material is 2-3m3/h。
According to the present invention, the rotation speed of the impeller 530 is increased to form a turbulent flow in the mixed slurry in the main body 110, thereby reducing the adhesion of the material to the filter medium 630 and facilitating the discharge of the waste liquid. Therefore, it is preferable that the rotation speed of the impeller 530 is adjusted so that the mixed slurry forms a turbulent flow; more preferably, the rotation speed of the impeller 530 is 50-300 r/min; further preferably, the rotation speed of the impeller 530 is 150 and 200 r/min.
In the present invention, the power unit provides pressure to push the mixed slurry to be transported while the transported slurry is filtered on the filtering unit 600 to remove the waste liquid. Increasing the pressure within the body 100 may increase the solids content of the material discharged by the discharge unit. However, too high a pressure in the body 100 may cause the impeller to be dead, which may affect the operation. Preferably, the pressure inside the body 100 is 0.08-0.6 MPa; more preferably, the pressure inside the body 100 is 0.08-0.4MPa, and even more preferably, the pressure inside the body 100 is 0.08-0.1 MPa.
By the cleaning method of the molecular sieve crystallization slurry, the crystallized molecular sieve slurry can be cleaned to remove metal cations in the crystallized molecular sieve slurry and reduce the conductivity of the molecular sieve crystallization slurry.
In the present invention, the molecular sieve in the molecular sieve crystallization slurry can be various molecular sieves which need to be cleaned after crystallization in the field, for example, the molecular sieve can be one or more of mordenite molecular sieve, ZSM-5 molecular sieve, ZSM-12 molecular sieve, NU-87 molecular sieve and beta zeolite molecular sieve. Preferably, the molecular sieve in the molecular sieve crystallization slurry is a mordenite molecular sieve.
According to the invention, when the cleaning equipment disclosed by the invention is used for cleaning the molecular sieve crystallization slurry, the material can be repeatedly cleaned by the cleaning equipment according to the characteristics of the molecular sieve crystallization slurry and the effect required by cleaning.
In the present invention, after the washing, preferably, the conductivity of the material obtained after the washing is 5mS/cm or less; more preferably, the conductivity of the material obtained after washing is 3mS/cm or less.
The present invention will be described in detail below by way of examples, but the present invention is not limited to the following examples.
In the following examples and comparative examples, a mordenite molecular sieve crystallized slurry was used, having a solid content of 25 wt%; the original conductivity was 21 mS/cm.
In the following examples and comparative examples, the ammonia gas concentration at the outer periphery of the apparatus was measured at a position 1m from the outer periphery of the apparatus using an ammonia gas detector (PGM-2500D, Wash instruments).
In the following examples and comparative examples, the conductivity was measured by a conductivity meter.
Example 1
The method is carried out by adopting the equipment shown in FIG. 1, and the equipment comprises a main body 100, wherein one end of the main body 100 is provided with a feeding unit 110, and the other end is provided with a discharging unit 120; the upper end of the main body 100 is provided with a washing water inlet unit 200, the lower end is provided with a waste liquid discharge unit 300, and the inside of the main body 100 is provided with a mixing and transferring unit 500 and a filtering unit 600; the apparatus further includes a power unit coupled to the feed unit 110 for powering the feed unit 110, the power unit selected from a diaphragm pump.
The washing water inlet unit 200 includes washing water inlet valves 210, and the number of the washing water inlet valves is 7.
The waste liquid discharge unit 300 includes 9 waste liquid discharge valves 310.
The discharging unit 120 includes a discharge valve 121.
The hybrid transmission unit 500 includes: a rotation shaft 510 at the center; a connection member 520 provided at a certain interval on the rotation shaft; an impeller 530 connected to the rotation shaft by a connection member 520; and a motor to provide power.
The number of the impellers is 10.
The filter units 600 are perpendicular to the rotation shaft 500, are alternately arranged with the impellers 530, and include filter plates 610; a chamber 620 located in the middle of the filter plate; and filter media 630 on the surface of the filter plate. The filter plate 610 has a circular hole at the center thereof, the rotation shaft 510 passes through the circular hole, and an annular space is left between the circular hole and the rotation shaft 510, and one end of the chamber 620 is connected to the waste liquid discharge unit 300.
The filter medium is a metal filter screen, and the number of the filter units is 9.
The specific steps of cleaning are as follows:
1) opening the discharge valve 121, cleaning water inlet valve 210, and wasteA liquid discharge valve 310 and an impeller 530, and an inflow rate of washing water is 3.75m3/h,
2) The diaphragm pump is opened and the material is fed from the feed unit 110 at a rate of 2.25m3The rotating speed of the impeller is 200 r/min;
3) adjusting the discharge rate of waste liquid to 3.75m3H, material discharge rate of 2.25m3H; the pressure in the main body 100 was 0.09 MPa.
When the cleaning equipment is in normal operation, the concentration of ammonia gas on the periphery of the equipment fluctuates between 8 ppm and 9 ppm.
The discharge valve obtains a material with the conductivity of 3mS/cm after being cleaned, namely 4.5m3When the amount of the washing water used is 7.5m3
On average, 0.41m of washing water is required per conductivity reduction of 1mS/cm3
Comparative example 1
The material was cleaned with a belt filter (manufactured by Huzhou Juxing mechanical manufacturing Co., Ltd., model No. PBF25/1800-A) whose peripheral ammonia concentration fluctuated between 56-60ppm during normal operation.
The same volume (4.5 m) as in example 1 was obtained3) The total amount of washing water used is 15m for the washed material of the same conductivity (3mS/cm)3
On average, 0.83m of washing water is required per 1mS/cm of conductivity reduction3
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 (10)

1. A cleaning device for molecular sieve crystallization slurry is characterized by comprising a main body (100), a feeding unit (110), a discharging unit (120), a cleaning water inlet unit (200), a waste liquid discharge unit (300), a mixing and conveying unit (500) and a filtering unit (600),
the feeding unit (110) and the discharging unit (120) are respectively arranged at two ends of the main body (100) and are respectively used for feeding materials into and discharging the materials;
the washing water inlet unit (200) is disposed at an upper end of the main body (100) and is used for allowing washing water to enter the washing apparatus;
the waste liquid discharge unit (300) is arranged at the lower end of the main body (100) and is used for discharging waste liquid in the cleaning equipment;
the mixing and transferring unit (500) is provided inside the main body (100), and includes a rotating shaft (510) positioned at the center, a coupling member (520) provided at a certain interval on the rotating shaft, and an impeller (530) coupled to the rotating shaft through the coupling member (520);
the filter unit (600) is arranged inside the main body (100), is perpendicular to the rotating shaft (500) and is alternately arranged with the impeller (530), and comprises a filter plate (610), a chamber (620) positioned in the middle of the filter plate and a filter medium (630) positioned on the surface of the filter plate, wherein a round hole is arranged at the center of the filter plate (610), the rotating shaft (510) penetrates through the round hole, an annular gap is reserved between the round hole and the rotating shaft (510), and one end of the chamber (620) is connected with the waste liquid discharge unit (300).
2. The cleaning apparatus according to claim 1, wherein the cleaning apparatus further comprises a power unit for powering the feed unit (110) for conveying the material;
preferably, the power unit is selected from one or more of a diaphragm pump, a hydraulic power pump and a magnetic force driven pump.
3. The washing apparatus according to claim 1 or 2, wherein the impeller (530) is rotated by the rotating shaft (500) during which the material entered from the feed unit (100) is mixed with the washing water entered from the washing water entry unit (200) while the mixed slurry of the washing water and the material is pushed to be transferred.
4. The cleaning device according to any one of claims 1 to 3, wherein the number of the filter units (600) is more than one, preferably 8 to 9;
preferably, the number of the impellers (530) is more than one, and more preferably 9-10.
5. The washing apparatus according to any one of claims 1 to 3, wherein one or more washing water inlet units (200) are provided, the washing water inlet unit (200) includes a washing water inlet valve (210) for controlling an inlet of washing water, and an inlet amount of washing water is controlled by adjusting an opening degree of the washing water inlet valve (210);
preferably, one or more waste liquid discharge units (300) are provided, the waste liquid discharge unit (300) comprises a waste liquid discharge valve (310) for controlling the discharge of waste liquid, and the discharge amount of waste liquid is controlled by adjusting the opening degree of the waste liquid discharge valve (310);
preferably, the discharge unit (120) comprises a discharge valve (121) for controlling the discharge of material.
6. A cleaning device according to any one of claims 1-3, said filter medium (630) being selected from a filter mesh;
preferably, the filter medium (630) is selected from a metal filter mesh and/or a ceramic filter mesh.
7. A method for cleaning molecular sieve crystallization slurry, which is characterized by being carried out by using the cleaning equipment of any one of claims 1 to 6, and the method comprises the following steps: mixing the materials with the washing water from the washing water inlet unit (200) under the action of the mixing and conveying unit (500), and filtering and washing the materials through the filtering unit (600).
8. The washing method as claimed in claim 7, wherein the washing water is introduced at a rate of 0.5 to 5m3H; the material inlet speed is 1-10m3H; the discharge rate of the waste liquid is 1-7m3H; the discharge rate of the material is 0.5-8m3H; impeller(530) The rotating speed of (A) is 50-300 r/min; the pressure in the main body (100) is 0.08-0.6 MPa;
preferably, the entry rate of the washing water is 3 to 4m3/h;
Preferably, the material has an entry rate of 2 to 3m3/h;
Preferably, the discharge rate of the waste liquid is 3 to 4m3/h;
Preferably, the discharge rate of the material is 2-3m3/h;
Preferably, the rotating speed of the impeller is 150-;
preferably, the pressure inside the body (100) is between 0.08 and 0.4 MPa;
more preferably, the pressure inside the body (100) is between 0.08 and 0.1 MPa.
9. The cleaning method according to claim 7 or 8, wherein the molecular sieve in the molecular sieve crystallization slurry is one or more of mordenite molecular sieve, ZSM-5 molecular sieve, ZSM-12 molecular sieve, NU-87 molecular sieve and beta zeolite molecular sieve;
preferably, the molecular sieve in the molecular sieve crystallization slurry is a mordenite molecular sieve.
10. The method according to any one of claims 7 to 9, wherein the conductivity of the material obtained after washing is 5mS/cm or less; more preferably 3mS/cm or less.
CN202011171833.6A 2020-10-28 2020-10-28 Molecular sieve crystallization slurry cleaning equipment and cleaning method Pending CN114477218A (en)

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CN202011171833.6A CN114477218A (en) 2020-10-28 2020-10-28 Molecular sieve crystallization slurry cleaning equipment and cleaning method

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CN114477218A true CN114477218A (en) 2022-05-13

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2609632Y (en) * 2002-10-28 2004-04-07 长沙高新技术产业开发区开通科技有限公司 Cross flow rotation blade dynamic pressure filter
CN101518749A (en) * 2009-03-05 2009-09-02 华东理工大学 Ion exchange process for multistage reverse flow zeolite molecular sieve of band filter
WO2013086767A1 (en) * 2011-12-15 2013-06-20 中国石油天然气股份有限公司 Heavy oil catalytic cracking catalyst and preparation method therefor
CN103723742A (en) * 2013-12-31 2014-04-16 中国天辰工程有限公司 Post-treatment method for washing, drying and calcining SAPO (silicoaluminophosphate) molecular sieve
CN103785438A (en) * 2012-10-26 2014-05-14 中国石油化工股份有限公司 Catalytic cracking catalyst production apparatus
CN105214381A (en) * 2015-10-14 2016-01-06 中国石油化工股份有限公司 The separating and filtering method of SAPO Crystallization of Zeolite slurry

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2609632Y (en) * 2002-10-28 2004-04-07 长沙高新技术产业开发区开通科技有限公司 Cross flow rotation blade dynamic pressure filter
CN101518749A (en) * 2009-03-05 2009-09-02 华东理工大学 Ion exchange process for multistage reverse flow zeolite molecular sieve of band filter
WO2013086767A1 (en) * 2011-12-15 2013-06-20 中国石油天然气股份有限公司 Heavy oil catalytic cracking catalyst and preparation method therefor
CN103785438A (en) * 2012-10-26 2014-05-14 中国石油化工股份有限公司 Catalytic cracking catalyst production apparatus
CN103723742A (en) * 2013-12-31 2014-04-16 中国天辰工程有限公司 Post-treatment method for washing, drying and calcining SAPO (silicoaluminophosphate) molecular sieve
CN105214381A (en) * 2015-10-14 2016-01-06 中国石油化工股份有限公司 The separating and filtering method of SAPO Crystallization of Zeolite slurry

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