CN112299432A - Molecular sieve production device - Google Patents

Molecular sieve production device Download PDF

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Publication number
CN112299432A
CN112299432A CN202011117744.3A CN202011117744A CN112299432A CN 112299432 A CN112299432 A CN 112299432A CN 202011117744 A CN202011117744 A CN 202011117744A CN 112299432 A CN112299432 A CN 112299432A
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kneader
molecular sieve
telescopic
shell
scraper
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CN112299432B (en
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胡佳怡
冯伟豪
陈玲
叶伟强
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Meier China Environmental Technology Co ltd
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Meier China Environmental Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B37/00Compounds having molecular sieve properties but not having base-exchange properties
    • 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

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  • Organic Chemistry (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • General Life Sciences & Earth Sciences (AREA)
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  • Materials Engineering (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

The invention discloses a molecular sieve production device which comprises a raw material storage tank, a screening instrument, a buffer tank, a mixing tank, a kneading machine, an extruder, a hot cutting box, an oven, a finished product tank, a detection device, a control system and corresponding connecting pipelines. The device has the advantages of high automation degree, simple operation, safety and controllability, diversified molding types, automatic generation of detection reports, realization of high-precision comprehensive central control and suitability for automatic large-scale production of molded molecular sieves. The raw materials are put into a raw material storage tank, uniformly refined powder is obtained through a screening instrument, a buffer tank and a mixing tank, the uniformly refined powder is uniformly mixed with liquid materials in a kneading machine and is extruded and molded, the molded molecular sieve with set micro-morphology, functions and appearance is obtained through hot cutting and hot drying and shearing in a hot cutting box and is sintered in an oven, and the molecular sieve prepared by the device has the advantages of regular shape, high strength, excellent and stable adsorption performance.

Description

Molecular sieve production device
Technical Field
The invention relates to a molecular sieve production device, which is suitable for the engineering forming preparation of porous materials and belongs to the technical field of material forming.
Background
The molecular sieve is a new adsorbent developed in the seventies of the last century and is a synthetic adsorbent with sieveSelecting molecular hydrated aluminosilicate or natural zeolite. The chemical general formula is (M' 2M) O.Al2O3·xSiO2·yH2O, M', M are respectively monovalent and divalent cations such as K+、Na+And Ca2+、Ba2+And the like. The molecular sieve has uniform pore passages and regular holes, and consists of molecular sieves with different pore diameters according to different Si/Al ratios. The types of the medicine are as follows: 3A (potassium A type), 4A (sodium A type), 5A (calcium A type), 10Z (calcium Z type), 13Z (sodium Z type), Y (sodium Y type), sodium mordenite type, etc. The molecular sieve has a special microporous structure and a nanometer space, shows high thermal stability, selective adsorption and enrichment functions and extremely high reaction activity, is widely used in organic chemical industry and petrochemical industry, and is increasingly emphasized in the fields of industrial nitrogen production and hydrogen production, sewage treatment, coal gas dehydration, organic waste gas purification and the like.
However, the existing molecular sieve production device has the problems of dependence on skilled labor, time and labor consumption of labor, uneven product size, high unreliable degree, unstable product performance, high rejection rate caused by untimely detection and the like. In the current production and preparation process of the molecular sieve, due to the real-time change of the viscosity of the material, the sticky and dry parts are easy to cause material jamming to cause the motor failure of the kneader, and further cause the shutdown error; in addition, the extrusion device is mostly of a double-screw complex structure, discharging in the production device is difficult, operators are required to use tools to transfer the molecular sieve, the production process is extremely unsafe, and accidents such as coiling into a kneader are easy to happen. The residual tank body of the high-viscosity molecular sieve slurry is easy to generate stubborn scales, the follow-up material proportion is influenced, the equipment is promoted to be corroded and aged, each batch of production needs manual cleaning, and the mass production time is occupied.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a molecular sieve production device which has the advantages of high automation degree, simple operation, diversified molding types, capability of automatically generating a detection report, regular shape, high strength and excellent and stable adsorption performance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the molecular sieve production device is characterized by comprising a raw material storage tank 100, a screening instrument 200, a buffer tank 300, a mixing tank 400 and a kneader 500 which are sequentially connected through a pump-containing pipeline, wherein one side, far away from the pump-containing pipeline, of the kneader 500 is connected to the inlet of an extruder 600 through a pipeline 1600, the outlet of the extruder 600 is connected with a hot cutting box 700, the hot cutting box 700 is connected with one end of an oven 800 through a bottom vertical pipe 1700, and the other end of the oven 800 is connected with a finished product tank 900;
the production device and the inspection device 1000 are electrically connected to a control system 1100, and the control system 1100 is capable of generating an inspection report, transmitting a report, and archiving the same.
Further, openings 504 are provided at both ends of the kneader 500, and the kneader can be connected in series or in parallel with another kneader 500, the openings 504 of the disconnected apparatuses are sealed by sealing rings, and the specifications of the kneaders 500 can be the same or different.
Further, the kneader 500 comprises a base 501, a kneading rod 517, a scraper 508, a sampler 511, a kneader shell 514 and a plurality of telescopic rods electrically connected with a control system, wherein the kneader shell 514 is connected to a side column of the base 501 through a bearing 515, a base side rod is arranged outside one end of the side column of the base 501, and the scraper 508 and the sampler 511 are fixed on the base side rod through the telescopic rods.
The outer side of the bearing 515 is connected with a driver, the inner side of the bearing is connected into the inner cavity of the kneading machine shell 514 and is connected with a kneading rod 517, and the upper plane of the kneading machine shell 514 is provided with a feeding hole 509, a water inlet 510 and an alarm 513 electrically connected with a control system 1100.
Furthermore, a heating wire 516 is arranged in the kneading rod 517, and the heating wire 516 is connected with a thermocouple through the ring groove snap 503 on the kneading machine shell 514, so as to realize real-time data transmission and temperature control.
Further, the telescopic rods comprise a first telescopic rod 507 and a second telescopic rod 506, one end of the first telescopic rod 507, which is far away from the side rod of the base, is fixed with a scraper 508, the scraper 508 is vertically placed close to the upper surface of the kneading machine shell 514, and one end of the second telescopic rod 506, which is far away from the side rod of the base, is connected with the sampler 511;
be provided with between base 501 and the second telescopic link 506 and be no less than 2 telescopic links, stretch into kneading machine casing 514 inside, its one end of keeping away from the base side lever is C type or I shape, can fixed scraper blade 508.
Further, the kneader shell 514 is a heat-insulating interlayer or a heat-insulating material, the outer interlayer of the heat-insulating interlayer of the kneader shell 514 is provided with a graphite heating layer, the graphite heating layer radiates heat to the inner cavity of the kneader shell 514, and the outer side of the graphite heating layer is provided with a cooling jacket or a fan for cooling the inner cavity of the kneader shell 514.
Furthermore, the sampling port of the sampler 511 is provided with one or more than one sampling ports, and can be contracted and expanded in multiple stages, and can rotate to sample at the contraction node, and the sampler 511 is made of stainless steel, hastelloy, cyanate resin polymer, carbon fiber or carbon nanotube.
Further, the scraper 508 includes an upper block surface 5085, a hollow column 5083, a central shaft 5081 and a plurality of telescopic blades; the telescopic blade comprises a first telescopic blade 5082, a second telescopic blade 5084 and a third telescopic blade 5086;
the upper end of the upper blocking surface 5085 is provided with an open hole area, two ends of the open hole area are provided with hollow columns 5083, and one end of each hollow column 5083, which is far away from the upper blocking surface, is connected with a first telescopic blade 5082 which stands oppositely; a central shaft 5081 is arranged below the upper blocking surface 5085, and second telescopic blades 5084 are respectively arranged on two sides of the central shaft 5081. The opposite surface of the telescopic blade 5084 is a third telescopic blade 5086 fixed on the side edge of the scraper 508; the scraper 508 is connected with the control system 1100, and can sense the positions of the kneading rod 517 and the sprayer 512 and adjust the stretching length and the speed.
Further, the hot cutting box 700 comprises a housing 703, a central shaft 702, an infrared lamp 707, a diaphragm 708, a sprayer 706, a motor 705, a discharge port 701 and a plurality of blades 709;
the top end of the central shaft 702 is connected with a motor 705 and is arranged outside a shell 703, the shaft body of the central shaft 702 is connected with a plurality of blades 709, the inner side of the upper part of the shell 703 is provided with a sprayer 706, the side surface of the shell 703 is provided with a side opening 704 and is sequentially connected with an infrared lamp 707 and a diaphragm 708, the bottom of the shell 703 is provided with a discharge hole 701, and a liquid outlet 710 is arranged beside the discharge hole 701;
wherein the infrared lamp 707 can be replaced by an ultraviolet lamp or a microwave source.
Further, the inner surface of the kneader shell 514 is also provided with a sprayer 512, the flow rate of the sprayer 512 is adjustable, the size of the sprayed liquid drops is adjustable, the rotating angle is a hemispherical surface in the cavity, and the sprayer can be switched to be connected with the feed inlet 509 or the water inlet 510 at will, so that the switching between feeding and self-cleaning is realized.
Compared with the prior art, the invention has the following beneficial effects:
1. by utilizing the molecular sieve production method provided by the invention, the obtained molecular sieve has the advantages of high strength, excellent adsorption performance, stable batch-to-batch, regular shape and diversified molding types.
2. The molecular sieve production device provided by the invention has the advantages of high automation degree, simplicity and easiness in operation, safety and controllability, high-precision comprehensive central control, no dependence on skilled and special skills and suitability for automatic large-scale production of the formed molecular sieve.
3. The detection device greatly facilitates real-time monitoring and adjustment, improves product stability, saves manpower and material resources, can automatically generate and file a detection report when being integrated into the control system, and is convenient and accurate in system calling.
4. Be provided with the spray thrower in the kneading machine, can cleaning equipment, extension equipment life reduces artifical work and reduces the potential safety hazard.
Drawings
FIG. 1 is a schematic structural diagram of a molecular sieve production apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic view of the structure of a kneader according to an embodiment of the present invention;
FIG. 3 is a schematic view of a squeegee configuration according to an embodiment of the invention;
FIG. 4 is a schematic structural diagram of a hot cutting box according to an embodiment of the present invention;
in the figure: 100. a raw material storage tank; 101. a weighing module; 200. a screening instrument; 201. a telescopic rod; 300. a buffer tank; 301. a weighing module; 400. a mixing tank; 401. a weighing module; 500. a kneader; 501. a base; 502. a fourth telescopic rod; 503. the ring groove is buckled; 504. an opening; 505. a third telescopic rod; 506. a second telescopic rod; 507. a first telescopic rod; 508. a squeegee; 5081. a central shaft; 5082. a first retractable blade; 5083. a hollow column; 5084. a second retractable blade; 5085. an upper blocking surface; 5086. a third retractable blade; 509. a feed inlet; 510. a water inlet; 511. a sampler; 512. a sprayer; 513. an alarm; 514. a kneader shell; 515. a bearing; 516. heating wires; 517. a kneading bar; 600. an extruder; 601. a top cap; 602. a screw; 700. hot cutting the box; 701. a discharge port; 702. a central shaft; 703. a housing; 704. opening the side; 705. a motor; 706. a sprayer; 707. an infrared lamp; 708. a diaphragm; 709. a blade; 710. a liquid outlet; 800. an oven; 801. slope combination; 900. a finished product tank; 901. a weighing module; 1000. a detection device; 1100. a control system; 1200. a pump-containing conduit; 1300. a pump-containing conduit; 1400. a pump-containing conduit; 1500. a pump-containing conduit; 1600. a pipeline; 1700. a vertical tube.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
Example 1
As shown in fig. 1, a schematic structural diagram of a molecular sieve production apparatus provided in an embodiment of the present invention includes a raw material storage tank 100, a sieving instrument 200, a buffer tank 300, a mixing tank 400, a kneader 500, an extruder 600, a hot-cutting box 700, an oven 800, a finished product tank 900, a detection apparatus 1000, a control system 1100, and corresponding connection pipelines and circuits.
The bottom surface of the 100 tanks of the raw material storage tank transmits materials to the screening instrument 200 through the pump-containing pipeline 1200, one side of the upper end of the screen of the screening instrument 200 is connected with a telescopic rod, and the telescopic rod can be used for opening, repairing and maintaining the cover. The lower end of the screen of the sieving instrument 200 transmits the sieved materials to the buffer tank 300 through the pipeline 1300 containing the pump. One end of the buffer tank 300, which is far away from the pump-containing pipeline 1300, is connected with the mixing tank 400 through the pump-containing pipeline 1400, and the bottom of the mixing tank 400 transmits the materials to the kneader 500 through the pump-containing pipeline 1500. The side of the kneader 500 remote from the pump-containing pipe 1500 is connected to a section of pipe 1600, and the side of the pipe 1600 remote from the kneader 500 is connected to an extruder 600. The end of extruder 600 remote from conduit 1600 extends into hot box 700. The bottom of the hot-cutting box 700 is provided with a vertical pipe 1700, one end of the vertical pipe 1700, which is far away from the hot-cutting box 700, is provided with an opening, the materials are shaken off on the slope combination 801 at the inlet of the oven 800, and the materials slide to the caterpillar track through the smooth slope combination 801 and are transmitted to the finished product tank 900.
The raw material storage tank 100, the sieving instrument 200, the buffer tank 300, the mixing tank 400, the kneading machine 500, the hot-cutting box 700, the oven 800 and the finished product tank 900 are provided with sampling ports, and are transmitted to the detection device 1000 through a collection pipeline for inspection, and the detection device 1000 feeds back detection data to the control system 1100 through electric connection. The raw material storage tank 100, the sieving instrument 200, the buffer tank 300, the mixing tank 400, the kneader 500, the extruder 600, the hot cutting box 700, the oven 800 and the finished product tank 900 are provided with sensors, and are integrated into the control system 1100 through electrical connection. The molecular sieve automation device is connected with a ground wire.
The bottom of the supporting foot of the raw material storage tank 100 is provided with a weighing module 101, the bottom of the buffer tank 300 is provided with a weighing module 301, the bottom of the supporting foot of the mixing tank 400 is provided with a weighing module 401, and the bottom of the supporting foot of the finished product tank 900 is provided with a weighing module 901.
The raw material storage tank 100 may be opened and may also be uncovered for maintenance and service by means of a telescopic rod 201, which may be hydraulically or pneumatically controlled.
The sizer 200 may be stacked with one or more layers of mesh for fine sizing. The screen frame connected with the supporting rod can be the uppermost layer, and can also be a middle layer or a plurality of layers which are respectively connected. The layer connecting the pump-containing pipeline 1300 and the sieving instrument 200 can be an upper material layer, a middle material layer or a bottom material layer.
The end of the buffer vessel 300 remote from the sifter device 200 may be connected directly to the buffer vessel 300 via a pump-containing line 1300 or may merge with one or more buffer vessels into the mixing tank 400.
The mixing tank 400 may have 1 or more layers of blades, each layer of blades may have 2 to 20 blades, each layer of blades may have an equal inclination angle, and the inclination angle may be 10 to 80 °, and preferably 30 to 60 °. The blades of different layers can be at the same or different inclination angles, and preferably, the upper layer is 30-50 degrees, and the lower layer is 40-60 degrees, and more preferably 45-50 degrees. The mixing tank 400 can be provided with an anchor type paddle for scraping off the materials with high humidity or viscosity and playing the effect of mixing the materials at the bottom into the materials at the middle upper part and mixing the materials uniformly. The blades are made of antistatic materials and lead static out through the conductive central shaft.
The kneader 500 is left open at both ends, and one end near the mixing tank 400 may be connected to one or more mixing tanks through a pipe 1500 including a pump, or may be connected to one or more kneaders through a pipe. The opening of the kneader 500 near the end of the extruder 600 may be connected to one or more extruders via a line 1600, or may be integrated into one extruder with one or more kneaders. The opening of the kneader 500 is sealed with a high-strength gasket when not connected to other devices.
Conduit 1600 may be a bent or straight conduit to which an auxiliary heating or cooling device may be added.
The screw 602 of the extruder 600 can be a single screw or a double screw, the screw thread pitch can be 0.5-5 cm, and the screw thread pitch can be adjusted according to the viscosity of the material. The top cap 601 of the extruder 600 may have 1 or more openings, preferably 3-10 holes, and the openings may be circular holes or square holes or parallelogram holes, and the center of the holes may be a partial solid body or a full hollow body. Preferably, the opening of the top cap 601 is 3-6 medium solid holes arranged at the hexagonal vertex angle position, and can also be honeycomb holes with the interval of 0.5-1 mm and the aperture of 0.5-1.5 mm. The shell layer of the extruder 600 can be used as a jacket type auxiliary heating or cooling device, and a drip irrigation device can be arranged, so that the material viscosity is suitable and the extrusion is easy.
One end of the hot cutting box 700 is open, into which the extruder 600 extends, and one or more openings for placing into the discharge end of the extruder may be provided, which extend in one or more directions or angles.
The oven 800 may be tunnel, ring, parallel-row split-flow, batch box, etc., and the oven heat source may be blast, infrared, microwave, etc. Preferably, an infrared tunnel oven is used. The oven 800 can be provided with rollers for moving, and can also be provided with fixed support legs for accurate material collection. The number of the ovens 800 for receiving the materials thrown out by the heat cutting machine 700 can be one or more, and one or more ovens are matched with one or more types of ovens for heat treatment.
The finished product tank 900 may be open or closed, may be provided with one or more than one oven, and may be connected to an automatic packaging apparatus.
As shown in FIG. 2, which is a schematic view of the structure of the kneader in the embodiment of the present invention, the kneader 500 supports the respective components by a base 501. A kneader housing 514 is supported and fixed on the base 501. The two sides of the shell are connected with the side columns extending out of the two sides of the base 501 through bearings 515, the outer sides of the bearings 515 are connected with drivers, the inner sides of the drivers are connected into the inner cavity of the kneader and connected with an S-shaped kneading rod 517. The kneading rod 517 is internally provided with a heating wire 516, the heating wire 516 is respectively matched with the ring groove elastic buckles 503 at the positions of the kneading machine shells at the two sides, and the heating wire is electrically connected through the ring groove elastic buckles 503 in the rotating process along with the kneading rod. One end of the ring groove elastic buckle 503, which is far away from the heating wire, is respectively connected with the thermocouple, so that data transmission and temperature control are realized. The kneader body 514 is provided with openings 504 near both ends of the ring groove snaps 503, and the openings can be connected with a kneader or a buffer tank or an extruder. The upper plane of the kneading machine shell 514 is provided with an alarm 513, a feed inlet 509 and a water inlet 510, and the inner surface of the upper plane cavity is provided with a sprayer 512. The alarm 513 is electrically connected to the control system 1100. The feed port 509 is connected to a pump-containing conduit 1500. The water inlet 510 is connected to a water tank or a tap water pipe. The sprayer 512 is connected to the feed port 509 and the water inlet 510, and can be switched arbitrarily. A fourth telescopic rod 502, a third telescopic rod 505, a second telescopic rod 506 and a first telescopic rod 507 are arranged on the side rods of the base 501, one end of the first telescopic rod 507 far away from the side rods of the base is fixed with the upper end of a scraper 508, and the scraper 508 is tightly attached to the upper surface of the kneading machine shell 514 and is vertically placed. The end of the second telescoping rod 506 away from the side bar is connected to the sampler 511. The fourth expansion link 502 and the third expansion link 505 are far from the side bar, and extend into the kneader housing 514, and the top thereof is C-shaped or i-shaped for fixing the scraper 508 transmitted by the first expansion link 507.
The kneading machine shell can be provided with a graphite heating layer, and the heat is quickly and safely radiated to the inner cavity by utilizing the high heat transfer coefficient characteristic of the graphite. The outside of the graphite heating layer can be provided with a cooling jacket, the inner cavity can be rapidly cooled through the graphite layer with high heat conductivity, and a fan cooling inner cavity can also be arranged.
The heating wire 516 may be made of metal, graphite, or nano material.
The sprayer 512 can spray liquid materials such as silica sol, water, nitric acid, or high pressure water or alkali solution to clean the inner cavity. The flow rate is adjustable, the size of the sprayed liquid drops is adjustable, the rotating angle is a hemispherical surface in the cavity, and the liquid drops can be randomly switched to be connected with the feeding port 509 or the water inlet 510, so that the switching between feeding and self-cleaning is realized.
The fourth telescopic rod 502, the third telescopic rod 505, the second telescopic rod 506 and the first telescopic rod 507 may be hydraulically or pneumatically arranged.
The first telescopic rod 507 can move in the vertical and horizontal directions, and the scraper 508 is fed into the inner cavity of the kneader or taken out after being accurately positioned. The upper surfaces of the scraper 508 and the kneader shell 514 are provided with narrow openings, so that the scraper can pass through smoothly, the narrow openings are closed when the scraper is taken out of the containing cavity, and the narrow openings can be controlled to open and close pneumatically. The top ends of the fourth telescopic rod 502 and the third telescopic rod 505 can move in the horizontal direction parallel to the kneading rod, receive and fix the scraper 508 transferred by the telescopic rod 507, and horizontally push the scraper 508 to move towards the opposite side in the cavity. Further, the scraper 508 can move back and forth at an adjustable speed, which can be 5-1500 cm/min or 20-1300 cm/min, preferably 800 and 1000 cm/min, and the scraper 508 can be horizontally fed into the cavity outside the housing 514.
The sampler 511 can be made of stainless steel, hastelloy, cyanate resin, etc., carbon fiber, carbon nanotube material, and has 1 or more sampling ports, which can be contracted and expanded in multiple stages, and can rotate at the contraction node for omnibearing sampling.
The alarm 513 may be an audible, visual or combination alarm.
As shown in fig. 3, which is a schematic view of the scraper structure in the embodiment of the present invention, the upper blocking surface 5085 of the scraper 508 is reserved with a middle upper end opening region for passing through the shower 512, and the middle upper end opening region is respectively provided with a hollow column 5083 connecting the two side blocking surfaces, and one end of the hollow column far from the blocking surfaces is respectively connected with the first telescopic blades 5082 which are opposite and vertical. A central shaft 5081 is provided at the center below the upper retaining surface 5085, and second retractable blades 5084 are provided at both sides of the central shaft 5081. The second telescoping blade 5084 is opposite a third telescoping blade 5086 secured to the side of the squeegee 508. The first retractable blade 5082, the second retractable blade 5084 and the third retractable blade 5086 are respectively controlled by the control system 1100 to extend and retract in length and speed, and sensors are provided to automatically sense the position of the kneading bar 517, avoid collision and push out the material in all directions.
Referring to fig. 4, which is a schematic structural view of the hot-cutting box in the embodiment of the present invention, a rotatable central shaft 702 is disposed near the center of the hot-cutting box 700, an upper end of the central shaft 702 is connected to a motor 705, and a blade 709 is attached to a middle and lower edge of the central shaft. The blades 709 may be of sickle, triangular, semi-circular or diamond design, arranged in 1 layer or more, each layer may be one or more.
The housing 703 of the hot-cutting box 700 is provided with a side opening 704 near the end of the extruder 600, which is closed against the inner wall by a corrosion-resistant sealing ring. An infrared lamp 707 is fixed at one end of the housing 703 far away from the extruder 600. A transparent membrane 708 is fixed between the infrared lamp 707 and the central shaft 702 for protecting the infrared lamp 707. The inner wall of the upper surface of the housing 703 near the transparent membrane 708 is provided with a sprayer 706 which can be used for cleaning fluids such as water, alkali, acid, etc. During the cleaning process, the discharge port 701 and the liquid outlet 710 are closed, and the liquid outlet 710 is intermittently opened to discharge waste liquid. And closing the discharge hole 710 and opening the discharge hole 701 after the cleaning is finished.
The discharge port 701 and the discharge port 710 may be controlled by a solenoid valve.
Wherein the infrared lamp 707 may be replaced by an ultraviolet lamp or a microwave source.
The transparent diaphragm 708 can penetrate one or more of infrared ray, ultraviolet ray and microwave, and is made of high-toughness and high-strength material with light transmittance of more than 95%.
Each device and pipeline sets process flow and parameters through the control system 1100, sends signals and coordinates operation. Wherein the raw material storage tank 100 controls the material quality; the screening instrument 200 controls the start and stop of the telescopic rod and the material quality; the buffer tank 300 controls the quality of the material; the mixing tank 400 controls the mixing ratio and the quality; the kneader 500 controls the position and the moving speed of the scraper, the rotating speed, the direction and the temperature of the kneading rod, the temperature in the cavity, the liquid material sprayed by the sprayer and the flow rate, the start and stop of the alarm, the opening and closing of the feed inlet and the water inlet, the position and the sampling quantity of the sampling point; the extruder 600 controls extrusion speed, pressure, temperature; the hot cutting box 700 controls the cutting angular speed, the box body temperature and the cleaning process; the oven 800 controls the temperature and the transmission speed of the oven body; the product tank 900 controls material quality.
Each device can sample as required and send to the detection system 1000 for detection and feedback of the result. The detection system 1000 of the invention comprises any one or more of a scanning electron microscope, a transmission electron microscope, an X-ray diffractometer, a laser particle analyzer, a specific surface tester, an intensity tester, a water content tester and a viscometer. The present automation device is not limited to the above control and detection contents.
Example 2
Based on the schematic structural diagram of a molecular sieve production device in example 1, this example provides a preparation method of a molecular sieve, which includes the following steps:
step 1): the powder raw material is put into a raw material storage tank and is transmitted to a screening instrument to screen out uniform powder with required granularity.
Step 2): and (3) collecting the uniform powder obtained in the step (1) in a buffer tank.
Step 3): and (3) conveying the powder collected in the step (2) to a mixing tank, and uniformly shearing at a high speed to obtain refined powder.
Step 4): and (3) uniformly mixing the refined powder obtained in the step (3) with liquid materials and the like in a kneading machine to obtain viscous materials.
Step 5): and (4) extruding and molding the viscous material obtained in the step (4) by an extruder.
Step 6): and (5) simultaneously drying and shearing the molding material obtained in the step (5) into a semi-dry product with a required shape.
Step 7): and (4) carrying out heat treatment on the semi-dry product obtained in the step (6) in an oven to obtain a finished product, and collecting the finished product in a finished product tank to finish the production of the molecular sieve with the regular shape.
In the preparation method, the powder collected in the step 2 can be one or a combination of at least two of a molecular sieve, an extrusion aid, a dispersant, a modifier and the like.
Wherein the molecular sieve can be one or more of beta-molecular sieve, TS-1, Y-type molecular sieve, mordenite, carbon molecular sieve, ZSM-5, ZSM-11, ZSM-34, Pd/Pt/Cu/Ag/Au modified molecular sieve, etc.
The extrusion aid can be one or more of plant powder, corn flour, sesbania powder, hide glue, rosin, ethylene-vinyl acetate copolymer, polyurethane, silicone, stearate, ethanol, ethylene glycol, propylene glycol, nitric acid, etc.
The dispersant can be one or the combination of at least two of arachidic acid, KH-560, acrylic acid-2-acrylamide-2-methylpropanesulfonic acid multipolymer, acrylic acid-acrylate-sulfonate terpolymer, polyepoxysuccinic acid (sodium), polyaspartic acid (sodium), sodium polyacrylate, sodium lignosulfonate, Tween-80, P-123, F-127, F-68, BYK-1900, OP-10, SDS, SDBS, NNO and the like.
The modifier can be AgNO3、Cu(NO3)2、TiO2Carbon nanotube, carbon fiber, carbon black, silver powder, graphite powder, activated carbon, and the like.
The high-speed shearing blade in the step 3 can be segmented, the rotating speed is selected from 100-. More preferably, the upper layer rotation speed is 1200-.
In the step 4, the liquid material can be one or more than one of diluent, dispersant and the like. Wherein the diluent is selected from water, methanol, ethanol, acetone, diethyl ether, tetrahydrofuran, hexane, ethyl acetate, benzene, cyclohexane, acetonitrile, isopropanol, etc. Wherein the dispersant can be polyethylene glycol, sodium carboxymethylcellulose, OP-10, NNO, etc.
In the step 4, the materials can sequentially pass through one or more kneading machines, one or more of more diluents, dispersing agents and the like can be added into the front-end kneading machine through a feed inlet and a liquid inlet, and the newly added feeding amount is reduced at the rear end. The front end kneading machine can increase the rotating speed, increase or reduce the temperature to promote the full mixing, and the rear end kneading machine properly reduces the rotating speed according to the material viscosity and the like, and increases the cavity temperature, so as to achieve the effect of concentrating the material to the best extrusion characteristic.
The kneader in the step 4 can be used for multi-point and multi-time detection until the indexes of the materials such as viscosity, granularity, morphology and the like reach a set range. The kneading bar rotation speed may be 5 to 150 rpm.
And 5, adjusting the temperature and the rotating speed of the extruder in real time along with the sampling detection result. During implementation, materials with low viscosity and overlarge water content can be wholly or locally heated to promote the diluent or the solvent to evaporate until indexes meet, and for an excessively viscous material feedback system, the excessively viscous material feedback system returns to the kneader to be reprocessed. The temperature is set at 2-200 deg.C, preferably 20-70 deg.C, and the rotation speed is 5-100 rpm, preferably 10-40 rpm.
The rotating speed of the blades of the hot cutting machine in the step 6 can be selected to be 6-600 rpm, preferably 60-180 rpm according to the material characteristics. The molecular sieve with low auxiliary material thermal stability can be selected by an infrared lamp, the molecular sieve containing the ultraviolet curing component can be selected by an ultraviolet lamp, and the molecular sieve containing poor conductivity and low water content can be dried by microwave.
Example 3
Based on the molecular sieve production device of the above example 1, a method for producing a Y-type molecular sieve is provided, which comprises the following steps:
step 1): 100 parts of Y-type molecular sieve, 8 parts of stearate, 2 parts of plant powder, F-1270.7 parts and Cu (NO)3)20.5 part of the powder is put into a raw material storage tank and respectively transmitted to a sieving instrument to sieve out uniform powder with required granularity.
Step 2): and collecting the uniform powder in a buffer tank.
Step 3): and shearing in a mixing tank at the rotating speed of 4000 rpm of blades to obtain refined powder.
Step 4): the refined powder is evenly mixed with 15 parts of methanol, 170 parts of ethanol and OP-102 parts in a kneader, the rotation speed of a kneading rod is 120 rpm, the mixture is kneaded for 1.5 h at room temperature to obtain thinner material, the temperature is raised to 75 ℃ by a second kneader, the rotation speed of the kneading rod is 55 rpm, and the kneading is carried out for 0.5 h.
Step 5): extruding the viscous material into 50 × 30 mm diamond-shaped unit honeycomb strips, controlling the temperature at 30 ℃ and rotating at 50 rpm.
Step 6): the honeycomb strips were maintained in an environment of 60 ℃ under infrared lamps and the blades rotated at 10 rpm.
Step 7): and (3) treating the semi-dry honeycomb for 1 h at 130 ℃ by using a crawler-type oven, treating for 3.6 h at 530 ℃, and putting into a finished product tank to finish the production of the Cu modified Y-shaped rhombic single-honeycomb molecular sieve.
Placing the obtained molecular sieve in a kettle-type adsorption tower, and allowing 17.5 ppm CO to flow through2 The mixed gas of = 87:13v.v has an initial efficiency of 91.5% for adsorbing CO and an adsorption rate of 0.41% at 70% of the service life.
Example 4
Based on the molecular sieve production device in the embodiment 1, the method for producing the carbon molecular sieve comprises the following steps:
step 1): 100 parts of carbon molecular sieve, 12 parts of porous carbon fiber, 5 parts of bamboo charcoal activated carbon, P-1231.5 parts and 0.75 part of SDS are put into a raw material storage tank, and powder is sieved out in a sieving instrument.
Step 2): and collecting the uniform powder in a buffer tank.
Step 3): and shearing at 2700 rpm of blades at the upper end and 3600 rpm of blades at the lower end in the mixing tank and 190 rpm of the anchor type to obtain the refined powder.
Step 4): and uniformly mixing the refined powder with 200 parts of ethyl acetate and 7 parts of polyethylene glycol in a kneader, and kneading at the rotating speed of a kneading rod of 165 rpm for 2 hours at room temperature to obtain a thinner material. Heating to 85 ℃ in a second kneader, kneading at the rotating speed of a kneading rod of 40 rpm for 0.6 h, adding 25 parts of photocurable slurry, kneading for 0.5 h, and feeding into an extruder.
Step 5): extruding the viscous material into a cylindrical continuous strip with the side length of 1 mm, the square hollow and the diameter of 2.5 mm, controlling the temperature to be 10 ℃ and rotating the speed to be 100 rpm.
Step 6): the hollow column strips were irradiated under an ultraviolet lamp and the blade was rotated at 26 rpm.
Step 7): treating the semi-dry honeycomb by a drawer type oven at 550 ℃ for 4 h, and putting the treated semi-dry honeycomb into a finished product tank to prepare the high-strength hollow strip carbon molecular sieve, wherein the BET is measured to be 1070 m2/g。
The resulting molecular sieve pairs contained 52.5 vt.% CH4Gas separation, CH4The volume fraction reaches 94.2 percent, the recovery rate is 93.6 percent, and the method is suitable for enriching CH from coal bed gas by PSA4
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A molecular sieve production device is characterized by comprising a raw material storage tank 100, a screening instrument 200, a buffer tank 300, a mixing tank 400 and a kneader 500 which are sequentially connected through a pump-containing pipeline, wherein one side, far away from the pump-containing pipeline, of the kneader 500 is connected to the inlet of an extruder 600 through a pipeline 1600, the outlet of the extruder 600 is connected with a hot cutting box 700, the hot cutting box 700 is connected with one end of an oven 800 through a bottom vertical pipe 1700, and the other end of the oven 800 is connected with a finished product tank 900;
the production device and the inspection device 1000 are electrically connected to a control system 1100, and the control system 1100 is capable of generating an inspection report, transmitting a report, and archiving the same.
2. The molecular sieve production device according to claim 1, wherein the kneader 500 is provided with openings 504 at both ends thereof, and can be connected in series or in parallel with another kneader 500, the openings 504 of the non-connected devices are sealed by sealing rings, and the sizes of the kneaders 500 are the same or different.
3. The molecular sieve production device according to claim 1, wherein the kneader 500 comprises a base 501, a kneading bar 517, a scraper 508, a sampler 511, a kneader shell 514 and a plurality of telescopic bars electrically connected with a control system, the kneader shell 514 is connected to the side column of the base 501 through a bearing 515, a base side rod is arranged outside one end of the side column of the base 501, and the scraper 508 and the sampler 511 are fixed on the base side rod through the telescopic bars;
the outer side of the bearing 515 is connected with a driver, the inner side of the bearing is connected into the inner cavity of the kneading machine shell 514 and is connected with a kneading rod 517, and the upper plane of the kneading machine shell 514 is provided with a feeding hole 509, a water inlet 510 and an alarm 513 electrically connected with a control system 1100.
4. The molecular sieve production device according to claim 3, wherein the kneading bar 517 is internally provided with a heating wire 516, and the heating wire 516 is connected with a thermocouple through the ring groove snap 503 on the kneader shell 514 for real-time data transmission and temperature control.
5. The molecular sieve production device of claim 3, wherein the telescopic rods comprise a first telescopic rod 507 and a second telescopic rod 506, one end of the first telescopic rod 507 away from the side rods of the base is fixed with a scraper 508, and the scraper 508 is vertically placed close to the upper surface of the kneader shell 514;
be provided with between base 501 and the second telescopic link 506 and be no less than 2 telescopic links, stretch into kneading machine casing 514 inside, its one end of keeping away from the base side lever is C type or I shape, can fixed scraper blade 508.
6. The molecular sieve production device according to claim 3, wherein the kneader housing 514 is a heat insulating sandwich or a heat insulating material, a graphite heating layer is disposed on an outer sandwich of the heat insulating sandwich of the kneader housing 514 to radiate heat to the inner cavity of the kneader housing 514, and a cooling jacket or a fan is disposed on an outer side of the graphite heating layer to cool the inner cavity of the kneader housing 514.
7. The molecular sieve production apparatus of claim 3, wherein the sampler 511 is provided with at least one sampling port, and is capable of multi-stage contraction and expansion, and is capable of rotating to sample at the contraction node, and the sampler 511 is made of stainless steel, hastelloy, cyanate resin polymer, carbon fiber or carbon nanotube.
8. The molecular sieve production device of claim 3, wherein the scraper 508 comprises an upper baffle surface 5085, a hollow column 5083, a central shaft 5081 and a plurality of telescopic blades; the telescopic blade comprises a first telescopic blade 5082, a second telescopic blade 5084 and a third telescopic blade 5086;
the upper end of the upper blocking surface 5085 is provided with an open hole area, two ends of the open hole area are provided with hollow columns 5083, and one end of each hollow column 5083, which is far away from the upper blocking surface, is connected with a first telescopic blade 5082 which stands oppositely; a central shaft 5081 is arranged below the upper blocking surface 5085, second telescopic blades 5084 are respectively arranged on two sides of the central shaft 5081, and the opposite surface of each telescopic blade 5084 is a third telescopic blade 5086 fixed on the side edge of the scraper 508; the scraper 508 is connected with the control system 1100, and can sense the positions of the kneading rod 517 and the sprayer 512 and adjust the stretching length and the speed.
9. The molecular sieve production apparatus of claim 1, wherein the hot-cutting box 700 comprises a housing 703, a central shaft 702, an infrared lamp 707, a diaphragm 708, a sprayer 706, a motor 705, a discharge port 701, and a plurality of blades 709;
the top end of the central shaft 702 is connected with a motor 705 and is arranged outside a shell 703, the shaft body of the central shaft 702 is connected with a plurality of blades 709, the inner side of the upper part of the shell 703 is provided with a sprayer 706, the side surface of the shell 703 is provided with a side opening 704 and is sequentially connected with an infrared lamp 707 and a diaphragm 708, the bottom of the shell 703 is provided with a discharge hole 701, and a liquid outlet 710 is arranged beside the discharge hole 701;
wherein the infrared lamp 707 can be replaced by an ultraviolet lamp or a microwave source.
10. The molecular sieve production device according to claim 3, wherein the inner surface of the kneader housing 514 is further provided with a sprayer 512, and the rotation angle of the sprayer 512 is a hemispherical surface in the kneader cavity, and can be switched to be connected with the feed port 509 or the water inlet 510, so that the switching between feeding and self-cleaning is realized.
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JP2006104028A (en) * 2004-10-07 2006-04-20 Ngk Insulators Ltd Method for manufacturing zeolite formed body
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JP2001048525A (en) * 1999-08-09 2001-02-20 Nobuko Hasuyama Method for producing zeolite and device for producing zeolite
JP2006104028A (en) * 2004-10-07 2006-04-20 Ngk Insulators Ltd Method for manufacturing zeolite formed body
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* Cited by examiner, † Cited by third party
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