CN219942790U - Recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves - Google Patents

Recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves Download PDF

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CN219942790U
CN219942790U CN202321454414.2U CN202321454414U CN219942790U CN 219942790 U CN219942790 U CN 219942790U CN 202321454414 U CN202321454414 U CN 202321454414U CN 219942790 U CN219942790 U CN 219942790U
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tank
filtrate
mother liquor
zsm
nay
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邹戊申
欧海月
张明远
卓润生
张静
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Runhe Catalytic Materials Zhejiang Co ltd
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Runhe Catalytic Materials Zhejiang Co ltd
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Abstract

The utility model provides a recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves, belongs to the technical field of molecular sieve production, and solves the problem of low silicon utilization rate in the prior art. The device comprises at least two settling tanks, wherein each settling tank is connected with an overflow pipe, one overflow pipe is connected with a silica-alumina gel reaction kettle, the other overflow pipe is connected with a silicon-containing liquid blending tank, and the silicon-containing liquid blending tank is connected with a silica gel preparation kettle. The filtered liquid is respectively conveyed into two settling tanks, the liquid separated from the two settling tanks is respectively fed into a silicon-aluminum glue preparation tank and a silicon-containing liquid preparation tank, the silicon-containing liquid preparation tank is used for preparing the liquid and then conveying the liquid into a silica gel preparation tank to prepare the silica gel, under the premise of ensuring stable product quality, the utilization rate of the silicon is improved, the cost is saved, the discharge pollution of waste water and waste residues is reduced, and meanwhile, the long-period continuous and stable operation of production is realized.

Description

Recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves
Technical Field
The utility model belongs to the technical field of molecular sieve production, and particularly relates to a recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves.
Background
Molecular sieves are a material containing precise and single minute pores that can be used to adsorb gases or liquids. Molecular sieves are often used in the petroleum industry, particularly for purifying gases, such as silica gel, which can adsorb mercury from natural gas for corrosion of aluminum pipelines and other liquefaction equipment. The Y-type and shape selective (ZSM-5) molecular sieves are the two main molecular sieves commonly used in the production of refinery catalysts.
In the synthesis process of the NaY molecular sieve and the ZSM-5 molecular sieve, the silicon-aluminum ratio of the material is far higher than that of the product, so that the crystallization mother liquor and the water washing filtrate contain a large amount of silicon, the silicon utilization rate is relatively low and is only 60 percent, if the direct discharge is likely to cause the loss of the silicon, the product cost is increased, and meanwhile, the environment is polluted. In order to avoid the problems, in the prior art, the crystallization mother liquor and filtrate are mostly adopted to directly react with aluminum sulfate to prepare the silica-alumina gel, so that the reuse of silicon is realized, and the silica-alumina gel is used as a raw material for synthesizing the NaY molecular sieve. The main process flow is as follows: mixing mother liquor, zero-order filtrate and primary filtrate, inputting the mixture into a filtering device for filtering, inputting the filtered liquid into a settling tank for further separating solid particles and liquid, and conveying the separated liquid into a silica-alumina gel reaction kettle for reaction to prepare the silica-alumina gel.
In the actual industrial production process, because the mother liquor contains certain molecular sieve particles, repeated recycling for a plurality of times can lead to the enrichment of molecular sieve impurity crystals, the generation of the impurity crystals is easy to induce in the crystallization process, the quality of NaY molecular sieve products is seriously affected, long-period continuous and stable recycling is not facilitated, the quality is ensured, and meanwhile, the recycling proportion of a silicon source is limited to a certain extent, so that the utilization rate of silicon in the existing process is only 75%, more silicon-containing waste liquid is generated, the utilization rate of raw materials is reduced, the treatment capacity of silicon-containing sewage is increased, and the operation cost is increased.
Disclosure of Invention
Aiming at the problems, the utility model aims to provide a recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves, wherein the filtered liquid is respectively conveyed into two settling tanks, the liquid separated by the two settling tanks is respectively conveyed into a silica-alumina gel preparation kettle and a silicon-containing liquid preparation tank, the silicon-containing liquid preparation tank is used for preparing liquid, and then the liquid is conveyed into a silica gel preparation kettle to prepare silica gel, so that the utilization rate of silicon is improved on the premise of ensuring stable product quality, and long-period continuous and stable operation of production is realized.
The technical scheme adopted by the utility model is as follows:
the utility model provides a reuse system of mother liquor and filtrate of NaY and ZSM-5 molecular sieve, includes two at least settling casks, the settling cask is connected with the overflow pipe, and wherein an overflow pipe is connected with silica-alumina gel reation kettle, and another overflow pipe is connected with the silicon-containing liquid blending jar, and silicon-containing liquid blending jar is connected with silica gel preparation cauldron.
Preferably, the device further comprises a mother liquid tank, a zero-level liquid filtering tank and a first-level liquid filtering tank, wherein the mother liquid tank, the zero-level liquid filtering tank and the first-level liquid filtering tank are connected with a mixing pipeline through pipelines, the outlet end of the mixing pipeline is connected with a filtering device, and the liquid outlet end of the filtering device is connected with a settling tank.
Preferably, the liquid outlet pipes of the mother liquid tank, the zero-level liquid filtering tank and the first-level liquid filtering tank are provided with first flow control valves.
Preferably, the device further comprises a plurality of delivery pumps arranged in the pipeline, wherein the water inlet end of the delivery pump and the pipeline of the water outlet pipe are respectively provided with a first valve.
Preferably, a second flow control valve is arranged in the liquid inlet pipe of the settling tank.
Preferably, the bottom of the settling tank is connected with a discharging pipe, and a second valve is arranged in the discharging pipe.
Preferably, the discharging pipe is connected with a beating tank, and the beating tank is provided with a receiving hopper.
Preferably, a first overflow cavity communicated with the overflow pipe is arranged in the sedimentation tank.
Preferably, a filter screen member is disposed in the first overflow chamber.
Preferably, the filter screen piece is movably arranged in the first overflow cavity, an opening is formed in the upper end face of the settling tank, a sealing plate connected with the filter screen piece is movably arranged in the opening in a sealing mode, a support is arranged on the settling tank, and a lifting mechanism for controlling the lifting of the sealing plate is arranged on the support.
In summary, due to the adoption of the technical scheme, the beneficial effects of the utility model are as follows:
the filtered liquid is respectively conveyed into two settling tanks, the liquid separated from the two settling tanks is respectively fed into a silicon-aluminum glue preparation tank and a silicon-containing liquid preparation tank, the silicon-containing liquid preparation tank is used for preparing the liquid and then conveying the liquid into a silica gel preparation tank to prepare the silica gel, under the premise of ensuring stable product quality, the utilization rate of the silicon is improved, the cost is saved, the discharge pollution of waste water and waste residues is reduced, and meanwhile, the long-period continuous and stable operation of production is realized.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present utility model, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present utility model and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a process flow provided in an embodiment of the present utility model;
FIG. 2 is a schematic diagram of a settling tank according to an embodiment of the present utility model;
fig. 3 is a schematic view of a cleaning state of a filter element according to an embodiment of the present utility model.
Description of the drawings: 1-a mother liquid tank; 2-zero-order filtrate tank; 3-a first-stage filtrate tank; 4-a filtering device; a 5-settling tank; 6-pulping tank; 7-a silica-alumina gel reaction kettle; 8-a silicon-containing liquid blending tank; 9-a silica gel preparation kettle; 10-a first flow control valve; 11-a transfer pump; 12-a first valve; 13-a second flow control valve; 14-a first overflow chamber; 15-overflow pipe; 16-a filter screen member; 17-connecting rods; 18-sealing plate; 19-a bracket; 20-screw rod; 21-a screw lifter; 22-a guide rod; 23-mixing pipes; 24-second valve.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present utility model more apparent, the technical solutions of the embodiments of the present utility model will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present utility model, and it is apparent that the described embodiments are some embodiments of the present utility model, but not all embodiments of the present utility model. The components of the embodiments of the present utility model generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the utility model, as presented in the figures, is not intended to limit the scope of the utility model, as claimed, but is merely representative of selected embodiments of the utility model. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
In the description of the present utility model, it should be noted that, if the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate an azimuth or a positional relationship based on that shown in the drawings, or an azimuth or a positional relationship in which a product of the application is conventionally put in use, it is merely for convenience of describing the present utility model and simplifying the description, and it is not indicated or implied that the referred device or element must have a specific azimuth, be constructed and operated in a specific azimuth, and thus should not be construed as limiting the present utility model.
The present utility model will be described in detail with reference to fig. 1 to 3.
Examples
The utility model provides a recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieve, includes two at least settling casks 5, and settling cask 5 is connected with overflow pipe 15, and wherein an overflow pipe 15 is connected with silica-alumina gel reation kettle 7, and another overflow pipe 15 is connected with silicon-containing liquid blending tank 8, and silicon-containing liquid blending tank 8 is connected with silica gel preparation cauldron 9. Wherein the silicon-containing liquid blending tank 8 is used for mixing the ZSM-5 recycled filtrate, water glass and liquid output by the settling tank 5, thereby increasing the concentration of silicon dioxide.
As shown in fig. 1, the liquid of one settling tank 5 enters a silica-alumina gel reaction kettle 7 and simultaneously aluminum sulfate and steam are input for reaction, so that silica-alumina gel is prepared; the liquid in the other sedimentation tank 5 enters a silicon-containing liquid blending tank 8 to be mixed with ZSM-5 recycling filtrate and water glass, and then is conveyed into a silica gel preparation kettle 9 to react with sulfuric acid and steam to generate silica gel.
As shown in fig. 1, the mother liquor and filtrate of NaY and ZSM-5 molecular sieves further comprises a mother liquor tank 1, a zero-order filtrate tank 2 and a first-order filtrate tank 3, wherein the mother liquor tank 1, the zero-order filtrate tank 2 and the first-order filtrate tank 3 are connected with a mixing pipeline 23 through pipelines, the outlet end of the mixing pipeline 23 is connected with a filtering device 4, and the liquid outlet end of the filtering device 4 is connected with a settling tank 5. The mother liquor tank 1, the zero-order filtrate tank 2 and the first-order filtrate tank 3 collect mother liquor, zero-order filtrate and first-order filtrate respectively, and the mother liquor, the zero-order filtrate and the first-order filtrate are conveyed to the filtering device 4 for filtering after being mixed in the mixing pipeline 23. The filter device 4 is a plate-and-frame filter press, which has high solid recovery rate and can fully collect solid particles in filtrate.
In order to ensure the quality of the final product, the mother liquor, the zero-order filtrate and the first-order filtrate are required to be mixed according to a certain proportion, so that a first flow control valve 10 is arranged in the liquid outlet pipes of the mother liquor tank 1, the zero-order filtrate tank 2 and the first-order filtrate tank 3, and the first flow control valve 10 monitors and controls the flow. Wherein the mixing proportion of the mother solution, the zero-order filtrate and the primary filtrate is mixed according to the mass ratio, and the specific mass ratio is (0.8-1.5) mother solution: (0.8-1.5) zero order filtrate: (0.5-1.0) primary filtrate.
The mother liquor and filtrate of NaY and ZSM-5 molecular sieves further comprise a plurality of delivery pumps 11 arranged in the pipeline, and first valves 12 are arranged in the pipeline of the water inlet end and the water outlet pipe of the delivery pumps 11. The liquid of the whole system is conveyed by the conveying pump 11, the first valve 12 is arranged in front of and behind the conveying pump 11, and when the conveying pump 11 is maintained, the first valve 12 is directly closed, so that the conveying pump 11 is maintained conveniently, and the loss of the liquid is reduced.
A second flow control valve 13 is arranged in the feed pipe of the settling tank 5. The liquid feed amount of the two settling tanks 5 is also required to be controlled at a certain ratio, and thus the second flow control valve 13 is provided to control the liquid feed amount of the settling tanks 5. The liquid inlet amount of the sedimentation tank 5 connected with the silica-alumina gel reaction kettle 7 is 60-70% of the liquid outlet amount of the filtering device 4, the residual liquid of the filtering device 4 enters another sedimentation tank 5, the production is carried out according to the proportion, and the silicon utilization rate can reach more than 95%
After sedimentation of the sedimentation tank 5, the liquid is discharged from the overflow pipe 15, solid particles are accumulated at the bottom of the sedimentation tank 5, a discharge pipe is connected to the bottom of the sedimentation tank 5 for conveniently discharging the solid particles, and a second valve 24 is arranged in the discharge pipe; the second valve 24 is opened again after a period of system operation to discharge solid particles. Further, the bottom of the settling tank 5 is arranged to be conical, so that solid particles are conveniently collected at the bottom of the settling tank 5 and discharged.
The discharging pipe is connected with the beating tank 6, and the discharging pipe carries the liquid that contains a large amount of solid particles to the beating tank 6 in carry out the beating, and the hopper that connects on the beating tank 6 is collected the filter cake in the filter equipment 4, and the liquid that the discharging pipe carried is followed to the cooperation is beaten again, reduces the use of other liquids. After the pulping tank 6 pulps, the slurry is sent to a NaY molecular sieve for crystallization.
A first overflow cavity 14 communicated with an overflow pipe 15 is arranged in the sedimentation tank 5, and the first overflow cavity 14 separates the liquid inlet area of the sedimentation tank 5, so that the liquid is kept relatively calm again than the first overflow cavity 14, and the sedimentation effect of solid particles is ensured. The second overflow cavities are arranged in the silica-alumina reaction kettle 7 and the silica gel preparation kettle 9, so that the solutions conveyed by the silica-alumina reaction kettle 7 and the silica gel preparation kettle 9 can be stably and continuously output.
Further, a filter screen member 16 is disposed in the first overflow chamber 14, and the filter screen member 16 filters and intercepts part of the non-settled solid particles, so as to improve the separation effect of the solid particles and the liquid.
The filter screen piece 16 is movably arranged in the first overflow cavity 14, an opening is formed in the upper end face of the sedimentation tank 5, a sealing plate 18 connected with the filter screen piece 16 is movably arranged in the opening in a sealing mode, a support 19 is arranged on the sedimentation tank 5, and a lifting mechanism for controlling the lifting of the sealing plate 18 is arranged on the support 19. The elevating system goes up and down to closing plate 18 and filter screen spare 16, and when closing plate 18 shutoff opening, filter screen spare 16 is located the inlet below of overflow pipe 15 to the inner wall in first overflow chamber 14 is laminated to the lateral wall of filter screen spare 16, after using a period, promotes filter screen spare 16 out of settling cask 5 and washs, in order to guarantee the filtration ability of filter screen spare 16.
The lifting mechanism can be in a screw rod transmission mode or a telescopic transmission mode. The utility model uses screw drive. The concrete structure is as follows: the lead screw lifter 21 is arranged on the support 19, the lead screw lifter 21 is meshed with the lead screw 20, the lead screw 20 movably penetrates through the support 19 and is in rotary connection with the sealing plate 18, the sealing plate 18 is fixedly connected with the guide rod 22 movably penetrating through the support 19, and the lead screw lifter 21 drives the lead screw 20 to move up and down so as to realize lifting control on the sealing plate 18, and the guide rod 22 prevents the sealing plate 18 from horizontally rotating in the lifting process of the sealing plate 18. Wherein the sealing plate 18 is connected to the sieve element 16 by means of a connecting rod 17.
The above is only a preferred embodiment of the present utility model, and is not intended to limit the present utility model, but various modifications and variations can be made to the present utility model by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present utility model should be included in the protection scope of the present utility model.

Claims (10)

1. The utility model provides a recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieve, its characterized in that includes two at least settling casks (5), settling cask (5) are connected with overflow pipe (15), and wherein an overflow pipe (15) are connected with silica-alumina gel reation kettle (7), and another overflow pipe (15) are connected with silicon-containing liquid blending tank (8), and silicon-containing liquid blending tank (8) are connected with silica gel preparation cauldron (9).
2. The recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves according to claim 1, further comprising a mother liquor tank (1), a zero-order filtrate tank (2) and a primary filtrate tank (3), wherein the mother liquor tank (1), the zero-order filtrate tank (2) and the primary filtrate tank (3) are connected with a mixing pipeline (23) through pipelines, the outlet end of the mixing pipeline (23) is connected with a filtering device (4), and the liquid outlet end of the filtering device (4) is connected with a settling tank (5).
3. The recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves according to claim 2, characterized in that the first flow control valve (10) is arranged in the liquid outlet pipes of the mother liquor tank (1), the zero-order filtrate tank (2) and the primary filtrate tank (3).
4. The recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves according to claim 1, further comprising a plurality of delivery pumps (11) arranged in the pipeline, wherein the water inlet end of the delivery pumps (11) and the pipeline of the water outlet pipe are respectively provided with a first valve (12).
5. The recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves according to claim 1, characterized in that a second flow control valve (13) is arranged in the feed pipe of the settling tank (5).
6. The recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves according to claim 1, characterized in that the bottom of the settling tank (5) is connected with a discharge pipe, and a second valve (24) is arranged in the discharge pipe.
7. The recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves according to claim 6, wherein the discharging pipe is connected with a beating tank (6), and a receiving hopper is arranged on the beating tank (6).
8. The recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves according to claim 1, characterized in that a first overflow cavity (14) communicating with an overflow pipe (15) is provided in the settling tank (5).
9. The NaY and ZSM-5 molecular sieve mother liquor and filtrate recycling system according to claim 8, characterized in that a filter screen member (16) is provided in the first overflow chamber (14).
10. The recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves according to claim 9, characterized in that the filter screen member (16) is movably arranged in the first overflow cavity (14), an opening is formed in the upper end face of the settling tank (5), a sealing plate (18) connected with the filter screen member (16) is movably arranged in the opening in a sealing manner, a support (19) is arranged on the settling tank (5), and a lifting mechanism for controlling the lifting of the sealing plate (18) is arranged on the support (19).
CN202321454414.2U 2023-06-08 2023-06-08 Recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves Active CN219942790U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202321454414.2U CN219942790U (en) 2023-06-08 2023-06-08 Recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202321454414.2U CN219942790U (en) 2023-06-08 2023-06-08 Recycling system of mother liquor and filtrate of NaY and ZSM-5 molecular sieves

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CN219942790U true CN219942790U (en) 2023-11-03

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