CN105483372B - A kind of reaction, separation, washing, evaporation and drying integrated device and method - Google Patents

Abstract

A device and method integrating reaction, separation, washing, evaporation and drying belong to the field of hydrometallurgy and chemical industry. The device of the present invention is mainly composed of unitized compartments and auxiliary equipment. The compartments are connected by perforated partitions. According to different process combinations such as leaching reaction, separation and washing, crystallization and drying, and different processing objects, the perforated partitions are equipped with selected specific filter membranes. And install the upper and lower sealing rings to achieve the sealing of the compartment. According to the different processing objects, any several processes of leaching reaction, separation and washing, crystallization and drying are continuously completed in the compartment. The independent compartment space with high diameter-to-height ratio is conducive to the control of reaction conditions such as pressure, temperature, and stirring rate. The stirring scraper with holes is easy to accelerate solid-liquid two-phase with high solid-liquid ratio and high-concentration liquid phase reaction. Increase mass transfer rate. The invention has strong adaptability to process flow and processing capacity, can recycle energy, water and medicine, is clean and environment-friendly, and is easy to operate.

Description

An integrated device and method for reaction, separation, washing, evaporation and drying

technical field

The invention belongs to the field of hydrometallurgy and chemical industry, and relates to a high solid-liquid ratio solid-liquid two-phase, or high-concentration liquid phase leaching reaction, separation and washing, crystallization and drying in an integrated device and method. The device is mainly composed of a main device and an auxiliary device. The compartments are unitized, and the number of compartments is set according to the processing capacity. Compartment space with high diameter-to-height ratio, stirring scraper with holes is easy to accelerate solid-liquid two-phase with high solid-liquid ratio, and high-concentration liquid phase reaction and improve mass transfer efficiency, and the independent space is easy to pressure, temperature, stirring rate According to the different processing objects, several processes in the process of reaction, separation, washing, evaporation, crystallization and drying can be completed continuously and stably.

The invention has strong adaptability to technological process and processing capacity, can recycle energy, water and medicine, is clean and environment-friendly, easy to operate, and has broad application prospects.

Background technique

The leaching reaction is the process of selectively separating the target substance (valuable component or impurity) in the solid with the help of a solution. Even if the valuable component or harmful impurity in the solid material is selectively dissolved into the solvent, it usually depends on the participation of chemical reactions. In most cases Next, the processed materials are conventional metallurgical raw materials such as ores and concentrates. The traditional leaching reaction device is a reaction kettle, and the reaction materials are put into the reaction kettle, and the stirring leaching reaction is carried out at a certain temperature and pressure. Washing is usually to put the finished material into the dense pool for concentration, and use the countercurrent washing method to wash the reaction slag. The overflow part is collected as precious liquid and subjected to subsequent extraction process, and the underflow part is subjected to the second dense washing operation. The thickening overflow can be used as wash water for one thickening operation, and so on.

The patent "Multi-stage acid leaching, washing and filter press metal extraction integrated device" (CN203451588) includes a membrane filter press, an acid storage tank, a gas blowing tank and a back blowing gas tank, a pre-compression gas tank and a high-pressure gas tank. The device can Avoid slag filter cake breakage and maximize metal extraction. This device directly injects the metal acid leaching solution into the diaphragm filter press for press filtration. The leaching reaction and filtration operation are not performed on the same equipment. The second-stage acid leaching is carried out in the diaphragm filter press, but there is no stirring and heating function, so the second-stage Insufficient acid leaching reaction. The patent "a method of reflux leaching and washing mineral leaching materials" (CN102618720A) improves on the basis of the original classic dense washing, effectively utilizes unreacted residual acid, increases the vanadium content in the solution, and reduces follow-up operations The amount of solution, and reduce the amount of wastewater treatment, saving production costs. However, the washing method is dense washing, and a large amount of unreacted and complete residual acid still remains in the underflow solid phase, so the residual acid must be washed by increasing the number of washings. The leaching reaction and dense washing are carried out in different equipment, which increases the equipment cost. The equipment occupies a large area and the operation is cumbersome, and none of the above devices involves the technical fields of evaporation, crystallization and drying, and the reaction is limited to the traditional leaching reaction.

In view of the frequent transfer of materials in the traditional reaction, separation and washing process, the equipment occupies a large area and the effect of leaching, filtration and washing is not good, the reaction liquid phase is large and difficult to concentrate and purify, a set of reaction, separation, washing, evaporation and drying is designed. The device and method realize the perfect combination of the leaching device and the filtering and washing device. The equipment occupies a small area, has good thermal insulation performance, is easy to operate, clean water and chemicals are recycled, clean and environmentally friendly, and has broad application prospects.

Contents of the invention

The purpose of the present invention is to integrate the leaching reaction generator and the separation and washing device on the basis of the traditional leaching, filtering, and washing processes, so as to avoid the transfer of materials in each equipment, enhance the leaching and washing effects, and improve the protection of valuable components. Recovery, and this equipment can realize evaporation, crystallization and drying operations. The device and method of the present invention can carry out stirring and leaching reaction under the condition of certain pressure and temperature, and after the reaction is finished, can carry out decompression filtration on the device, and can also carry out countercurrent washing on the reaction slag phase through the device. And washing liquid and waste heat of exhaust gas can be recycled.

The present invention provides a high solid-liquid ratio, or high-concentration liquid-liquid leaching, pressure filtration, and washing device. The reaction device is divided into multiple compartments by partitions to form a high-diameter-height ratio reaction chamber. The reaction conditions are easy to control, and It is easy to carry out high solid-liquid ratio, or liquid-liquid ratio reaction. The compartments and other devices form a reaction system, a filter press system and a cleaning system. Multiple compartments work at the same time to continuously complete the leaching reaction, filter press and washing processes.

The integrated device for reaction, separation, washing, evaporation and drying is composed of a main device and an auxiliary device. The main device is composed of upper compartment sealing ring, partition, filter membrane, compartment lower sealing ring, device wall, heating system, safety valve, device top cover, multiple compartments, stirring scraper, device bottom plate, main shaft, set It is composed of liquid chamber, device bracket and shaft sleeve. The accessory device consists of pipeline, stirring paddle, liquid outlet valve A, liquid outlet valve B, liquid outlet valve C, liquid outlet valve D, clean water tank, washing liquid tank C, washing liquid tank B, washing liquid tank A, leaching liquid tank, cleaning liquid Water pump, third lotion pump C, second lotion pump B, lotion pump A, stirring motor, raw material tank, raw material pump, liquid inlet valve, raw material valve, flange, discharge door, air inlet and outlet valve, induced draft fan, connection Composed of trough and spindle motor.

The leaching, filtering and washing are all completed in the same compartment, that is, the compartment is a common part of the leaching system, the filtering system and the washing system. The compartments are connected by a partition, the partition is covered with a filter membrane, the lower sealing ring of the compartment is placed on the filter membrane, the upper sealing ring of the compartment is located on the top of the compartment, under the partition; the stirring scraper The device is welded on the shaft sleeve of the main shaft. There are round holes of uniform size in the middle and upper part of the stirring scraper. There is a discharge door on the wall of the device. The discharge door is equipped with an air inlet and outlet valve, a raw material valve, and a liquid inlet valve.

The reaction system includes a stirring motor, a raw material tank, a raw material pump, a raw material valve, a compartment, a main shaft, a main shaft motor, a stirring scraper, an air inlet and outlet valve, condensed water, and a condensed liquid tank. The evaporated gas passes through the condensing device, and the condensed water cools the gas evaporated from the compartment into a liquid, which is collected in the condensate tank.

The separation system includes an induced draft fan, liquid outlet valve A, liquid outlet valve B, liquid outlet valve C, liquid outlet valve D, leaching liquid tank or washing liquid tank A, or washing liquid tank B, or washing liquid tank C, or clean water The main shaft motor of the tank, the main shaft, the stirring scraper, the discharge door, and the receiving tank are composed. The safety valve in the filter press system is located at the top of the top cover of the device, the induced draft fan is connected to each compartment through the pipeline, and the liquid collection chamber is connected to the leachate tank through the pipeline and the liquid outlet valve.

The cleaning system includes a clean water pump, a lotion pump C, a lotion pump B, a lotion pump A, a clean water tank, a lotion tank C, a lotion tank B, a lotion tank A, an inlet valve, a spindle motor, a spindle, Stir scraper composition. In the cleaning system, the clean water tank, lotion tank C, lotion tank B, and lotion tank A are connected to each compartment through pipelines and corresponding screw pumps, and the clean water tank or lotion tank A, or lotion tank B, or lotion tank C is connected to the liquid collection chamber through pipes, liquid outlet valve A, liquid outlet valve B, liquid outlet valve C, and liquid outlet valve D, and the induced draft fan is connected to each compartment through pipes.

The compartment is composed of a discharge door, a lower sealing ring of the compartment, a filter membrane, a partition, an upper sealing ring of the compartment, and a stirring scraper, wherein the upper and lower sealing rings of the compartment and the sealing ring of the discharge door make the compartment It has good sealing performance, prevents the leakage of reaction liquid, slag or gas during the reaction, and ensures the independent space of each compartment. The diameter and aspect ratio of the compartments are determined according to the reaction requirements, and the number of compartments is determined by the production volume.

The distance between the edge of the stirring scraper and the device wall and the partition is between 0.5cm-1cm, and the middle and upper part of the stirring scraper has round holes of uniform size, and the diameter of the round hole is between 0.5cm-2cm; the partition Round holes are evenly distributed on the top, and the diameter of the round holes is between 1mm-3mm; the inner wall of the compartment in contact with the material and the stirring scraper are all materials with good corrosion resistance, such as polytetrafluoroethylene, Hastelloy, etc.; the separator The circular holes are evenly distributed on the top to ensure that the liquid phase can flow down through the partition to the liquid collection chamber and be collected during press filtration.

The integrated device for reaction, separation, washing, evaporation and drying is suitable for all solid-liquid two-phase or liquid-liquid reactions within a certain pressure range, specifically, including hydrometallurgy, solid The dissolution and crystallization of chemical industry products include solid-liquid two-phase reactions, hydrolysis of solid organic matter and other reactions.

A method for integrating reaction, separation, washing, evaporation and drying, which comprises the following steps when performing a liquid-solid two-phase leaching reaction without gas discharge:

1) Add the solids and liquids participating in the reaction into the raw material tank according to the ratio of the experimental design, turn on the stirring motor, rotate the stirring paddle to mix the reaction materials evenly, open the raw material pump and the raw material valve, and the raw material pump will transfer the reaction materials in the raw material tank through The pipeline is driven into each compartment, so that the material is just completely submerged on the top of the stirring scraper, and the raw material pump and raw material valve are closed;

2) Open the inlet and outlet valves, the exhaust gas with a certain temperature is pressed into each compartment, and close the inlet and outlet valves after the pressure is increased to 0.3MPa;

3) Turn on the main shaft motor, driven by the motor, the stirring scraper starts to rotate, so that the materials in the compartment are fully mixed;

4) Control the heating system to heat the materials in each compartment, and carry out solid-liquid two-phase leaching reaction at a temperature of 30-125°C;

5) After the reaction is finished, open the safety valve on the top of the device, start the induced draft fan, and perform pressure filtration on each compartment. The liquid phase permeates through the filter membrane and the partition with holes, and is collected in the liquid collection chamber. After the pressure filtration is complete, close the Induced fan, open the outlet valve D, collect the leachate in the leachate tank, close the outlet valve D;

6) Open the lotion pump B and the liquid inlet valve, input a certain amount of secondary lotion into each compartment, close the lotion pump B and the liquid inlet valve, turn on the spindle motor, and clean the leached residue once. , turn off the main shaft motor, start the induced draft fan, and perform a washing and pressure filtration on the leach slag; turn off the induced draft fan, open the liquid outlet valve C, collect the washing liquid once in the washing liquid tank A, and close the liquid outlet valve C;

7) Open the lotion pump C and the liquid inlet valve, input a certain amount of tertiary lotion into each compartment, close the lotion pump C, the liquid inlet valve, turn on the spindle motor, and perform secondary cleaning on the leached slag. , turn off the main shaft motor, start the induced draft fan, perform secondary washing and pressure filtration on the leached slag; close the induced draft fan, open the liquid outlet valve B, collect the secondary washing liquid in the washing liquid tank B, and close the liquid outlet valve B;

8) Turn on the clean water pump and liquid inlet valve, input a certain amount of clean water into each compartment, turn off the clean water pump and liquid inlet valve, turn on the main shaft motor, and clean the leached slag three times. Fan, wash and filter the leached slag three times; close the induced draft fan, open the liquid outlet valve A, collect the three times of washing liquid in the washing liquid tank C, and close the liquid outlet valve A;

9) Turn on the main shaft motor, the leaching slag is scraped up by the stirring scraper and concentrated on the edge of the compartment, turn off the main shaft motor, open the discharge door, manually collect the leaching slag in the receiving tank, and close the discharge door.

Above-mentioned step 1) and step 2) and step 3) can be carried out simultaneously, promptly feeding, air intake and agitation operation can be carried out simultaneously; In step 3) the distance of the edge of agitating scraper and device wall, dividing plate is appropriate, in During the leaching reaction, the solid material will not settle at the bottom of the compartment; the middle and upper part of the stirring scraper has circular holes of uniform size, and the lower layer of material is stirred up and passes through the circular hole in the middle and upper part of the stirring scraper. The materials in each reaction compartment are mixed evenly; in step 4), each reaction compartment is provided with a heating system, and the temperature control of the leaching reaction is realized by a temperature control device; the pore size of the filter membrane in step 5) is determined by the properties of the processed material However, during the leaching reaction, the liquid phase cannot pass through the filter membrane and enter the reaction compartment of the next layer.

Said step 5), step 6), step 7), and step 8) obtained leachate, primary lotion, secondary lotion, and the concentration of three lotions are successively reduced; wherein, the primary lotion obtained in step 6) can be obtained by a The lotion pump A is pumped into the raw material tank for reuse.

A method integrating reaction, separation, evaporation, crystallization and drying, when performing evaporation, crystallization and drying reactions with gas discharge, the following steps are included:

1) Add the solids and liquids participating in the reaction into the raw material tank according to the ratio of the experimental design, turn on the raw material stirring motor, rotate the stirring paddle to mix the reaction materials evenly, open the raw material pump and the raw material valve, and the raw material pump will transfer the reaction materials in the raw material tank Drive into each compartment through the pipeline, make the material just completely submerge the top of the stirring scraper, and close the raw material pump and raw material valve;

2) Turn on the main shaft motor, driven by the motor, the stirring scraper starts to rotate, so that the materials in the compartment are fully mixed;

3) Open the air inlet and outlet valves, control the heating system to heat the materials in each compartment, and carry out solid-liquid two-phase or liquid-liquid two-phase reaction at a temperature of 80°C;

4) Pass in condensed water to condense the steam passing through the inlet and outlet valves into a liquid phase and collect it in the condensate tank;

5) After the reaction is over, start the induced draft fan to perform pressure filtration on each compartment. The liquid phase permeates through the filter membrane and the perforated partition and is collected in the liquid collection chamber. After the pressure filtration is complete, close the induced draft fan and open the outlet Liquid valve D, collect the leachate in the leachate tank, close the liquid outlet valve D;

6) Turn on the lotion pump B and the liquid inlet valve, input a certain amount of secondary lotion into each compartment, close the lotion pump B and the liquid inlet valve, turn on the spindle motor, and clean the leached slag once. , turn off the main shaft motor, start the induced draft fan, and perform a washing and pressure filtration on the leach slag; turn off the induced draft fan, open the liquid outlet valve C, collect the washing liquid once in the washing liquid tank A, and close the liquid outlet valve C;

7) Open the lotion pump C and the liquid inlet valve, input a certain amount of tertiary lotion into each compartment, close the lotion pump C and the liquid inlet valve, turn on the main shaft motor, and perform secondary cleaning on the leached slag. , turn off the main shaft motor, start the induced draft fan, and perform secondary washing and pressure filtration on the leached slag; close the induced draft fan, open the liquid outlet valve B, collect the secondary washing liquid in the washing liquid tank B, and close the liquid outlet valve B;

8) Turn on the clean water pump and liquid inlet valve, input a certain amount of clean water into each compartment, close the clean water pump and liquid inlet valve, turn on the main shaft motor, and clean the leached slag three times. Fan, wash and filter the leached slag three times; close the induced draft fan, open the liquid outlet valve A, collect the three times of washing liquid in the washing liquid tank C, and close the liquid outlet valve A;

9) Turn on the main shaft motor, the leaching slag is scraped up by the stirring scraper and concentrated on the edge of the compartment, turn off the main shaft motor, open the discharge door, manually collect the leaching slag in the receiving tank, and close the discharge door.

The above steps 1) and 2) can be carried out simultaneously, that is, the feeding and stirring operations can be carried out simultaneously; each reaction compartment is provided with a heating system, and the temperature control of the leaching reaction is realized by a temperature control device; in step 5), The pore size of the filter membrane is determined by the properties of the material to be processed. During the leaching reaction, the liquid phase cannot pass through the filter membrane and enter the reaction compartment of the next layer.

The concentration of valuable ingredients and chemicals in the three washing liquids can determine the washing effect, and the number of washings can be reduced or increased according to the washing effect.

Compared with the prior art, a device and method integrating reaction, separation, washing, evaporation, crystallization and drying described in the present invention is composed of a plurality of high-diameter-height ratio compartments and auxiliary equipment to form a reaction device. The feature is: the compartment with high diameter-to-height ratio can realize the solid-liquid two-phase or high-concentration liquid phase leaching reaction with high liquid-solid ratio, which increases the concentration of valuable components in the leachate, which is beneficial to the subsequent concentration and purification of valuable components; The independent compartment space with a high diameter-to-height ratio is conducive to the control of reaction conditions such as pressure, temperature, and stirring rate; the leaching reaction, separation, washing, crystallization, and drying are carried out in the same device, avoiding the transmission and transportation of materials on various equipment According to the processing object, any of the above-mentioned processes can be completed continuously, and the operation is simple and convenient; each compartment is a unit that independently completes the above-mentioned processes, and the compartments are stacked on each other in space according to the processing capacity, which reduces the equipment occupation. Land area; the full use of tail gas has been realized. The tail gas can not only heat, but also increase the reaction pressure, promote the reaction, and improve the recovery rate of valuable components; the medicament in the primary washing liquid can be used again for leaching reaction , Due to the countercurrent cleaning of the reaction slag, the amount of cleaning water is saved, the cleaning effect is improved, and the content of pharmaceuticals and valuable components in the slag is reduced.

Description of drawings

Figure 1 is a schematic diagram of a device integrating reaction, separation, washing, evaporation, crystallization and drying.

Fig. 2 is the process flow diagram of the method of the present invention.

In Fig. 1, 1, stirring paddle, 2-5, liquid outlet valve, 6, clear water tank, 7, washing liquid tank C, 8, washing liquid tank B,

9, lotion tank A, 10, leaching solution tank, 11, clean water pump, 12, lotion pump C, 13, lotion pump B,

14. Lotion pump A, 15. Stirring motor, 16. Raw material tank, 17. Raw material pump,

18. Compartment upper sealing ring, 19. Partition plate, 20. Filter membrane, 21. Compartment lower sealing ring, 22. Device wall,

23. Liquid inlet valve, 24. Raw material valve, 25. Heating system, 26. Safety valve, 27. Device top cover,

28. Flange, 29. Discharge door, 30. Inlet and outlet valve, 31. Compartment, 32. Exhaust gas,

33. Stirring scraper, 34. Induced fan, 35. Feed tank, 36. Device bottom plate, 37. Main shaft motor,

38, main shaft, 39, liquid collection chamber, 40, device support, 41, axle sleeve, 42, condensed water,

43. Condensate tank.

Detailed ways

The present invention will be described in further detail below in conjunction with the accompanying drawings and specific embodiments. After being made into a material with a high liquid-solid ratio, leaching, separation, and washing are carried out according to the present invention. The specific steps have been introduced in detail in the specification of the present invention and will not be repeated here.

Example 1

High pressure and high temperature leaching, impurity removal, separation and washing of clay vanadium ore

The test raw material was taken from a clay vanadium mine in Hubei, and its chemical composition is shown in the following table:

It can be seen from the table that the main chemical components of the clay are SiO ₂ and Al ₂ O ₃ , and the grade of V ₂ O ₅ is 1.72%.

Crush the ore until the particle size is less than 3mm and account for 100%, add leaching aid MnO ₂ , the dosage is 3% to account for the mass fraction of clay vanadium ore, add sulfuric acid with a mass fraction of 20% to make a slurry with a solid-to-liquid ratio of 1:1.5 , pump the slurry into the reaction compartment, the stirring speed of the stirring scraper is 150r/min, feed the tail gas to pressurize the reaction pressure to 0.3MPa, heat the material in the reaction compartment through the heating device, at 80 ℃, The reaction pressure is 0.3Pa for leaching, and after 3 hours of reaction, filter to obtain the leaching liquid, wash the reaction residue three times, and discharge the leaching residue.

The grade of the obtained leaching residue was 0.184%, the leaching rate of vanadium after leaching was 96.35%, and the concentration of V ₂ O ₅ in the three washing liquids was 0.03g/L.

Experimental example 2

Acid leaching vanadium solution precipitation vanadium

The vanadium solution in this example is the leaching solution obtained by leaching in Example 1, the pH of the solution is adjusted to be 2.4, and the tetravalent vanadium ions are extracted with P204 organic phase, and then the sulfuric acid solution of 1.5mol/L is used as a stripping agent to remove Impurities in the acid leaching vanadium solution obtain a relatively pure vanadium-containing solution, and the solution composition is as shown in the table below:

Adjust the pH of the solution to 5, add the vanadium-containing solution and 250g/L NH ₄ Cl into the reaction compartment in equal volumes, the ammonium addition coefficient at this time is K=5, and the stirring speed of the stirring scraper is 150r/min, The liquid phase in the reaction compartment is heated by a heating device, and reacted at 30°C for 1 hour at a reaction pressure of 0.3 MPa to form precipitated sodium ammonium decavanadate. The sodium was washed twice, and finally the solid sodium ammonium decavanadate was collected.

The vanadium deposition rate is 98.53%.

Example 3

Straw Hydrolysis Sugar

The straw in this example is taken from a farmland in Xiaogan, Hubei, China. After natural air-drying, it is crushed to below 20 meshes. Its main components are hemicellulose, cellulose, lignin, and reducing sugar, and its moisture content is 6.23%.

Take straw samples under 20 mesh and mix them with sulfuric acid with a mass fraction of 5% to make a material with a solid-to-liquid ratio of 1:2. Use a pump to pump the mixture into the reaction compartment, and the stirring speed of the stirring scraper is 150r /min, feed tail gas and pressurize to the reaction pressure of 0.3MPa, soak in water at 125°C, react for 2 hours, filter to obtain the leachate, and wash the reaction slag three times with the washing method adopted in the present invention, and discharge Leach residue.

The hydrolyzed reducing sugar yield was 57.30%.

Experimental example 4

Fermentation of Corn Raw Meal to Ethanol

Test raw materials: corn flour, the starch content was determined to be 65.5%, the water content was 12.5%, the crude protein was 8.13%, the crude fiber was 0.94%, the crude fat was 4.03%, and the ash content was 1.09%.

Grinding the raw materials means that the particle size of the test raw materials is less than 0.35mm, the mass ratio of raw materials and water is: 1:2, and an appropriate amount of enzyme is added to promote fermentation. The type and amount of enzyme added are: glucoamylase 250u/g is the enzyme activity value unit), liquefaction enzyme 5u/g, acid protease 10u/g. The stirring speed of the stirring scraper is 50r/min, ferment at 30°C for 3 days, heat the fermentation liquid through the heating system, ethanol can be volatilized at 80°C, open the air inlet and outlet valves, pass in condensed water, and collect the ethanol liquid.

The concentration of ethanol was 76.7%, and the utilization rate of starch was 93.1%.

Experimental example 5

Magnesite acid leaching, impurity removal and crystallization to produce magnesium sulfate

The present embodiment raw material is low-grade magnesite, and its chemical element composition is as shown in the table:

The magnesite and sulfuric acid (volume ratio 1:1) solution is made into slurry according to the solid-to-liquid ratio of 1:1.5 (mass ratio), and it is quickly poured into the reaction compartment, and the inlet and outlet valves are opened to make the CO ₂ produced by the reaction Overflow through the condenser tube (or use the CO ₂ gas for other purposes), the stirring speed of the stirring scraper is 100r/min, react at 80°C for 2h, add hydrogen peroxide to oxidize Fe ²⁺ to Fe ³⁺ , use ammonia water Adjust the pH of the solution to 6, precipitate the Al ³⁺ and Fe ³⁺ generated in the reaction, press filter, wash the leaching residue 3 times to obtain a higher purity MgSO ₄ solution, clean up the slag in the reactor, and replace The specific filter membrane required for the crystallization of magnesium sulfate. Pump the collected _MgSO4 solution into the reaction compartment of the device again, the stirring speed of the scraper is 100r/min, heat the solution at 80°C, evaporate the water in the solution, and adjust the Baumé degree of the solution It is 46°Bé, and MgSO ₄ is crystallized at 80°C to obtain high-purity MgSO ₄ crystals.

Claims (8)

1. reaction unit, is divided into multiple by a kind of reaction, separation, washing, evaporation and drying integrated device by dividing plate (19) High blade diameter length ratio compartment (31), reaction condition is easily controllable, and is easy to carry out high solid-liquid ratio reaction, compartment (31) and other device groups Into reaction system, piece-rate system, purging system, multiple compartments (31) work simultaneously, are continuously finished Leach reaction, separation and washing Technological process；It is characterized in that：

1) integrated apparatus is made up of agent set and auxiliary equipment；Agent set by 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), every Room (31), stirring scratch board device (33), device bottom plate (36), main shaft (38), liquid collecting room (39), appliance stand (40), axle sleeve (41) Composition；Auxiliary equipment is by pipeline, agitating paddle (1), liquid valve A (2), liquid valve B (3), liquid valve C (4), liquid valve D (5), clear Water pot (6), washing lotion tank C (7), washing lotion tank B (8), washing lotion tank A (9), leach flow container (10), clarified water pump (11), lotion pumps C (12), Lotion pumps B (13), lotion pumps A (14), stirring motor (15), head tank (16), raw material pump (17), liquid feed valve (23), feed valve (24), flange (28), discharge door (29), air valve (30), air-introduced machine (34), splicing groove (35), spindle motor (37) composition；

The reaction, separation and washing are completed in same compartment (31), i.e., compartment (31) is leaching system, segregative line System, the common portion of washing system；Connected between compartment and compartment by dividing plate (19), filter membrane (20) covered on dividing plate (19), Compartment lower seal (21) is positioned on filter membrane (20), and sealing ring (18) is located at the top of compartment (31) on compartment, in dividing plate (19) under；Stirring scratch board device (33) is welded on the axle sleeve (41) of main shaft (38), and the middle and upper part of stirring scratch board device (33) is provided with Circular hole of uniform size, discharge door (29) is provided with device wall (22), air valve (30), raw material are housed on discharge door (29) Valve (24), liquid feed valve (23)；

Compartment (31) by sealing ring (18) on discharge door (29), compartment lower seal (21), filter membrane (20), dividing plate (19), compartment, Stirring scratch board device (33) form, wherein, compartment upper-lower seal circle (18), (21) and discharge door (29) sealing ring make compartment with compared with Good airtight performance, the leakage of reaction solution, slag or gas in reaction is prevented, ensure the space of each compartment independence, required according to reaction The diameter and blade diameter length ratio of compartment are determined, compartment quantity is determined by output；

The edge and device wall (22) of stirring scratch board device (33), the distance of dividing plate (19) are between 0.5cm-1cm, stirring scratch board device (33) Circularhole diameter is between 0.5cm-2cm；

Dividing plate is uniformly distributed circular hole on (19), and Circularhole diameter is between 1mm-3mm；To ensure that liquid phase can pass through when press filtration separates Dividing plate (19) is downwardly towards in liquid collecting room (39) and is collected；

Compartment (31), inwall, dividing plate (19), filter membrane (20), stirring scratch board device (33), sealing ring, the material of valve and pump, by it is anti- Product property determines after answering material and reaction；

2) reaction system includes stirring motor (15), head tank (16), raw material pump (17), feed valve (24), compartment (31), main shaft (38), spindle motor (37), stirring scratch board device (33), air valve (30), condensed water (42), condensate drum (43)；

3) piece-rate system include air-introduced machine (34), liquid valve A (2), liquid valve B (3), liquid valve C (4), liquid valve D (5), Leach flow container (10) or washing lotion tank A (9) or washing lotion tank B (8) or washing lotion tank 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；

Air-introduced machine (34) in piece-rate system is connected through pipeline with each compartment (31), and liquid collecting room (39) is through pipeline and liquid valve A (2), liquid valve B (3), liquid valve C (4), liquid valve D (5) are connected with leaching flow container (10)；

4) purging system includes clarified water pump (11), lotion pumps C (12), lotion pumps B (13), lotion pumps A (14), clean water tank (6), washing lotion tank C (7), washing lotion tank B (8), washing lotion tank A (9), liquid feed valve (23), spindle motor (37), main shaft (38), stirring are scraped Plate device (33) forms；

Clean water tank (6) in purging system, washing lotion tank C (7), washing lotion tank B (8), washing lotion tank A (9) through pipeline and corresponding screw pump with Each compartment (31) connection, clean water tank (6) or washing lotion tank A (9) or washing lotion tank B (8) or washing lotion tank C (7) are through pipeline and liquid valve A (2), liquid valve B (3), liquid valve C (4), liquid valve D (5) are connected with liquid collecting room (39), air-introduced machine (34) by pipeline with it is each Compartment (31) connects.

2. a kind of carry out liquid-solid two-phase using reaction, separation, washing, evaporation and drying integrated device described in claim 1 Or liquid-liquid diphase material reaction, separation, washing, evaporation and the method for drying, it is characterised in that carrying out the liquid without gas discharge Gu during two-phase Leach reaction, comprise the following steps：

1) solid for participating in reaction and liquid are empirically designed into proportioning to add in head tank (16), opens raw material stirring motor (15), agitating paddle (1), which rotates, is well mixed reaction mass, raw material pump (17) and feed valve (24) is opened, by raw material pump (17) Reaction mass in head tank (16) is squeezed into each compartment (31) through pipeline, material is just totally submerged stirring scratch board device (33) top, raw material pump (17) and feed valve (24) are closed；

2) air valve (30) is opened, the tail gas (32) with certain temperature is pressed into each compartment (31), increased to Air valve (30) is closed after 0.3MPa pressure；

3) spindle motor (37) is opened, under the drive of motor, stirring scratch board device (33) starts to rotate, and makes in compartment (31) Material is sufficiently mixed；

4) control heating system (25) to heat the material in each compartment (31), solid-liquid two is carried out at a temperature of 30-125 DEG C Phase, or liquid-liquid diphase reaction；

5) after question response terminates, start air-introduced machine (34), press filtration is carried out to each compartment (31), liquid phase passes through filter membrane (20) and band Hole dividing plate (19), it is collected in liquid collecting room (39), after press filtration is complete, closes air-introduced machine (34), open liquid valve D (5), receive Collect leachate in leaching in flow container (10), close liquid valve D (5)；

6) lotion pumps B (13), liquid feed valve (23) are opened, a certain amount of secondary cleaning water of input into each compartment (31), closes washing lotion Pump B (13) and liquid feed valve (23), spindle motor (37) is opened, leached mud is once cleaned, after cleaning terminates, close main shaft Motor (37), start air-introduced machine (34), once washing press filtration is carried out to leached mud；Air-introduced machine (34) is closed, opens liquid valve C (4) primary wash liquor, is collected in washing lotion tank A (9), closes liquid valve C (4)；

7) lotion pumps C (12) is opened, liquid feed valve (23), a certain amount of washing lotion three times of input into each compartment (31), closes washing lotion Pump C (12) and liquid feed valve (23), spindle motor (37) is opened, secondary cleaning is carried out to leached mud, after cleaning terminates, close main shaft Motor (37), start air-introduced machine (34), secondary washing press filtration is carried out to leached mud；Air-introduced machine (34) is closed, opens liquid valve B (3) secondary cleaning water, is collected in washing lotion tank B (8), closes liquid valve B (3)；

8) clarified water pump (11) is opened, liquid feed valve (23), a certain amount of clear water of input into each compartment (31), closes clarified water pump (11) With liquid feed valve (23), spindle motor (37) is opened, leached mud is cleaned three times, after cleaning terminates, close spindle motor (37), start air-introduced machine (34), washing and filter pressing three times is carried out to leached mud；Air-introduced machine (34) is closed, opens liquid valve A (2), is received Collect washing lotion three times and in washing lotion tank C (7), close liquid 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), closes Spindle motor (37), discharge door (29) is opened, leached mud is artificially collected among splicing groove (35), close discharge door (29).

3. a kind of liquid-solid two-phase according to claim 2 or liquid-liquid diphase material reaction, separation, washing, evaporation and drying Method, it is characterised in that the step 1) and step 2) and step 3) are carried out simultaneously.

A kind of 4. liquid-solid two-phase or liquid-liquid diphase material reaction, separation, washing, evaporation and drying according to claim 2 Method, it is characterised in that leachate that the step 5), step 6), step 7), step 8) obtain, primary wash liquor, secondary wash The concentration of liquid, three times washing lotion reduces successively；Wherein, the primary wash liquor that step 6) obtains can squeeze into head tank by lotion pumps A (14) (16) reuse.

5. a kind of carry out liquid-solid two-phase using reaction, separation, washing, evaporation and drying integrated device described in claim 1 Or liquid-liquid diphase material reaction, separation, washing, evaporation and the method for drying, have evaporation, crystallization that gas discharges and dry During dry reaction, it is characterised in that comprise the following steps：

1) solid for participating in reaction and liquid or liquid phase+liquid phase are empirically designed into proportioning to add in head tank (16), opened former Expect stirring motor (15), agitating paddle (1), which rotates, is well mixed reaction mass, opens raw material pump (17) and feed valve (24), by Raw material pump (17) squeezes into the reaction mass in head tank (16) in each compartment (31) through pipeline, material is just totally submerged At the top of stirring scratch board device (33), raw material pump (17) and feed valve (24) are closed；

2) spindle motor (37) is opened, under the drive of motor, stirring scratch board device (33) starts to rotate, and makes in compartment (31) Material is sufficiently mixed；

3) air valve (30) is opened, control heating system (25) heats to the material in each compartment (31), in 80 DEG C of temperature The reaction of the lower liquid-liquid diphase generation solid phase of degree, or it is evaporated crystallizing and drying operation；

4) condensed water (42) is passed through, the steam by air valve (30) is condensed into liquid phase, and be collected in condensate drum；

5) after question response terminates, start air-introduced machine (34), press filtration is carried out to each compartment (31), liquid phase passes through filter membrane (20) and band Hole dividing plate (19), it is collected in liquid collecting room (39), after press filtration is complete, closes air-introduced machine (34), open liquid valve D (5), receive Collect leachate in leaching in flow container (10), close liquid valve D (5)；

6) lotion pumps B (13), liquid feed valve (23) are opened, a certain amount of secondary cleaning water of input into each compartment (31), closes washing lotion Pump B (13) and liquid feed valve (23), spindle motor (37) is opened, solid phase is once cleaned, after cleaning terminates, close main shaft electricity Machine (37), start air-introduced machine (34), once washing press filtration is carried out to solid phase；Air-introduced machine (34) is closed, opens liquid valve C (4), is received Collect primary wash liquor in washing lotion tank A (9), close liquid valve C (4)；

7) lotion pumps C (12) is opened, liquid feed valve (23), a certain amount of washing lotion three times of input into each compartment (31), closes washing lotion Pump C (12) and liquid feed valve (23), spindle motor (37) is opened, secondary cleaning is carried out to solid phase, after cleaning terminates, close main shaft electricity Machine (37), start air-introduced machine (34), secondary washing press filtration is carried out to solid phase；Air-introduced machine (34) is closed, opens liquid valve B (3), is received Collect secondary cleaning water in washing lotion tank B (8), close liquid valve B (3)；

8) clarified water pump (11) is opened, liquid feed valve (23), a certain amount of clear water of input into each compartment (31), closes clarified water pump (11) With liquid feed valve (23), spindle motor (37) is opened, solid phase is cleaned three times, after cleaning terminates, closing spindle motor (37), Start air-introduced machine (34), washing and filter pressing three times is carried out to solid phase；Air-introduced machine (34) is closed, opens liquid valve A (2), is collected three times Washing lotion closes liquid valve A (2) in washing lotion tank C (7)；

9) spindle motor (37) is opened, solid phase is stirred scraper plate device (33) and sweeps and concentrate on the edge of compartment (31), closes master Spindle motor (37), discharge door (29) is opened, solid phase is artificially collected among splicing groove (35), close discharge door (29).

6. a kind of liquid-solid two-phase or liquid-liquid diphase material reaction, separation, washing, steaming according to claim 2 or claim 5 Hair and the method dried, it is characterised in that stirred in the step 2) of the step 3) or claim 6 of claim 2 The edge and device wall (22) of scraper plate device (33), the distance of dividing plate (19) are appropriate, and during Leach reaction, solid material is not Compartment (31) bottom can be fallen to；The middle and upper part of stirring scratch board device (33) point has circular opening of uniform size, lower floor's material It is stirred, through the circular hole of stirring scratch board device (33) middle and upper part, is well mixed each reaction compartments (31) interior material.

7. a kind of liquid-solid two-phase or liquid-liquid diphase material reaction, separation, washing, steaming according to claim 2 or claim 5 Hair and the method dried, it is characterised in that depending on the aperture of the filter membrane (20) in the step 5) is by handled material properties, leaching Going out liquid phase in course of reaction can not pass through in the reaction compartments that filter membrane (20) enters next layer.

8. a kind of liquid-solid two-phase or liquid-liquid diphase material reaction, separation, washing, steaming according to claim 2 or claim 5 Hair and the method dried, it is characterised in that each reaction compartments (31) are provided with heating system (25), and are realized by temperature control device The temperature of Leach reaction is controlled.