CN113813908B - Integrated reaction and separation system, process and application - Google Patents
Integrated reaction and separation system, process and application Download PDFInfo
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- CN113813908B CN113813908B CN202111235224.7A CN202111235224A CN113813908B CN 113813908 B CN113813908 B CN 113813908B CN 202111235224 A CN202111235224 A CN 202111235224A CN 113813908 B CN113813908 B CN 113813908B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01D—SEPARATION
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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Abstract
The invention discloses an integrated reaction and separation system, which comprises: a feeding device for storing and conveying the 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 is connected with a washing device. The separation assembly comprises a hollow rotating shaft which is arranged in the middle of the reaction kettle shell in a penetrating way, a plurality of hollow separation diaphragms are arranged on the hollow rotating shaft at intervals, a cavity of the hollow rotating shaft is communicated with an inner cavity of the separation diaphragms, a first end of the hollow rotating shaft along the axial direction is connected with the driving element, and a second end of the hollow rotating shaft is used for outputting separated mother liquor clear liquid and washing waste liquid; the upper space of the separation membrane in the reaction kettle is also provided with a liquid distributor which is communicated with the feeding device; the bottom is provided with a discharge hole. And simultaneously, the integrated reaction and separation process and application are provided to improve the reaction efficiency and the separation and washing effects.
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 reaction of generating fine suspended solid particles usually involves liquid-solid, gas-liquid-solid and the like, after the reaction process is finished, solid-liquid separation is usually needed to be carried out on materials so as to separate solid particle products from mother liquor, and the solid particles prepared by partial synthesis reaction also need to enter a next treatment section after the mother liquor remained on the surface of the solid particles is removed through a washing process.
In the existing process flow, the reaction, the liquid-solid separation and the product washing are usually carried out in different equipment respectively, wherein a reaction kettle only can provide stirring and meet the necessary process conditions of the reaction, but has no solid-liquid separation function and washing function, an in-vitro separation unit is required to be added to realize the solid-liquid separation and an in-vitro washing unit is required to realize the slurry washing, so that the complexity of the process flow is increased, and the production cost is higher; on the other hand, when the concentrated slurry with high solid content flows back to the reaction kettle, the concentration and the uniform distribution of the particles in the reaction kettle are affected, so that the reaction efficiency is affected, and the consistency of the growth formation of the product particles and the product quality is poor when the reaction process is carried out on the particles. Aiming at the technical defect, in the prior art, the influence on the growth morphology of the reaction kettle product particles is slowed down by reducing the reflux quantity of the concentrated solution of the in-vitro solid-liquid separation unit in the process of synthesizing the 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 extremely easy to form a filter cake in the separation process, reduces flux and separation efficiency, and has the advantages of long process flow, large occupied area and complicated control operation. In the washing process, the problems of material running, uneven washing, environmental protection caused by a large amount of washing wastewater and the like exist in the conventional filter cake washing process such as a plate frame, a centrifugal machine and the like.
Based on this, it is necessary for those skilled in the art to provide an integrated reaction and separation system, process and application, so as to simplify the process flow, improve the reaction efficiency, and improve the separation and washing effects, thereby effectively reducing the production cost under the existing process and effectively solving the environmental emission problem from the source.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide an integrated reaction and separation system, a process and application thereof, so as to simplify the process flow, improve the reaction efficiency, and improve the separation and washing effects, thereby realizing the effective reduction of the production cost under the prior art and the effective solution of the environmental protection emission problem from the source.
The technical scheme provided by the invention is as follows:
an integrated reaction and separation system comprising:
a feeding device for storing and conveying the reaction raw materials;
the integrated reaction and separation device comprises a reaction kettle connected to the downstream of the feeding device; the reaction kettle is internally provided with at least one group of separation components for dynamic separation of solid and liquid phases during raw material reaction, the separation components comprise a hollow rotating shaft which is penetrated in the middle of a reaction kettle shell, a plurality of hollow separation diaphragms are arranged on the hollow rotating shaft at intervals, the cavity of the hollow rotating shaft is communicated with the inner cavity of the separation diaphragms, 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.
Preferably, a liquid distributor is further arranged in the reaction kettle and parallel to the hollow rotating shaft, and the liquid distributor is communicated with the feeding device;
and a discharge hole is arranged at the bottom of the separation membrane in the reaction kettle.
Preferably, the separating membrane is of a hollow disc-shaped structure, the membrane aperture is 1 nm-50 μm, and the diameter of the separating membrane is 50-5000 mm.
Preferably, the reaction kettle is connected with a washing device, 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, the lower stream of the reaction kettle is sequentially connected with a washing waste liquid tank and a multi-stage membrane separation unit, the multi-stage membrane separation unit adopts a nanofiltration membrane and/or a reverse osmosis membrane and is used for separating washing waste liquid after washing, the multi-stage membrane separation unit is provided with a concentrated liquid outlet and a clear liquid outlet, and the clear liquid outlet is circularly connected to a water supply tank.
Further, the washing device further comprises a washing pipeline with a washing liquid flow valve, and the washing pipeline is connected to the liquid distributor; the bottom of the reaction kettle is also provided with a drain port for draining the waste liquid and residual mother liquid after cleaning, and the front end of the washing waste liquid tank is communicated with the heat exchange unit and is used for reducing the temperature of the washing waste liquid.
Furthermore, a turbulent flow element is also arranged in the reaction kettle; the cross section of the turbulence element is in a comb shape, and a plurality of comb teeth which are uniformly distributed at intervals are inserted into the interval areas of the adjacent separation diaphragms.
Further, the feed device comprises a raw material storage unit connected to the liquid distributor through a feed pipe with a feed valve.
Further, the reaction kettle is also connected with a back flushing device, the back flushing device comprises a back flushing pipeline with a back flushing valve, the back flushing pipeline is connected to a back flushing tank, and the bottom of the back flushing tank is also 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 the buffer tank; and a clear liquid viewing mirror is arranged on the connecting pipeline of the buffer tank, the backflushing tank and the mother liquor tank.
Further, 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.
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; and 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 provided, and the integrated reaction and separation process comprises the following steps:
s1, continuously metering the reaction raw materials into a reaction kettle of an integrated reaction and separation device, controlling the pressure in the reaction kettle by adjusting the feeding flow, and separating mother liquor clear liquid and solid materials from the reacted materials by a separation assembly while the reaction raw materials react in the kettle;
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 physical and chemical characteristics of the solid materials in the technical scheme comprise the particle size, tap density, specific surface area and the like of the reaction products, and the catalytic activity of the solid catalyst, and the physical and chemical characteristics adopted by different reaction systems can 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 slurry in the reaction kettle by the washing medium under the drive 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, and slurry concentration is performed by controlling the rotation speed of the separation assembly, so that the solid material gradually forms a filter cake on the surface of the membrane of the separation assembly; the residual mother liquor is discharged and the washing process is started for the solid particles.
Further, the steps are more specifically as follows:
in the step S1, the reaction raw materials react in the kettle, and meanwhile, the first end of a hollow rotating shaft positioned in the middle of the reaction kettle in the separation assembly is driven to rotate, separation diaphragms which are arranged on the hollow rotating shaft at intervals and are mutually communicated are driven to rotate, mother liquor clear liquid generated by the reaction permeates from the surfaces of the separation diaphragms into a cavity of the hollow rotating shaft under the driving of pressure and is discharged through the second end of the hollow rotating shaft, and solid particles in the reaction system are trapped on the surfaces of the separation diaphragms; under the combined action of the rotation of the separating membrane and the turbulence element, solid particles in the reaction kettle are uniformly suspended and distributed in the reaction kettle;
in the step S3, a water washing pump at the outlet of a water supply tank in the washing device is started, the rotating speed of the hollow rotating shaft is controlled, and washing media permeate from the surface of the separation membrane to the hollow rotating shaft under the driving of pressure, after the slurry is washed and discharged from the second end of the hollow rotating shaft, the slurry is cooled by a heat exchange unit and then stored in a washing waste liquid tank; the method comprises the steps of sampling and detecting the qualified impurity content of a slurry product in a reaction kettle, and discharging the slurry to a qualified product storage tank; washing waste liquid in the washing waste liquid tank is separated by nanofiltration membranes and/or reverse osmosis membranes of the multistage membrane separation unit, and 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, the clear liquid of the mother solution is discharged to a mother solution tank, and the solid material is discharged to a product storage tank through a discharge valve and enters the subsequent treatment process.
Preferably, in the process, back flushing is carried out on the reaction kettle according to the requirement; the back flushing process is as follows:
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 washing waste liquid in the backflushing tank is pushed by backflushing air pressure to permeate from the inner side of the membrane of the separation membrane to the surface of the membrane through the hollow rotating shaft, and sediment on the surface of the separation membrane is removed through backflushing.
When the system runs for a long time and the back flushing does not completely recover the clear liquid flux, the materials of the system equipment are drained at regular intervals, cleaning liquid is added into the reaction kettle through a cleaning pipeline to clean the reaction kettle, and the waste liquid after cleaning is drained from the drain; and after the cleaning is finished, the washing 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 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 beneficial effects of the invention are as follows:
(1) The invention can provide a reaction and dynamic separation integrated device and process, which utilizes the separation membrane to perform in-situ reaction and dynamic separation, and ensures high flux of the membrane and low leakage filtering capacity of solid particles. The invention is suitable for occasions of preparing ultrafine powder or preparing the catalyst additive into fine particles by a liquid phase method, can realize the reaction of raw materials of the reaction while separating filtrate, and improves the reaction efficiency and the utilization rate of the catalyst.
(2) The invention also provides a system and a process integrating the reaction, dynamic separation and washing, wherein the solid materials generated by the reaction are uniformly and suspended in the reaction kettle by utilizing the combined action of the rotation of the separation membrane and the turbulent flow element, so that the dynamic 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 especially suitable for occasions of preparing ultrafine powder by a liquid phase method, such as titanium oxide, aluminum oxide, battery anode materials, precursors thereof and the like, and can realize the reaction of reaction raw materials, separation of filtrate, direct washing process after the reaction is completed, and recycling of washing waste liquid after treatment.
(3) The invention integrates the reaction and dynamic separation processes in the integrated reaction and separation device, can integrate the washing process, can react while feeding, dynamically separate while feeding, has high reaction integration level, can ensure that solid particles uniformly grow in situ in the reaction kettle, avoids adverse growth factors caused by external transfer on products, and can regenerate the integrated reaction and separation device according to actual requirements through the back flushing 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. The method 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 productivity, low production cost and the like.
(4) According to the integrated reaction and separation device, the hollow rotating shaft is driven by the driving element to drive the separation membrane to rotate, meanwhile, the stirring effect on materials in the reaction kettle is better, 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 diagram of the integrated reaction and separation system according to an embodiment of the present invention.
FIG. 2 is a schematic diagram of the integrated reaction and separation system according to another embodiment of the present invention.
The meaning of the reference symbols in the figures is as follows:
10-feeding device, 100-reaction raw material storage unit, 110-feeding valve, 120-feeding pump and 121-feeding pump outlet check valve;
20-an integrated reaction and separation device, 200-a reaction kettle, 210-a driving element, 220-a reaction kettle shell, 230-a separation diaphragm, 240-a hollow rotating shaft, 250-a turbulence element, 260-a liquid distributor, 270-a clear liquid sight glass, 280-a reaction kettle heat source flow valve, 281-an exhaust flow valve, 282-a discharge valve, 283-a pressure gauge, 284-a temperature sensor, 285-a drain port and 290-a buffer tank;
300-mother liquor tank, 310-mother liquor discharge valve, 320-mother liquor tank discharge valve;
400-qualified product storage tanks, 410-qualified material discharge valves;
500-washing waste liquid tanks, 510-booster pumps, 511-booster pump outlet check valves and 520-washing waste liquid discharge valves;
600-multistage membrane separation units, 610-membrane separation clear liquid valves, 620-membrane separation concentrate valves;
70-backwashing device, 700-backwashing tank and 710-backwashing valve;
80-washing device, 800-water supply tank, 810-water supplementing 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, 831-water washing pump outlet check valve;
900-heat exchange unit.
Detailed Description
The technical scheme of the present invention will be clearly and completely described in the following in connection with specific embodiments. The following examples are only for more clearly illustrating the technical aspects of the present invention, and are not intended to limit the scope of the present invention.
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 includes: a feeding device 10 for storing and transporting the reaction raw materials;
an integrated reaction and separation device 20, the integrated reaction and separation device 20 comprising a reaction vessel 200 connected downstream of the feeding device 10; at least one group of separation components are arranged in the reaction kettle 200 and are 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 are performed in the integrated reaction and separation device 20, so that the mother solution can be dynamically separated while the reaction is performed, the reaction integration level is high, adverse factors caused by external transfer to the reaction are avoided, and the method is suitable for the situation that reactants or products or catalytic additives of multiphase reactions such as liquid-solid, gas-liquid-solid and the like 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, the hollow cavity of the hollow rotating shaft 240 is communicated with the inner cavity of the separation membrane 230, a first end of the hollow rotating shaft 240 along the axial direction is connected with 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 rotates under the drive of the driving element 210, and can play a good role in stirring materials in the reaction kettle 200; the reaction kettle 200 is internally provided with a liquid distributor 260 parallel to 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 the embodiment, the reaction raw materials enter the reaction kettle 200 through the liquid distributor 260 by the feeding device 10, the hollow rotating shaft 240 is driven by the driving element 210 to drive the separation membrane 230 to rotate, the materials in the reaction kettle 200 are driven to form mixed flow, a pressure difference is formed in the space between the feeding and the discharging of the reaction kettle, the solid particles in the reaction system are trapped on the surface of the separation membrane 230, the solid particles in the reaction kettle are uniformly suspended and distributed in the reaction kettle under the mixed flow effect, and the mother liquor clear liquid after the reaction is permeated and converged to the hollow rotating shaft 240 from the surface of the separation membrane 230 under the driving of the pressure, is discharged through the second end of the hollow rotating shaft 240, and particularly 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 mixing effect.
In practical application, the separation membrane 230 on the hollow rotating shaft 240 is in a hollow disc shape, 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 has a hollow column shape, 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 adopting a mechanical sealing device, and the driving element 210 and the hollow rotating shaft 240 realize rotary rotation through a connecting shaft transmission or a belt transmission or a gear transmission.
By combining the above, the integrated reaction and separation system can work in a closed and positive pressure environment, so that the mutual contact between a reaction system and an external air environment is avoided, the reaction system is influenced, the environment is polluted, and the reliability is improved.
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 materials. By integrating 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 multiphase reactions such as liquid-solid, gas-liquid-solid and the like are fine particles. Wherein the washing apparatus 80 includes a water supply tank 800 for supplying a washing medium, and the water supply tank 800 is connected to the liquid distributor 260 through a liquid supply valve 820.
Preferably, the washing apparatus 80 further comprises a washing pipe with a washing liquid flow valve 822, said washing pipe being connected to the liquid distributor 260; the bottom of the reaction kettle 200 is also provided with a drain port 285 for draining the waste liquid and residual mother liquid after cleaning.
As a preferred further embodiment, the water supply tank 800 is provided with a water supply pipe with a water supply valve 810; the water supply tank 800 is connected to the liquid distributor 260 through a liquid supply valve 820 after passing through a wash pump 830 and a wash pump outlet check valve 831 for controlling the flow of the washing medium into 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 is provided, and the temperature sensor 811 is electrically connected to the water supply tank heat source flow valve 821, so that the temperature of the washing medium such as pure water in the water supply tank 800 is adjusted according to the measured temperature value in combination with the processing demand. Generally, the water washing temperature is controlled to be 0 to 150 ℃. According to the present embodiment, the products in the reaction vessel 200 can be washed by the washing device 80 to obtain a qualified product. In the reaction gap, cleaning liquid can be added into the cleaning pipeline to clean the separation assembly, and the waste liquid after cleaning is discharged outside through the drain port 285. In addition, after the cleaning is finished, the cleaning medium such as pure water can be used for washing again, so that the 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 discharging, the discharging opening is arranged in a funnel shape. Wherein, the discharge port discharges the product to the qualified product storage tank 400 by controlling the opening of the discharge valve 282, and the product enters the subsequent process through the qualified material tank discharge valve 410.
Furthermore, a turbulence element 250 is further disposed in the reaction kettle 200; the cross section of the turbulence element 250 is in a comb shape, and a plurality of comb teeth with uniform intervals are inserted into the interval area of the adjacent separation membrane 230, so as to further form turbulence effect. In addition, the turbulence element 250 may adopt a mechanical turbulence comb, an air-differential turbulence or a jet turbulence. 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 degree 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 good, and the method is suitable for the production of the particles with different particle size grades.
As a preferred further embodiment, the feeding device 10 comprises a raw material storage unit 100, which raw material storage unit 100 is connected to the liquid distributor 260 by a feeding pipe with a feeding pump 120 and a feeding valve 110; and the liquid distributor 260 is disposed along the axial direction of the vessel wall parallel to the hollow rotation shaft 240, as shown in fig. 1, so that the reaction raw materials can be sufficiently and uniformly distributed on each separation membrane 230, improving the sufficiency of the reaction and the solid-liquid separation. To ensure uniformity of the feeding process, the feeding device 10 may be provided with a plurality of raw material feeding ports on the reaction kettle 200, and symmetrically and uniformly distributed along the reaction kettle 200, and respectively communicated with the liquid distributor 260 in the kettle. In addition, the raw material storage unit 100 may include a plurality of raw materials according to kinds of raw materials required for actual reaction, and each communicates with the liquid distributor 260 through a feed port.
As a preferred further embodiment, a back flushing device 70 is further connected to the reaction kettle 200, the back flushing device 70 includes a back flushing pipe with a back flushing valve 710, the back flushing pipe is connected to the back flushing tank 700, and the bottom of the back flushing tank 700 is further communicated with the second end of the hollow rotating shaft 240, so as to receive a part of separated mother liquor clear liquid and washing waste liquid for back flushing.
According to the embodiment, the back flushing device 70 can regenerate the separation components in the integrated reaction and separation device 20 according to actual requirements, and simultaneously, the reaction efficiency and the product quality are effectively improved. Specifically, the back flushing device 70 can utilize the mother liquor clear liquid or the washing waste liquid which is generated by the reaction and is discharged after dynamic separation, and permeate from the inner side of the separation membrane 230 to the outer surface of the separation membrane through the hollow rotating shaft 240 under the pushing of back flushing gas, and remove the sediment on the surface of the separation membrane 230 through back flushing; the reaction vessel 200 is backwashed and the membrane flux of the separation membrane 230 is recovered.
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 multi-stage membrane separation unit 600, the multi-stage membrane separation unit 600 adopts nanofiltration membranes and/or reverse osmosis membranes for treating and recycling the washed washing waste liquid, the multi-stage membrane separation unit 600 is provided with a concentrated liquid outlet and a clear liquid outlet, the clear liquid outlet is circularly connected to a water supply tank 800, the clear liquid is circularly utilized 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 ends of the hollow shaft 240 in the axial direction are connected to the backwash tank 700 and the mother liquor tank 300 through the buffer tank 290, respectively; the buffer tank 290 and the backflushing tank 700 and the mother liquor tank 300 are connected by a clear liquid sight glass 270. Thereby facilitating the observation of the clarity of the mother liquor supernatant discharged from the reaction vessel 200. So as to find and observe the reaction condition in time and make the switching adjustment of the corresponding working procedure in time. A mother liquor discharge valve 310 is provided in a pipe between the buffer tank 290 and the mother liquor tank 300 to adjust a discharge amount of the mother liquor. The mother liquor tank 300 discharges the reaction mother liquor to the next process through the mother liquor tank discharge valve 320.
In practical use, 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.
Accordingly, the materials in the reaction kettle 200 can be washed by the washing device 80, the obtained washing waste liquid can be recycled by combining the process conditions and requirements, for example, when the solid materials in the reaction kettle meet the physicochemical characteristics, the feeding pump 120 and the feeding valve 110 of the reaction kettle 200 are closed, the feeding to the reaction kettle 200 is stopped, the rotating speed of the hollow rotating shaft 240 is controlled, for example, the rotating speed is reduced or stopped, the scouring action of the cross flow separation membrane 230 is reduced, so that the solid materials gradually form filter cakes on the membrane surface of the separation membrane 230, and after the residual mother liquid is discharged through the drain port 285, the washing process is started on the filter cakes by the washing device 80, and the specific steps are as follows: 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, simultaneously slowly rotating the hollow rotating shaft 240 at the initial stage of washing, gradually recovering to a normal rotating speed after a filter cake forms slurry, penetrating and converging a washing medium such as pure water into a cavity of the hollow rotating shaft 240 from the surface of the separation membrane 230 under the driving of pressure, discharging the washing medium from the second end, entering a heat exchange unit 900 through a buffer tank 290 and a backflushing tank 700, storing the washing medium into a washing waste liquid tank 500 after heat exchange and cooling, discharging the slurry into a qualified product storage tank 400 after the impurity content of a product in a sampling detection reaction kettle is qualified, and discharging the slurry to a subsequent process through a qualified product 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 is pressurized by the booster pump 510 and passes through the multi-stage membrane separation unit 600, 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 nanofiltration and/or reverse osmosis; the recovery rate of the clear liquid of the multistage membrane separation unit 600 is not less than 70%.
In addition, the reaction kettle 200 is provided with a reaction kettle heat source flow valve 280 for adjusting the temperature of a system in the reaction kettle; the reaction kettle 200 is also provided with an exhaust port, and the exhaust port is communicated with an exhaust pipeline with an exhaust flow valve 281 to regulate the pressure in the reaction kettle 200. The reaction vessel 200 is also provided with a pressure gauge 283 for monitoring the operating pressure in the reaction vessel 200.
In the above embodiment, the reaction vessel 200 may be of a horizontal type or a vertical type. The heating mode of the kettle body of the reaction kettle 200 can be a clamping sleeve or pipe type, and the heating medium is heat conduction oil or saturated steam and the like.
It should be noted that, according to different requirements of washing the reaction materials, the washing medium in the water supply tank 800 may be pure water, alkali solution, alcohols, etc., and the number of the water supply tanks 800 may be set to be plural according to different requirements of washing sequences.
According to another embodiment of the present invention, as shown in fig. 1, an integrated reaction and separation process is provided, comprising the following steps:
s1, continuously metering the reaction raw materials into a reaction kettle 200 of an integrated reaction and separation device 20, controlling the pressure in the reaction kettle 200 by adjusting the feeding flow, and separating mother liquor clear liquid and solid materials from the reacted materials by a separation assembly 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, specific steps further include:
s3, adding a washing medium into the reaction kettle 200 through the washing device 80, washing slurry in the reaction kettle 200 by the washing medium under the drive of pressure, and storing the generated washing waste liquid into a 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.
Or, in step S2, when the washing process is not set, and the solid content in the reaction kettle 200 is continuously increased to a predetermined value, the mother liquor clear liquid 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 steps of the integrated reaction and separation process include:
in step S1: continuously metering reaction raw materials into a reaction kettle 200 of an integrated reaction and separation device, controlling the pressure in the reaction kettle 200 through a feed valve 110 of the integrated device, driving a first end of a hollow rotating shaft 240 positioned in the middle of the reaction kettle 200 in a separation assembly to rotate while the reaction raw materials react in the kettle, driving separation diaphragms 230 which are arranged at intervals on the hollow rotating shaft and are mutually communicated to rotate, and penetrating and converging mother liquor clear liquid generated by the reaction from the surface of the separation diaphragms 230 into a cavity of the hollow rotating shaft 240 under the driving of the pressure, discharging the mother liquor through a second end of the hollow rotating shaft, wherein solid particles generated by the reaction are trapped on the surface of the separation diaphragms 230; in addition, 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 between the separation membranes 230 to prevent the solid matters generated by the reaction from depositing on the surfaces of the membranes, the surfaces of the membranes are smooth all the time and no filter cake is generated, thus ensuring the membranes to have stable high clear liquid flux;
In step S3: concentrating the slurry by controlling the rotating speed of the separation assembly, so that a filter cake is gradually formed on the surface of a membrane of the separation assembly by the solid material; discharging residual mother liquor, and starting a washing process for the filter cake; starting a water washing pump 830 at the outlet of the water supply tank 800 in the washing device 80, simultaneously, slowly rotating the hollow rotating shaft 240 until a filter cake forms slurry in the initial stage of washing, then recovering the normal rotating speed, and storing washing water such as pure water after the washing of the slurry is completed and discharged from the second end of the hollow rotating shaft 240 after penetrating and converging to the hollow rotating shaft 240 from the surface of the separation membrane 230 under the driving of pressure, and cooling the washing water by the heat exchange unit 900 and storing the washing water in the washing waste liquid tank 500; wherein, for the slurry product in the reaction kettle 200, sampling and detecting that the impurity content in the product is qualified, and then discharging the slurry to a qualified product storage tank 400; after the washing waste liquid generated in the washing process is separated by the nanofiltration membrane and/or the reverse osmosis membrane of the multi-stage membrane separation unit 600 under the supercharging action of the booster pump 510, clear liquid flows back to the water supply tank 800 for recycling, and concentrated liquid enters the recovery system.
According to the embodiment, the reaction raw materials are subjected to the integrated treatment of reaction and dynamic separation in the integrated reaction and separation device, the whole process is high in integration level, 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 this step S1, the reaction liquid fills the integrated reaction and separation device (or the exhaust amount of the gas outlet and the pressure in the reaction tank are controlled when the integrated reaction and separation system is opened, so that the liquid level in the tank is kept at a proper position when the reaction is normally performed), and the opening of the mother liquor discharge valve 310 is adjusted so that the mother liquor discharge amount and the actual capacity of the device are adapted. The residence time of the slurry in the apparatus is controlled by adjusting the mother liquor discharge flow according to the different product reaction rates or crystallization rates. When the specified conversion rate or physical and chemical characteristics of the solid product are reached, the reaction is complete. The invention can also arrange an inlet-outlet pressure difference alarm device on the reaction kettle 200, comprising a pressure gauge 283 and an alarm arranged on the reaction kettle 200, so as to monitor the blockage condition of the solid material to the separation membrane 230.
Preferably, in the reaction, separation and washing processes in the steps S1 to S3, under the condition that the operation 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 rate of the washing waste liquid discharged in the washing process into the washing waste liquid tank 500 is reduced to 80% of the initial state, or when the internal pressure difference of the reaction kettle 200 exceeds the limit value, back flushing is performed on the reaction kettle 200 by introducing back flushing gas, wherein the back flushing process is as follows:
The clear liquid discharged from the hollow rotation shaft 240 enters the backflushing tank 700 through the buffer tank 290, the clear liquid in the backflushing tank 700 is pushed by backflushing air pressure, permeates from the inner side of the membrane of the separation membrane 230 to the surface of the membrane through the hollow rotation shaft 240, and removes the sediment on the surface of the separation membrane 230 through backflushing. Wherein, the drop of the clear liquid flux can be observed through the clear liquid 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 back-flushed and then repeatedly put into reaction. The back flushing step is the same as the above process.
Further, when the clear liquid flux is not completely recovered by back flushing after the system runs for a long time, the materials of the system equipment are drained periodically, cleaning liquid is added to clean the system equipment through a cleaning pipeline, and the waste liquid after cleaning is drained from the drain port 285; and, after the washing is completed, the washing medium such as pure water in the water supply tank 800 is used for washing, so that the pollution of the residual washing 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 feeding flow of the reaction raw materials is controlled to be 0-5000L/h; the revolution of the hollow rotating shaft is 0-1500 r/min; and controlling the solid content in the reaction kettle to be 0-70%; the pH of the reaction 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.
According to the reaction system and the process provided by the embodiment of the invention, the reaction system and the process can be applied to the reaction for generating a solid product by a liquid phase method or the fluidized bed reaction of a powder catalyst. Specific examples of applications are provided below:
application example 1 recovery of oximation catalyst in caprolactam production
At present, cyclohexanone oxime is prepared by catalyzing cyclohexanone ammoximation through a titanium-silicon molecular sieve at home.
Reaction and dynamic separation process
By utilizing the integrated reaction and separation system shown in fig. 1, tertiary butanol, ammonia gas and catalyst respectively enter a liquid distributor 260 from different feed inlets through a feed device 10, the reaction is carried out in a reaction kettle 200, the catalyst concentration is 3wt%, after the reaction is completed, the reaction liquid containing the catalyst is separated by a separation membrane 230 in the reaction kettle 200, mother liquor clear liquid enters a mother liquor tank 300 through a mother liquor discharge valve 310, and cyclohexanone oxime is obtained through a subsequent process, thereby producing caprolactam. The catalyst is retained in the reaction kettle 200 to continue the reaction until the catalyst activity is reduced to the point that the catalyst needs to be regenerated, the feeding is stopped, and the catalyst needing to be regenerated is discharged through a discharge valve 282 of the reaction kettle and then enters the subsequent treatment process.
Backflushing and cleaning recovery process
Under the condition of keeping the operation pressure difference in the reaction kettle 200 unchanged, when the flow rate of the 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 is needed, a mother liquor discharge valve 310 is closed, a back flushing valve 710 is opened, the back flushing gas gauge pressure is controlled to be 0.1MPa, clear liquid in a buffer tank 290 enters the reaction kettle 200 under the back flushing gas pressure effect, back flushing is carried out on catalyst powder on the surface of a separation membrane, the back flushing time lasts for 30 seconds each time, and the flux of the separation membrane is recovered to be more than 90% of that in the initial state after the back flushing; and (3) periodically checking the pollution and blockage conditions of the membrane in the production gap, and cleaning the separation membrane by using special cleaning liquid in time to recover the membrane flux. The cleaning liquid flow valve 822 is opened, cleaning liquid enters the reaction kettle 200 from the raw material inlet, the stirring motor serving as the driving element 210 is started to clean the separation membrane 230 in the reaction kettle, and the cleaned waste liquid enters the sewage drain pipeline through the drain port 285.
Application example 2 reaction, dynamic separation and washing of ternary Material precursor
Reaction and dynamic separation process
With the integrated reaction and separation system of fig. 2, the reaction raw materials (sulfate mixed solution, alkali solution, and 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 sulfate mixed solution, alkali solution, and ammonia solution are symmetrically distributed at the inlet positions and uniformly distributed in the reaction kettle 200 through the liquid distributor 260. The driving element 210 is started, the reaction raw materials react in the reaction kettle 200 to generate mother liquor containing solid matters, the mother liquor is subjected to solid-liquid separation through the separation membrane 230, separated mother liquor clear liquid is discharged from the second end of the hollow rotating 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 capacity of the device, the total flow of the sulfate mixed solution, the alkali solution and the ammonia water solution is 400L/h; by setting the operating frequency of the stirring motor as the driving element 210, the revolution number of the hollow rotating shaft 240 and the separation membrane 230 is controlled to 350r/min, and the reaction temperature in the reaction vessel 200 is controlled by the reaction vessel heat source flow valve 280, and the reaction temperature is constant at 60±1 ℃. The absolute pressure in the reaction kettle 200 is controlled by adjusting the feed valve 110, the mother liquor discharge 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 discharge flow of the mother liquor clear liquid is automatically maintained to be equal to the total feed flow of the reaction kettle because the reaction kettle 200 is full of liquid and the liquid is incompressible.
Washing and multistage membrane separation process
When the particle size of the solid material in the reaction vessel 200 meets the requirement, the reaction is completed, the reaction raw material feed pump 120 is stopped, the feed valve 110 and the mother liquor discharge valve 310 are closed, the rotation speed of the hollow rotation shaft 240 and the separation membrane 230 is reduced until the rotation is stopped, the solid material forms a filter cake on the surface of the membrane, and the residual mother liquor 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 is started;
by controlling the heat source flow valve 821 of the water supply tank, the temperature of pure water in the water supply tank 800 is kept at 75 ℃, hot water enters the reaction kettle 200 from a feeding pipeline and is uniformly distributed through the fluid distributor 260 in the kettle, meanwhile, the hollow rotating shaft 240 slowly rotates to form slurry by a filter cake at the initial stage of washing, then the normal rotating speed is recovered, pure water permeates from the surface of the separation membrane 230 to the hollow rotating shaft 240 under the driving of pressure, after the formed washing waste liquid is discharged through the second end of the hollow rotating shaft 240, the formed washing waste liquid sequentially flows through the clear liquid sight glass 270 and the backflushing tank 700 along a pipeline, then enters the washing waste liquid tank 500 after being cooled to 45 ℃ through the heat exchanger serving as the heat exchange unit 900, when the liquid level in the washing waste liquid tank 500 reaches the upper limit value, the booster pump 510 is started, the clear liquid is obtained after the separation of the washing waste liquid by the multi-stage membrane separation unit 600 and flows back to the water supply tank 800 as washing make-up water, and the concentrated liquid obtained after the membrane separation is discharged to the subsequent process through the membrane separation concentrated liquid valve 620 for recovery treatment, and the water recovery rate of the multi-stage membrane separation unit 600 is not lower than 70%; the water supply valve 810 is controlled to supplement a washing medium such as pure water according to the liquid level in the water supply tank 800, so that balance of the washing process is ensured, and after the impurity content of the product in the sampling and detecting reaction vessel is qualified, the liquid supply valve 820 and the washing waste liquid discharge valve 520 of the water supply tank 800 are closed, and the washing pump 830 is stopped. At this time, the discharge valve 282 of the reaction tank is opened, and the washed acceptable product is discharged to the acceptable product storage tank 400.
Backflushing and cleaning recovery process
Under the condition of keeping the operation pressure difference in the reaction kettle 200 unchanged, when the flow rate of the mother liquor clear liquid flowing into the mother liquor tank 300 in the reaction process or the flow rate of the washing waste liquid flowing into the washing waste liquor tank 500 in the washing process is reduced to 80% of 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 gauge pressure of backflushing gas 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, powder on the surface of the separation membrane 230 is backflushed, the backflushing time lasts for 30 seconds each time, and the membrane flux after backflushing is recovered to more than 95% of the initial state; the pollution and blockage condition of the separation membrane 230 is checked at regular intervals in the production gap, specifically, the separation membrane 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 is cleaned by special cleaning liquid in time, so that the membrane flux is recovered. The cleaning liquid inlet flow valve 822 is opened, 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 drain pipeline through the drain port 285.
It should be noted that the above embodiments can be freely combined as needed. The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (15)
1. An integrated reaction and separation process is characterized by comprising the following steps:
s1, continuously metering reaction raw materials into a reaction kettle of an integrated reaction and separation device, controlling the pressure in the reaction kettle by adjusting the feeding flow, driving a first end of a hollow rotating shaft positioned in the middle of the reaction kettle to rotate while the reaction raw materials react in the kettle, driving separation diaphragms which are arranged on the hollow rotating shaft at intervals and are mutually communicated to rotate, and under the driving of the pressure, penetrating mother liquor clear liquid generated by the reaction from the surface of the separation diaphragms into a cavity of the hollow rotating shaft and discharging the mother liquor clear liquid through a second end of the hollow rotating shaft, wherein solid particles in a reaction system are trapped on the surface of the separation diaphragms;
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;
S3, concentrating the slurry by controlling the rotating speed of the separation assembly, so that a filter cake is gradually formed on the surface of the membrane of the separation assembly by the solid material; discharging residual mother liquor, and starting a washing process for the filter cake;
the washing process specifically comprises the following steps: adding a washing medium into the reaction kettle through a washing device, washing 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.
2. The integrated reaction and separation process of claim 1, wherein:
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.
3. The integrated reaction and separation process of claim 1, wherein:
in the step S3, a water washing pump at the outlet of a water supply tank in the washing device is started, the rotating speed of the hollow rotating shaft is controlled, and washing media permeate from the surface of the separation membrane to the hollow rotating shaft under the driving of pressure, after the slurry is washed and discharged from the second end of the hollow rotating shaft, the slurry is cooled by a heat exchange unit and then stored in a washing waste liquid tank; the method comprises the steps of sampling and detecting the qualified impurity content of a slurry product in a reaction kettle, and discharging the slurry to a qualified product storage tank; washing waste liquid in the washing waste liquid tank is separated by nanofiltration membranes and/or reverse osmosis membranes of the multistage membrane separation unit, and clear liquid flows back to the water supply tank for recycling.
4. The integrated reaction and separation process according to any one of claims 1 to 3, characterized in that,
back flushing the reaction kettle according to the requirement; the back flushing process is as follows: 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 washing waste liquid in the backflushing tank is pushed by backflushing air pressure to permeate from the inner side of the membrane of the separation membrane to the surface of the membrane through the hollow rotating shaft, and sediment on the surface of the separation membrane is removed through backflushing;
and/or;
adding cleaning liquid into the reaction kettle through a cleaning pipeline according to the requirement to clean the reaction kettle, and discharging the cleaned waste liquid from the exhaust port; after the cleaning is finished, the washing medium in the water supply tank is used for flushing;
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.
5. The integrated reaction and separation process of claim 1, comprising:
a feeding device for storing and conveying the reaction raw materials;
the integrated reaction and separation device comprises a reaction kettle connected to the downstream of the feeding device; the reaction kettle is internally provided with at least one group of separation components for dynamically separating solid and liquid phases during raw material reaction, the separation components comprise a hollow rotating shaft which is penetrated in the middle of the reaction kettle shell, a plurality of hollow separation diaphragms are arranged on the hollow rotating shaft at intervals, the cavities of the hollow rotating shaft are communicated with the inner cavities of the separation diaphragms, 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 the washing device is connected to the upstream of the reaction kettle and is used for washing the solid materials after reaction separation.
6. The integrated reaction and separation process of claim 5, wherein:
the reaction kettle is internally provided with a liquid distributor which is parallel to the hollow rotating shaft and is communicated with the feeding device;
and a discharge hole is arranged at the bottom of the separation membrane in the reaction kettle.
7. The integrated reaction and separation process of claim 6, wherein:
the separation membrane is of a hollow disc-shaped structure, and the membrane aperture of the separation membrane is 1 nm-50 mu m;
and/or;
the separating membrane is of a circular structure and has a diameter of 50-5000 mm.
8. The integrated reaction and separation process of claim 5, wherein:
the washing apparatus includes a water supply tank for supplying a washing medium, the water supply tank being connected to the reaction tank through a liquid supply valve.
9. The integrated reaction and separation process of claim 8, wherein:
the low reaches of reation kettle connect gradually washing waste liquid jar and multistage membrane separation unit, multistage membrane separation unit adopts nanofiltration membrane and/or reverse osmosis membrane for the washing waste liquid after the washing is separated, multistage membrane separation unit is equipped with thick liquid export and clear solution export, and clear solution export circulation is connected to the supply tank.
10. The integrated reaction and separation process of claim 9, wherein:
the washing device further comprises a washing pipeline with a washing liquid flow valve, and the washing pipeline is connected to the reaction kettle; the bottom of the reaction kettle is also provided with a drain port for draining the waste liquid and residual mother liquid after cleaning, and the front end of the washing waste liquid tank is communicated with the heat exchange unit and is used for reducing the temperature of the washing waste liquid.
11. The integrated reaction and separation process of claim 5, wherein:
a turbulent flow element is also arranged in the reaction kettle;
the cross section of the turbulence element is in a comb shape, and a plurality of comb teeth which are uniformly distributed at intervals are inserted into the interval areas of the adjacent separation diaphragms.
12. The integrated reaction and separation process of claim 5, wherein:
the reaction kettle is also connected with a back flushing device, the back flushing device comprises a back flushing pipeline with a back flushing valve, the back flushing pipeline is connected to a back flushing tank, and the bottom of the back flushing tank is also communicated with the second end of the hollow rotating shaft.
13. The integrated reaction and separation process of claim 12, 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 the buffer tank; and a clear liquid viewing mirror is arranged on the connecting pipeline of the buffer tank, the backflushing tank and the mother liquor tank.
14. The integrated reaction and separation process of claim 8, 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; and the reaction kettle is also provided with a pressure gauge for monitoring the operating pressure in the reaction kettle.
15. Use of an integrated reaction and separation process according to any one of claims 1 to 14 in a liquid phase process for the production of solid products or in a powder catalyst fluidized bed reaction.
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| 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 |
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