CN219003093U - Reaction device for preparing coal gas slag-based zeolite adsorbent - Google Patents

Reaction device for preparing coal gas slag-based zeolite adsorbent Download PDF

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CN219003093U
CN219003093U CN202223328747.9U CN202223328747U CN219003093U CN 219003093 U CN219003093 U CN 219003093U CN 202223328747 U CN202223328747 U CN 202223328747U CN 219003093 U CN219003093 U CN 219003093U
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kettle body
ultrasonic vibration
zeolite adsorbent
preparing
heat conduction
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余方可
张蓓
朱碧湘
陈映宏
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The utility model provides a reaction device for preparing a coal gas slag-based zeolite adsorbent, and belongs to the technical field of recycling of coal gas slag. The device includes the support of the cauldron body and cauldron body bottom, and cauldron body top is equipped with the charge door, and the bottom is equipped with the bin outlet, can dismantle on the charge door and be connected with sealed lid, and the cauldron body outside sets up the heat conduction and presss from both sides the cover, and the heat conduction presss from both sides the cover lateral wall and is equipped with conduction oil entry, conduction oil export, and the conduction oil export is located conduction oil entry top, and the internal lateral wall of cauldron sets up the inside lining, is equipped with mechanical stirring mechanism, ultrasonic vibration stick in the cauldron, and ultrasonic vibration stick upper portion is fixed in cauldron body roof, and the ultrasonic vibration stick lower extreme stretches into the internal middle lower part of cauldron. The reaction device adopts an ultrasonic wave assisted hydrothermal method to treat the coal gas slag to synthesize zeolite, and the zeolite has uniform crystallization nucleation and high crystallinity; the materials can be fully and uniformly mixed, and the time of hydrothermal polymerization reaction is shortened; the kettle body is provided with a polytetrafluoroethylene lining, so that the durability of the kettle body is improved.

Description

Reaction device for preparing coal gas slag-based zeolite adsorbent
Technical Field
The utility model belongs to the technical field of recycling of coal gas slag, and particularly relates to a reaction device for preparing a coal gas slag-based zeolite adsorbent.
Background
At present, the gas slag has the advantages of high yield, low utilization rate, high treatment cost and environmental threat, and the piling and landfill are still the main disposal modes of the gas slag. How to effectively utilize the carbon residue in the gas slag and the richer resources such as ferro-silico-aluminum. The gas-stripping slag comprises fine slag and coarse slag. The prior study finds that the coal gasification coarse slag is granular or sheet-shaped, has smooth surface, and part of slag sample is thoroughly melted and agglomerated into spheres; the fine slag is in a floc shape, the surface of the fine slag is similar to a honeycomb shape, and the fine slag is more developed than the coarse slag in a pore structure and is more suitable for being used as an adsorption material. Therefore, the pore structure of the gas slag also provides an important basis for the fields of the adsorbent, the catalyst carrier and the like.
The coal gasification fine slag can be used as a raw material for synthesizing zeolite molecular sieve, which is an important high-value utilization way of the coal gasification fine slag. The hydrothermal method is one of the methods for preparing zeolite by utilizing coal gasification fine slag, the coal gasification fine slag and sodium hydroxide are added into a hydrothermal reaction kettle according to a certain solid-to-liquid ratio, and the hydrothermal reaction is carried out under a certain temperature and stirring condition after the sealing, and the zeolite is obtained after ageing, filtering, washing and drying.
CN213050517U provides a hydrothermal reaction kettle, and this reation kettle adopts the lift mode to open the cauldron body upper cover, avoids staff direct contact cauldron body upper cover to the problem of being scalded. The reaction kettle can be used for preparing the gas slag-based zeolite adsorbent, but has the defects of low efficiency of mixed materials, overlong hydrothermal reaction time and poor uniformity of zeolite crystallization nucleation if a stirring mechanism is lacked.
Disclosure of Invention
The utility model aims to solve the technical problems of overcoming the defects in the prior art and providing a reaction device for preparing a coal gas slag-based zeolite adsorbent, which can shorten the time of hydrothermal reaction and improve the crystallinity of zeolite.
In order to achieve the aim, the technical scheme adopted by the utility model is that the reaction device for preparing the coal gasification slag-based zeolite adsorbent comprises a kettle body and a bracket at the bottom of the kettle body, wherein the top of the kettle body is provided with a feed inlet, the bottom of the kettle body is provided with a discharge outlet, a sealing cover is detachably connected to the feed inlet, a heat conducting jacket is arranged at the outer side of the kettle body, a heat conducting oil inlet and a heat conducting oil outlet are arranged on the side wall of the heat conducting jacket, the heat conducting oil outlet is positioned above the heat conducting oil inlet, a lining is arranged at the inner side wall of the kettle body, a mechanical stirring mechanism and an ultrasonic vibration rod are arranged in the kettle body, the upper part of the ultrasonic vibration rod is fixed on the top wall of the kettle body, and the lower end of the ultrasonic vibration rod stretches into the middle lower part of the kettle body.
Further, mechanical stirring mechanism includes (mixing) shaft, helical blade, and helical blade sets up on the (mixing) shaft, (mixing) shaft upper end and agitator motor output shaft coaxial coupling, and (mixing) shaft upper portion rotates with the cauldron body roof to be connected. The mixing speed of the materials is accelerated by the stirring mechanism, so that the materials are homogenized.
Preferably, the spiral blade is uniformly provided with a plurality of through holes.
Further, the number of the ultrasonic vibration bars is 2, and the 2 ultrasonic vibration bars are symmetrically arranged around the stirring shaft and are positioned outside the spiral blade. Ultrasonic waves are generated by an ultrasonic vibration rod to serve as energy, ultrasonic crystallization is carried out under the assistance of the ultrasonic waves, zeolite crystallization is enabled to be uniform in nucleation, and hydrothermal reaction time is shortened.
Further, the bottom surface of the sealing cover body is concentrically provided with an inner convex ring body and an outer convex ring body, a groove is formed between the inner convex ring body and the outer convex ring body, a first sealing ring is arranged in the groove, the upper end of a charging hole is inserted into the groove, the outer side of the charging hole is fixedly connected with a limiting seat, and the limiting seat is connected with the sealing cover body through a bolt. The sealing cover and the charging port form a labyrinth structure, so that the sealing effect is improved.
Preferably, a groove which can be inserted into the lower part of the outer convex ring body is formed between the limiting seat and the charging hole, and a second sealing ring is arranged in the groove.
Further, a three-way valve is arranged on the discharge port, one outlet of the three-way valve is used for discharging materials in the kettle body out of the kettle body, the other outlet is connected with a circulating pump, the circulating pump is fixed on the support, the liquid outlet end of the circulating pump is connected with a return pipe, and the upper end of the return pipe is communicated with the upper part of the kettle body. The materials in the kettle body are circularly mixed through the three-way valve, the circulating pump and the return pipe, so that the materials are more fully polymerized.
Preferably, the outlet at the upper end of the return pipe is horizontally arranged and tangentially arranged with the side wall at the upper part of the kettle body. The circulating material tangentially enters the kettle body, swirls along the inner wall of the kettle body, and improves the heat exchange efficiency with the heat conduction oil in the heat conduction jacket through the side wall of the kettle body.
Compared with the prior art, the utility model has the beneficial technical effects that due to the adoption of the technical scheme, the utility model has the following advantages: the reaction device for preparing the coal gas slag-based zeolite adsorbent adopts an ultrasonic wave-assisted hydrothermal method to treat coal gas slag to synthesize zeolite, and the zeolite has uniform crystallization nucleation and high crystallinity; the materials can be fully and uniformly mixed, and the time of hydrothermal polymerization reaction is shortened; the kettle body is provided with a polytetrafluoroethylene lining, so that the durability of the kettle body is improved.
Drawings
FIG. 1 is a schematic structural view of a reaction apparatus for preparing a gas-based slag zeolite adsorbent according to an embodiment of the present utility model;
FIG. 2 is an enlarged view of a portion of FIG. 1 at A;
reference numerals: the device comprises a 1-kettle body, a 2-heat conducting jacket, a 3-bracket, a 4-stirring shaft, 5-helical blades, a 6-stirring motor, a 7-liner, an 8-charging opening, a 9-sealing cover, a 901-inward convex ring body, a 902-outward convex ring body, a 10-ultrasonic vibration rod, an 11-discharging opening, a 12-three-way valve, a 13-circulating pump, a 14-return pipe, a 15-heat conducting oil inlet, a 16-heat conducting oil outlet, a 17-first sealing ring, a 18-limiting seat, a 19-second sealing ring and a 20-bolt.
Detailed Description
The utility model will be further described in detail by means of preferred embodiments in order to make the objects, technical solutions and advantages of the utility model more apparent.
Examples
Referring to fig. 1, the reaction device for preparing a gasifiable slag-based zeolite adsorbent in this embodiment includes a kettle body 1 and a support 3 at the bottom of the kettle body 1, wherein a feed inlet 8 is provided at the top of the kettle body 1, a discharge outlet 11 is provided at the bottom of the kettle body, a sealing cover 9 is detachably connected to the feed inlet 8, a heat conducting jacket 2 is provided at the outside of the kettle body 1, a heat conducting oil inlet 15 and a heat conducting oil outlet 16 are provided at the side wall of the heat conducting jacket 2, the heat conducting oil outlet 16 is located above the heat conducting oil inlet 15, a liner 7 is provided at the inner side wall of the kettle body 1, the liner 7 is made of polytetrafluoroethylene material, a mechanical stirring mechanism and an ultrasonic vibration rod 10 are provided in the kettle body 1, the upper part of the ultrasonic vibration rod 10 is fixed on the top wall of the kettle body 1, and the lower end of the ultrasonic vibration rod 10 extends into the middle lower part of the kettle body 1.
Specifically, in order to accelerate the material mixing rate in the cauldron body 1, mechanical stirring mechanism includes (mixing) shaft 4, helical blade 5, and helical blade 5 sets up on (mixing) shaft 4, and (mixing) shaft 4 upper end and (mixing) motor 6 output shaft coaxial coupling, (mixing) shaft 4 upper portion and cauldron body 1 roof rotate to be connected, evenly set up a plurality of through-holes on the helical blade 5. The stirring mechanism is used for homogenizing materials and is convenient for uniform heating.
Specifically, in order to make zeolite crystallization nucleation uniform and shorten the hydrothermal reaction time, the number of the ultrasonic vibration bars 10 is 2, and the 2 ultrasonic vibration bars 10 are symmetrically arranged about the stirring shaft 4 and are positioned outside the helical blades 5. Ultrasonic waves are generated by the ultrasonic vibration rod 10 as energy sources, ultrasonic crystallization is assisted by the ultrasonic waves, and zeolite crystallization is uniformly nucleated. The ultrasonic vibration rod 10 is of the type HDG-1000, the working frequency is 15-60kHz, and the working temperature is 100-500 ℃.
Specifically, in order to improve the sealing effect between the sealing covers 9 of the kettle body for 1 month and reduce heat loss, the bottom surface of the cover body of the sealing cover 9 is concentrically provided with an inner convex ring body 901 and an outer convex ring body 902, a groove is formed between the inner convex ring body 901 and the outer convex ring body 902, a first sealing ring 17 is arranged in the groove, the upper end of a charging port 8 is inserted into the groove, the outer side of the charging port 8 is fixedly connected with a limiting seat 18, and the limiting seat 18 is connected with the cover body of the sealing cover 9 through a bolt 20; a groove which can be inserted into the lower part of the outer convex ring body 902 is formed between the limiting seat 18 and the charging hole 8, and a second sealing ring 19 is arranged in the groove. The sealing cover 9 and the charging hole 8 form a labyrinth structure, so that the sealing effect is improved.
Specifically, in order to make the material in the kettle body 1 more fully carry out the polymerization, set up three-way valve 12 on the bin outlet 11, one of them export of three-way valve 12 is used for discharging the material in the kettle body 1 outside the kettle body 1, and another exit linkage has circulating pump 13, and circulating pump 13 is fixed in on the support 3, and the back flow 14 is connected to the liquid outlet end of circulating pump 13, and back flow 14 upper end and kettle body 1 upper portion intercommunication. The materials in the kettle body 1 are circularly mixed through a three-way valve 12, a circulating pump 13 and a return pipe 14.
Specifically, the outlet at the upper end of the return pipe 14 is horizontally arranged and tangentially arranged with the side wall of the upper part of the kettle body 1. The circulating material tangentially enters the kettle body 1 from the outlet at the upper end of the return pipe 14, swirls along the inner wall of the kettle body 1, and improves the heat exchange efficiency with the heat conduction oil in the heat conduction jacket 2 through the side wall of the kettle body 1.
When the reaction device for preparing the coal gasification slag-based zeolite adsorbent is used, coal gasification fine slag and sodium hydroxide solution are sequentially added through the feed inlet 8, the sealing cover 9 is covered after being adjusted according to a certain solid-to-liquid ratio, the sealing cover 9 is in sealing connection with the feed inlet 8 by adopting the bolts 20, the stirring motor 6 is started to stir materials, meanwhile, heat conduction oil is injected into the heat conduction jacket 2 through the heat conduction oil inlet 15, the materials in the kettle body 1 are heated to 100 ℃, and the circulating pump 13 is started to enable the materials at the lower part of the kettle body 1 to circularly flow into the upper part of the kettle body 1; after 1.5 hours, the stirring motor 6 and the circulating pump 13 stop working; and starting the ultrasonic vibration rod 10 to generate ultrasonic waves, performing ultrasonic crystallization for 1h, stopping injecting heat conduction oil into the heat conduction jacket 2 after the ultrasonic waves are finished, standing to room temperature to obtain a product, discharging the material in the kettle body 1 out of the kettle body 1 through one of a discharge port 11 and a three-way valve 12, and sending the material to the next filtering equipment.
The foregoing description of the preferred embodiments of the utility model has been presented for the purpose of illustration and description, and it will be apparent to those skilled in the art that various changes, substitutions and alterations can be made therein without departing from the spirit and principles of the utility model.

Claims (8)

1. A reaction unit for preparation of coal gas slag-based zeolite adsorbent, including cauldron body (1) and support (3) of cauldron body (1) bottom, its characterized in that: the utility model discloses a kettle, including a kettle body (1), a kettle cover (2), a heat conduction jacket (2), a heat conduction oil inlet (15), a heat conduction oil outlet (16), a mechanical stirring mechanism, an ultrasonic vibration stick (10) are arranged at the top of the kettle body (1), a sealing cover (9) is detachably connected to the top of the kettle body (1), the heat conduction jacket (2) is arranged at the outer side of the kettle body (8), the heat conduction oil inlet (15) and the heat conduction oil outlet (16) are arranged on the side wall of the heat conduction jacket (2), a lining (7) is arranged on the inner side wall of the kettle body (1), the mechanical stirring mechanism and the ultrasonic vibration stick (10) are arranged in the kettle body (1), the upper part of the ultrasonic vibration stick (10) is fixed on the top wall of the kettle body (1), and the lower end of the ultrasonic vibration stick (10) stretches into the middle lower part of the kettle body (1).
2. The reaction apparatus for preparing a gas-based zeolite adsorbent according to claim 1, wherein: the mechanical stirring mechanism comprises a stirring shaft (4) and a spiral blade (5), the spiral blade (5) is arranged on the stirring shaft (4), the upper end of the stirring shaft (4) is coaxially connected with the output shaft of the stirring motor (6), and the upper part of the stirring shaft (4) is rotationally connected with the top wall of the kettle body (1).
3. The reaction apparatus for preparing a gas-based zeolite adsorbent according to claim 2, characterized in that: a plurality of through holes are uniformly formed in the spiral blade (5).
4. The reaction apparatus for preparing a gas-based zeolite adsorbent according to claim 1, wherein: the number of the ultrasonic vibration rods (10) is 2, and the 2 ultrasonic vibration rods (10) are symmetrically arranged about the stirring shaft (4) and are positioned outside the spiral blades (5).
5. The reaction apparatus for preparing a gas-based zeolite adsorbent according to claim 1, wherein: the sealing cover is characterized in that an inner convex ring body (901) and an outer convex ring body (902) are concentrically arranged on the bottom surface of the cover body of the sealing cover (9), a groove is formed between the inner convex ring body (901) and the outer convex ring body (902), a first sealing ring (17) is arranged in the groove, the upper end of a charging hole (8) is inserted into the groove, the outer side of the charging hole (8) is fixedly connected with a limiting seat (18), and the limiting seat (18) is connected with the cover body of the sealing cover (9) through a bolt (20).
6. The reaction apparatus for preparing a gas-based zeolite adsorbent according to claim 5, wherein: a groove which can be inserted into the lower part of the outer convex ring body (902) is formed between the limiting seat (18) and the charging hole (8), and a second sealing ring (19) is arranged in the groove.
7. The reaction apparatus for preparing a gas-based zeolite adsorbent according to claim 1, wherein: the three-way valve (12) is arranged on the discharge port (11), one outlet of the three-way valve (12) is used for discharging materials in the kettle body (1) out of the kettle body (1), the other outlet is connected with the circulating pump (13), the circulating pump (13) is fixed on the support (3), the liquid outlet end of the circulating pump (13) is connected with the return pipe (14), and the upper end of the return pipe (14) is communicated with the upper part of the kettle body (1).
8. The reaction apparatus for preparing a gas-based zeolite adsorbent according to claim 7, wherein: the outlet at the upper end of the return pipe (14) is horizontally arranged and tangentially arranged with the side wall at the upper part of the kettle body (1).
CN202223328747.9U 2022-12-13 2022-12-13 Reaction device for preparing coal gas slag-based zeolite adsorbent Active CN219003093U (en)

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CN202223328747.9U CN219003093U (en) 2022-12-13 2022-12-13 Reaction device for preparing coal gas slag-based zeolite adsorbent

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CN202223328747.9U CN219003093U (en) 2022-12-13 2022-12-13 Reaction device for preparing coal gas slag-based zeolite adsorbent

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117299375A (en) * 2023-10-24 2023-12-29 西安科技大学 Device and method for sorting coal gasification fine slag by ultrasonic cavitation and oil agglomeration

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117299375A (en) * 2023-10-24 2023-12-29 西安科技大学 Device and method for sorting coal gasification fine slag by ultrasonic cavitation and oil agglomeration
CN117299375B (en) * 2023-10-24 2024-03-08 西安科技大学 Device and method for sorting coal gasification fine slag by ultrasonic cavitation and oil agglomeration

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