CN105483372A - Reaction, separation, washing, evaporation and drying integrated device and method - Google Patents
Reaction, separation, washing, evaporation and drying integrated device and method Download PDFInfo
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- CN105483372A CN105483372A CN201610035239.1A CN201610035239A CN105483372A CN 105483372 A CN105483372 A CN 105483372A CN 201610035239 A CN201610035239 A CN 201610035239A CN 105483372 A CN105483372 A CN 105483372A
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Abstract
The invention provides a reaction, separation, washing, evaporation and drying integrated device and method and belongs to the field of hydrometallurgy and the chemical industry. The device is mainly composed of unit partition chambers and accessory equipment. The partition chambers are connected through partition plates with holes, and according to different process combinations of the leaching reaction process, the separation and washing process, the crystallization and drying process and the like and different treatment objects, specific filtering films are selected and used for the partition plates with the holes, and upper sealing rings and lower sealing rings are arranged to seal the partition chambers. According to the different treatment objects, certain process procedures of the leaching reaction process, the separation and washing process and the crystallization and drying process are finished continuously in the partition chambers. By the adoption of the high-diameter high-ratio independent partition chamber space, control over the pressure, the temperature, the stirring speed and other reaction conditions is facilitated; and by the adoption of stirring scrapper devices with holes, the high-solid-liquid-ratio solid-liquid phase reaction and the high-concentration liquid phase reaction are easy to accelerate, and the mass transfer rate is increased. By the adoption of the method, adaptability to the procedures and treatment capacity is high, energy, water and chemicals can be used in a cyclic manner, cleanness and environment friendliness are achieved, and operation is convenient.
Description
Technical field
The invention belongs to hydrometallurgy and chemical field, relate to a kind of high solid-liquid ratio solid-liquid two-phase, or high density liquid phase Leaching reaction, separation and washing, crystallization and drying are in integrated apparatus and method.This device is formed primarily of agent set and auxiliary equipment, and compartment is having unit structure, according to treatment capacity setting compartment quantity.The compartment space of high blade diameter length ratio, stirring scratch board device with holes is easy to the solid-liquid two-phase accelerating high solid-liquid ratio, and high density liquid phase reaction and improve mass-transfer efficiency, and independently space is easy to the controls such as pressure, temperature, stir speed (S.S.), according to the difference of processing object, the several flow processs in reaction, separation, washing, evaporation, crystallization and drying process continuously, stably can be completed.
The present invention to technical process and processing power strong adaptability, energy, water and medicament reusable edible, clean environment firendly, easy to operate, have broad application prospects.
Background technology
Leaching reaction is exactly the process by desired substance in solution-selective separate solid (valuable constituent or impurity), even if the valuable constituent in solid materials or detrimental impurity are selectively dissoluted in solvent, usually the participation of chemical reaction is depended on, in most cases, handled material is that the metallurgical raw material of routine is as ore, concentrate.Tradition Leaching reaction device is reactor, is added by reaction mass in reactor, under certain temperature and pressure, carries out agitation leach reaction.The material that reaction terminates normally is squeezed into thickening pond and is concentrated by washing, the method of countercurrent washing is adopted to wash reaction slag, overflow portion as your liquid is collected and is carried out subsequent extracted technique, underflow part carries out the dense laundry operation of secondary, the dense overflow portion of secondary can be used as once the washing water of dense operation, the like.
Patent " the METAL EXTRACTION integrated apparatus of multistage acidleach, washing and press filtration " (CN203451588) comprises diaphragm filter press, sour storage tank, air blowing tank and blowback gas tank, precompressed gas tank and high pressure gas holder, this device can avoid slag filtrate cake bursting, and at utmost can extract metal.Metal acid immersion liquid is directly squeezed into diaphragm filter press and is carried out press filtration by this device, and not on the same device, two-stage acid leaching carries out in diaphragm filter press for Leaching reaction and filter operation, but does not stir and heating function, so two-stage acid leaching reaction is insufficient.Patent " a kind of method of leaching that refluxes, washing leaching of ores material " (CN102618720A) is improved on the basis of the dense washing of original classics, effectively utilize unreacted spent acid, improve the vanadiumcontent in solution simultaneously, decrease the amount of solution of subsequent job, and decrease wastewater treatment capacity, save production cost.But its washing methods is dense washing, still the complete spent acid of a large amount of unreacted is remained in underflow solid phase, spent acid could be cleaned so washing times will be increased, Leaching reaction and dense washing are carried out in different equipment, add equipment cost, equipment takes up an area comparatively large and complex operation, and above device does not all relate to the technical field of evaporation, crystallization and drying, and is confined to traditional Leaching reaction by reacting.
In view of classical inverse should, be separated and the transfer of washing process material frequent, occupation area of equipment is large and leach filtration washing poor effect, reaction solution phasor is greatly and not easily concentrated purifies, design and a kind ofly integrate reaction, separation, washing, evaporation and the device and method of drying, achieve the perfect adaptation of leaching device and filtration wash unit, the little and good heat insulating of occupation area of equipment, easy and simple to handle, clear water and medicament are recycled, and clean environment firendly has broad application prospects.
Summary of the invention
The object of the invention is on the basis of tradition leaching, filtration, washing process, by Leaching reaction producer and separating, washing apparatus integration, avoid the transfer of material in each equipment, strengthen leaching and washing effect, improve the recovery to valuable constituent, and this equipment can realize evaporation, crystallization and drying operation.Apparatus of the present invention and method both can carry out agitation leach reaction under the condition of certain pressure intensity and temperature, after question response terminates, can carry out filtration under diminished pressure on the apparatus again, also carry out countercurrent washing by this device mutually to reaction slag, medicament and washing lotion and using waste heat from tail gas all can be recycled.
A kind of high solid-liquid ratio provided by the invention, or high density liquid immersion goes out, press filtration, washing device, by dividing plate 19, reaction unit is divided into multiple compartment, forms high blade diameter length ratio reaction chamber, reaction conditions is easy to control, and is easy to carry out high solid-liquid ratio, or the reaction of liquid liquor ratio.Compartment and other device anabolic reaction system, press filteration system and cleaning system, multiple compartment works simultaneously, completes Leaching reaction, press filtration and washing process flow process continuously.
Described one reaction, separation, washing, evaporation and drying integrated gasifying device are made up of agent set and auxiliary equipment.Agent set is made up of sealing-ring, dividing plate, filter membrane, compartment lower seal, device wall, heating system, safety valve, device top cover, multiple compartment, stirring scratch board device, device base plate, main shaft, liquid collecting room, appliance stand, axle sleeve on compartment.Auxiliary equipment is made up of pipeline, stirring rake, liquid-outlet valve A, liquid-outlet valve B, liquid-outlet valve C, liquid-outlet valve D, clean water tank, washing lotion tank C, washing lotion tank B, washing lotion tank A, leaching flow container, fresh water pump, three lotion pumps C, two lotion pumps B, lotion pumps A, agitator motor, head tank, feedstock pump, liquid feed valve, feed valve, flange, discharge door, air valve, induced draft fan, splicing groove, spindle motor.
Described leaching, press filtration, washing are all complete in same compartment, and namely compartment is the public part of leaching system, press filteration system, washing system.Be connected by dividing plate between compartment with compartment, dividing plate covers filter membrane, compartment lower seal is positioned on filter membrane, and on compartment, sealing-ring is positioned at compartment top, under dividing plate; Stirring scratch board device is welded on the axle sleeve of main shaft, and the middle and upper part of stirring scratch board device is provided with circular hole of uniform size, and device wall is provided with discharge door, discharge door is equipped with air valve, feed valve, liquid feed valve.
Described reactive system agitator motor, head tank, feedstock pump, feed valve, compartment, main shaft, spindle motor, stirring scratch board device, air valve, water of condensation, condensate drum.Vaporised gas is through condensing works, and the gas cooling be evaporated by compartment is liquid by water of condensation, and is collected in condensate drum.
Described separation system comprises induced draft fan, liquid-outlet valve A, liquid-outlet valve B, liquid-outlet valve C, liquid-outlet valve D, leaches flow container or washing lotion tank A, or washing lotion tank B, or washing lotion tank C, or clean water tank spindle motor, main shaft, stirring scratch board device, discharge door, splicing groove composition.Safety valve in press filteration system is positioned at device top cover top, and induced draft fan is connected with each compartment through pipeline, and liquid collecting room is connected with leaching flow container with liquid-outlet valve through pipeline.
Described cleaning system comprises fresh water pump, lotion pumps C, lotion pumps B, lotion pumps A, clean water tank, washing lotion tank C, washing lotion tank B, washing lotion tank A, liquid feed valve, spindle motor, main shaft, stirring scratch board device composition.In cleaning system, clean water tank, washing lotion tank C, washing lotion tank B, washing lotion tank A are connected with each compartment with corresponding spiral pump through pipeline, clean water tank or washing lotion tank A, or washing lotion tank B, or washing lotion tank C is connected with liquid collecting room with liquid-outlet valve A, liquid-outlet valve B, liquid-outlet valve C, liquid-outlet valve D through pipeline, induced draft fan is connected with each compartment by pipeline.
Described compartment is made up of sealing-ring, stirring scratch board device on discharge door, compartment lower seal, filter membrane, dividing plate, compartment, wherein, compartment upper-lower seal circle and discharge door sealing-ring make compartment have good airtight performance, prevent the leakage of reaction solution, slag or gas in reacting, ensure each compartment independently space.Diameter and the blade diameter length ratio of determining compartment is required, by turnout determination compartment quantity according to reaction.
The distance of the edge of stirring scratch board device and device wall, dividing plate is between 0.5cm-1cm, and the middle and upper part of stirring scratch board device is divided and had circular hole of uniform size, and Circularhole diameter is between 0.5cm-2cm; Dividing plate is uniformly distributed circular hole, and Circularhole diameter is between 1mm-3mm; Compartment contacts inwall with material and stirring scratch board device is the good material of erosion resistance, such as tetrafluoroethylene, Hastelloy etc.; Dividing plate is uniformly distributed circular hole, is collected to ensure that when press filtration liquid phase flows in liquid collecting room by dividing plate downwards.
Described a kind of reaction, separation, washing, evaporation and drying are applicable to all solid-liquid two-phases within the scope of certain pressure intensity in the device of integration, or the reaction between liquid liquid, specifically, comprise field of hydrometallurgy, the dissolving of solid, crystallization, chemical field resultant contains the reaction such as the reaction of solid-liquid two-phase, the hydrolysis of SOLID ORGANIC matter.
Reaction, separation, washing, evaporation and a drying integrated method, when carrying out the liquid-solid two-phase Leaching reaction of discharging without gas, comprise the following steps:
1) solid and liquid that participate in reaction empirically being designed proportioning adds in head tank, open agitator motor, stirring rake rotates and reaction mass is mixed, open feedstock pump and feed valve, by feedstock pump, the reaction mass in head tank is squeezed in each compartment through pipeline, make material just complete submergence stirring scratch board device top, close feedstock pump and feed valve;
2) open air valve, the tail gas with certain temperature is pressed in each compartment, closes air valve after being increased to certain pressure;
3) open spindle motor, under the drive of electric motor, stirring scratch board device starts to rotate, and the material in compartment is fully mixed;
4) control heating system to heat the material in each compartment, carry out solid-liquid two-phase Leaching reaction at a certain temperature;
5) question response terminates rear opening unit top safety valve, and start induced draft fan, carry out press filtration to each compartment, liquid phase is through filter membrane and apertured partition, be collected in liquid collecting room, after press filtration completely, close induced draft fan, open liquid-outlet valve D, collect leach liquor in leaching flow container, close liquid-outlet valve D;
6) open lotion pumps B, liquid feed valve, in each compartment, input a certain amount of secondary cleaning water, close lotion pumps B, liquid feed valve, open spindle motor, leached mud is once cleaned, after cleaning terminates, close spindle motor, start induced draft fan, once washing press filtration is carried out to leached mud; Close induced draft fan, open liquid-outlet valve C, collect primary wash liquor in washing lotion tank A, close liquid-outlet valve C;
7) open lotion pumps C, liquid feed valve, in each compartment, input a certain amount of three washing lotions, close lotion pumps C, liquid feed valve, opens spindle motor, carries out secondary cleaning to leached mud, after cleaning terminates, close spindle motor 37, start induced draft fan, secondary washing press filtration is carried out to leached mud; Close induced draft fan, open liquid-outlet valve B, collect secondary cleaning water in washing lotion tank B, close liquid-outlet valve B;
8) open fresh water pump, liquid feed valve, in each compartment, input a certain amount of clear water, close fresh water pump, liquid feed valve, opens spindle motor, carries out three cleanings to leached mud, after cleaning terminates, close spindle motor, start induced draft fan, three washing and filter pressings are carried out to leached mud; Close induced draft fan, open liquid-outlet valve A, collect three washing lotions in three washing lotion tanks, close liquid-outlet valve A;
9) open spindle motor, leached mud is stirred scraper plate device and sweeps and the edge concentrating on compartment, closes spindle motor, opens discharge door, artificially collected by leached mud among splicing groove, closes discharge door.
Above-mentioned steps 1) and step 2) and step 3) can carry out, i.e. charging, air inlet and stirring operation can carry out simultaneously; simultaneously Described step 2) in pressure between 2-3 normal atmosphere; Step 3) in the edge of stirring scratch board device and device wall, dividing plate distance suitable, in the process of Leaching reaction, solid materials can not fall to cell bottom; The middle and upper part of stirring scratch board device is divided and is had circular opening of uniform size, and lower floor's material is stirred, and through the circular hole of stirring scratch board device middle and upper part, makes mixing of materials in each reaction compartments even; Step 4) in each reaction compartments be provided with heating system, and realize control to the temperature of Leaching reaction by temperature control unit; Step 5) in the aperture of filter membrane determined by handled material properties, in Leaching reaction process, liquid phase can not enter in the reaction compartments of lower one deck through filter membrane.
Described step 5), step 6), step 7), step 8) obtain leach liquor, primary wash liquor, secondary cleaning water, three washing lotions concentration reduce successively; Wherein, step 6) primary wash liquor that obtains can squeeze into head tank reuse by a lotion pumps A.
Integrate a method for reaction, separation, evaporation, crystallization and drying, the evaporation carrying out having gas to discharge, crystallization and dry reaction time, comprise the following steps:
1) solid and liquid that participate in reaction empirically being designed proportioning adds in head tank, open raw material stirring motor, stirring rake rotates and reaction mass is mixed, open feedstock pump and feed valve, by feedstock pump, the reaction mass in head tank is squeezed in each compartment through pipeline, make material just complete submergence stirring scratch board device top, close feedstock pump and feed valve;
2) open spindle motor, under the drive of electric motor, stirring scratch board device starts to rotate, and the material in compartment is fully mixed;
3) open air valve, control heating system and the material in each compartment is heated, carry out solid-liquid two-phase at a certain temperature, or liquid-liquid diphase reaction;
4) pass into water of condensation, make to become liquid phase by the vapor condensation of air valve, and be collected in condensate drum;
5), after question response terminates, start induced draft fan, carry out press filtration to each compartment, liquid phase is through filter membrane and apertured partition (19), be collected in liquid collecting room, after press filtration completely, close induced draft fan, open liquid-outlet valve D, collect leach liquor in leaching flow container, close liquid-outlet valve D;
6) open lotion pumps B, liquid feed valve, in each compartment, input a certain amount of secondary cleaning water, close two lotion pumps B and liquid feed valve, open spindle motor, leached mud is once cleaned, after cleaning terminates, close spindle motor, start induced draft fan, once washing press filtration is carried out to leached mud; Close induced draft fan, open liquid-outlet valve C, collect primary wash liquor in a washing lotion tank, close liquid-outlet valve C;
7) open lotion pumps C, liquid feed valve, in each compartment, input a certain amount of three washing lotions, close lotion pumps C and liquid feed valve, open spindle motor, secondary cleaning is carried out to leached mud, after cleaning terminates, close spindle motor, start induced draft fan, secondary washing press filtration is carried out to leached mud; Close induced draft fan, open liquid-outlet valve B, collect secondary cleaning water in two washing lotion tanks, close liquid-outlet valve B;
8) open fresh water pump, liquid feed valve, in each compartment, input a certain amount of clear water, close fresh water pump and liquid feed valve, open spindle motor, three cleanings are carried out to leached mud, after cleaning terminates, close spindle motor, start induced draft fan, three washing and filter pressings are carried out to leached mud; Close induced draft fan, open liquid-outlet valve A, collect three washing lotions in washing lotion tank C, close liquid-outlet valve A;
9) open spindle motor, leached mud is stirred scraper plate device and sweeps and the edge concentrating on compartment, closes spindle motor, opens discharge door, artificially collected by leached mud among splicing groove, closes discharge door.
Above-mentioned steps 1) and step 2) can carry out, namely charging and stirring operation can carry out simultaneously; simultaneously Each reaction compartments is provided with heating system, and realizes the control to the temperature of Leaching reaction by temperature control unit; Step 5) in the aperture of filter membrane determined by handled material properties, in Leaching reaction process, liquid phase can not enter in the reaction compartments of lower one deck through filter membrane.
In three washingss, the concentration of valuable constituent and medicament can judge washing effect, can reduce or increase washing times according to washing effect.
Compared with prior art, a kind of device and method integrating reaction, separation, washing, evaporation, crystallization and drying of the present invention, reaction unit is formed by multiple high blade diameter length ratio compartment and auxiliary facility, its feature is: the compartment of high blade diameter length ratio can realize solid-liquid two-phase or the high density liquid phase Leaching reaction of high liquid-solid ratio, add the concentration of valuable constituent in leach liquor, be conducive to the follow-up concentrated purification to valuable constituent; The individual compartment space of high blade diameter length ratio, is beneficial to the control realized reaction conditionss such as pressure, temperature, stir speed (S.S.)s; By Leaching reaction be separated and wash, crystallization and drying carry out in the same apparatus, avoids material on each equipment, transmit transport and the loss that causes, according to handling object, complete above-mentioned any several flow process continuously, simple to operation; Each compartment is the unit of the above-mentioned flow process of complete independently, according to treatment capacity, compartment is spatially mutually stacking, decreases occupation area of equipment; Achieve making full use of tail gas, tail gas both had heat effect, also can increase reaction pressure simultaneously, promoted the carrying out of reaction, improved the rate of recovery to valuable constituent; Medicament in primary wash liquor can be used as Leaching reaction again, owing to carrying out reflux type cleaning to reaction slag, saves the consumption of rinse water, improves cleaning performance, decrease the content of slag Chinese medicine and valuable constituent.
Accompanying drawing explanation
Fig. 1 is a kind of reaction, separation, washing, evaporation, crystallization and drying integrated device schematic diagram.
Fig. 2 is the process flow sheet of the inventive method.
In Fig. 1,1, stirring rake, 2-5, liquid-outlet valve, 6, clean water tank, 7, washing lotion tank C, 8, washing lotion tank B,
9, washing lotion tank A, 10, leach flow container, 11, fresh water pump, 12, lotion pumps C, 13, lotion pumps B,
14, lotion pumps A, 15, agitator motor, 16, head tank, 17, feedstock pump,
18, sealing-ring on compartment, 19, dividing plate, 20, filter membrane, 21, compartment lower seal, 22, device wall,
23, liquid feed valve, 24, feed valve, 25, heating system, 26, safety valve, 27, device top cover,
28, flange, 29, discharge door, 30, air valve, 31, compartment, 32, tail gas,
33, stirring scratch board device, 34, induced draft fan, 35, splicing groove, 36, device base plate, 37, spindle motor,
38, main shaft, 39, liquid collecting room, 40, appliance stand, 41, axle sleeve, 42, water of condensation,
43, condensate drum.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described in detail.After being made into high liquid-solid ratio material, undertaken leaching by the present invention, be separated, wash, concrete steps are introduced in detail in specification sheets of the present invention, repeat no more here.
Embodiment 1
The leaching of clay vanadium mineral high pressure-temperature, removal of impurities, separation and washing
Test raw material takes from Hubei clay vanadium mineral, and its chemical composition is as shown in the table:
As seen from table, in this clay, main chemical compositions is SiO
2and Al
2o
3, wherein with V
2o
5the grade of meter is 1.72%.
Ore reduction to particle diameter is less than 3mm and accounts for 100%, add leaching agent MnO
2, consumption is 3% massfraction accounting for clay vanadium mineral, add massfraction be 20% sulfuric acid be made into the ore pulp that solid-to-liquid ratio is 1:1.5, with pump, ore pulp is squeezed into reaction compartments, the stir speed (S.S.) of stirring scratch board device is 150r/min, and passing into tail gas, to be forced into reaction pressure be 0.3MPa, by heating unit to heating material in reaction compartments, 80 DEG C, reaction pressure leaches under being 0.3Pa, after reaction 3h, filter, obtain leach liquor, reaction slag carries out 3 washings, discharges leaching slag.
The leaching cinder grade obtained is 0.184%, and after leaching, the leaching yield of vanadium is V in 96.35%, three washingss
2o
5concentration be 0.03g/L.
Experimental example 2
The precipitation of acidleach vanadium liquid
Vanadium solution in the present embodiment is for leaching the leach liquor obtained in embodiment 1, regulator solution pH is 2.4, adopt P204 organic extractant phase tetravalent vanadium ion, then reverse-extraction agent is done with the sulphuric acid soln of 1.5mol/L, the impurity in acidleach vanadium liquid can be removed, obtain purer containing vanadium solution, solution composition is as shown in the table:
Regulator solution pH is 5, and this is contained the NH of vanadium solution and 250g/L
4cl equal-volume adds in reaction compartments, the ammonium coefficient that adds now is K=5, the stir speed (S.S.) of stirring scratch board device is 150r/min, by heating unit to liquid phase heating in reaction compartments, at 30 DEG C, under reaction pressure 0.3MPa, react 1h, generate precipitation ten ammonium vanadate sodium, reaction terminates rear press filtration and is separated solid-liquid two-phase, and washs 2 times with distilled water to ten ammonium vanadate sodium, finally collects solid ten ammonium vanadate sodium.
Precipitation rate is 98.53%.
Embodiment 3
Stalk hydrolysis sugaring
Stalk in this example takes from Hubei China Xiaogan farmland, and after natural air drying, be crushed to below 20 orders, its essential substance consists of hemicellulose, Mierocrystalline cellulose, xylogen, reducing sugar, and water ratio is 6.23%.
Get the lower straw sample of below 20 orders sieve, the sulfuric acid being 5% with massfraction mixes, and is made into the material that solid-to-liquid ratio is 1:2, with pump, mixture is squeezed into reaction compartments, the stir speed (S.S.) of stirring scratch board device is 150r/min, pass into tail gas and be forced into reaction pressure 0.3MPa, at 125 DEG C of temperature, carry out water logging, after reaction 2h, filter, obtain leach liquor, and with the mode of washing adopted in the present invention, 3 washings are carried out to reaction slag, discharge leaching slag.
Reductive hydrolysis sugar yield is 57.30%.
Experimental example 4
Ethanol Fermentation With Uncooked Corn
Test raw material: Semen Maydis powder, starch content is 65.5% after measured, moisture 12.5%, crude protein 8.13%, robust fibre 0.94%, crude fat 4.03%, ash content 1.09%.
That test raw material granularity is less than 0.35mm by raw material pulverizing, the mass ratio of raw material and water is: 1:2, and add appropriate enzymatic and to set out ferment, the kind and the consumption that add enzyme are: saccharifying enzyme 250u/g (wherein, u/g is the energy value unit of enzyme), α-amylase 5u/g, aspartic protease 10u/g.The stirring velocity of stirring scratch board device is 50r/min, and 30 DEG C of bottom fermentations 3 days, heated fermented liq by heating system, ethanol can evaporate at 80 DEG C, opens air valve, passes into water of condensation, collects containing ethanol liquid.
Alcohol concn is 76.7%, and starch utilization ratio is 93.1%.
Experimental example 5
Magnesite acidleach, removal of impurities, crystallization Sulphuric acid magnesium
The present embodiment raw material is low-grade magnesite, and it is as shown in the table for its chemical element composition:
Be that 1:1.5 (mass ratio) is made into ore pulp by this magnesite and sulfuric acid (volume ratio 1:1) solution by solid-to-liquid ratio, squeeze into rapidly in reaction compartments, open air valve, make the CO that reaction generates
2(or mobile phone CO is overflowed by prolong
2gas is separately used as him), the stirring velocity of stirring scratch board device is 100r/min, reacts 2h, adds hydrogen peroxide, make Fe at 80 DEG C
2+be oxidized to Fe
3+, be 6 with ammoniacal liquor regulator solution pH, make the Al generated in reaction
3+, Fe
3+precipitation, press filtration, washing leached mud 3 times, obtains the MgSO that purity is higher
4solution, cleans out the slag in reactor, and changes the specific filter membrane be applicable to required for magnesium sulfate crystallization.The MgSO obtained will be collected
4solution pump is squeezed in the reaction compartments of this device again, and the stirring velocity of stirring scratch board device is 100r/min, heats this solution, moisture in evaporating solns at 80 DEG C, and regulator solution degree Beaume is 46 ° of B é, and makes MgSO at 80 DEG C
4crystallization, obtains high-purity MgSO
4crystal.
Claims (10)
1. a reaction, separation, washing, evaporation and drying integrated device, by dividing plate (19), reaction unit is divided into multiple high blade diameter length ratio compartment (31), reaction conditions is easy to control, and be easy to carry out high solid-liquid ratio reaction, compartment (31) and other device anabolic reaction system, separation system, cleaning systems, multiple compartment (31) works simultaneously, completes Leaching reaction, separation and washing process flow process continuously; It is characterized in that:
1) integrated apparatus is made up of agent set and auxiliary equipment, agent set is made up of sealing-ring on compartment (18), dividing plate (19), filter membrane (20), compartment lower seal (21), device wall (22), heating system (25), safety valve (26), device top cover (27), compartment (31), stirring scratch board device (33), device base plate (36), main shaft (38), liquid collecting room (39), appliance stand (40), axle sleeve (41), auxiliary equipment is by pipeline, stirring rake (1), liquid-outlet valve A (2), liquid-outlet valve B (3), liquid-outlet valve C (4), liquid-outlet valve D (5), clean water tank (6), washing lotion fills with C (7), washing lotion fills with B (8), washing lotion fills with A (9), leach flow container (10), fresh water pump (11), lotion pumps C (12), lotion pumps B (13), lotion pumps A (14), agitator motor (15), head tank (16), feedstock pump (17), liquid feed valve (23), feed valve (24), flange (28), discharge door (29), air valve (30), induced draft fan (34), splicing groove (35), spindle motor (37) forms,
Described reaction, separation and washing are all complete in same compartment (31), and namely compartment (31) is the public part of leaching system, separation system, washing system; Be connected by dividing plate (19) between compartment with compartment, dividing plate (19) covers filter membrane (20), compartment lower seal (21) is positioned on filter membrane (20), on compartment, sealing-ring (18) is positioned at compartment (31) top, under dividing plate (19); Stirring scratch board device (33) is welded on the axle sleeve (41) of main shaft (38), the middle and upper part of stirring scratch board device (33) is provided with circular hole of uniform size, device wall (22) is provided with discharge door (29), discharge door (29) is equipped with air valve (30), feed valve (24), liquid feed valve (23);
2) reactive system comprises agitator motor (15), head tank (16), feedstock pump (17), feed valve (24) compartment (31), main shaft (38), spindle motor (37), stirring scratch board device (33), air valve (30), water of condensation (42), condensate drum (43);
3) described separation system comprise induced draft fan (34), liquid-outlet valve A (2), liquid-outlet valve B (3), liquid-outlet valve C (4), liquid-outlet valve D (5), leach flow container (10) or washing lotion fill with A (9) washing lotion fill with B (8) or washing lotion fill with C (7) or clean water tank (6), spindle motor (37), main shaft (38), stirring scratch board device (33), discharge door (29), splicing groove (35) composition;
Induced draft fan (34) in separation system is connected with each compartment (31) through pipeline, and liquid collecting room (39) is connected with leaching flow container (10) with liquid-outlet valve A (2), liquid-outlet valve B (3), liquid-outlet valve C (4), liquid-outlet valve D (5) through pipeline;
4) described cleaning system comprises fresh water pump (11), lotion pumps C (12), lotion pumps B (13), lotion pumps A (14), clean water tank (6), washing lotion fills with C (7), washing lotion fills with B (8), washing lotion fills with A (9), liquid feed valve (23), spindle motor (37), main shaft (38), stirring scratch board device (33) composition;
In cleaning system, clean water tank (6), washing lotion tank C (7), washing lotion tank B (8), washing lotion tank A (9) are connected with each compartment (31) with corresponding spiral pump through pipeline, clean water tank (6) or washing lotion fill with A (9) or washing lotion fills with B (8) or washing lotion filling C (7) is connected with liquid collecting room (39) with liquid-outlet valve A (2), liquid-outlet valve B (3), liquid-outlet valve C (4), liquid-outlet valve D (5) through pipeline, and induced draft fan (34) is connected with each compartment (31) by pipeline.
2. a kind of reaction according to claim 1, separation, washing, evaporation and drying integrated device, is characterized in that,
1) compartment (31) is made up of sealing-ring (18), stirring scratch board device (33) on discharge door (29), compartment lower seal (21), filter membrane (20), dividing plate (19), compartment, wherein, compartment upper-lower seal circle (18), (21) and discharge door (29) sealing-ring make compartment have good airtight performance, prevent the leakage of reaction solution, slag or gas in reacting, ensure each compartment independently space, diameter and the blade diameter length ratio of determining compartment is required, by turnout determination compartment quantity according to reaction;
2) distance of the edge of stirring scratch board device (33) and device wall (22), dividing plate (19) is between 0.5cm-1cm, the middle and upper part of stirring scratch board device (33) is divided and is had circular hole of uniform size, and Circularhole diameter is between 0.5cm-2cm;
3) dividing plate (19) is uniformly distributed circular hole, Circularhole diameter is between 1mm-3mm; To ensure that liquid phase flows in liquid collecting room (39) by dividing plate (19) and is collected when press filtration is separated downwards;
4) material of compartment (31), inwall, dividing plate (19), filter membrane (20), stirring scratch board device (33), sealing-ring, valve and pump, is determined by institute's reaction mass and reaction after product characteristic.
3. one kind adopt described in claim 1 or 2 react, be separated, washing, evaporation and drying integrated device carry out liquid-solid two-phase or liquid-liquid diphase material reaction, be separated, washing, evaporation and drying method, it is characterized in that, when carrying out the liquid-solid two-phase Leaching reaction of discharging without gas, comprising the following steps:
1) solid and liquid that participate in reaction empirically being designed proportioning adds in head tank (16), open raw material stirring motor (15), stirring rake (1) rotates and reaction mass is mixed, open feedstock pump (17) and feed valve (24), by feedstock pump (17), the reaction mass in head tank (16) is squeezed in each compartment (31) through pipeline, make material just complete submergence stirring scratch board device (33) top, close feedstock pump (17) and feed valve (24);
2) open air valve (30), the tail gas (32) with certain temperature is pressed in each compartment (31), closes air valve (30) after being increased to certain pressure;
3) open spindle motor (37), under the drive of electric motor, stirring scratch board device (33) starts to rotate, and the material in compartment (31) is fully mixed;
4) control heating system (25) to heat the material in each compartment (31), carry out solid-liquid two-phase at a certain temperature, or liquid-liquid diphase reaction;
5) after question response terminates, start induced draft fan (34), press filtration is carried out to each compartment (31), liquid phase, through filter membrane (20) and apertured partition (19), is collected in liquid collecting room (39), after press filtration completely, close induced draft fan (34), open liquid-outlet valve D (5), collect leach liquor in leaching flow container (10), close liquid-outlet valve D (5);
6) lotion pumps B (13), liquid feed valve (23) is opened, a certain amount of secondary cleaning water of input in each compartment (31), close lotion pumps B (13) and liquid feed valve (23), open spindle motor (37), leached mud is once cleaned, after cleaning terminates, close spindle motor (37), start induced draft fan (34), once washing press filtration is carried out to leached mud; Close induced draft fan (34), open liquid-outlet valve C (4), collect primary wash liquor in washing lotion tank A (9), close liquid-outlet valve C (4);
7) lotion pumps C (12) is opened, liquid feed valve (23), a certain amount of three washing lotions of input in each compartment (31), close lotion pumps C (12) and liquid feed valve (23), open spindle motor (37), secondary cleaning is carried out to leached mud, after cleaning terminates, close spindle motor (37), start induced draft fan (34), secondary washing press filtration is carried out to leached mud; Close induced draft fan (34), open liquid-outlet valve B (3), collect secondary cleaning water in washing lotion tank B (8), close liquid-outlet valve B (3);
8) fresh water pump (11) is opened, liquid feed valve (23), a certain amount of clear water of input in each compartment (31), close fresh water pump (11) and liquid feed valve (23), open spindle motor (37), three cleanings are carried out, after cleaning terminates to leached mud, close spindle motor (37), start induced draft fan (34), three washing and filter pressings are carried out to leached mud; Close induced draft fan (34), open liquid-outlet valve A (2), collect three washing lotions in washing lotion tank C (7), close liquid-outlet valve A (2);
9) spindle motor (37) is opened, leached mud is stirred scraper plate device (33) and sweeps and concentrate on the edge of compartment (31), close spindle motor (37), open discharge door (29), leached mud is artificially collected among splicing groove (35), close discharge door (29).
4. the method for a kind of liquid-solid two-phase according to claim 3 or liquid-liquid diphase material reaction, separation, washing, evaporation and drying, is characterized in that, described step 2) in pressure between 2-3 normal atmosphere.
5. the method for a kind of liquid-solid two-phase according to claim 3 or liquid-liquid diphase material reaction, separation, washing, evaporation and drying, is characterized in that, described step 1) and step 2) and step 3) carry out simultaneously.
6. a kind of method of liquid-solid two-phase or liquid-liquid diphase material reaction, separation, washing, evaporation and drying according to claim 3, it is characterized in that, described step 5), step 6), step 7), step 8) obtain leach liquor, primary wash liquor, secondary cleaning water, three washing lotions concentration reduce successively; Wherein, step 6) primary wash liquor that obtains can squeeze into head tank (16) reuse by lotion pumps A (14).
7. adopt a method for a kind of liquid-solid two-phase described in claim 1 or 2 or liquid-liquid diphase material reaction, separation, washing, evaporation and drying, the evaporation carrying out having gas to discharge, crystallization and dry reaction time, it is characterized in that comprising the following steps:
1) solid and liquid (or liquid phase+liquid phase) that participate in reaction empirically being designed proportioning adds in head tank (16), open raw material stirring motor (15), stirring rake (1) rotates and reaction mass is mixed, open feedstock pump (17) and feed valve (24), by feedstock pump (17), the reaction mass in head tank (16) is squeezed in each compartment (31) through pipeline, make material just complete submergence stirring scratch board device (33) top, close feedstock pump (17) and feed valve (24);
2) open spindle motor (37), under the drive of electric motor, stirring scratch board device (33) starts to rotate, and the material in compartment (31) is fully mixed;
3) open air valve (30), control heating system (25) and heat the material in each compartment (31), liquid-liquid diphase generates the reaction of solid phase at a certain temperature, or carries out evaporative crystallization drying operation;
4) pass into water of condensation (42), make to become liquid phase by the vapor condensation of air valve (30), and be collected in condensate drum;
5) after question response terminates, start induced draft fan (34), press filtration is carried out to each compartment (31), liquid phase, through filter membrane (20) and apertured partition (19), is collected in liquid collecting room (39), after press filtration completely, close induced draft fan (34), open liquid-outlet valve D (5), collect leach liquor in leaching flow container (10), close liquid-outlet valve D (5);
6) lotion pumps B (13), liquid feed valve (23) is opened, a certain amount of secondary cleaning water of input in each compartment (31), close lotion pumps B (13) and liquid feed valve (23), open spindle motor (37), solid phase is once cleaned, after cleaning terminates, close spindle motor (37), start induced draft fan (34), once washing press filtration is carried out to solid phase; Close induced draft fan (34), open liquid-outlet valve C (4), collect primary wash liquor in washing lotion tank A (9), close liquid-outlet valve D (4);
7) three lotion pumps (12) are opened, liquid feed valve (23), a certain amount of three washing lotions of input in each compartment (31), close three lotion pumps (12) and liquid feed valve (23), open spindle motor (37), secondary cleaning is carried out to solid phase, after cleaning terminates, close spindle motor (37), start induced draft fan (34), secondary washing press filtration is carried out to solid phase; Close induced draft fan (34), open liquid-outlet valve (3), collect secondary cleaning water in two washing lotion tanks (8), close liquid-outlet valve (3);
8) fresh water pump (11) is opened, liquid feed valve (23), a certain amount of clear water of input in each compartment (31), close fresh water pump (11) and liquid feed valve (23), open spindle motor (37), three cleanings are carried out, after cleaning terminates to solid phase, close spindle motor (37), start induced draft fan (34), three washing and filter pressings are carried out to solid phase; Close induced draft fan (34), open liquid-outlet valve A (2), collect three washing lotions in washing lotion tank C (7), close liquid-outlet valve A (2);
9) spindle motor (37) is opened, solid phase is stirred scraper plate device (33) and sweeps and concentrate on the edge of compartment (31), close spindle motor (37), open discharge door (29), solid phase is artificially collected among splicing groove (35), close discharge door (29).
8. a kind of method of liquid-solid two-phase or liquid-liquid diphase material reaction, separation, washing, evaporation and drying according to claim 3 or claim 7, it is characterized in that, described step 3) in the edge of stirring scratch board device (33) and device wall (22), dividing plate (19) distance suitable, in the process of Leaching reaction, solid materials can not fall to compartment (31) bottom; The middle and upper part of stirring scratch board device (33) is divided and is had circular opening of uniform size, and lower floor's material is stirred, and through the circular hole of stirring scratch board device (33) middle and upper part, makes each reaction compartments (31) interior mixing of materials even.
9. a kind of method of liquid-solid two-phase or liquid-liquid diphase material reaction, separation, washing, evaporation and drying according to claim 3 or claim 7, it is characterized in that, described step 5) in the aperture of filter membrane (20) determined by handled material properties, in Leaching reaction process, liquid phase can not enter in the reaction compartments of lower one deck through filter membrane (20).
10. a kind of method of liquid-solid two-phase or liquid-liquid diphase material reaction, separation, washing, evaporation and drying according to claim 3 or claim 7, it is characterized in that, each reaction compartments (31) is provided with heating system (25), and realizes controlling the temperature of Leaching reaction by temperature control unit.
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| CN111494985A (en) * | 2020-05-25 | 2020-08-07 | 张掖征峰科技有限公司 | Multistage continuous countercurrent washing leaching equipment and method |
| CN117463394A (en) * | 2023-12-27 | 2024-01-30 | 内蒙古工业大学 | Preparation method and application of sulfate radical adsorption self-assembled PDI photocatalyst |
| CN117463394B (en) * | 2023-12-27 | 2024-03-12 | 内蒙古工业大学 | Preparation method and application of sulfate radical adsorption self-assembled PDI photocatalyst |
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