CN113813908A - Integrated reaction and separation system, process and application - Google Patents
Integrated reaction and separation system, process and application Download PDFInfo
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- CN113813908A CN113813908A CN202111235224.7A CN202111235224A CN113813908A CN 113813908 A CN113813908 A CN 113813908A CN 202111235224 A CN202111235224 A CN 202111235224A CN 113813908 A CN113813908 A CN 113813908A
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/147—Microfiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/16—Rotary, reciprocated or vibrated modules
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
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Abstract
The invention discloses an integrated reaction and separation system, which comprises: the feeding device is used for storing and conveying reaction raw materials; an integrated reaction and separation device comprising a reaction vessel connected downstream of the feed device; the reaction kettle is provided with a separation component for dynamic separation of solid and liquid phases during raw material reaction, and the reaction kettle is connected with a washing device. The separation assembly comprises a hollow rotating shaft which penetrates through the middle part of the reaction kettle shell, a plurality of hollow separation membranes are arranged on the hollow rotating shaft at intervals, the cavity of the hollow rotating shaft is communicated with the inner cavity of each separation membrane, the first end of the hollow rotating shaft along the axial direction is connected with a driving element, and the second end of the hollow rotating shaft is used for outputting separated mother liquor clear liquid and washing waste liquid; a liquid distributor is also arranged in the upper space of the separation membrane in the reaction kettle and is communicated with the feeding device; the bottom is provided with a discharge outlet. Meanwhile, an integrated reaction and separation process and application are provided, so that the reaction efficiency is improved, and the separation and washing effects are improved.
Description
Technical Field
The invention belongs to the technical field of chemical treatment and preparation, and relates to an integrated reaction and separation system, a process and application.
Background
In the fields of chemical industry, pharmacy, material synthesis and the like, the method generally relates to the reaction of generating fine suspended solid particles such as liquid-solid, liquid-solid, gas-liquid-solid and the like, after the reaction processes are finished, solid-liquid separation is often needed to be carried out on materials immediately so as to separate solid particle products from mother liquor, and the solid particles prepared by partial synthesis reaction enter the next treatment working section after the residual mother liquor on the surfaces of the solid particles is removed through a washing process.
In the existing process flow, reaction, liquid-solid separation and product washing are usually carried out in different devices respectively, wherein a reaction kettle only can provide stirring and meet the process conditions necessary for the reaction, and does not have a solid-liquid separation function and a washing function, and an in-vitro separation unit is required to be added to realize solid-liquid separation and an in-vitro washing unit to realize slurry washing, so that the complexity of the process flow is increased, and the production cost is high; on the other hand, when the concentrated high-solid-content slurry flows back to the reaction kettle, the uniform concentration of the particles in the reaction kettle is influenced, so that the reaction efficiency is influenced, and the growth forming of the product particles and the consistency of the product quality are poor in the process of preparing the particles. Aiming at the technical defect, in the prior art, the influence on the growth morphology of product particles in a reaction kettle is alleviated by reducing the backflow amount of concentrated liquid of an in-vitro solid-liquid separation unit in the process of synthesizing a ternary material precursor by a precipitation method, but the working efficiency is reduced at the same time. In addition, the conventional in-vitro solid-liquid separation unit is easy to form a filter cake in the separation process, the flux and the separation efficiency are reduced, the process flow is long, the occupied area is large, and the control operation is complicated. In the washing process, the traditional filter cake washing processes of plate frames, centrifuges and the like have the problems of material running, uneven washing, environmental protection caused by a large amount of washing wastewater and the like.
Therefore, there is a need for providing an integrated reaction and separation system, process and application thereof to simplify the process flow, improve the reaction efficiency, and simultaneously improve the separation and washing effects, thereby effectively reducing the production cost and solving the environmental emission problem in the prior art.
Disclosure of Invention
In view of the above problems in the prior art, the present invention aims to provide an integrated reaction and separation system, a process and an application thereof, so as to simplify the process flow, improve the reaction efficiency, and simultaneously improve the separation and washing effects, thereby effectively reducing the production cost in the prior art and effectively solving the problems of environmental protection and discharge from the source.
The technical scheme provided by the invention is as follows:
an integrated reaction and separation system comprising:
the feeding device is used for storing and conveying reaction raw materials;
an integrated reaction and separation device comprising a reaction vessel connected downstream of the feed device; the reaction kettle is provided with at least one group of separation assemblies for dynamic separation of solid and liquid phases during raw material reaction, each separation assembly comprises a hollow rotating shaft penetrating through the middle of the reaction kettle shell, a plurality of hollow separation membranes are arranged on the hollow rotating shaft at intervals, cavities of the hollow rotating shafts are communicated with inner cavities of the separation membranes, the hollow rotating shafts are connected with a driving element along the axial first ends, and the second ends are used for outputting mother liquor clear liquid after separation.
Preferably, a liquid distributor is further arranged in the reaction kettle in parallel with the hollow rotating shaft, and the liquid distributor is communicated with the feeding device;
and a discharge outlet is formed in the reaction kettle and positioned at the bottom of the separation membrane.
Preferably, the separation membrane is a hollow disc-shaped structure, the membrane aperture of the separation membrane is 1 nm-50 μm, and the diameter of the separation membrane is 50-5000 mm.
Preferably, a washing device is connected to the reaction kettle, the washing device comprises a water supply tank for supplying a washing medium, and the water supply tank is connected to the liquid distributor through a liquid supply valve and is used for washing the separated solid materials.
Preferably, washing waste liquid jar and multistage membrane separation unit are connected gradually to reation kettle's low reaches, multistage membrane separation unit adopts and receives filter membrane and/or reverse osmosis membrane for wash waste liquid after the washing separates, multistage membrane separation unit is equipped with dense solution export and clear solution export, clear solution export cyclic connection to feed water tank.
Further, the washing device further comprises a cleaning pipeline with a cleaning liquid flow valve, and the cleaning pipeline is connected to the liquid distributor; the bottom of the reaction kettle is also provided with a discharge port for discharging the cleaned waste liquid and the residual mother liquid, and the front end of the washing waste liquid tank is communicated with the heat exchange unit for reducing the temperature of the washing waste liquid.
Furthermore, a turbulence element is also arranged in the reaction kettle; the cross section of the turbulence element is comb-shaped, and a plurality of comb teeth which are uniformly distributed at intervals are inserted into the interval area of the adjacent separation membranes at intervals.
Further, the feeding device comprises a raw material storage unit which is connected to the liquid distributor through a feeding pipeline with a feeding valve.
Furthermore, a back washing device is connected to the reaction kettle and comprises a back washing pipeline with a back washing valve, the back washing pipeline is connected to a back washing tank, and the bottom of the back washing tank is communicated with the second end of the hollow rotating shaft.
Further, the second end of the hollow rotating shaft along the axial direction is respectively connected to the backflushing tank and the mother liquor tank through a buffer tank; and a clear liquid viewing mirror is arranged on a connecting pipeline of the buffer tank, the backflushing tank and the mother liquid tank.
Furthermore, a water supply tank heat source flow valve is arranged on the water supply tank, and a temperature sensor is arranged on the water supply tank and used for adjusting the temperature of the washing medium in the water supply tank.
Further, a reaction kettle heat source flow valve is arranged on the reaction kettle and used for adjusting the temperature of a system in the reaction kettle; an exhaust pipeline with an exhaust flow valve is also arranged on the reaction kettle; the reaction kettle is also provided with a pressure gauge for monitoring the operating pressure in the reaction kettle.
According to the integrated reaction and separation system provided by the invention, an integrated reaction and separation process can be further provided, and the integrated reaction and separation process comprises the following steps:
s1, continuously metering reaction raw materials into a reaction kettle of the integrated reaction and separation device, controlling the pressure in the reaction kettle by adjusting the feed flow, and separating mother liquor clear liquid and solid materials from the reacted materials by a separation component while the reaction raw materials react in the kettle;
and S2, stopping feeding the reaction kettle when the solid materials in the reaction kettle meet the physicochemical characteristics, and obtaining a slurry product in the reaction kettle. The physicochemical characteristics of the solid material in the technical scheme comprise the particle size, tap density and specific surface area of a reaction product, the catalytic activity of a solid catalyst and the like, and the physicochemical characteristics adopted by different reaction systems may be different.
Further, the integrated reaction and separation process further comprises the following steps:
s3, adding a washing medium into the reaction kettle through a washing device, washing the slurry in the reaction kettle by the washing medium under the driving of pressure, and storing the generated washing waste liquid into a washing waste liquid tank; and storing the qualified slurry product washed in the reaction kettle into a qualified product storage tank through a discharge valve.
Preferably, the step S3 includes a concentration process of the slurry product before washing, in which the slurry concentration is performed by controlling the rotation speed of the separation module, so that the solid material gradually forms a filter cake on the surface of the membrane of the separation module; the residual mother liquor was drained and the washing process was started for the solid particles.
Further, the above steps are more specifically:
in the step S1, when the reaction raw materials react in the kettle, a first end of a hollow rotating shaft in the separation assembly, which is positioned in the middle of the reaction kettle, is driven to rotate, separation membranes which are arranged on the hollow rotating shaft at intervals and are communicated with each other are driven to rotate, mother liquor clear liquid generated by the reaction permeates from the surfaces of the separation membranes to converge into a cavity of the hollow rotating shaft under the drive of pressure and is discharged through a second end of the hollow rotating shaft, and solid particles in a reaction system are intercepted on the surfaces of the separation membranes; moreover, the solid particles in the reaction kettle are uniformly suspended and distributed in the reaction kettle under the combined action of the rotation of the separation membrane and the turbulence element;
in step S3, a washing pump at an outlet of a water supply tank in the washing device is turned on, and at the same time, the rotation speed of the hollow rotating shaft is controlled, and a washing medium permeates and converges from the surface of the separation membrane to the hollow rotating shaft under the driving of pressure, so that the washing of the slurry is completed, and the slurry is discharged from the second end of the hollow rotating shaft, cooled by the heat exchange unit, and then stored in a washing waste liquid tank; wherein, for slurry products in the reaction kettle, after sampling and detecting that the impurity content in the products is qualified, the slurry is discharged to a qualified product storage tank; and after the washing waste liquid in the washing waste liquid tank is separated by a nanofiltration membrane and/or a reverse osmosis membrane of the multistage membrane separation unit, clear liquid flows back to the water supply tank for recycling.
Further, the step S2 includes: when the solid content in the reaction kettle is continuously increased to a specified value, mother liquor clear liquid is discharged to a mother liquor tank, and solid materials are discharged to a product storage tank through a discharge valve and enter a subsequent treatment process.
Preferably, in the process, the reaction kettle is backwashed as required; the back washing process comprises the following steps:
mother liquor clear liquid or washing waste liquid discharged from the hollow rotating shaft enters the backflushing tank through the buffer tank, the mother liquor clear liquid or the washing waste liquid in the backflushing tank permeates from the membrane side to the membrane surface of the separation membrane through the hollow rotating shaft under the push of backflushing air pressure, and sediments on the surface of the separation membrane are removed through backflushing.
When the system runs for a long time and the clear liquid flux is not completely recovered by backwashing, periodically draining the system equipment materials, adding cleaning liquid through a cleaning pipeline to clean the reaction kettle, and discharging the cleaned waste liquid from a drain port; and moreover, after cleaning is finished, the cleaning medium in the water supply tank is used for washing, so that the pollution of residual cleaning liquid to products is avoided.
Preferably, the revolution of the hollow rotating shaft is controlled to be 0-1500 r/min; the operating pressure in the reaction kettle is 0-5 bar.
According to the integrated reaction and separation system and the process provided by the invention, the application of the integrated reaction and separation system can be further provided, and the integrated reaction and separation system can be particularly used for the reaction of generating a solid product by a liquid phase method or the fluidized bed reaction of a powder catalyst.
The invention has the beneficial effects that:
(1) the invention can provide a device and a process integrating reaction and dynamic separation, which utilize a separation membrane to carry out in-situ reaction and dynamic separation, and ensure high flux of the membrane and low leakage filtration of solid particles. The invention is suitable for the occasions of preparing ultrafine powder or catalytic additives into fine particles by a liquid phase method, can realize reaction raw material reaction and filtrate separation at the same time, and improves the reaction efficiency and the utilization rate of the catalyst.
(2) The invention also provides a system and a process integrating reaction, dynamic separation and washing, wherein the solid materials generated by the reaction are uniformly suspended and distributed in the reaction kettle by utilizing the combined action of the rotation of the separation membrane and the turbulence element in the reaction kettle, so that the dynamic and uniform separation and washing without filter cakes are realized, the high-definition liquid flux of the separation membrane is ensured, and the separation and washing efficiency is higher. The method is particularly suitable for occasions of preparing superfine powder by a liquid phase method, such as titanium oxide, aluminum oxide, battery anode materials and precursors thereof, and the like, can realize reaction raw material reaction and filtrate separation, directly performs a washing process after the reaction is finished, and recycles washing waste liquid after the treatment.
(3) The invention integrates the reaction and dynamic separation processes in the integrated reaction and separation device, also integrates the washing process, can carry out reaction while feeding, and carry out dynamic separation, has high reaction integration level, can ensure that solid particles can keep uniform growth in situ in a reaction kettle, avoids adverse growth factors caused by in vitro transfer to products, can regenerate the integrated reaction and separation device according to actual requirements through a back washing device, and simultaneously effectively improves the reaction efficiency and the product quality. Therefore, the whole process can realize intermittent or semi-intermittent semi-continuous or continuous production, and the production efficiency is improved. And has the characteristics of small occupied area of the whole system, short reaction flow, high reaction solid content, high volume utilization rate of the reaction kettle, high yield, low production cost and the like.
(4) The integrated reaction and separation device provided by the invention has the advantages that the hollow rotating shaft is driven by the driving element to drive the separation membrane to rotate, meanwhile, the material in the reaction kettle is well stirred, the stirring device in the traditional reaction kettle can be replaced, the energy consumption is obviously reduced, and the purposes of energy conservation and environmental protection are achieved.
(5) The integrated reaction and separation device is easy to clean, is suitable for flexible switching among different series of products, and has high industrial popularization value.
Drawings
FIG. 1 is a schematic view of an integrated reaction and separation system according to an embodiment of the present invention.
FIG. 2 is a schematic view of an integrated reaction and separation system according to another embodiment of the present invention.
The notations in the figures have the following meanings:
10-a feed device, 100-a reaction raw material storage unit, 110-a feed valve, 120-a feed pump, 121-a feed pump outlet check valve;
20-integrated reaction and separation device, 200-reaction kettle, 210-driving element, 220-reaction kettle shell, 230-separation membrane, 240-hollow rotating shaft, 250-turbulence element, 260-liquid distributor, 270-clear liquid sight glass, 280-reaction kettle heat source flow valve, 281-exhaust flow valve, 282-discharge valve, 283-pressure gauge, 284-temperature sensor, 285-exhaust port, 290-buffer tank;
300-mother liquor tank, 310-mother liquor discharge valve, 320-mother liquor tank discharge valve;
400-qualified material storage tank, 410-qualified material discharge valve;
500-washing waste liquid tank, 510-booster pump, 511-booster pump outlet check valve, 520-washing waste liquid discharge valve;
600-multistage membrane separation unit, 610-membrane separation clear liquid valve, 620-membrane separation concentrated liquid valve;
70-backwashing device, 700-backwashing tank, 710-backwashing valve;
80-washing device, 800-water supply tank, 810-water replenishing valve, 811-temperature sensor, 820-liquid supply valve, 821-water supply tank heat source flow valve, 822-cleaning liquid flow valve, 830-water washing pump and 831-water washing pump outlet check valve;
900-heat exchange unit.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the specific embodiments. 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.
According to an embodiment of the present invention, as shown in fig. 1, an integrated reaction and separation system according to an embodiment of the present invention comprises: a feeding device 10 for storing and delivering reaction raw materials;
an integrated reaction and separation device 20, the integrated reaction and separation device 20 comprising a reaction vessel 200 connected to the downstream of the feeding device 10; at least one group of separation assemblies is arranged in the reaction kettle 200 and is used for synchronously carrying out dynamic separation of solid and liquid phases during raw material reaction. According to the embodiment, the integrated reaction and dynamic separation device 20 integrates reaction and dynamic separation, can feed reaction and dynamically separate mother liquor, has high reaction integration level, avoids adverse factors caused by external transfer to the reaction, is suitable for the occasions that reactants or products or catalytic additives of liquid-solid, liquid-solid, gas-liquid-solid and other multi-phase reactions are fine particles, and can improve the reaction efficiency and the catalyst utilization rate.
As a preferred embodiment, the separation assembly includes a hollow rotating shaft 240 penetrating through the middle of the reaction kettle shell 220, a plurality of hollow separation membranes 230 are disposed on the hollow rotating shaft 240 at intervals, and the cavities of the hollow rotating shaft 240 are communicated with the inner cavities of the separation membranes 230, a first end of the hollow rotating shaft 240 along the axial direction is connected to a driving element 210 such as a stirring motor, a second end is used for outputting separated mother liquor clear liquid, and the separated mother liquor clear liquid is output to a buffer tank 290; the separation assembly is driven by the driving element 210 to rotate, and can better stir the materials in the reaction kettle 200; a liquid distributor 260 is further arranged in the reaction kettle 200 in parallel with the hollow rotating shaft 240, and the liquid distributor 260 is communicated with the feeding device 10; a discharge port is arranged at the bottom of the separation membrane 230 in the reaction kettle 200, and solid materials are discharged through a discharge valve 282.
According to this embodiment, the reaction raw material enters the reaction vessel 200 through the liquid distributor 260 via the feeding device 10, the hollow rotating shaft 240 is driven by the driving element 210 to rotate the separation membrane 230, so as to drive the materials in the reaction vessel 200 to form a mixed flow, a pressure difference is formed in the space between the feeding and discharging of the reaction vessel, the solid particles in the reaction system are trapped on the surface of the separation membrane 230, the solid particles in the reaction vessel are uniformly suspended and distributed in the reaction vessel under the mixed flow, and the mother liquor clear liquid after the reaction is driven by the pressure, permeates through the surface of the separation membrane 230, converges to the hollow rotating shaft 240, and is discharged through the second end of the hollow rotating shaft 240, specifically, the mother liquor clear liquid can be discharged to the mother liquor tank 300 through the buffer tank 290. Preferably, the separation membranes 230 are uniformly spaced along the axial direction of the hollow rotating shaft 240, so as to improve the mixed flow effect.
In practical application, the separation membrane 230 on the hollow rotating shaft 240 is in the shape of a hollow disc, the membrane aperture on the separation membrane 230 is 1 nm-50 μm, and the diameter of the separation membrane 230 is 50-5000 mm. The hollow rotating shaft 240 is in a hollow cylindrical structure, the outer diameter of the hollow rotating shaft 240 is 10-500 mm, and the wall thickness is 2-25 mm. The hollow rotating shaft 240 and the reaction kettle shell 220 are sealed by a mechanical sealing device, and the driving element 210 and the hollow rotating shaft 240 realize rotary rotation through shaft transmission, belt transmission or gear transmission.
In combination with the above, the integrated reaction and separation system of the invention can work in a closed and positive pressure environment, thereby avoiding the mutual contact between the reaction system and the external air environment, influencing the reaction system, polluting the environment and improving the reliability.
In order to improve the applicability of the system, as shown in fig. 2, a washing device 80 is connected to the reaction kettle 200 for washing the separated solid material. Through the integration of washing, batch or semi-batch semi-continuous or continuous production can be realized, and the production efficiency is improved. The method is suitable for the occasions that reactants or products of liquid-solid, liquid-solid, gas-liquid-solid and other multiphase reactions are fine particles. Wherein the washing device 80 includes a water supply tank 800 for supplying a washing medium, the water supply tank 800 being connected to the liquid distributor 260 through a liquid supply valve 820.
Preferably, the washing apparatus 80 further comprises a cleaning conduit with a cleaning fluid flow valve 822, the cleaning conduit being connected to the liquid distributor 260; the bottom of the reaction kettle 200 is further provided with a drain 285 for discharging the waste liquid and the residual mother liquid after cleaning.
As a further preferred embodiment, a water replenishing pipeline with a water replenishing valve 810 is provided on the water supply tank 800; the water supply tank 800 is connected to the liquid distributor 260 through a water washing pump 830 and a water washing pump outlet check valve 831 via a liquid supply valve 820 for controlling the flow of the washing medium entering the liquid distributor 260.
The water supply tank 800 is further provided with a heat source pipe having a water supply tank heat source flow valve 821, and a temperature sensor 811, and the temperature sensor 811 is electrically connected to the water supply tank heat source flow valve 821 to adjust the temperature of the washing medium, such as pure water, in the water supply tank 800 according to the measured temperature value in accordance with the process requirement. Generally, the washing temperature is controlled to be 0-150 ℃. According to this embodiment, the washing apparatus 80 may be used to wash the product in the reaction kettle 200 to obtain a qualified material. In the reaction gap, cleaning liquid can be added through the cleaning pipeline to clean the separation assembly, and the cleaned waste liquid is discharged through the exhaust port 285. In addition, after cleaning, a washing medium such as pure water can be used for washing again, and pollution of residual cleaning liquid to products is avoided. Thereby further ensuring the quality of the slurry product collected by the reaction.
In order to further facilitate the discharge, the discharge opening is funnel-shaped. Wherein, the product is discharged to the qualified material storage tank 400 at the discharge outlet by controlling the opening of the discharge valve 282, and enters the subsequent process through the discharge valve 410 of the qualified material tank.
Furthermore, a flow disturbing element 250 is also arranged in the reaction kettle 200; the cross section of the turbulent flow element 250 is comb-shaped, and a plurality of comb teeth uniformly distributed at intervals are inserted into the interval area of the adjacent separation membrane 230 at intervals to further form a turbulent flow effect. In addition, the flow perturbation element 250 may employ a mechanical flow perturbation comb or a flow perturbation by air difference or a jet flow perturbation. Under the combined action of the rotation of the separation membrane 230 and the turbulence element 250, the solid particles are uniformly suspended, the saturation in the reaction system is uniform all the time, the solid particles grow uniformly, the uniformity of the particle size of the solid particles generated by the reaction is better, and the method is suitable for the production of particles with different particle size grades.
As another preferred embodiment, the feeding device 10 includes a raw material storage unit 100, the raw material storage unit 100 is connected to the liquid distributor 260 through a feeding pipe with a feeding pump 120 and a feeding valve 110; and the liquid distributor 260 is arranged along the axial direction of the kettle wall parallel to the hollow rotating shaft 240, as shown in fig. 1, so that the reaction raw materials can be fully and uniformly distributed on each separation membrane 230, and the sufficiency of reaction and solid-liquid separation is improved. In order to ensure the uniformity of the feeding process, a plurality of raw material feeding holes are formed on the reaction kettle 200 for the feeding device 10, and are symmetrically and uniformly distributed along the reaction kettle 200 and are respectively communicated with the liquid distributor 260 in the kettle. In addition, the raw material storage unit 100 may include a plurality according to the kind of raw material required for an actual reaction, and each communicates with the liquid distributor 260 through the feed port.
As a preferred further embodiment, a back washing device 70 is further connected to the reaction vessel 200, the back washing device 70 comprises a back washing pipeline with a back washing valve 710, the back washing pipeline is connected to a back washing tank 700, and the bottom of the back washing tank 700 is further communicated with the second end of the hollow rotating shaft 240 to receive a part of the separated mother liquor clear liquid and washing waste liquid as a back washing liquid.
According to the embodiment, the back washing device 70 can regenerate the separation components in the integrated reaction and separation device 20 according to actual requirements, and meanwhile, the reaction efficiency and the product quality are effectively improved. Specifically, the back-flushing device 70 may utilize the mother liquor clear liquid or the washing waste liquid generated by the reaction and discharged after the dynamic separation, and under the pushing of the back-flushing gas, permeate from the inner side of the separation membrane 230 to the outer surface of the separation membrane through the hollow rotating shaft 240, and remove the sediment on the surface of the separation membrane 230 through the back-flushing; back flushing of reaction vessel 200 is achieved and membrane flux of separation membrane 230 is restored.
As a preferred further embodiment, the upper portion of the backflushing tank 700 is further communicated with a heat exchange unit 900, the downstream of the heat exchange unit 900 is sequentially connected with a washing waste liquid tank 500 and a multistage membrane separation unit 600, the multistage membrane separation unit 600 adopts a nanofiltration membrane and/or a reverse osmosis membrane for treating and recycling the washed washing waste liquid, the multistage membrane separation unit 600 is provided with a concentrated liquid outlet and a clear liquid outlet, the clear liquid outlet is circularly connected to the water supply tank 800, the clear liquid is recycled as washing make-up water, the water consumption is effectively reduced, and the concentrated liquid enters a recovery system for treatment.
In the above embodiment, the second end of the hollow rotating shaft 240 in the axial direction is respectively connected to the backflushing tank 700 and the mother liquor tank 300 through the buffer tank 290; and a clear liquid viewing mirror 270 is arranged on a connecting pipeline of the buffer tank 290, the backflushing tank 700 and the mother liquor tank 300. Thereby facilitating observation of the clarity of the mother liquor supernatant discharged from the reaction tank 200. So as to find and observe the reaction condition in time and make switching adjustment of corresponding procedures in due time. Further, a mother liquor discharge flow valve 310 is provided on a pipe between the buffer tank 290 and the mother liquor tank 300 for adjusting a mother liquor discharge amount. The mother liquor tank 300 discharges the reaction mother liquor to the next treatment process through a mother liquor tank discharge valve 320.
In practical applications, the outlet of the heat exchange unit 900 is connected to the washing waste liquid tank 500 through a washing waste liquid discharge pipe with a washing waste liquid discharge valve 520. The heat exchange unit 900 can effectively reduce the temperature of the washing waste liquid through the heat exchange medium, thereby ensuring that the subsequent multistage membrane separation unit 600 works at a lower temperature and prolonging the service life of the membrane element.
In view of the above, accessible washing device 80 washes the interior material of reation kettle 200, the washing waste liquid that obtains can combine the technology condition to carry out recycle with the demand, for example, when waiting the solid material in the reation kettle to satisfy the materialization characteristic, close reation kettle 200's charge-in pump 120 and feed valve 110, stop the feeding to reation kettle 200, the rotational speed of control cavity pivot 240, if reduce or stop rotating, reduce the scouring action of cross-flow to separation membrane 230, make the solid material form the filter cake gradually on separation membrane 230's membrane surface, after residual mother liquor discharges through arranging exhaust opening 285, begin the washing process to the filter cake through washing device 80, it is specific: starting a water washing pump 830 at the outlet of the water supply tank 800, opening a liquid supply valve 820, controlling a certain washing temperature, pressure and washing flow, slowly rotating the hollow rotating shaft 240 at the initial stage of washing, gradually returning to a normal rotating speed after filter cakes form slurry, allowing a washing medium such as pure water to permeate from the surface of the separation membrane 230 and converge into the cavity of the hollow rotating shaft 240 under the driving of pressure, discharging from the second end, allowing the washing medium to enter a heat exchange unit 900 through a buffer tank 290 and a backflushing tank 700, storing into a washing waste liquid tank 500 after heat exchange and cooling, washing until the impurity content of a product in the sampling detection reaction kettle is qualified, discharging the slurry to a qualified product storage tank 400, and discharging to subsequent processes through a qualified material discharge valve 410; the reaction kettle 200 enters the next batch of production after being back-flushed; the washing waste liquid generated in the washing process passes through the multistage membrane separation unit 600 under the pressurization effect of the booster pump 510, the separated clear liquid flows back to the water supply tank 800 through the membrane separation clear liquid valve 610 for recycling, and the concentrated liquid enters the recovery system through the membrane separation concentrated liquid valve 620. Wherein the multi-stage membrane separation unit 600 is of the nanofiltration and/or reverse osmosis type; the clear solution recovery rate of the multi-stage membrane separation unit 600 is not less than 70%.
In addition, a reaction kettle heat source flow valve 280 is arranged on the reaction kettle 200 and used for adjusting the temperature of a system in the reaction kettle; the reaction kettle 200 is further provided with an exhaust port, and the exhaust port is connected with an exhaust pipeline with an exhaust flow valve 281 so as to adjust the pressure in the reaction kettle 200. A pressure gauge 283 is also arranged on the reaction kettle 200 and used for monitoring the operation pressure in the reaction kettle 200.
In the above embodiment, the reaction vessel 200 may be of a horizontal type or a vertical type. The heating mode of the reaction kettle 200 can be a clamp sleeve or a pipe type, and the heating medium is heat conduction oil or saturated steam.
It should be noted that the washing medium in the water supply tank 800 may be pure water, alkali solution, alcohol, etc. according to different requirements of washing the reaction materials, and the number of the water supply tanks 800 may be set to be plural according to different requirements of the washing sequence.
According to another embodiment of the present invention, shown in fig. 1, an integrated reaction and separation process comprises the following steps:
s1, continuously metering reaction raw materials into a reaction kettle 200 of the integrated reaction and separation device 20, controlling the pressure in the reaction kettle 200 by adjusting the feed flow, and separating mother liquor clear liquid and solid materials from the reacted materials by a separation component while the reaction raw materials react in the kettle;
s2, stopping feeding the reaction kettle 200 when the solid materials in the reaction kettle meet the physicochemical characteristics, and obtaining a slurry product in the reaction kettle 200.
In step S2, when a washing process is provided, as shown in fig. 2, the specific steps further include:
s3, adding a washing medium into the reaction kettle 200 through the washing device 80, washing the slurry in the reaction kettle 200 by the washing medium under the driving of pressure, and storing the generated washing waste liquid into the washing waste liquid tank 500; and storing the qualified slurry product washed in the reaction kettle 200 into a qualified product storage tank 400 through a discharge valve.
Alternatively, in step S2, when the washing process is not performed and the solid content in the reaction kettle 200 is continuously increased to a predetermined value, the mother liquor is discharged to the mother liquor tank 300, and the solid material is discharged to the product storage tank through the discharge valve 282 and enters the subsequent processing process.
Specifically, the integrated reaction and separation process comprises the following steps:
in step S1: reaction raw materials are continuously metered into a reaction kettle 200 of the integrated reaction and separation device, the pressure in the reaction kettle 200 is controlled through a feed valve 110 of the integrated device, the reaction raw materials react in the kettle, a first end of a hollow rotating shaft 240 in the middle of the reaction kettle 200 in a separation assembly is driven to rotate, separation membranes 230 which are arranged on the hollow rotating shaft at intervals and are communicated with each other are driven to rotate, mother liquor clear liquid generated by reaction is driven by the pressure to permeate from the surfaces of the separation membranes 230 to converge into a cavity of the hollow rotating shaft 240 and is discharged through a second end of the hollow rotating shaft, and solid particles generated by the reaction are intercepted on the surfaces of the separation membranes 230; moreover, the solid particles generated in the reaction kettle are uniformly suspended and distributed in the reaction kettle under the combined action of the rotation of the separation membrane 230 and the turbulence element 250; wherein, the reaction slurry forms cross flow among the separation membranes 230, which prevents the deposition of the solid generated by the reaction on the membrane surface, and the membrane surface is always smooth without filter cake, thus ensuring the membrane to have stable high-definition liquid flux;
in step S3: the slurry is concentrated by controlling the rotating speed of the separation assembly, so that solid materials gradually form a filter cake on the surface of a membrane of the separation assembly; discharging residual mother liquor, and starting a washing process for a filter cake; starting a water washing pump 830 at the outlet of a water supply tank 800 in the washing device 80, slowly rotating the hollow rotating shaft 240 at the initial stage of washing until a filter cake forms slurry, then recovering to a normal rotation speed, permeating washing water such as pure water from the surface of the separation membrane 230 under the driving of pressure, converging the washing water to the hollow rotating shaft 240, completing the washing of the slurry, discharging the washing water through the second end of the hollow rotating shaft 240, cooling the washing water through a heat exchange unit 900, and storing the washing water to the washing waste liquid tank 500; wherein, for the slurry product in the reaction kettle 200, after sampling and detecting that the impurity content in the product is qualified, the slurry is discharged to a qualified product storage tank 400; washing waste liquid generated in the washing process is subjected to pressurization by a booster pump 510 and is separated by a nanofiltration membrane and/or a reverse osmosis membrane of the multistage membrane separation unit 600, clear liquid flows back to the water supply tank 800 for recycling, and concentrated liquid enters a recovery system.
According to the embodiment, the reaction raw materials are subjected to integrated treatment of reaction and dynamic separation in the integrated reaction and separation device, the integration level of the whole process is high, and the overall production efficiency is improved. And the economic benefit is improved by integrating the washing process and the treatment and recycling of the washing waste liquid.
In addition, in step S1, the reaction solution fills the integrated reaction and separation device (or the exhaust amount of the gas outlet and the pressure in the reaction vessel when the integrated reaction and separation system is turned on so that the liquid level in the reaction vessel is kept at a suitable position when the reaction is normally performed), and the opening of the mother solution discharge valve 310 is adjusted and controlled so that the mother solution discharge amount is adapted to the actual capacity of the device. The residence time of the slurry in the device is controlled by adjusting the discharge flow of the mother liquor according to the reaction rate or crystallization rate of different products. When the specified conversion rate or physicochemical characteristic index of the solid product is reached, the reaction is complete. The invention can also be provided with an inlet-outlet pressure difference alarm device on the reaction kettle 200, which comprises a pressure gauge 283 and an alarm arranged on the reaction kettle 200, so as to monitor the blockage condition of the solid material on the separation membrane 230.
Preferably, in the reaction, separation and washing processes in steps S1-S3, under the condition that the operating pressure difference (i.e. pressure) in the reaction kettle 200 is kept unchanged, when the flux of the mother liquor clear liquid discharged in the reaction process is reduced or the flow of the washing waste liquid in the washing process is reduced to 80% of the initial state when the flow of the washing waste liquid flowing into the washing waste liquid tank 500 is reduced, or when the pressure difference in the reaction kettle 200 exceeds a limit value, the reaction kettle 200 is back-flushed by introducing a back-flushing gas, wherein the back-flushing process is as follows:
the clear liquid discharged from the hollow rotating shaft 240 enters the backflushing tank 700 through the buffer tank 290, the clear liquid in the backflushing tank 700 permeates from the membrane side of the separation membrane 230 to the membrane surface through the hollow rotating shaft 240 under the push of the backflushing air pressure, and the sediment on the surface of the separation membrane 230 is removed through backflushing. Wherein, the clear liquid flux decline can be observed by a clear liquid viewing mirror 270; the pressure difference exceeding the limit value can be monitored by an inlet-outlet pressure difference alarm device arranged on the reaction kettle 200.
After step S3, the reaction vessel 200 is subjected to back washing and then repeatedly put into reaction. The back washing step is the same as the above process.
Further, when the system runs for a long time and the clear liquid flux is not completely recovered by backwashing, the system equipment materials are periodically drained, cleaning liquid is added through a cleaning pipeline for cleaning, and the cleaned waste liquid is discharged from the drain opening 285; and, after the cleaning is finished, the cleaning medium such as pure water in the water supply tank 800 is used for washing, so that the pollution of the residual cleaning liquid to the product is avoided.
In the reaction process, in order to further improve the production quality and efficiency of the product, the total feed flow of the reaction raw materials is controlled to be 0-5000L/h; the revolution number of the hollow rotating shaft is 0-1500 r/min; controlling the solid content in the reaction kettle to be 0-70%; the reaction pH is 0-14; the reaction temperature is 0-150 ℃; the operating pressure in the reaction kettle is 0-5 bar; the reaction time is 0-200 h.
The reaction system and the process provided by the embodiment of the invention can be applied to the reaction of generating a solid product by a liquid phase method or the fluidized bed reaction of a powder catalyst. Specific application examples are provided below:
application example 1 recovery of oximation catalyst in caprolactam production Process
At present, the titanium silicalite molecular sieve is used for catalyzing cyclohexanone ammoximation to prepare cyclohexanone oxime in China.
Reaction and dynamic separation process
By using the integrated reaction and separation system shown in fig. 1, the tert-butyl alcohol, the ammonia gas and the catalyst respectively enter the liquid distributor 260 from different feed inlets through the feeding mechanism 10, and react in the reaction kettle 200, the concentration of the catalyst is 3 wt%, after the reaction is completed, the reaction liquid containing the catalyst is separated by the separation membrane 230 inside the reaction kettle 200, the clear mother liquor enters the mother liquor tank 300 through the mother liquor discharge valve 310, and the cyclohexanone oxime is obtained through the subsequent process, thereby producing caprolactam. The catalyst is retained in the reaction kettle 200 to continue the reaction until the activity of the catalyst is reduced to the level required for regeneration, the feeding is stopped, and the catalyst required for regeneration is discharged through a discharge valve 282 of the reaction kettle and enters the subsequent treatment process.
Backwash and cleaning recovery process
Under the condition that the operation pressure difference in the reaction kettle 200 is kept unchanged, when the flow rate of mother liquor clear liquid flowing into the mother liquor tank 300 in the reaction process is reduced to 80% of that in the initial state, a back flushing process needs to be carried out, the mother liquor discharge valve 310 is closed, the back flushing valve 510 is opened, the back flushing gas gauge pressure is controlled to be 0.1MPa, the clear liquid in the buffer tank 500 enters the reaction kettle 200 under the action of the back flushing gas pressure, back flushing is carried out on catalyst powder on the surface of the separation membrane, the back flushing time lasts for 30 seconds each time, and the flux of the separation membrane returns to the initial state by more than 90% after back flushing; the pollution and blockage conditions of the membrane are regularly checked in the production gap, a special cleaning solution is required to clean the separation membrane in time, and the membrane flux is recovered. And (3) opening a cleaning liquid flow valve 822, enabling cleaning liquid to enter the reaction kettle 200 from the raw material inlet, opening a stirring motor serving as a driving element 210 to clean the separation membrane 230 in the reaction kettle, and enabling the cleaned waste liquid to enter a sewage discharge pipeline through a drain outlet 285.
Application example 2 reaction, dynamic separation and washing of ternary Material precursors
Reaction and dynamic separation process
By using the integrated reaction and separation system of fig. 2, the reaction raw materials (the sulfate mixed solution, the alkali solution, and the ammonia solution) in the reaction raw material storage unit 100 continuously and stably enter the reaction kettle 200 through the feed pump 120, and the inlet positions of the sulfate mixed solution, the alkali solution, and the ammonia solution are symmetrically distributed and uniformly distributed in the reaction kettle 200 through the liquid distributor 260. The driving element 210 is turned on, the reaction raw material reacts in the reaction kettle 200 to generate a mother liquor containing solid substances, the solid-liquid separation is performed through the separation membrane 230, and the separated mother liquor clear liquor is discharged from the second end of the idle shaft 240, and is discharged to the mother liquor tank 300 and the backflushing tank 700 through the buffer tank 290.
Wherein: according to the design productivity of the device, the total flow of the sulfate mixed solution, the alkali solution and the ammonia water solution is 400L/h; the number of revolutions of the hollow rotary shaft 240 and the separation membrane 230 was controlled to 350r/min by setting the operating frequency of the stirring motor as the driving element 210, the reaction temperature in the reaction vessel 200 was controlled by the reaction vessel heat source flow valve 280, and the reaction temperature was constantly maintained at 60 + -1 deg.C. The absolute pressure in the reaction kettle 200 is controlled by adjusting the feed valve 110, the mother liquor discharge flow valve 310 is adjusted, the pressure difference between the inlet and the outlet of the reaction kettle 200 is controlled to be 0.2Mpa, and the mother liquor clear liquid discharge flow is automatically maintained to be equal to the total feed flow of the reaction kettle because the reaction kettle 200 is filled with liquid and the liquid is incompressible.
Washing and multistage membrane separation process
When the particle size of the solid material in the reaction kettle 200 meets the requirement, the reaction is finished, the reaction raw material feeding pump 120 is stopped, the feeding valve 110 and the mother liquid discharge flow valve 310 are closed, the rotating speeds of the hollow rotating shaft 240 and the separation membrane 230 are reduced until the rotation is stopped, the solid material forms a filter cake on the surface of the membrane, and the residual mother liquid is discharged; the liquid supply valve 820 and the washing waste liquid discharge valve 520 of the water supply tank 800 are opened, the washing pump 830 is started, and the washing process starts;
by controlling the heat source flow valve 821 of the water supply tank, keeping the temperature of the pure water in the water supply tank 800 at 75 ℃, the hot water enters the reaction kettle 200 from the feeding pipeline under the action of the washing pump 830 and is uniformly distributed by the fluid distributor 260 in the kettle, at the same time, the hollow rotating shaft 240 slowly rotates to filter cakes to form slurry at the initial stage of washing, then the normal rotating speed is recovered, the pure water permeates and converges to the hollow rotating shaft 240 from the surface of the separation membrane 230 under the driving of pressure to complete the washing of the slurry, the formed washing waste liquid is discharged from the second end of the hollow rotating shaft 240, sequentially flows through the clear liquid viewing mirror 270 and the backflushing tank 700 along the pipeline, is subjected to heat exchange by the heat exchanger serving as the heat exchange unit 900 and is cooled to 45 ℃ and then enters the washing waste liquid tank 500, when the liquid level in the washing waste tank 500 reaches the upper limit value, the booster pump 510 is started, the washing waste liquid is separated by the multistage membrane separation unit 600 to obtain clear liquid which is refluxed to the water supply tank 800, concentrated solution obtained after membrane separation is discharged to subsequent processes through a membrane separation concentrated solution valve 620 for recovery treatment, and the water recovery rate of the multistage membrane separation unit 600 is not lower than 70%; and (3) adding a washing medium such as pure water according to the liquid level control water supplementing valve 810 in the water supply tank 800 to ensure the balance of the washing process, and when the impurity content of the product in the reaction kettle is detected to be qualified by sampling, closing the liquid supply valve 820 and the washing waste liquid discharge valve 520 of the water supply tank 800, and stopping the washing pump 830. At this time, the discharge valve 282 of the reaction vessel is opened, and the washed acceptable product is discharged to the acceptable material storage tank 400.
Backwash and cleaning recovery process
Under the condition that the operation pressure difference in the reaction kettle 200 is kept unchanged, when the flow rate of mother liquor clear liquid flowing into the mother liquor tank 300 in the reaction process or washing waste liquid flowing into the washing waste liquid tank 500 in the washing process is reduced to 80% of that in the initial state, the mother liquor discharge valve 310 and the washing waste liquid discharge valve 520 are closed, the backflushing valve 710 is opened, the backflushing gas gauge pressure is controlled to be 0.1MPa, clear liquid in the backflushing tank 700 enters the separation membrane 230 through the second end of the hollow rotating shaft 240 under the action of the backflushing gas pressure, the backflushing time lasts 30 seconds each time, and the membrane flux returns to the original state by more than 95% after backflushing; the pollution blockage condition of the separation membrane 230 is periodically checked in a production gap, specifically, the pollution blockage condition can be checked according to the attenuation condition of the clear liquid flux and the pressure difference value in the reaction kettle, and the separation membrane needs to be cleaned by special cleaning liquid in time to recover the membrane flux. The cleaning liquid inlet flow control valve 822 is opened, the cleaning liquid enters the reaction kettle 200 from the raw material inlet, the driving element 210 is opened to rotationally clean the separation membrane 230 in the reaction kettle, and the cleaned waste liquid enters the sewage discharge pipeline through the exhaust port 285.
It should be noted that the above embodiments can be freely combined as necessary. The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (18)
1. An integrated reaction and separation system, comprising:
the feeding device is used for storing and conveying reaction raw materials;
an integrated reaction and separation device comprising a reaction vessel connected downstream of the feed device; the reaction kettle is provided with at least one group of separation assemblies for dynamic separation of solid and liquid phases during raw material reaction, each separation assembly comprises a hollow rotating shaft penetrating through the middle of the reaction kettle shell, a plurality of hollow separation membranes are arranged on the hollow rotating shaft at intervals, cavities of the hollow rotating shafts are communicated with inner cavities of the separation membranes, the hollow rotating shafts are connected with a driving element along the axial first ends, and the second ends are used for outputting mother liquor clear liquid after separation.
2. The integrated reaction and separation system of claim 1, wherein:
a liquid distributor is arranged in the reaction kettle in parallel with the hollow rotating shaft and is communicated with the feeding device;
and a discharge outlet is formed in the reaction kettle and positioned at the bottom of the separation membrane.
3. The integrated reaction and separation system of claim 2, wherein:
the separation membrane is of a hollow disc-shaped structure, and the membrane aperture of the separation membrane is 1 nm-50 microns;
and/or;
the separation membrane is of a circular structure, and the diameter of the separation membrane is 50-5000 mm.
4. The integrated reaction and separation system of claim 1, wherein:
the reaction kettle is connected with a washing device, the washing device comprises a water supply tank for supplying washing media, and the water supply tank is connected to the reaction kettle through a liquid supply valve and used for washing the solid materials after reaction and separation.
5. The integrated reaction and separation system of claim 4, wherein:
washing waste liquid jar and multistage membrane separation unit are connected gradually to reation kettle's low reaches, multistage membrane separation unit adopts and receives filter membrane and/or reverse osmosis membrane for wash waste liquid after the washing separates, multistage membrane separation unit is equipped with dense liquid export and clear liquid export, clear liquid export cyclic connection to feed tank.
6. The integrated reaction and separation system of claim 5, wherein:
the washing device also comprises a cleaning pipeline with a cleaning liquid flow valve, and the cleaning pipeline is connected to the reaction kettle; the bottom of the reaction kettle is also provided with a discharge port for discharging the cleaned waste liquid and the residual mother liquid, and the front end of the washing waste liquid tank is communicated with the heat exchange unit for reducing the temperature of the washing waste liquid.
7. The integrated reaction and separation system of claim 1, wherein:
a turbulence element is also arranged in the reaction kettle;
the cross section of the turbulence element is comb-shaped, and a plurality of comb teeth which are uniformly distributed at intervals are inserted into the interval area of the adjacent separation membranes at intervals.
8. The integrated reaction and separation system of claim 1, wherein:
the reaction kettle is further connected with a back washing device, the back washing device comprises a back washing pipeline with a back washing valve, the back washing pipeline is connected to a back washing tank, and the bottom of the back washing tank is further communicated with the second end of the hollow rotating shaft.
9. The integrated reaction and separation system of claim 8, wherein:
the second end of the hollow rotating shaft along the axial direction is respectively connected to the backflushing tank and the mother liquor tank through a buffer tank; and a clear liquid viewing mirror is arranged on a connecting pipeline of the buffer tank, the backflushing tank and the mother liquid tank.
10. The integrated reaction and separation system of claim 4, wherein:
the water supply tank is provided with a water supply tank heat source flow valve and a temperature sensor for adjusting the temperature of the washing medium in the water supply tank;
and/or;
the reaction kettle is provided with a reaction kettle heat source flow valve for adjusting the temperature of a system in the reaction kettle; an exhaust pipeline with an exhaust flow valve is also arranged on the reaction kettle; the reaction kettle is also provided with a pressure gauge for monitoring the operating pressure in the reaction kettle.
11. An integrated reaction and separation process is characterized by comprising the following steps:
s1, continuously metering reaction raw materials into a reaction kettle of the integrated reaction and separation device, controlling the pressure in the reaction kettle by adjusting the feed flow, and separating mother liquor clear liquid and solid materials from the reacted materials by a separation component while the reaction raw materials react in the kettle;
and S2, stopping feeding the reaction kettle when the solid materials in the reaction kettle meet the physicochemical characteristics, and obtaining a slurry product in the reaction kettle.
12. The integrated reaction and separation process of claim 11, further comprising the steps of:
s3, adding a washing medium into the reaction kettle through a washing device, washing the slurry in the reaction kettle by the washing medium under the driving of pressure, and storing the generated washing waste liquid into a washing waste liquid tank; and storing the qualified slurry product washed in the reaction kettle into a qualified product storage tank through a discharge valve.
13. The integrated reaction and separation process of claim 12, wherein step S3 comprises a concentration step of the slurry product before washing, wherein the slurry concentration step is performed by controlling the rotation speed of the separation module, so that the solid material forms a filter cake on the membrane surface of the separation module; the residual mother liquor was drained and the washing process was started for the solid particles.
14. The integrated reaction and separation process of claim 11, wherein:
in the step S1, when the reaction raw materials react in the kettle, a first end of a hollow rotating shaft in the separation assembly, which is positioned in the middle of the reaction kettle, is driven to rotate, separation membranes which are arranged on the hollow rotating shaft at intervals and are communicated with each other are driven to rotate, mother liquor clear liquid generated by the reaction permeates from the surfaces of the separation membranes to converge into a cavity of the hollow rotating shaft under the drive of pressure and is discharged through a second end of the hollow rotating shaft, and solid particles in a reaction system are intercepted on the surfaces of the separation membranes; and the solid particles in the reaction kettle are uniformly suspended and distributed in the reaction kettle under the combined action of the rotation of the separation membrane and the turbulence element.
15. The integrated reaction and separation process of claim 12, wherein:
in step S3, a washing pump at an outlet of a water supply tank in the washing device is turned on, and at the same time, the rotation speed of the hollow rotating shaft is controlled, and a washing medium permeates and converges from the surface of the separation membrane to the hollow rotating shaft under the driving of pressure, so that the washing of the slurry is completed, and the slurry is discharged from the second end of the hollow rotating shaft, cooled by the heat exchange unit, and then stored in a washing waste liquid tank; wherein, for slurry products in the reaction kettle, after sampling and detecting that the impurity content in the products is qualified, the slurry is discharged to a qualified product storage tank; and after the washing waste liquid in the washing waste liquid tank is separated by a nanofiltration membrane and/or a reverse osmosis membrane of the multistage membrane separation unit, clear liquid flows back to the water supply tank for recycling.
16. The integrated reaction and separation process of claim 14, wherein step S2 comprises: when the solid content in the reaction kettle is continuously increased to a specified value, mother liquor clear liquid is discharged to a mother liquor tank, and solid materials are discharged to a product storage tank through a discharge valve and enter a subsequent treatment process.
17. The integrated reaction and separation process of claim 14, 15 or 16,
back flushing the reaction kettle according to the requirement; the back washing process comprises the following steps: mother liquor clear liquid or washing waste liquid discharged from the hollow rotating shaft enters a backflushing tank through a buffer tank, the mother liquor clear liquid or the washing waste liquid in the backflushing tank permeates from the membrane side to the membrane surface of the separation membrane through the hollow rotating shaft under the push of backflushing air pressure, and sediments on the surface of the separation membrane are removed through backflushing;
and/or;
cleaning liquid is added into the reaction kettle through a cleaning pipeline according to needs to clean the reaction kettle, and the waste liquid after cleaning is discharged from a discharge port; after cleaning, washing by using a washing medium in a water supply tank;
and/or;
controlling the revolution of the hollow rotating shaft to be 0-1500 r/min; the operating pressure in the reaction kettle is 0-5 bar.
18. The application of the integrated reaction and separation system is characterized in that the integrated reaction and separation system is used for the reaction of generating a solid product by a liquid phase method or the fluidized bed reaction of a powder catalyst.
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| Publication number | Priority date | Publication date | Assignee | Title |
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Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3401607A1 (en) * | 1983-01-19 | 1984-07-19 | Politechnika Warszawska, Warszawa | Dynamic filter |
| US5254250A (en) * | 1991-05-30 | 1993-10-19 | Membrex, Inc. | Rotary filtration device and filter pack therefor |
| US6419835B1 (en) * | 1998-06-25 | 2002-07-16 | Outokumpu Oyj | Method for producing a filter cake |
| WO2002085492A1 (en) * | 2001-04-23 | 2002-10-31 | Baker Hughes Incorporated | Rotatable disc filters with shower systems and methods of use |
| CN1590316A (en) * | 2003-09-05 | 2005-03-09 | 中国科学技术大学 | Biological rotary disk device having filtration cavity |
| CN102703712A (en) * | 2012-06-29 | 2012-10-03 | 阳光凯迪新能源集团有限公司 | Combined filtration process for recovering noble metal catalyst from fischer-tropsch synthesis products |
| CN102728123A (en) * | 2012-06-29 | 2012-10-17 | 阳光凯迪新能源集团有限公司 | High-efficiency dynamic slurry separation filtering apparatus and filtering method thereof |
| CN103041705A (en) * | 2012-12-29 | 2013-04-17 | 上海安赐机械设备有限公司 | Device and method for coupling catalyst recovery process with dynamic disc membrane separation process |
| CN203075844U (en) * | 2012-12-29 | 2013-07-24 | 上海安赐机械设备有限公司 | Dynamic disc film device applied to recovery of superfine solid catalyst |
| CN104592036A (en) * | 2014-12-24 | 2015-05-06 | 上海安赐机械设备有限公司 | Nitrobenzene/dinitrobenzene catalyst recovery device and recovery method thereof |
| CN107213800A (en) * | 2017-07-10 | 2017-09-29 | 上海闰铭精密技术有限公司 | A kind of novel cross flow rotary ceramic membranous system |
| CN107570011A (en) * | 2017-09-26 | 2018-01-12 | 上海安赐环保科技股份有限公司 | A kind of ultrafiltration apparatus and its technique that slurry oil is thrown away applied to catalytic cracking process |
| CN110947219A (en) * | 2019-12-27 | 2020-04-03 | 湖南邦普循环科技有限公司 | Device and method for recycling materials in ternary precursor washing wastewater and recycling wastewater |
| CN113750946A (en) * | 2021-10-22 | 2021-12-07 | 上海安赐环保科技股份有限公司 | Reaction for preparing battery anode material precursor and purification system and process thereof |
| CN113856476A (en) * | 2021-10-22 | 2021-12-31 | 上海安赐环保科技股份有限公司 | Dynamic disc membrane washing system and process |
| CN216419373U (en) * | 2021-10-22 | 2022-05-03 | 上海安赐环保科技股份有限公司 | Integrated reaction and separation system |
-
2021
- 2021-10-22 CN CN202111235224.7A patent/CN113813908B/en active Active
Patent Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3401607A1 (en) * | 1983-01-19 | 1984-07-19 | Politechnika Warszawska, Warszawa | Dynamic filter |
| US5254250A (en) * | 1991-05-30 | 1993-10-19 | Membrex, Inc. | Rotary filtration device and filter pack therefor |
| US6419835B1 (en) * | 1998-06-25 | 2002-07-16 | Outokumpu Oyj | Method for producing a filter cake |
| WO2002085492A1 (en) * | 2001-04-23 | 2002-10-31 | Baker Hughes Incorporated | Rotatable disc filters with shower systems and methods of use |
| CN1590316A (en) * | 2003-09-05 | 2005-03-09 | 中国科学技术大学 | Biological rotary disk device having filtration cavity |
| CN102703712A (en) * | 2012-06-29 | 2012-10-03 | 阳光凯迪新能源集团有限公司 | Combined filtration process for recovering noble metal catalyst from fischer-tropsch synthesis products |
| CN102728123A (en) * | 2012-06-29 | 2012-10-17 | 阳光凯迪新能源集团有限公司 | High-efficiency dynamic slurry separation filtering apparatus and filtering method thereof |
| CN103041705A (en) * | 2012-12-29 | 2013-04-17 | 上海安赐机械设备有限公司 | Device and method for coupling catalyst recovery process with dynamic disc membrane separation process |
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| CN115155495A (en) * | 2022-07-14 | 2022-10-11 | 洛阳中硅高科技有限公司 | Preparation system and preparation method |
| CN115155495B (en) * | 2022-07-14 | 2024-03-19 | 洛阳中硅高科技有限公司 | Preparation system and preparation method |
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