CN116119676B - Integrated process method and device for series three-phase flow pickling high-purity quartz sand - Google Patents
Integrated process method and device for series three-phase flow pickling high-purity quartz sand Download PDFInfo
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Abstract
The utility model belongs to the field of quartz sand purification, and relates to an integrated process method and device for series three-phase flow pickling high-purity quartz sand, wherein quartz sand with purity of 99.6-99.8% and granularity of 120-40 meshes is selected, quartz sand to be washed sequentially enters a 1 st-stage pickling tank, a 2 nd-stage pickling tank … … nth-stage pickling tank and is finally discharged from the nth-stage pickling tank; the pickling solution sequentially enters an N-level pickling tank … …, a 2-level pickling tank and a 1-level pickling tank; the upper part of the pickling tank is cylindrical, the lower part of the pickling tank is conical, the bottom of the pickling tank is connected with an air inlet pipeline, and compressed gas is introduced through the air inlet pipeline to form a gas-solid-liquid upward mixed flow. Replaces the rotary dynamic cleaning mode of the reaction kettle, and reduces the energy consumption. The reverse acid washing is adopted, the acid washing driving force is improved, the purity of quartz sand is gradually improved, and the purity can reach 99.99% -99.999%.
Description
Technical Field
The utility model belongs to the field of high-purity quartz sand purification, and particularly relates to an integrated process method and device for pickling high-purity quartz sand by using a series three-phase flow.
Background
The quartz is a silicate mineral with hardness, wear resistance and stable chemical property, and the quartz sand is quartz particles prepared by the steps of crushing, screening, acid washing, water washing, calcining and the like. China generally subdivides quartz sand by the difference of silicon dioxide and ferric oxide contents, and mainly divides the quartz sand into common quartz sand, refined quartz sand and high-purity quartz sand.
Common quartz sand: siO (SiO) 2 The content is more than or equal to 90-99%, fe 2 O 3 The content is less than or equal to 0.06-0.02 percent, and the main application is as follows: common glass, casting, refractory materials;
refining quartz sand: siO (SiO) 2 The content is more than or equal to 99 to 99.5 percent, fe 2 O 3 The content is less than or equal to 0.005 percent, and the main application is as follows: optical, instrument glass, etc.;
high-purity quartz sand: siO (SiO) 2 The content is more than or equal to 99.5 to 99.9 percent, fe 2 O 3 The content is less than or equal to 0.001 percent, and the main application is as follows: the optical glass and special glass are produced, the semiconductor material is widely applied to high-end manufacturing industries such as semiconductors, optical fibers, photovoltaic materials, light source materials, aerospace and the like, is also the most important raw material for producing monocrystalline silicon, and has higher added value.
The export unit price of the high-purity quartz sand is quite different, wherein the export unit price of the high-purity quartz deep-processing products is higher in the United states, japan, korea, germany and other countries. And China, spanish and the like mainly export high-purity quartz primary products. Especially, the demand for silicon crystal materials is higher and higher, and impurities are removed from high-purity quartz sand through deep purification again, so that SiO is obtained 2 The purity of (3) reaches 99.99 percent,even 99.999 percent, the refining difficulty is very high and the cost is high.
The purification of high-purity quartz sand is very serious in environmental pollution unlike the pickling process used in the purification process of the natural quartz sand and gangue quartz sand reproduction quartz sand, that is, the pickling production of quartz sand is strictly controlled by the country. The high-purity quartz sand is obtained by magnetic separation and acid floatation of quartz sand with low natural grade (generally SiO) 2 Less than 99.9%) and purifying again. In the purification process of high-purity quartz sand, the particle size of the raw quartz sand is 0.1mm, namely 100 microns, and the raw quartz sand is even finer, so that the smaller the particle size is, the better the purification effect of the quartz sand is, but the smaller the quartz sand is, the more expensive the quartz sand processing itself is.
CN206970230U discloses a dynamic high-temperature pickling device for high-purity quartz sand, which comprises a reaction kettle, wherein the reaction kettle is in a double-cone shape, and a hollow hot oil jacket is wrapped on the outer wall of the reaction kettle; the hot oil jacket is connected with the heating system through a heat conduction oil pipe; the upper end and the lower end of the reaction kettle are respectively provided with an openable end cover, and the end covers are communicated with a vacuum system through vacuum pipes and can be used for vacuumizing the reaction kettle; the two sides of the reaction kettle are provided with rotating shafts which are respectively connected with two groups of rotating support units, so that the reaction kettle can rotate up and down; the vacuum tube is provided with a plurality of quick connectors, and other pipelines are connected after the quick connectors are convenient to detach. The working process is as follows: the upper end cover is opened first, the material to be treated is then filled with strong acid solution, such as hydrofluoric acid, hydrochloric acid, etc. or strong alkali solution, such as sodium hydroxide, etc. according to the material characteristic. Simultaneously, a heating system is started, the temperature of the hot oil furnace is increased, and the highest temperature of the heat conduction oil is controlled to be 200 ℃. And (5) covering an end cover to enable the reaction kettle to rotate. According to the product requirement, the temperature of the heat conduction oil is arbitrarily selected to be constant before reaching 160 ℃ by a manual measurement method. And stopping rotating the reaction kettle after the constant temperature is finished. Simultaneously, the heating system is closed, and the pickling solution in the reaction kettle is discharged. Then the upper end cover is opened, the quick connector of the vacuum tube on the lower end cover is detached, and then the water pipe is connected to inject pure water into the reaction kettle. Pure water overflows from the upper port after passing through the materials from bottom to top, so that the materials in the reaction kettle are washed. The overflowed aqueous solution is collected via a water tray. The water washing process is carried out until the aqueous solution of the cleaning material reaches neutrality. After the cleaning, stopping water injection, and removing free water in the material from the water injection port. Then, cover the end cover, make reation kettle rotatory, open heating system and vacuum system simultaneously, heat and the evacuation to reation kettle, dry the material. And after the materials are dried, opening the end cover, discharging the materials, and packaging and warehousing.
CN206970230U is a process device for pickling high-purity quartz sand applied by Jiangsu Pacific quartz corporation, and the process device realizes dynamic cleaning through a rotary reaction kettle, but has too high energy consumption, and cannot realize continuous production, and more importantly, pickling solution is not well recycled, a treatment method of pickling waste liquid is not written, practical application is difficult, and the environment may be damaged.
CN112441590a discloses a quartz sand pickling method and device, comprising a pickling bed with a cavity for placing quartz sand; one side of the pickling bed is provided with a pickling device for conveying acid liquor from the lower part of the cavity to the bottom of the quartz sand and a gas supply device for conveying compressed air into the cavity. The inside adopts a gas distribution device, compressed air is utilized to be introduced into quartz sand submerged by acid liquid to promote bubbling in an acid bed, and the whole gas-liquid-solid mixed state is formed, so that the efficiency is low and the energy consumption is high. And the device is only provided with one pickling bed, if the concentration of the pickling liquid is low, the pushing of the pickling process is small, the time spent is long, the treatment capacity in unit time is reduced, and the efficiency is reduced. If the concentration of the pickle liquor discharged is too high, the subsequent treatment difficulty increases, and the cost also increases.
CN215516658U discloses a quartz sand pickling device, which comprises a pickling net barrel, wherein the pickling net barrel can be rotatably arranged in a pickling cylinder; the lower end of the tray is fixed on the inner bottom wall of the pickling cylinder through a first bearing; a transmission rod linked with the output end of the driving device is fixedly arranged at the lower end of the tray; the transmission rod is hollow, the cavity in the transmission rod is a first air guide cavity, a second air guide cavity is formed in the tray, a plurality of impact nozzles are formed in the tray, and the first air guide cavity is connected with a compressed air pipeline through a second bearing. The utility model claims that the quartz sand can be fully billowed and mixed longitudinally and transversely, so that the quartz sand can be more fully pickled, and the pickling effect is improved. But is not suitable for treating quartz sand with the granularity of 120-40 meshes in practice, because the aperture of the net barrel cannot be smaller than 120 meshes, even if the aperture is achieved, the strength cannot meet the requirement, the net barrel is easy to deform, the supporting function cannot be realized, the net hole is small, the net hole is easy to block, and gas cannot be sprayed in. In addition, this patent also fails to achieve solid-liquid separation after acid washing.
In addition, the patents are all single pickling tanks, and continuous production cannot be realized. How to relatively optimize thermodynamically, dynamically and economically in the process and how to improve the utilization rate of acid and the acid washing efficiency, and realizing continuous production are the technical problems to be solved in the application.
Disclosure of Invention
The utility model aims to overcome the defects of the prior art and provide an integrated process for pickling high-purity quartz sand by using three-phase flow in series, wherein gas in a jet three-phase fluidized bed forms three-phase flow of gas, liquid and solid in a pickling system by means of upward impact force of the gas, the three-phase flow of the gas, the liquid and the solid in the pickling system, and the pickling solution and the quartz sand in the system can easily form circulation due to a specific conical structure, and can form relative speed difference due to density difference of the pickling solution and the quartz sand, so that a certain scrubbing effect can be achieved, and the concentration gradient of a liquid film on a solid-liquid contact surface is effectively reduced due to the speed difference of the pickling solution and the quartz sand, so that the chemical reaction of hydrogen ions and impurity oxides is promoted, and the pickling efficiency is promoted; the circulation replaces a dynamic cleaning mode of the rotation of the reaction kettle, so that the energy consumption is reduced; reverse pickling is adopted for the series connection of a plurality of kettles, so that the purity of quartz sand is gradually improved, and the pickling efficiency of sulfuric acid solution is improved; the final-stage low-concentration pickling solution is subjected to a reverse osmosis separation device to obtain high-purity water, the high-purity water is used for preparing water for preparing the pickling solution, and the obtained concentrated water is reused to realize the closed loop of the process. The method is relatively optimized in thermodynamics, dynamics and process economy, has high efficiency and high acid liquor utilization rate, and can realize continuous production.
The technical scheme adopted for solving the technical problems is as follows:
the utility model provides an integrated process method for series three-phase flow pickling high-purity quartz sand, which selects quartz sand with purity of 99.6-99.8% and granularity of 120-40 meshes after flotation, quartz sand to be washed sequentially enters a 1 st-stage pickling tank and a 2 nd-stage pickling tank … … nth-stage pickling tank, and finally is discharged from the nth-stage pickling tank, the purity of quartz sand in the 1 st-stage pickling tank is the lowest, and the purity of quartz sand in the nth-stage pickling tank is the highest; the pickling solution sequentially enters an N-level pickling tank … …, a 2-level pickling tank and a 1-level pickling tank, wherein the concentration of the pickling solution in the N-level pickling tank is highest, and the concentration of the pickling solution in the 1-level pickling tank is lowest; the pickling solution is discharged from a 1 st-stage pickling tank and enters a reverse osmosis device, and pure water after reverse osmosis separation is used for preparing the pickling solution, wherein N is more than or equal to 3;
the pickling tank adopts a jet fluidized bed, the upper part is cylindrical, the lower part is conical, the bottom of the pickling tank is connected with an air inlet pipeline, compressed air is led in through the air inlet pipeline, air flow forms upward radiation flow, a negative pressure space is formed at an injection port, quartz sand and pickling solution are entrained by the air flow and flow from bottom to top to form air-solid-liquid upward mixed flow, surrounding pickling solution and quartz sand can flow downwards by depending on self gravity to form quite stable circulation, and the pickling solution and quartz sand always flow under the circulation. The gas is air, the solid is quartz sand, and the liquid is pickling solution. The quartz sand, the pickling solution and the air form a jet fluidized bed technology, three-phase substances form the largest three-phase speed difference under the jet action, and form an integral circulation, so that the acid liquor and the particulate matters have better contact and scrubbing processes.
Further, the pickling solution is discharged from a discharging pipeline at the bottom of the pickling tank, is collected in a storage tank, and is pumped into a top liquid inlet of the next-stage pickling tank through a water pump.
Further, quartz sand is discharged from a discharge pipeline at the bottom of the pickling tank to enter a solid-liquid separation conveying belt after pickling, solid-liquid separation is carried out while conveying, pickling solution is stored in a storage tank, and the quartz sand after solid-liquid separation is conveyed to a sand inlet at the top of the next-stage pickling tank.
Further, the pickling solution is sulfuric acid solution with the concentration of 5-10wt%.
The second aspect of the present utility model provides a process apparatus for implementing the above process method, including a plurality of pickling units, which are a first stage pickling unit and a second stage pickling unit … …, an nth stage pickling unit, where N is greater than or equal to 3, and each of the pickling units includes:
the top of the pickling tank is provided with a sand inlet and a liquid inlet, the bottom of the pickling tank is provided with an outlet, and the outlet is connected with two pipelines, namely an air inlet pipeline and a discharge pipeline;
the air pump is arranged on the air inlet pipe line;
the inlet of the solid-liquid separation conveying belt is connected with a discharge pipeline of the pickling tank;
the storage tank is arranged below the solid-liquid separation conveying belt and is provided with an outlet;
a water pump mounted on an outlet line of the sump;
the sand inlet of the pickling tank of the first-stage pickling unit is connected with a quartz sand raw material conveying pipeline to be pickled, the outlet of the solid-liquid separation conveying belt of the first-stage pickling unit is connected to the top sand inlet … … of the pickling tank of the second-stage pickling unit through a pipeline, and the outlet of the solid-liquid separation conveying belt of the N-1-stage pickling unit is connected to the top sand inlet of the pickling tank of the N-stage pickling unit through a pipeline;
the liquid inlet of the pickling tank of the N-stage pickling unit is connected with the new pickling solution distribution storage tank through a pickling solution conveying pipeline, the water pump outlet pipeline of the N-stage pickling unit is connected to the liquid inlet … … of the pickling tank of the N-1 stage pickling unit, and the water pump outlet pipeline of the second stage pickling unit is connected to the liquid inlet of the pickling tank of the first stage pickling reaction unit.
Further, the device also comprises a reverse osmosis separation device, wherein the inlet of the reverse osmosis separation device is connected with the outlet pipeline of the water pump of the first-stage pickling unit.
Further, the plurality of pickling units are arranged laterally side by side or in a stepped arrangement, wherein the first stage pickling unit is uppermost and the nth stage pickling unit is lowermost.
The utility model has the advantages and positive effects that:
1. the jet gas forms three-phase flow of gas, liquid and solid, quartz stone forms circulation in the pickling tank from top to bottom, and then forms circulation from bottom to top under the action of the gas flow, so that the contact of dilute acid and quartz sand and the collision and friction between quartz sand are quickened, the mass transfer resistance of a liquid film on the solid-liquid surface is reduced, and the chemical reaction of hydrogen ions and impurity oxides is promoted. Replaces the rotary dynamic cleaning mode of the reaction kettle, and reduces the energy consumption.
2. The utility model adopts a reverse pickling and multisection pickling linkage system, firstly adopts low-concentration acid to mix with quartz sand with relatively high impurity content, improves the pickling driving force, gradually improves the purity of the quartz sand, and can reach 99.99% -99.999%. The utility model can effectively utilize the pickling solution, can realize energy conservation and emission reduction, and maximally utilizes the effective action of the acid solution on the quartz sand.
3. The pure water after reverse osmosis separation can be directly recycled to the system to prepare dilute sulfuric acid solution.
Drawings
Fig. 1 is a schematic diagram of an integrated process flow of a series three-phase flow acid-washed high purity quartz sand according to an embodiment of the present utility model.
Reference numerals in the drawings: 1 is a pickling tank, 2 is a reverse osmosis separation device, 3 is an air pump, 4 is an air inlet pipeline, 5 is a discharge pipeline, 6 is a solid-liquid separation conveyer belt, 7 is a storage tank, 8 is a water pump, and 9 is a novel pickling solution storage tank.
Description of the embodiments
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The utility model will be described in detail below with reference to the drawings in connection with embodiments.
It is noted that all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs unless otherwise indicated.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more of the described features. In the description of the present utility model, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The utility model relates to an integrated process for pickling high-purity quartz sand by a series three-phase flow, which is shown in figure 1, and comprises a plurality of pickling units, namely a first-stage pickling unit and a second-stage pickling unit … … Nth-stage pickling unit, wherein N is more than or equal to 3, and each of the pickling units comprises: the device comprises a pickling tank 1, an air pump 3, a solid-liquid separation conveying belt 6, a storage tank 7 and a water pump 8, wherein the upper part of the pickling tank 1 is cylindrical, the lower part of the pickling tank is conical, the top of the pickling tank 1 is provided with a sand inlet and a liquid inlet, the bottom of the pickling tank is provided with an outlet, and the outlet is connected with two pipelines, namely an air inlet pipeline 4 and a discharge pipeline 5; the air pump 3 is arranged on the air inlet pipeline 4; the inlet of the solid-liquid separation conveying belt 6 is connected with a discharge pipeline 5 of the pickling tank 1; the storage tank 7 is arranged below the solid-liquid separation conveying belt 6, and the storage tank 7 is provided with an outlet; the water pump 8 is mounted on the outlet line of the sump 7.
The plurality of pickling units can be transversely arranged side by side as shown in fig. 1 or arranged in a step-shaped manner, wherein the first-stage pickling unit is arranged at the uppermost part, and the Nth-stage pickling unit is arranged at the lowermost part, so that the energy consumption is further reduced.
The sand inlet of the pickling tank of the first-stage pickling unit is connected with a quartz sand raw material conveying pipeline to be pickled, the outlet of the solid-liquid separation conveying belt of the first-stage pickling unit is connected to the top sand inlet … … of the pickling tank of the second-stage pickling unit through a pipeline, and the outlet of the solid-liquid separation conveying belt of the N-1-stage pickling unit is connected to the top sand inlet of the pickling tank of the N-stage pickling unit through a pipeline;
the liquid inlet of the pickling tank of the N-stage pickling unit is connected with the novel pickling solution distribution storage tank 9 through a pickling solution conveying pipeline, the water pump outlet pipeline of the N-stage pickling unit is connected to the liquid inlet … … of the pickling tank of the N-1 stage pickling unit, and the water pump outlet pipeline of the second stage pickling unit is connected to the liquid inlet of the pickling tank of the first stage pickling reaction unit.
The device also comprises a reverse osmosis separation device 2, wherein the inlet of the reverse osmosis separation device 2 is connected with the outlet pipeline of the water pump of the first-stage pickling unit.
Injecting the newly-prepared pickling solution into a pickling tank of an N-th pickling unit, discharging the cleaned pickling solution from a discharging pipeline at the bottom of the pickling tank, collecting the cleaned pickling solution in a storage tank, pumping the cleaned pickling solution into the pickling tank of the N-1 th pickling unit through a water pump, pumping the cleaned pickling solution into a pickling tank of a first-stage pickling unit after the cleaned pickling solution is used in a second-stage pickling tank, wherein the concentration of the pickling solution in the pickling tank of the N-th pickling unit is the highest, and the concentration of the pickling solution in the pickling tank of the first-stage pickling unit is the lowest;
and the quartz sand raw material to be pickled is put into the pickling tank of the first-stage pickling unit, is discharged from a discharge pipeline at the bottom of the pickling tank and enters a solid-liquid separation conveying belt after being pickled, is conveyed and subjected to solid-liquid separation, the pickling solution is stored in a storage tank, quartz sand after being pickled at the first stage sequentially enters the pickling tank of the N-stage pickling unit of the second-stage pickling unit … … to finish pickling, and is discharged from the solid-liquid separation conveying belt of the N-stage pickling unit, wherein the quartz sand in the pickling tank of the first-stage pickling unit has the lowest purity, and the quartz sand in the pickling tank of the N-stage pickling unit has the highest purity.
And (3) opening an air pump in the cleaning process of the pickling tank of each stage of pickling unit, and introducing compressed air into the pickling tank to form three-phase flow of gas, liquid and solid so as to form circulation of quartz sand in the pickling tank.
The pickling solution pumped from the water pump of the first-stage pickling unit enters the reverse osmosis separation device 2 to obtain high-purity water, which is used for preparing water for newly-prepared pickling solution, and the obtained concentrated water is reused.
Preferably, the pickling solution is a sulfuric acid solution with the concentration of 5-10wt%.
The utility model relates to a four-step series three-phase flow pickling quartz sand purification innovative process, wherein each stage of pickling unit is a relatively independent pickling device, and the whole process is formed by connecting four identical units in series; the upper part of the pickling tank is cylindrical, the lower part of the pickling tank is conical, quartz sand with different purities is placed in the pickling tank, dilute sulfuric acid solution is placed in the pickling tank, the liquid level is higher than the quartz sand, then the bottom of the pickling tank is aerated, the air flow forms upward radiation flow, a negative pressure space is formed in the jet orifice, the quartz sand and the dilute acid are easily entrained by the air flow, the air-solid-liquid upward mixed flow is formed by flowing from bottom to top, the speed of the air is higher than the speed of the liquid, the speed of the liquid is higher than the speed of the solid, the liquid film on the surface of the liquid is thinned due to speed difference, particles collide and rub each other, the mass transfer resistance of hydrogen ions and metal ions in the water film is reduced, the quartz sand is continuously contacted with the dilute acid solution, the dissociation of the hydrogen ions to metal oxides is accelerated, and the chemical reaction of the dilute acid and impurities on the surface of the quartz sand is promoted, as shown in a chemical reaction equation (1), wherein M is expressed as metal, and the impurity metal oxides are converted into metal ions and water under the action of the hydrogen ions.
H + + M x O y =M n+ +H 2 O （1）
（M n+ ：Fe 3+ 、Al 3+ 、Ti 2+ 、Ca 2+ 、Mg 2+ ）
In order to improve the efficiency of acid washing and impurity removal, and effectively utilize sulfuric acid, the process adopts a three-phase flow acid washing process of a four-step method, and the purity of quartz sand is improved step by step, and the specific operation steps are as follows:
[1]quartz sand from flotation, siO thereof 2 Purity C0SiO of (C) 2 Generally 99.6-99.8%, the granularity is 120-40 mesh, the acid is sent into the pickling tank of the first-stage pickling unit by a conveyer belt, and then the dilute acid solution C2H stored in a storage tank after the pickling tank of the second-stage pickling unit finishes pickling 2 SO 4 Pumping the waste water into a pickling tank of a first-stage pickling unit through an acid-resistant and corrosion-resistant professional water pump until the liquid level is higher than that of quartz sand.
[2] After stabilization, an air pump is started to form jet flow, the solid and liquid at the bottom rapidly rise along with the air flow from bottom to top, and due to the difference of the air speed, the liquid speed and the solid particle speed, the contact of quartz sand and the solid particles and the collision and friction probability among the particles are accelerated, the pickling effect is promoted, under the action of continuous air flow, the quartz sand forms orderly circulation flow from top to bottom, then moves along with the air flow and the liquid from bottom to top under the entrainment of the air flow, and repeatedly moves along with the air flow, the quartz sand continuously forms dynamic contact with a dilute acid solution, a liquid film between the solid and the liquid becomes thinner, and under the action of turbulent flow and continuously updates, the chemical reaction of hydrogen ions and impurity oxides on the surface of the quartz sand is promoted, so that the impurity oxides are converted into metal ions and are separated from the quartz sand, and enter the solution, and the purpose of pickling and purification is realized.
[3] After a period of pickling time, the air pump is closed, the discharging valve is opened, the solid-liquid separation conveying belt at the upper part of the storage tank is opened, and the solid-liquid separation conveying belt is conveyed forward while draining, and finally conveyed into the pickling tank of the second-stage pickling unit.
[4] C1H 2 SO 4 The acid washing tank of the first-stage acid washing unit is used solution, the concentration of acid is relatively low, fe, al, ti, ca and Mg ions which are obtained by acid washing are directly sent to the reverse osmosis separation device 2 (RO), a large amount of high-purity water is obtained, the high-purity water is directly used for preparing water for the dilute acid solution at the front stage of the process, and the obtained concentrated water is used as another advanced treatment section, so that the acid washing tank is quite valuable.
[5]The four pickling units are synchronously carried out, and SiO is subjected to pickling by the first-stage pickling unit 2 The purity can reach C1SiO 2 :99.95%, siO after acid washing of the second-stage acid washing unit 2 The purity can reach C2SiO 2 :99.98%, siO after acid cleaning in third-stage acid cleaning unit 2 The purity can reach C3SiO 2 :99.993% of SiO after pickling in the fourth-stage pickling unit 2 The purity can reach C4SiO 2 :99.999%. After the pickling is finished, the pickling tank of the fourth-stage pickling unit starts to discharge materials, so that a high-purity quartz sand product can be obtained. Then discharging the quartz sand in a pickling tank of the third-stage pickling unit, and directly conveying the quartz sand to a pickling tank of the fourth-stage pickling unit; discharging the quartz sand in the pickling tank of the second-stage pickling unit, and directly conveying the quartz sand to the pickling tank of the third-stage pickling unit;and discharging the quartz sand in the pickling tank of the first-stage pickling unit, and directly conveying the quartz sand to the pickling tank of the second-stage pickling unit.
[6]Next, the fourth stage pickling unit is stored at a concentration of C4H 2 SO 4 Is fed into a pickling tank of a third-stage pickling unit, and the concentration stored in the third-stage pickling unit is C3H 2 SO 4 Is fed into a pickling tank of a second-stage pickling unit, and the concentration stored in the second-stage pickling unit is C2H 2 SO 4 Is fed into the pickling tank of the first-stage pickling unit.
[7]Acid solution (C0H) of the fourth stage pickling section pickling tank 2 SO 4 ) Acid solution from new configuration with concentration of C0H 2 SO 4 As is known from the four-step pickling process,
C0H 2 SO 4 > C4H 2 SO 4 > C3H 2 SO 4 > C2H 2 SO 4 > C1H 2 SO 4 ，
C4SiO 2 > C3SiO 2 > C2SiO 2 > C1SiO 2 > C0SiO 2 ：
the concentration of the stock solution of the sulfuric acid dilute solution of the whole system is the largest, the purity of the stock solution is 99.994 percent, the content of impurity oxides is only 0.006 percent after the quartz sand is washed by a third-stage acid washing unit in four-step acid washing, the stock solution acts, the pushing force of the stock solution is larger than that of a single acid washing tank, the high-purity quartz sand is easier to obtain, the former steps are equivalent to pretreatment of acid washing and purification, the solution of the front-stage acid washing is fully utilized to act with the quartz sand with relatively higher impurity concentration, and under the action of gas jet, the contact of the quartz sand and the dilute acid solution and the friction between particles are promoted, the mass transfer resistance in a liquid film is reduced, and the speed of the reaction (1) is accelerated.
The above description is only of the preferred embodiments of the present utility model and is not intended to limit the present utility model, but various modifications and variations can be made to the present utility model by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present utility model should be included in the protection scope of the present utility model.
Claims (7)
1. The integrated process method for the series three-phase flow pickling high-purity quartz sand is characterized in that quartz sand with the purity of 99.6-99.8% and granularity of 120-40 meshes after flotation is selected, quartz sand to be washed sequentially enters a 1 st-stage pickling tank, a 2 nd-stage pickling tank … … nth-stage pickling tank and is finally discharged from the nth-stage pickling tank, the purity of quartz sand in the 1 st-stage pickling tank is the lowest, and the purity of quartz sand in the nth-stage pickling tank is the highest; the pickling solution sequentially enters an N-level pickling tank … …, a 2-level pickling tank and a 1-level pickling tank, wherein the concentration of the pickling solution in the N-level pickling tank is highest, and the concentration of the pickling solution in the 1-level pickling tank is lowest; the pickling solution is discharged from a 1 st-stage pickling tank and enters a reverse osmosis device, and pure water after reverse osmosis separation is used for preparing the pickling solution, wherein N is more than or equal to 3;
the pickling tank adopts a jet fluidized bed, the upper part is cylindrical, the lower part is conical, the bottom of the pickling tank is connected with an air inlet pipeline, compressed gas is led in through the air inlet pipeline, air flow forms upward radiation flow, a negative pressure space is formed at an injection port, quartz sand and pickling solution are entrained by the air flow and flow from bottom to top to form a gas-solid-liquid upward mixed flow, the gas is air, the solid is quartz sand, and the liquid is pickling solution.
2. The process of claim 1 wherein the pickling solution is drained from the bottom discharge line of the pickling tank, collected in a sump and pumped into the top inlet of the next pickling tank by a water pump.
3. The process according to claim 2, wherein the quartz sand is discharged from a discharge pipeline at the bottom of the pickling tank to enter a solid-liquid separation conveying belt after pickling, and is conveyed and subjected to solid-liquid separation, the pickling solution is stored in a storage tank, and the quartz sand after solid-liquid separation is conveyed to a sand inlet at the top of the next-stage pickling tank.
4. The process of claim 1, wherein the pickling solution is a sulfuric acid solution with a concentration of 5-10wt%.
5. A process unit for implementing the process method of claim 1, comprising a plurality of pickling units, respectively a first stage pickling unit, a second stage pickling unit … …, and an nth stage pickling unit, wherein N is greater than or equal to 3, and each stage pickling unit comprises:
the pickling tank (1) is characterized in that the top of the pickling tank (1) is provided with a sand inlet and a liquid inlet, the bottom of the pickling tank is provided with an outlet, and the outlet is connected with two pipelines, namely an air inlet pipeline (4) and a discharging pipeline (5);
the air pump (3) is arranged on the air inlet pipeline (4);
the inlet of the solid-liquid separation conveying belt (6) is connected with the discharge pipeline (5) of the pickling tank (1);
a sump (7), the sump (7) being mounted below the solid-liquid separation conveyor belt (6), the sump (7) having an outlet;
a water pump (8), the water pump (8) being mounted on an outlet line of the sump (7);
the sand inlet of the pickling tank of the first-stage pickling unit is connected with a quartz sand raw material conveying pipeline to be pickled, the outlet of the solid-liquid separation conveying belt of the first-stage pickling unit is connected to the top sand inlet … … of the pickling tank of the second-stage pickling unit through a pipeline, the outlet of the solid-liquid separation conveying belt of the N-1-stage pickling unit is connected to the top sand inlet of the pickling tank of the N-stage pickling unit through a pipeline, the liquid inlet of the pickling tank of the N-stage pickling unit is connected with a new pickling liquid tank (9) through a pickling liquid conveying pipeline, the water pump outlet pipeline of the N-stage pickling unit is connected to the liquid inlet … … of the pickling tank of the N-1-stage pickling unit, and the water pump outlet pipeline of the second-stage pickling unit is connected to the liquid inlet of the pickling tank of the first-stage pickling reaction unit.
6. The process unit according to claim 5, further comprising a reverse osmosis separation unit (2), wherein the inlet of the reverse osmosis separation unit (2) is connected to the water pump outlet line of the first stage pickling unit.
7. The process unit of claim 6 wherein the plurality of acid wash units are arranged laterally side by side or in a stepped arrangement with the first stage acid wash unit uppermost and the nth stage acid wash unit lowermost.
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| JP2005200697A (en) * | 2004-01-15 | 2005-07-28 | Mitsubishi-Hitachi Metals Machinery Inc | Continuous pickling equipment |
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| CN112441590A (en) * | 2020-11-27 | 2021-03-05 | 中建材衢州金格兰石英有限公司 | Quartz sand pickling method and device |
| CN215516658U (en) * | 2021-08-18 | 2022-01-14 | 江苏福淼石英制品有限公司 | Quartz sand pickling device |
| CN114804129A (en) * | 2022-04-29 | 2022-07-29 | 江苏亨芯石英科技有限公司 | Method for purifying high-purity quartz sand |
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| JP2005200697A (en) * | 2004-01-15 | 2005-07-28 | Mitsubishi-Hitachi Metals Machinery Inc | Continuous pickling equipment |
| CN101475169A (en) * | 2009-01-21 | 2009-07-08 | 青岛科技大学 | Preparing apparatus for granular active carbon |
| CN109485050A (en) * | 2019-01-08 | 2019-03-19 | 临沂昊泉硅业科技有限公司 | A kind of cycle pickling method for conveniently removing deimpurity glass sand |
| CN112441590A (en) * | 2020-11-27 | 2021-03-05 | 中建材衢州金格兰石英有限公司 | Quartz sand pickling method and device |
| CN215516658U (en) * | 2021-08-18 | 2022-01-14 | 江苏福淼石英制品有限公司 | Quartz sand pickling device |
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