Technical background
The performance of nano material at aspects such as light, electricity, magnetic, mechanics and biology become the important subject of high and new technology, the general various materials that adopt the coprecipitation method preparation, especially after the nano-powder material synthetic reaction finishes, all can residual multiple zwitterion in the solution, and produce a large amount of by-product salt.Because the particle of nano-powder particle is little, specific area big, the surface chemistry effect is strong, have strong reunion trend, makes powder surface very easily adhere to foreign ion.When using the conventional method washing of unidirectional washing, foreign ion can not take off particle surface very soon and reach balance in washings, makes solid-liquid separation efficiency low, just makes that the utilization rate of washings is low, and consumes a large amount of washings, produces a large amount of industrial wastewaters simultaneously.Therefore under the condition of the performance that does not influence product, improve the washings utilization rate, not only be related to detersive efficiency and cost etc., and determined the benefit of factory, and problems such as service water and wastewater treatment.
Hydrotalcite layered crystal material (Layered Double Hydroxides for example, be called for short LDHs) in the coprecipitation production of industrial main employing, this method is mixed mixing salt solution and mixed ammonium/alkali solutions by suitable mode, make it to take place co-precipitation, then sedimentary suspension crystallization certain hour under the uniform temperature condition is obtained the LDHs slurries, go back a large amount of sodium salt of by-product (about 2 tons of/ton LDHs) simultaneously.And because also there is a large amount of raw material alkali in base excess in the system.LDHs product slurry deionized water flush away accessory substance sodium salt and excessive raw material alkali will be obtained.With getting the LDHs product slurry, finally obtain target product after the drying processing with deionized water flush away accessory substance sodium salt and excessive raw material alkali.
Produce in the production process of LDHs in coprecipitation, because the raw material base excess, a large amount of inorganic salts of by-product need wash with a large amount of water simultaneously.There is following shortcoming in traditional mode of washing: (1) washing methods is unidirectional water, the low salinity washings of the high salinity washings of last stage and after-stage all directly carry out waste water and reclaim, the washings utilization rate is low, water consumption is big, (2) washings of a large amount of saliferous and alkali directly discharging can cause the waste of raw material and, reclaim and then expend a large amount of energy the pollution of environment.Produce 1 ton of LDHs at present and need consume about 700 tons of water, not only wasted great amount of water resources, also reduced production efficiency, increased energy consumption, also limited the application of LDHs to a certain extent.Therefore the washing process of product becomes the key link that LDHs produces.
Separate the mother liquor that obtains after the crystallization owing to contain a large amount of by-product salt, generally all directly carry out wastewater treatment, but wherein contain a large amount of unreacted raw material alkali (0.6 ton of/ton LDHs), its pH value is more than 10, directly discharging has caused the significant wastage of raw material, how reasonably to recycle this part unreacted raw material alkali, also be problem demanding prompt solution always.
The research and the improvement of document [1] roll type PS version production line washing process, printed magazine, 2007 (7): among the 70-73, introduced the every grade of all corresponding recirculated water collection of washing storage tank in water-washing process, the aluminium plate that the technology groove high speed is moved continuously is after the flushing of many group spray booms, and washing water is collected through following cyclic water tank, pressurizes through centrifugal pump then, most of water is still beaten to former technology groove and is washed, the reach the last recirculated water storage tank of one-level of low amounts of water.The rest may be inferred, up to washing 1, the low amounts of water discharging arranged.Yet the method also is not suitable for being applied in the washing of superfine powder, otherwise can reduce the detersive efficiency of powder.
Document [2] has been introduced the membrane separation concentrated compression apparatus of superfine powder feed liquid in application number is 20050070757.4 patent application.This device is to use the filter membrane separating technology, makes to contain the continuous-flow in pipeline of superfine powder suspension liquid feed liquid, between circulation and inoranic membrane device and the material trough, liquid phase constantly sees through the separated collection of inoranic membrane, recycle stock is enrichment gradually, reaches the purpose of feed separation, has reduced running cost.
Summary of the invention
The purpose of this invention is to provide a kind of wash water jacket device of saving the washing nano-powder of washings consumption.
Washing separation device for wash water jacket of the present invention comprises: a slurry tank, a film separator-scrubber, a storage tank, a waste tank and one group of washings tank battery;
Slurry tank has a slurry inlet to be washed and DI inlet, and a discharging opening is connected with storage tank by blow-off valve; Slurry tank is connected with washings tank battery outlet pipe, and slurry tank is connected with the import of film separator-scrubber through dehvery pump;
Outlet of film separator-scrubber is connected with the slurry tank import, and another outlet is connected with the waste liquid tank import by three-way pipe and is connected with washings tank battery inlet;
The washings tank battery is composed in parallel by a plurality of storage tanks, and the entrance point of each storage tank is connected in parallel and is connected with film separator-scrubber outlet, and each port of export is connected in parallel through water pump and access slurry tank charging aperture after DI is in parallel; The quantity of tank battery is 3-10, and preferable is 4-6.
Waste tank is connected with the outlet of film separator-scrubber by draining valve.
The film separator-scrubber is made up of one group of film pipe and air compressor, and the quantity of film pipe is the 1-20 root, and the film pipe is parallel in the stainless steel bucket with parallel way, and described stainless steel bucket diameter is as the criterion can load the film pipe.The membrane aperture of said film pipe is 0.01~10 μ m, and film tube opening end is fixed on stainless steel bucket one end by a card and loam cake flange, and links to each other with mashing pump; Space between the film pipe links to each other with air compressor; The film pipe other end is fixed on the stainless steel bucket other end by flange, and links to each other with slurry tank by pipeline, and material can be circulated between film pipe and slurry tank.The material of film pipe can be pottery, metal or metal oxide.
The concrete operations step of this wash water jacket device is:
A. the washing of first slurry:
The 1st washing, squeeze into slurry tank (1) with waiting the slurry that washs powder, injecting deionized water also fully mixes, return slurry tank (1) after making slurry via film separating, washing unit (2) by mashing pump (6) and circulate, the fenestra of the saturating filmed passing tube of washings is discharged system in cyclic process, realizes that slurry concentrates; The washings of separating are entered in the waste liquid tank (5).
The 2nd washing, inject deionized water to slurry tank (1), fully after the mixing, return slurry tank (1) after making slurry via film separating, washing unit (2) by mashing pump (6) and circulate, in cyclic process, make the fenestra of the saturating filmed passing tube of washings discharge system, realize that slurry concentrates; The washings of separating are squeezed into washings storage tank (3
1) in.
The 3rd washing according to the washing operation second time, squeezed into washings storage tank (3 with washings
2) in.
Wash successively as stated above, to the n+1 time washing, add pure water, make the pH value less than 8, washings are squeezed into washings storage tank (3
n) in.
The phase I washing operation finishes, and the slurry in the slurry tank (1) is entered in the storage tank (4).
B. the washing of second batch of slurry:
The 1st washing squeezed into second batch of powdery pulp to be washed in the slurry tank (1) by inlet; Washings in the washings storage tank (31) are squeezed in the slurry tank (1); After fully mixing, return slurry tank (1) after making slurry via film separating, washing unit (2) by mashing pump (6), and circulate, realize that slurry concentrates; The washings of separating are entered in the waste liquid tank (5).
The 2nd washing is with washings storage tank (3
2) in washings squeeze in the slurry tank (1); After fully mixing, return slurry tank (1) after making slurry via film separating, washing unit (2) by mashing pump (6), slurry is circulated, and in cyclic process, make the fenestra of the saturating filmed passing tube of washings discharge system, realize that slurry concentrates; The washings of separating are squeezed into washings storage tank (3
1) in.
Wash successively as stated above, to the n+1 time washing, add pure water, make the pH value less than 8, washings are squeezed into washings storage tank (3
n) in.
After washing operation finishes, open bleeder valve K3, the solids slurry in the slurry tank (1) is entered in the storage tank (4).
C. the operation of repeating step B is washed the different batches slurry, adds pure water during to the n+1 time washing and washs, until washings storage tank (3
n) the pH value less than 8 o'clock, washing finishes;
Take out the full back of powdery pulp storage in the storage tank (4), obtains the powder finished product after drying.
The characteristics of this washing separation device for wash water jacket are: every grade of corresponding washings storage tank of washing.Slurry mixes with washings in the washings storage tank, be washed during by film separating, washing unit concentrate after, washings are put into waste liquid tank for the first time; Washings are collected the washings storage tank for the second time, carry out successively, wash with pure water when only washing the last time.The low salinity washings of the storage in the washings storage tank are used to wash the next batch product, and except that primary washings are put into the waste liquid tank, washings thereafter are stored in the washings storage tank again successively, cycling successively.Can be according to the quantity of the granularity that is washed slurry and impurity content design washings storage tank, and circulation cleaning number of times, i.e. 3≤n≤10.,
This washing separation device is applicable to the slurry washing of micron, submicron particle, for example hydrotalcite stratified material, ultrafine yttria, super fine zinc oxide etc.
Advantage of the present invention is:
1. can design the quantity of washings storage tank according to actual conditions, and the circulation cleaning number of times.
2. greatly improve the washings utilization rate, when guaranteeing clean result, reduced the slurry amount more than 70%, significantly reduced production cost, reached the purpose of energy-saving and emission-reduction.
3. the washing methods technology of Cai Yonging is simple, and cost is low, easy operating.
The specific embodiment
Referring to accompanying drawing, washing separation device for wash water jacket comprises: a slurry tank (1), it is volume 5m
3The polypropylene jar that stirs of band; Film separating, washing unit (2) is connected with slurry tank (1) through mashing pump (6), and employed film pipe is an inorganic film tube, and its film pipe number is 10, and membrane aperture is 0.05 μ m; With 5 10m
3Polypropylene washings storage tank import department be connected the discharge outlet of film separating, washing unit (2) through adapter, the port of export is connected with slurry tank (1) by water pump (7).Employed tube connector is a stainless steel tube between each equipment, and the 6-mashing pump is a plunger displacement pump,, the 7-water pump is centrifugal pump, wherein water valve is a stainless steel valve, blow-off valve is a stainless steel valve, 8-air compressor model is ZB-0.1/8; Intake valve is a stop valve; Pulp stock valve is a ball valve.
With hydrotalcite stratified material (LDHs) powdery pulp that this equipment for washing synthesizes with coprecipitation method, steps A-C washs according to aforesaid operations, to washings storage tank (3
n) the pH value less than 8 o'clock, washing finishes, and the slurry in the slurry tank (1) is entered in the storage tank (4), withdraws from circulation.Obtain the powder finished product after drying.
The LDHs powder that washing is obtained adopts means such as X-ray diffraction (XRD), fourier-transform infrared (FT-IR) and laser particle size analyzer to characterize the LDHs sample respectively, the LDHs sample that proof obtains has higher degree of crystallinity, grain size between 5-100nm, distribution of particles D
90(90% particle) less than 91nm, Na in the product
+Ion concentration is less than 0.01%, and product purity is greater than 99.9%.