A kind of thickener and be used for the method for liquid-solid separation
Technical field
The present invention relates to a kind of equipment that solia particle is separated from liquid continuously and and using method, more particularly, relate to a kind of thickener, and use this thickener to realize separating continuously of product liquid and solid catalyst particulate, and from catalyst concentration, remove the method for byproduct of reaction.
Background technology
Usually, in the liquid-phase catalysis course of reaction, in order to eliminate diffusion influence, the catalyst granules that uses is less, but also bring product to separate this difficult problem with catalyst granules thereupon, therefore, adopt a kind of separator that solid catalyst is separated from liquid product, become a key technology in the liquid-phase catalysis course of reaction.For example, the thickener that catalyst can be concentrated out from product in the outer setting of reactor, and the catalyst slurry after will concentrating sends back in the reactor and recycles, thereby reduces the amount of entrained catalyst in the product, makes the product that obtains meet the requirement of downstream processing technology.Especially when using expensive catalysts such as noble metal catalyst, catalyst granules is separated from product and recycled, the use cost of save catalyst greatly by thickener.
In Aniline Production technology, advantages such as reaction temperature is low, side reaction is few because liquid phase catalytic hydrogenation has, catalysis load height, equipment capacity is big, gross investment is low have caused people's attention in recent years.Yet, the producer of present domestic employing liquid phase catalytic hydrogenation technology system aniline such as Ningbo polyurethane Co., Ltd, the employed thickener of sky, Shanxi ridge group company are import equipment, cost an arm and a leg, because the domestic product that does not also occur similar technology at present, cause external product to monopolize market for a long time, thickener equipment cost height makes liquid phase catalytic hydrogenation system aniline technology be difficult at home obtain promote.But, in actual use, thereby because external thickener equipment adopts the driven by motor hydraulic pump, produces the multistage transmission that hydraulic oil passes to energy hydraulic motor, energy loss is big between this multistage transmission, causing its transmission efficiency only is 60%, and the every cover mechanically-sealing apparatus of this kind equipment all is equipped with a centralized oil supply station, the fault rate height, many cover sealing devices are equivalent to serial operation, if one of them oil pump station breaks down, then can influence the normal operation of its sealing device, thereby cause the sealing property of whole system to descend; And a plurality of oil pump stations operate more loaded down with trivial details, and security reliability is poor.
Summary of the invention
An object of the present invention is to provide and reclaim catalyst particles a kind of from product, the separation, simultaneously the thickener that byproduct of reaction is removed continuously.
In order to solve the problems of the technologies described above, the present invention has adopted a kind of like this thickener, but it comprises the filter disc 5 of hollow shaft 4, feed pipe 2 and at least two middle perforates of tank body 11, motor 9, reductor 10 axial rotation; Wherein, the upper end of tank body 11 is provided with concentrate discharging opening 7, and motor 9 directly links to each other with reductor 10 and drives hollow shaft by shaft coupling 12, and hollow shaft 4 runs through whole tank body along the axis of tank body, and the lower end of hollow shaft connects filtrate discharging opening 8; Described feed pipe 2 is arranged on tank interior and parallel with hollow shaft, and the lower end of feed pipe is a charging aperture 1, and the upper end is fixed on the tank body top; Described filter disc 5, is provided with an end between per two adjacent filter discs and is connected and the charging distributor pipe 3 of other end opening with feed pipe in hollow shaft by middle perforate vertical fixing, and scraper 6 is fixed in the charging distributor pipe abreast.
According to thickener provided by the invention, the filter disc 5 of 20~29 middle perforates is housed on hollow shaft 4 wherein.
According to thickener provided by the invention, its hollow mandrel 4 is provided with filtrate and enters hole 14 to collect filtrate, and each filtrate is advanced the corresponding filter disc in hole, and it is vertical with hollow shaft that filtrate is advanced the perforate direction in hole.According to thickener provided by the invention, the lower end of its hollow mandrel 4 is provided with discharge opening 15, and discharge opening 15 links to each other with filtrate discharging opening 8 by discharging ring 16, and discharging ring 16 is that filtrate is flowed out the thickener prerequisite for free air space through filtrate charging aperture 8.
According to thickener provided by the invention, wherein filter disc 5 is equipped with the filter medium that is selected from lamination filter screen, sintering filter screen, powder metallurgy plate, is preferably the sintering filter screen, metal sintering filter screen more preferably, and the pore size filter of filter medium is lower than the particle diameter of solid particle.
A preferred version according to thickener provided by the invention, wherein all filter discs are by the sealing of the O type circle between the filter disc wheel hub, O type circle guarantees that by the extruding force sealing between the folded filter disc that drops on together the dipping and heaving amount on its plane was less than 1.5 millimeters when filter disc rotated.Described sealing ring can adopt the corrosion-and high-temp-resistant material to make, and preferably adopts perfluor ether rubber to make.
According to thickener provided by the invention, wherein on the hollow shaft 4 above first charging distributor pipe, be provided with first agitator 18, be preferably and have the radially agitator of paddle of straight leaf, make the product after concentrating even with the catalyst mix of being struck off by scraper; In the end the hollow shaft 4 of a charging distributor pipe below is provided with second agitator 19, is preferably to have the radially agitator of paddle of hinging type, prevents to be accumulated in tank base by the catalyst that scraper strikes off.
According to thickener provided by the invention, be respectively equipped with sealing device 20 between the bottom of the top of its hollow mandrel and tank body, hollow shaft and tank body and hollow shaft and the discharging ring, the sealing device preferably adopts the Double End integrated mechanical sealing device that carries bearing; Described bearing can be the conventional bearing in this area, for example, to tank body top and being connected of hollow shaft adopting the double-row self-aligning roller bearing, play the effect of radial location, to tank base and being connected of hollow shaft adopting the circular cone roller bearing, play the effect of axial location by face-to-face layout.
According to thickener provided by the invention, wherein, required cooling and lubricated when adopting a centralized oil station 21 that sealing device 20 work are provided.
According to a preferred version of thickener provided by the invention, wherein, feed pipe 3 is fixed in tank body 11 by fixture 17, prevents the radially wobble effects scraper work of feed pipe, and allows 90 ° of feed pipe axial rotation; The design pressure of tank body is FV~2.0MPa, and design temperature is 30~120 ℃, and tank body is provided with chuck 13 outward, and by the reacting slurry of the Steam Heating HTHP in the chuck, the pressure of steam is 0.2~0.6MPa in the chuck, and the temperature of steam is 90~150 ℃; Except that special provision was arranged, each parts among the present invention in the chuck 13 of thickener, tank body 11 and the tank body adopted stainless steel to make, and preferably adopt stainless steel 304 to make.
Described " FV " is meant " vacuum ", is meant that actual when operation of going into operation is because inner high-temperature steam formed vacuum when unusual condensation.
Another object of the present invention is, providing a kind of adopts above-mentioned thickener to carry out the method that liquid-solid two-phase separates continuously, this method comprises: contain catalyst granules and liquid reacting product and enter tank body 11 by the charging aperture 1 of feed pipe 2 lower ends, under the driving of motor and speed reducer, filter disc 5, first agitator 18 and second agitator 19 and hollow shaft coaxial rotation, charging distributor pipe 3 will be introduced between adjacent two filter discs 5 equably from the slurries of feed pipe 2, catalyst granules forms filter cake at the filter disc surface sediment, the part that filter cake constantly thickens is struck off through scraper 6, struck off the solid catalyst that gets off and flowed out tank body 11, Returning reacting system through concentrate discharging opening 7; Gained filtrate is confluxed to enter hole 14 and enter hollow shaft to flow downward to the filtrate of hollow shaft 4 by the space of filter medium, flows out from discharge opening 15, comes together in discharging ring 16, discharges through filtrate discharging opening 8 again, is sent to the product purification system.
Compared with prior art, thickener of the present invention has the following advantages:
(1) adopts rotatable filter disc and doctor assemblies, can realize separating continuously of liquid and solid particle, and recycle catalyst;
(2) thickener of the present invention adopts driven by motor reductor direct coupled structure, and transmission efficiency reaches more than 95%;
(3) cooling and lubricatings of many cover sealing devices adopt a centralized oil station to realize that operation is reliable, keep in repair easyly, have reduced equipment volume and operating cost;
(4) thickener of the present invention adopts 304 stainless steels as equipment master material, can satisfy the manufacturing requirement of thickener, and compares with the same category of device of this area, and manufacturing cost reduces about 20%.
By the continuous method of separating of liquid-solid two-phase provided by the invention, can realize separating continuously of solid catalyst particle and product liquid, the catalyst granules Returning reacting system of separating continues to participate in reaction, product liquid after separating is sent to the product purification system to remove most of byproduct of reaction, reach the purpose of the catalyst that carries in concentration response product, the recovery product, also can remove byproduct of reaction with the catalyst granules Returning reacting system.
Description of drawings
Fig. 1 is the schematic diagram according to a preferred version of thickener of the present invention, and wherein 1 is charging aperture, and 2 is feed pipe, and 3 are the charging distributor pipe, 4 is hollow shaft, and 5 is filter disc, and 6 is scraper, and 7 is the concentrate discharging opening, 8 is the filtrate discharging opening, and 9 is motor, and 10 is reductor, and 11 is tank body, 12 is shaft coupling, and 13 is chuck, and 14 enter the hole for filtrate, 15 is discharge opening, and 16 are the discharging ring, and 17 is fixture, 18 is first agitator, and 19 is second agitator, and 20 is sealing device;
Fig. 2 is the local enlarged diagram of Fig. 1;
Fig. 3 is an exemplary operation principle schematic diagram with thickener of multilayer rotation filter disc of the present invention, and wherein direction of arrow representative contains the flow direction of liquid reacting product in thickener of catalyst granules.
The specific embodiment
Further specify embodiment of the present invention below in conjunction with embodiment.But the embodiment that the invention is not restricted to enumerate also should be included in other any known changes in the interest field of the presently claimed invention.
The design pressure of thickener tank body 11 is 0.1~1.6Mpa, and design temperature is 120 ℃.Adopt the alternating current generator 9 of IP55/DIIBT4, power output is 37kw, uses 380 volts power supply.Motor 9 and reductor 10 place the top of tank body 11, reductor is with the required rotating speed of high speed rotating conversion filter disc of motor, the rotational speed regulation scope of reductor 10 is 0~130rpm, motor, reductor drive hollow shaft by shaft coupling, hollow shaft is positioned at tank body central shaft position, its upper end links to each other the discharge opening 15 that it is 20mm that the lower end is provided with 10 diameters with shaft coupling.Feed pipe 2 is arranged on tank interior and parallel with hollow shaft, and the lower end of feed pipe is a charging aperture 1.The filter disc 5 of the middle perforate that it is 940mm that the hollow shaft 4 that is positioned at tank interior is provided with 20 diameters, all filter discs be fixed on the hollow shaft by middle perforate and with its coaxial rotation, be provided with an end between the adjacent filter disc and be connected and the charging distributor pipe 3 of other end opening with feed pipe, scraper 6 is fixed in the charging distributor pipe abreast.The upper end of feed pipe 2 is fixed 17 by feed pipe and is fixed on the tank body top, the wobble effects scraper work of feed pipe when preventing work, but 90 ° of feed pipe axial rotation.
Hollow shaft therein line position to be provided with diameter be that the filtrate of 10mm is entered hole 14, each filtrate is advanced the corresponding filter disc in hole, it is vertical with the axial direction of hollow shaft that filtrate is advanced the hole direction.Filter medium on the filter disc adopts the metal sintering screen pack, and scraper 6 is fixed in the charging distributor pipe.Discharge opening 15 links to each other with filtrate discharging opening 8 by discharging ring 16.Also install respectively on the hollow shaft have straight leaf radially paddle first agitator 18 and have second agitator 19 that hinged joint upwards disperses paddle.
Sealing device between hollow shaft and tank body top, hollow shaft and tank base and hollow shaft and the discharging ring is the Double End integrated mechanical sealing device that carries bearing.Wherein upper bearing adopts the double-row self-aligning roller bearing, and lower bearing adopts the circular cone roller bearing.The O type circle sealing that all filter discs are made by the perfluor ether rubber between the wheel hub.Required cooling and lubricated when adopting a centralized oil station 21 to guarantee described both-end mechanically-sealing apparatus work.
Also be provided with chuck 13 outside the tank body 11, can lead to steam in the chuck.Parts in the chuck of thickener, tank body and the tank body adopt stainless steel 304 to make.
Flow is 80m
3The aniline product that contains catalyst granules and accessory substance tar of/h (catalyst solid content is 1wt%) enters the feed pipe 2 of thickener through charging aperture 1, adopting pressure in the chuck is that 0.4Mpa, temperature are 120 ℃ the interior material of Steam Heating tank body, and the rotating speed of filter disc is 100rpm.Rotation by filter disc, charging distributor pipe 3 will be introduced between adjacent two filter discs equably from the product that feed pipe 2 is come in, the aniline product filters under the effect of metal sintering filter screen both sides pressure reduction, solid catalyst particle is piled up in screen surface and is formed certain thickness filter cake, and obtains containing the filtrate of aniline and tar accessory substance.Along with the continuous rotation of filter disc, the part that filter cake constantly thickens is struck off continuously through scraper, strikes off the solid catalyst that gets off and flow out thickener, Returning reacting system through concentrate discharging opening 7 under the stirring action of first agitator 18; The space of filtrate by filter screen is flowed to the filtrate of hollow shaft 4 and enters hole 14, and flow downward along hollow shaft, flow out and come together in discharging ring 16 from discharge opening 15, discharge through filtrate discharging opening 8 again, solids content in the filtrate satisfies the technological requirement of subsequent product refining system less than 0.2ppm.
Embodiment 2
Adopt with embodiment 1 in identical thickener, wherein the quantity with filter disc 5 changes 25 into.
Flow is 100m
3The aniline product that contains catalyst granules and accessory substance tar of/h (catalyst solid content is 1wt%) enters the feed pipe 2 of thickener through charging aperture 1, adopting pressure in the chuck is that 0.4Mpa, temperature are 120 ℃ the interior material of Steam Heating tank body, and the rotating speed of filter disc is 120rpm.Rotation by filter disc, charging distributor pipe 3 will be introduced between adjacent two filter discs equably from the aniline product that feed pipe 2 is come in, the aniline product filters under the effect of metal sintering filter screen both sides pressure reduction, solid catalyst particle is piled up in screen surface and is formed certain thickness filter cake, and obtains containing the filtrate of aniline and tar accessory substance.Along with the continuous rotation of filter disc, the part that filter cake constantly thickens is struck off continuously through scraper, strikes off the solid catalyst that gets off and mixes again under the stirring action of agitator up and down and flow out thickeners, Returning reacting system through concentrate discharging opening 7; The space of filtrate by filter screen is flowed to the filtrate of hollow shaft and enters the hole, and flow downward along hollow shaft, flow out and come together in discharging ring 16 from discharge opening 15, discharge through discharging opening 8 again, solids content in the filtrate satisfies the technological requirement of subsequent product refining system less than 0.2ppm.
Embodiment 3
Adopt with embodiment 1 in identical thickener, wherein the quantity with filter disc changes 29 into.
Flow is 120m
3The aniline product that will contain catalyst granules and accessory substance tar of/h (catalyst solid content is 1wt%) enters the feed pipe 2 of thickener through charging aperture 1, adopting pressure in the chuck is that 0.4Mpa, temperature are 120 ℃ the interior material of Steam Heating tank body, and the rotating speed of filter disc is 130rpm.Rotation by filter disc, charging distributor pipe 3 will be introduced between adjacent two filter discs equably from the aniline product that feed pipe 2 is come in, the aniline product filters under the effect of metal sintering filter screen both sides pressure reduction, solid catalyst particle is piled up in screen surface and is formed certain thickness filter cake, and obtains containing the filtrate of aniline and tar accessory substance.Along with the continuous rotation of filter disc, the part that filter cake constantly thickens is struck off continuously through scraper, strikes off the solid catalyst that gets off and mixes again under the stirring action of agitator up and down and flow out thickeners, Returning reacting system through concentrate discharging opening 7; The space of filtrate by filter screen is flowed to the filtrate of hollow shaft and enters the hole, and flow downward along hollow shaft, flow out and come together in discharging ring 16 from discharge opening 15, discharge through discharging opening 8 again, solids content in the filtrate satisfies the technological requirement of subsequent product refining system less than 0.2ppm.