CN105692629B - The method that acid-washed quartz sand is quickly cleaned - Google Patents
The method that acid-washed quartz sand is quickly cleaned Download PDFInfo
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- CN105692629B CN105692629B CN201610279069.1A CN201610279069A CN105692629B CN 105692629 B CN105692629 B CN 105692629B CN 201610279069 A CN201610279069 A CN 201610279069A CN 105692629 B CN105692629 B CN 105692629B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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Abstract
The invention discloses a kind of method that acid-washed quartz sand is quickly cleaned, it includes：Step 1: the quartz sand for treating pickling is put into pickling purifying plant, pickle is added, deviates from after 3~6h of pickling and collects pickle；Step 2: the quartz sand after pickling is delivered in water washing device, multiple absorbent packets are buried into quartz sand, all absorbent packets are taken out after 10~20min, clear water is added into water washing device and soaks 10~20min, then agitator treating, cleaning solution is discharged, absorbent packet absorption, clear water immersion, agitator treating is placed again into repeatedly to quartz sand surface in neutrality, merges the cleaning solution；Clean quartz sand is gone to 3~4h is dried in drier, obtain the quartz sand of purifying；Step 3: the pickle of collection and the cleaning solution merged are gone in anhydride recovery plant, the processing of spent acid and waste water is carried out.The advantages of anhydride recovery plant that the present invention designs has environmental protection and energy saving, easy to operate, and cost is cheap.
Description
Technical field
The present invention relates to the purification technique field of quartz sand.It is more particularly related to a kind of acid-washed quartz sand is fast
The clean method of speed.
Background technology
Quartz sand is very important nonmetallic ore raw material, is widely used in the row such as glass, ceramics, cement and refractory material
Industry.The height of quartz sand grade and the metal impurities mineral content for depending mainly on the size of quartz sand itself of value number,
Especially using impurity iron as represent metalliferous mineral content how much, to determine the self-value of quartz sand and use value.It is existing
The method of quartz sand iron removaling mainly have：1) multi-stage magnetic separation, this method are applied to the quartz sand purifying technique containing strong magnet, but
Its de-ferrous effect is difficult to get a desired effect and purpose；2) flotation is carried out again on the basis of 1), although can reach certain
Expected Results, but unstable product quality, it is difficult to which quartz is purified to trace level (0.5-20ppm) below；3) on basis 1)
Upper progress pickling iron removaling, it can not only get a desired effect, and product quality is stable, and energy large-scale mass production, is current
The maximally effective method of purifying quartz sand, but be that substantial amounts of spent acid and useless can be produced in pickling purification process the shortcomings that its is maximum
Water, pollute environment.
At present, the spent acid during pickling purifying quartz sand, waste water are mainly neutralized to PH=7, Ran Houzai using alkali lye
Discharge, but long-term discharge not only wastes substantial amounts of freshwater resources, but also certain pollution can be caused to environment.Therefore, need badly
A kind of acid formula for the iron ore material that can either thoroughly remove in quartz sand is found, can be good at handling acid-bearing wastewater again,
Acid-bearing wastewater after processing can also all be recycled and not influence the quickly clean process of product quality.
The content of the invention
It is an object of the invention to provide a kind of method that acid-washed quartz sand is quickly cleaned, it is in the quartz sand after overpickling
Middle addition absorbent packet, the residual acid in quartz sand is adsorbed, pure quartz sand is finally obtained by the washing of multiple clear water, devised
Anhydride recovery plant, sour composition volatile in heating recovery acid solution is first passed through, acid is converted into precipitation row by pH is overregulated
Go out, add alkali lye and discharge the iron tramp in acid solution, obtain the clear water that recyclable workshop recycles, the acid solution that the present invention designs
The advantages of retracting device has environmental protection and energy saving, easy to operate, and cost is cheap.
In order to realize according to object of the present invention and further advantage, there is provided what a kind of acid-washed quartz sand was quickly cleaned
Method, comprise the following steps：
Step 1: the quartz sand for treating pickling is put into pickling purifying plant, pickle is added, by pickling purifying plant
Temperature be heated to 60~85 DEG C, and ON cycle system makes the pickle circulation dynamic acid-washed quartz sand of heat, after 3~6h of pickling
Deviate from and collect pickle；
Step 2: the quartz sand after pickling is delivered in water washing device, embedded multiple absorbent packets into quartz sand, 10~
All absorbent packets are taken out after 20min, clear water is added into water washing device and soaks 10~20min, then agitator treating, by cleaning solution
Discharge, absorbent packet absorption, clear water immersion, agitator treating are placed again into repeatedly to quartz sand surface in neutrality, merges the washing
Liquid；Clean quartz sand is gone to 3~4h is dried in drier, obtain the quartz sand of purifying；
Wherein, the absorbent packet is NACF material, inside the absorbent packet particle diameter equipped with 1~5g for 0.2~
0.5mm green stone, the absorbent packet are fitted into after green stone before being put into quartz sand, have passed through pretreatment：Green grass or young crops will be housed
The absorbent packet of stone is put into 10~20min of immersion in the limewash of clarification, then takes out drying, stand-by；
Step 3: the pickle of collection and the cleaning solution merged are gone in anhydride recovery plant, spent acid and waste water are carried out
Processing.
Preferably, the method that described acid-washed quartz sand is quickly cleaned, the anhydride recovery plant include：
Tank body, it is the hollow structure closed up and down, and the top of the tank body is provided with inlet, and bottom is provided with leakage fluid dram,
The inside of the tank body is horizontal from top to bottom to be provided with the first flashboard and the second flashboard, and the tank interior is separated into and not connected mutually
Upper space, central space and lower space, the tank wall of the upper space is provided with heating mantle, first flashboard and
The top of second flashboard is respectively equipped with the first screen pack and the second screen pack；The upper space, the central space and
Agitator is equipped with the lower space；
Acid mist recovering mechanism, it is arranged in the upper space and is located at the inlet top, the acid mist recovery
Mechanism includes the pipe group that at least two row of horizontal are set, and the pipe group includes hollow pipe that is multiple horizontal and being parallel to each other, the sky
The both ends of heart pipe are detachably connected with the inner tank wall respectively, and the tube wall of the hollow pipe is provided with multiple through holes, the sky
Anion-cation exchange resin filled with absorption acid mist inside heart pipe；
First shower nozzle, it is arranged in the central space, and the inlet of first shower nozzle passes through the first flexible pipe and institute
The milk of lime holding vessel connection outside tank body is stated, the middle part of first flexible pipe is provided with the first valve；
Second shower nozzle, it is arranged on the lower space, the inlet of second shower nozzle by the second flexible pipe with it is described
The sodium hydrate aqueous solution holding vessel that mass fraction outside tank body is 2.5% connects, and the middle part of second flexible pipe is provided with the
Two valves；
First pH meter, it is arranged in the central space；
Second pH meter, it is arranged in the lower space；
First valve, second valve, first pH meter and second pH meter are electrically connected with the controller, institute
Controller is stated to be arranged to：Receive the first pH value that first pH meter detects liquid in the central space, and the 2nd pH
The second pH value of liquid in the lower space of detection is counted, if the first pH value is less than 6, the controller control described first
Valve is opened, and first shower nozzle conveys milk of lime to the central space, if the first pH value is not less than 6, the controller
First valve is controlled to close；If the second pH value is less than 8.5, the controller controls second valve to open, described
Second shower nozzle conveys sodium hydrate aqueous solution to the lower space, if the second pH value is not less than 8.5, the controller control
Second valve is closed.
Preferably, the method that described acid-washed quartz sand is quickly cleaned, the concrete operations of the step 3 are：By pickling
Liquid and cleaning solution import the upper space by the inlet, start the heating mantle heats to 40~50 DEG C, and stirring 1~
After 2h, stop heating, open first flashboard, liquid is imported into the central space, opens first valve, adjusts liquid
Body pH to 6~7, after stirring 20~30min, 10~20min is stood, second flashboard is opened, liquid is imported into the bottom
Space, second valve is opened, adjust liquid pH to 8.5~9, after stirring 20~30min, stand 10~20min, from described
Leakage fluid dram discharge liquid, and use careless acid for adjusting pH to 6~7, filter off except precipitation, obtain clear water be sent into workshop recycling.
Preferably, the method that described acid-washed quartz sand is quickly cleaned, the 3rd screen pack is connected in the leakage fluid dram.
Preferably, the method that described acid-washed quartz sand is quickly cleaned, the embedded density of the absorbent packet is 30g/.
Preferably, in the method that described acid-washed quartz sand is quickly cleaned, the both ends of the hollow pipe and the tank body
The position of wall contact is provided with sealing gasket.
Preferably, the method that described acid-washed quartz sand is quickly cleaned, adding in the limewash of clarification has volume fraction
For 0.1~0.3% hydrogen peroxide.
Preferably, the method that described acid-washed quartz sand is quickly cleaned, described pickle by 2~15 parts by weight hydrogen
Fluoric acid, the fluosilicic acid of 5~20 parts by weight, the oxalic acid of 4~25 parts by weight, the hydrochloric acid of 1~8 parts by weight and 50~90 parts by weight
Water forms.
Preferably, the method that described acid-washed quartz sand is quickly cleaned, the upper space, the central space and institute
The height ratio for stating lower space is 1.5:1:1.
The present invention comprises at least following beneficial effect：
1st, the present invention adds absorbent packet in the quartz sand after overpickling, the residual acid in quartz sand is adsorbed, by more
Secondary clear water washing finally obtains pure quartz sand, devises anhydride recovery plant, first passes through volatile in heating recovery acid solution
Sour composition, by overregulate pH by acid be converted into precipitation discharge, add alkali lye by acid solution iron tramp discharge, obtain returning
The clear water recycled between returning the vehicle to the garage and knock off, the anhydride recovery plant that the present invention designs can be good at handling acid-bearing wastewater, have environmental protection
Energy-conservation, easy to operate, the advantages of cost is cheap；
2nd, the main component of green stone is CaO, also containing a certain amount of MgO, can absorb the acid neutralized in acid solution, will fill
The absorbent packet for having green stone is buried in quartz sand, and the acid solution of the residual in quartz sand is slowly infiltrated through in absorbent packet, with green stone
Simultaneously with it neutralization reaction occurs for son contact, and absorbent packet can be adsorbed for NACF material caused by acid gas in quartz sand etc.
Peculiar smell, repeatedly absorption and clear water washing, so as to obtain pure quartz sand, rapidly and thoroughly cleans the miscellaneous of quartz sand surface residual
Matter and acid substance, the acid content in cleaning solution is reduced after absorption, reduce the difficulty of cleaning solution post-processing；
3rd, anhydride recovery plant is provided with upper, middle and lower space, first in upper space by easily waving in acid solution
The acid of hair realizes the recovery of acid mist, in case of heating, hydrochloric acid and hydrofluoric acid in acid solution etc. have volatilized by resin adsorption
Acid be adsorbed acid resin adsorption, after the completion of absorption, hollow pipe is taken out from upper space, and with the stripping liquids such as water will set
Acid recovery in fat, the pickle that restored acid can add certain quantity of fresh are re-used in the acid cleaning process of quartz sand；Acid mist
The acid solution of upper space is imported into central space after the completion of recovery, the first shower nozzle adds limewash, adjusted by controller thereto
Acid solution pH to 6~7 is saved, the fluosilicic acid in acid solution and oxalic acid are converted into calcium fluosilicate and calcium oxalate, remove the fluorine silicon in acid solution
Acid and oxalic acid, the dilute sulfuric acid that calcium fluosilicate and calcium oxalate on the second screen pack add equivalent is collected, generates fluosilicic acid and oxalic acid
It can be fed again into the Pickling-shop of quartz sand and recycle, the calcium sulfate of generation can make byproduct sale；Treat central space
After acid solution precipitation is complete, the second flashboard is opened, acid solution is imported in lower space, the second shower nozzle adds sodium hydroxide water thereto
Solution, pH to 8.5~9 is adjusted, the iron ion in acid solution forms ferric hydroxide precipitate in the basic conditions, removes the iron in acid solution
Ion, acid solution discharge anhydride recovery plant eventually through leakage fluid dram, careless acid for adjusting pH are added to 6~7, by the calcium ion in acid solution
Precipitation, filter clear water can be sent into workshop recycling, in whole process as far as possible by the utility recovery in acid solution simultaneously
Recycle, be finally reached zero-emission, no pollution.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Brief description of the drawings
Fig. 1 is the structural representation of anhydride recovery plant of the present invention.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples, to make those skilled in the art's reference
Specification word can be implemented according to this.
It should be noted that experimental method described in following embodiments, is conventional method unless otherwise specified, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained；In the description of the invention, term " transverse direction ", " vertical
To ", " on ", " under ", "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom ", " interior ", the instruction such as " outer " side
Position or position relationship are based on orientation shown in the drawings or position relationship, are for only for ease of the description present invention and simplify description,
It is not instruction or implies signified device or element there must be specific orientation, with specific azimuth configuration and operation, because
This is not considered as limiting the invention.
<Embodiment 1>
A kind of method that acid-washed quartz sand is quickly cleaned, comprises the following steps：
Step 1: the quartz sand for treating pickling is put into pickling purifying plant, pickle is added, by pickling purifying plant
Temperature be heated to 60 DEG C, and ON cycle system makes the pickle circulation dynamic acid-washed quartz sand of heat, deviates from simultaneously after pickling 3h
Collect pickle；
Wherein, described pickle by the hydrofluoric acid of 2 parts by weight, the fluosilicic acid of 5 parts by weight, 4 parts by weight oxalic acid, 1 weight
Measure the hydrochloric acid of part and the water composition of 50 parts by weight；
Step 2: the quartz sand after pickling is delivered in water washing device, multiple absorbent packets, the suction are buried into quartz sand
The embedded density of pocket is 30g/, and all absorbent packets are taken out after 10min, clear water immersion 10min is added into water washing device, so
Agitator treating afterwards, cleaning solution is discharged, be placed again into absorbent packet absorption, clear water immersion, agitator treating repeatedly to quartz sand surface
In neutrality, merge the cleaning solution；Clean quartz sand is gone to 3h is dried in drier, obtain the quartz sand of purifying；
Wherein, the absorbent packet is NACF material, and the particle diameter equipped with 1g is 0.2mm green grass or young crops inside the absorbent packet
Stone, the absorbent packet are fitted into after green stone before being put into quartz sand, have passed through pretreatment：By the absorption equipped with green stone
Bag, which is put into the limewash of clarification, soaks 10min, then takes out drying, stand-by；Wherein, being added in the limewash of clarification has volume
Fraction is 0.1% hydrogen peroxide；The present invention adds absorbent packet in the quartz sand after overpickling, adsorbs the residue in quartz sand
Acid, pure quartz sand is finally obtained by the washing of multiple clear water；The main component of green stone is CaO, also containing a certain amount of
MgO, the acid neutralized in acid solution can be absorbed, the absorbent packet equipped with green stone be buried in quartz sand, the residual in quartz sand
Acid solution slowly infiltrate through in absorbent packet, contact with green stone and neutralization reaction occur with it, absorbent packet is NACF material
Matter can adsorb peculiar smell caused by acid gas in quartz sand etc., repeatedly absorption and clear water washing, so as to obtain pure quartz sand,
The impurity and acid substance of quartz sand surface residual are rapidly and thoroughly cleaned, the acid content in cleaning solution, drop are reduced after absorption
The difficulty of low cleaning solution post-processing；
Step 3: the pickle of collection and the cleaning solution merged are gone in anhydride recovery plant, spent acid and waste water are carried out
Processing：Pickle and cleaning solution are imported into the upper space 5 by the inlet 1, start the heating mantle heats extremely
40 DEG C, after stirring 1h, stop heating, open first flashboard 3, liquid is imported into the central space 6, opens described first
Valve, liquid pH to 6 is adjusted, after stirring 20min, stand 10min, open second flashboard 4, liquid is imported into the bottom
Space 7, second valve is opened, adjust liquid pH to 8.5, after stirring 20min, 10min is stood, from the row of leakage fluid dram 2
Go out liquid, and with careless acid for adjusting pH to 6, filter off except precipitation, obtain clear water and be sent into workshop and recycle.
As shown in figure 1, in the method that described acid-washed quartz sand is quickly cleaned, the anhydride recovery plant includes：
Tank body, it is the hollow structure closed up and down, and the top of the tank body is provided with inlet 1, and bottom is provided with leakage fluid dram
2, the 3rd screen pack is connected in the leakage fluid dram 2, the inside of the tank body is horizontal from top to bottom to be provided with the first flashboard 3 and the second lock
Plate 4, the tank interior is separated into mutual disconnected upper space 5, central space 6 and lower space 7, the upper space
5 tank wall is provided with heating mantle, the top of first flashboard 3 and second flashboard 4 be respectively equipped with the first screen pack and
Second screen pack；Agitator is equipped with the upper space 5, the central space 6 and the lower space 7；The top
The height ratio in space 5, the central space 6 and the lower space 7 is 1.5:1:1；
Acid mist recovering mechanism, it is arranged in the upper space 5 and is located at the top of inlet 1, and the acid mist returns
Receiving mechanism includes the pipe group that at least two row of horizontal are set, and the pipe group includes hollow pipe 8 that is multiple horizontal and being parallel to each other, described
The both ends of hollow pipe 8 are detachably connected with the inner tank wall respectively, and the both ends of the hollow pipe 8 contact with the inner tank wall
Position be provided with sealing gasket, the tube wall of the hollow pipe 8 is provided with multiple through holes 9, and the inside of hollow pipe 8 is filled with adsorber acid
The anion-cation exchange resin of mist；
First shower nozzle 10, it is arranged in the central space 6, and the inlet 1 of first shower nozzle 10 is soft by first
Pipe connects with the milk of lime holding vessel outside the tank body, and the middle part of first flexible pipe is provided with the first valve；
Second shower nozzle 11, it is arranged on the lower space 7, and the inlet 1 of second shower nozzle 11 passes through the second flexible pipe
Connected with the sodium hydrate aqueous solution holding vessel that the mass fraction outside the tank body is 2.5%, the middle part of second flexible pipe
Provided with the second valve；
First pH meter, it is arranged in the central space 6；
Second pH meter, it is arranged in the lower space 7；
First valve, second valve, first pH meter and second pH meter electrically connect with controller 12,
The controller 12 is arranged to：Receive the first pH value that first pH meter detects liquid in the central space 6, and described the
Second pH value of liquid in the lower space 7 of two pH meters detection, if the first pH value is less than 6, the controller 12 controls
First valve is opened, and first shower nozzle 10 conveys milk of lime to the central space 6, if the first pH value is not less than 6,
The controller 12 controls first valve to close；If the second pH value is less than 8.5, the controller 12 controls described second
Valve is opened, and second shower nozzle 11 conveys sodium hydrate aqueous solution to the lower space 7, if the second pH value is not less than 8.5
When, the controller 12 controls second valve to close.
Anhydride recovery plant is provided with upper, middle and lower space 7, first in upper space 5 by easily waving in acid solution
The acid of hair realizes the recovery of acid mist, in case of heating, hydrochloric acid and hydrofluoric acid in acid solution etc. have volatilized by resin adsorption
Acid be adsorbed acid resin adsorption, after the completion of absorption, hollow pipe 8 is taken out from upper space 5, and with the stripping liquids such as water will
Acid recovery in resin, the pickle that restored acid can add certain quantity of fresh are re-used in the acid cleaning process of quartz sand；Acid
The acid solution of upper space 5 is imported into central space 6 after the completion of mist recovery, the first shower nozzle 10 adds limewash, passes through control thereto
Device 12 processed adjusts acid solution pH to 6~7, and the fluosilicic acid in acid solution and oxalic acid are converted into calcium fluosilicate and calcium oxalate, remove acid solution
In fluosilicic acid and oxalic acid, collect the dilute sulfuric acid that calcium fluosilicate and calcium oxalate on the second screen pack add equivalent, generate fluorine silicon
Acid and oxalic acid, which can be fed again into the Pickling-shop of quartz sand, to be recycled, and the calcium sulfate of generation can make byproduct sale；In treating
After the acid solution in portion space 6 precipitates completely, the second flashboard 4 is opened, acid solution is imported in lower space 7, the second shower nozzle 11 is thereto
Sodium hydrate aqueous solution is added, adjusts pH to 8.5~9, the iron ion in acid solution forms ferric hydroxide precipitate in the basic conditions,
The iron ion in acid solution is removed, acid solution discharges anhydride recovery plant eventually through leakage fluid dram 2, adds careless acid for adjusting pH to 6~7,
By the calcium ions precipitate in acid solution, filter clear water can be sent into workshop recycling, as far as possible by acid solution in whole process
Utility reclaim and recycle, be finally reached zero-emission, no pollution.
<Embodiment 2>
A kind of method that acid-washed quartz sand is quickly cleaned, comprises the following steps：
Step 1: the quartz sand for treating pickling is put into pickling purifying plant, pickle is added, by pickling purifying plant
Temperature be heated to 73 DEG C, and ON cycle system makes the pickle circulation dynamic acid-washed quartz sand of heat, deviates from simultaneously after pickling 5h
Collect pickle；
Wherein, described pickle is by the hydrofluoric acid of 9 parts by weight, the fluosilicic acid of 13 parts by weight, the oxalic acid of 14 parts by weight, 5
The hydrochloric acid of parts by weight and the water of 70 parts by weight composition；
Step 2: the quartz sand after pickling is delivered in water washing device, multiple absorbent packets, the suction are buried into quartz sand
The embedded density of pocket is 30g/, and all absorbent packets are taken out after 15min, clear water immersion 15min is added into water washing device, so
Agitator treating afterwards, cleaning solution is discharged, be placed again into absorbent packet absorption, clear water immersion, agitator treating repeatedly to quartz sand surface
In neutrality, merge the cleaning solution；Clean quartz sand is gone to 3.5h is dried in drier, obtain the quartz sand of purifying；
Wherein, the absorbent packet is NACF material, and the particle diameter equipped with 3g is 0.4mm green grass or young crops inside the absorbent packet
Stone, the absorbent packet are fitted into after green stone before being put into quartz sand, have passed through pretreatment：By the absorption equipped with green stone
Bag, which is put into the limewash of clarification, soaks 15min, then takes out drying, stand-by；Wherein, being added in the limewash of clarification has volume
Fraction is 0.2% hydrogen peroxide；The present invention adds absorbent packet in the quartz sand after overpickling, adsorbs the residue in quartz sand
Acid, pure quartz sand is finally obtained by the washing of multiple clear water；The main component of green stone is CaO, also containing a certain amount of
MgO, the acid neutralized in acid solution can be absorbed, the absorbent packet equipped with green stone be buried in quartz sand, the residual in quartz sand
Acid solution slowly infiltrate through in absorbent packet, contact with green stone and neutralization reaction occur with it, absorbent packet is NACF material
Matter can adsorb peculiar smell caused by acid gas in quartz sand etc., repeatedly absorption and clear water washing, so as to obtain pure quartz sand,
The impurity and acid substance of quartz sand surface residual are rapidly and thoroughly cleaned, the acid content in cleaning solution, drop are reduced after absorption
The difficulty of low cleaning solution post-processing；
Step 3: the pickle of collection and the cleaning solution merged are gone in anhydride recovery plant, spent acid and waste water are carried out
Processing：Pickle and cleaning solution are imported into the upper space 5 by the inlet 1, start the heating mantle heats extremely
45 DEG C, after stirring 1.5h, stop heating, open first flashboard 3, liquid is imported into the central space 6, open described the
One valve, adjust liquid pH to 6.5, after stirring 25min, stand 15min, open second flashboard 4, liquid is imported described in
Lower space 7, second valve is opened, adjust liquid pH to 8.8, after stirring 25min, 15min is stood, from the leakage fluid dram
2 discharge liquid, and use careless acid for adjusting pH to 6.5, filter off except precipitation, obtain clear water be sent into workshop recycling.
As shown in figure 1, in the method that described acid-washed quartz sand is quickly cleaned, the anhydride recovery plant includes：
Tank body, it is the hollow structure closed up and down, and the top of the tank body is provided with inlet 1, and bottom is provided with leakage fluid dram
2, the 3rd screen pack is connected in the leakage fluid dram 2, the inside of the tank body is horizontal from top to bottom to be provided with the first flashboard 3 and the second lock
Plate 4, the tank interior is separated into mutual disconnected upper space 5, central space 6 and lower space 7, the upper space
5 tank wall is provided with heating mantle, the top of first flashboard 3 and second flashboard 4 be respectively equipped with the first screen pack and
Second screen pack；Agitator is equipped with the upper space 5, the central space 6 and the lower space 7；The top
The height ratio in space 5, the central space 6 and the lower space 7 is 1.5:1:1；
Acid mist recovering mechanism, it is arranged in the upper space 5 and is located at the top of inlet 1, and the acid mist returns
Receiving mechanism includes the pipe group that at least two row of horizontal are set, and the pipe group includes hollow pipe 8 that is multiple horizontal and being parallel to each other, described
The both ends of hollow pipe 8 are detachably connected with the inner tank wall respectively, and the both ends of the hollow pipe 8 contact with the inner tank wall
Position be provided with sealing gasket, the tube wall of the hollow pipe 8 is provided with multiple through holes 9, and the inside of hollow pipe 8 is filled with adsorber acid
The anion-cation exchange resin of mist；
First shower nozzle 10, it is arranged in the central space 6, and the inlet 1 of first shower nozzle 10 is soft by first
Pipe connects with the milk of lime holding vessel outside the tank body, and the middle part of first flexible pipe is provided with the first valve；
Second shower nozzle 11, it is arranged on the lower space 7, and the inlet 1 of second shower nozzle 11 passes through the second flexible pipe
Connected with the sodium hydrate aqueous solution holding vessel that the mass fraction outside the tank body is 2.5%, the middle part of second flexible pipe
Provided with the second valve；
First pH meter, it is arranged in the central space 6；
Second pH meter, it is arranged in the lower space 7；
First valve, second valve, first pH meter and second pH meter electrically connect with controller 12,
The controller 12 is arranged to：Receive the first pH value that first pH meter detects liquid in the central space 6, and described the
Second pH value of liquid in the lower space 7 of two pH meters detection, if the first pH value is less than 6, the controller 12 controls
First valve is opened, and first shower nozzle 10 conveys milk of lime to the central space 6, if the first pH value is not less than 6,
The controller 12 controls first valve to close；If the second pH value is less than 8.5, the controller 12 controls described second
Valve is opened, and second shower nozzle 11 conveys sodium hydrate aqueous solution to the lower space 7, if the second pH value is not less than 8.5
When, the controller 12 controls second valve to close.
Anhydride recovery plant is provided with upper, middle and lower space 7, first in upper space 5 by easily waving in acid solution
The acid of hair realizes the recovery of acid mist, in case of heating, hydrochloric acid and hydrofluoric acid in acid solution etc. have volatilized by resin adsorption
Acid be adsorbed acid resin adsorption, after the completion of absorption, hollow pipe 8 is taken out from upper space 5, and with the stripping liquids such as water will
Acid recovery in resin, the pickle that restored acid can add certain quantity of fresh are re-used in the acid cleaning process of quartz sand；Acid
The acid solution of upper space 5 is imported into central space 6 after the completion of mist recovery, the first shower nozzle 10 adds limewash, passes through control thereto
Device 12 processed adjusts acid solution pH to 6~7, and the fluosilicic acid in acid solution and oxalic acid are converted into calcium fluosilicate and calcium oxalate, remove acid solution
In fluosilicic acid and oxalic acid, collect the dilute sulfuric acid that calcium fluosilicate and calcium oxalate on the second screen pack add equivalent, generate fluorine silicon
Acid and oxalic acid, which can be fed again into the Pickling-shop of quartz sand, to be recycled, and the calcium sulfate of generation can make byproduct sale；In treating
After the acid solution in portion space 6 precipitates completely, the second flashboard 4 is opened, acid solution is imported in lower space 7, the second shower nozzle 11 is thereto
Sodium hydrate aqueous solution is added, adjusts pH to 8.5~9, the iron ion in acid solution forms ferric hydroxide precipitate in the basic conditions,
The iron ion in acid solution is removed, acid solution discharges anhydride recovery plant eventually through leakage fluid dram 2, adds careless acid for adjusting pH to 6~7,
By the calcium ions precipitate in acid solution, filter clear water can be sent into workshop recycling, as far as possible by acid solution in whole process
Utility reclaim and recycle, be finally reached zero-emission, no pollution.
<Embodiment 3>
A kind of method that acid-washed quartz sand is quickly cleaned, comprises the following steps：
Step 1: the quartz sand for treating pickling is put into pickling purifying plant, pickle is added, by pickling purifying plant
Temperature be heated to 85 DEG C, and ON cycle system makes the pickle circulation dynamic acid-washed quartz sand of heat, deviates from simultaneously after pickling 6h
Collect pickle；
Wherein, described pickle is by the hydrofluoric acid of 15 parts by weight, the fluosilicic acid of 20 parts by weight, the oxalic acid of 25 parts by weight, 8
The hydrochloric acid of parts by weight and the water of 90 parts by weight composition；
Step 2: the quartz sand after pickling is delivered in water washing device, multiple absorbent packets, the suction are buried into quartz sand
The embedded density of pocket is 30g/, and all absorbent packets are taken out after 20min, clear water immersion 20min is added into water washing device, so
Agitator treating afterwards, cleaning solution is discharged, be placed again into absorbent packet absorption, clear water immersion, agitator treating repeatedly to quartz sand surface
In neutrality, merge the cleaning solution；Clean quartz sand is gone to 4h is dried in drier, obtain the quartz sand of purifying；
Wherein, the absorbent packet is NACF material, and the particle diameter equipped with 5g is 0.5mm green grass or young crops inside the absorbent packet
Stone, the absorbent packet are fitted into after green stone before being put into quartz sand, have passed through pretreatment：By the absorption equipped with green stone
Bag, which is put into the limewash of clarification, soaks 20min, then takes out drying, stand-by；Wherein, being added in the limewash of clarification has volume
Fraction is 0.3% hydrogen peroxide；The present invention adds absorbent packet in the quartz sand after overpickling, adsorbs the residue in quartz sand
Acid, pure quartz sand is finally obtained by the washing of multiple clear water；The main component of green stone is CaO, also containing a certain amount of
MgO, the acid neutralized in acid solution can be absorbed, the absorbent packet equipped with green stone be buried in quartz sand, the residual in quartz sand
Acid solution slowly infiltrate through in absorbent packet, contact with green stone and neutralization reaction occur with it, absorbent packet is NACF material
Matter can adsorb peculiar smell caused by acid gas in quartz sand etc., repeatedly absorption and clear water washing, so as to obtain pure quartz sand,
The impurity and acid substance of quartz sand surface residual are rapidly and thoroughly cleaned, the acid content in cleaning solution, drop are reduced after absorption
The difficulty of low cleaning solution post-processing；
Step 3: the pickle of collection and the cleaning solution merged are gone in anhydride recovery plant, spent acid and waste water are carried out
Processing：Pickle and cleaning solution are imported into the upper space 5 by the inlet 1, start the heating mantle heats extremely
50 DEG C, after stirring 2h, stop heating, open first flashboard 3, liquid is imported into the central space 6, opens described first
Valve, liquid pH to 7 is adjusted, after stirring 30min, stand 20min, open second flashboard 4, liquid is imported into the bottom
Space 7, second valve is opened, adjust liquid pH to 9, after stirring 30min, stood 20min, discharged from the leakage fluid dram 2
Liquid, and with careless acid for adjusting pH to 7, filtering off except precipitation, obtains clear water and is sent into workshop and recycle.
As shown in figure 1, in the method that described acid-washed quartz sand is quickly cleaned, the anhydride recovery plant includes：
Tank body, it is the hollow structure closed up and down, and the top of the tank body is provided with inlet 1, and bottom is provided with leakage fluid dram
2, the 3rd screen pack is connected in the leakage fluid dram 2, the inside of the tank body is horizontal from top to bottom to be provided with the first flashboard 3 and the second lock
Plate 4, the tank interior is separated into mutual disconnected upper space 5, central space 6 and lower space 7, the upper space
5 tank wall is provided with heating mantle, the top of first flashboard 3 and second flashboard 4 be respectively equipped with the first screen pack and
Second screen pack；Agitator is equipped with the upper space 5, the central space 6 and the lower space 7；The top
The height ratio in space 5, the central space 6 and the lower space 7 is 1.5:1:1；
Acid mist recovering mechanism, it is arranged in the upper space 5 and is located at the top of inlet 1, and the acid mist returns
Receiving mechanism includes the pipe group that at least two row of horizontal are set, and the pipe group includes hollow pipe 8 that is multiple horizontal and being parallel to each other, described
The both ends of hollow pipe 8 are detachably connected with the inner tank wall respectively, and the both ends of the hollow pipe 8 contact with the inner tank wall
Position be provided with sealing gasket, the tube wall of the hollow pipe 8 is provided with multiple through holes 9, and the inside of hollow pipe 8 is filled with adsorber acid
The anion-cation exchange resin of mist；
First shower nozzle 10, it is arranged in the central space 6, and the inlet 1 of first shower nozzle 10 is soft by first
Pipe connects with the milk of lime holding vessel outside the tank body, and the middle part of first flexible pipe is provided with the first valve；
Second shower nozzle 11, it is arranged on the lower space 7, and the inlet 1 of second shower nozzle 11 passes through the second flexible pipe
Connected with the sodium hydrate aqueous solution holding vessel that the mass fraction outside the tank body is 2.5%, the middle part of second flexible pipe
Provided with the second valve；
First pH meter, it is arranged in the central space 6；
Second pH meter, it is arranged in the lower space 7；
First valve, second valve, first pH meter and second pH meter electrically connect with controller 12,
The controller 12 is arranged to：Receive the first pH value that first pH meter detects liquid in the central space 6, and described the
Second pH value of liquid in the lower space 7 of two pH meters detection, if the first pH value is less than 6, the controller 12 controls
First valve is opened, and first shower nozzle 10 conveys milk of lime to the central space 6, if the first pH value is not less than 6,
The controller 12 controls first valve to close；If the second pH value is less than 8.5, the controller 12 controls described second
Valve is opened, and second shower nozzle 11 conveys sodium hydrate aqueous solution to the lower space 7, if the second pH value is not less than 8.5
When, the controller 12 controls second valve to close.
Anhydride recovery plant is provided with upper, middle and lower space 7, first in upper space 5 by easily waving in acid solution
The acid of hair realizes the recovery of acid mist, in case of heating, hydrochloric acid and hydrofluoric acid in acid solution etc. have volatilized by resin adsorption
Acid be adsorbed acid resin adsorption, after the completion of absorption, hollow pipe 8 is taken out from upper space 5, and with the stripping liquids such as water will
Acid recovery in resin, the pickle that restored acid can add certain quantity of fresh are re-used in the acid cleaning process of quartz sand；Acid
The acid solution of upper space 5 is imported into central space 6 after the completion of mist recovery, the first shower nozzle 10 adds limewash, passes through control thereto
Device 12 processed adjusts acid solution pH to 6~7, and the fluosilicic acid in acid solution and oxalic acid are converted into calcium fluosilicate and calcium oxalate, remove acid solution
In fluosilicic acid and oxalic acid, collect the dilute sulfuric acid that calcium fluosilicate and calcium oxalate on the second screen pack add equivalent, generate fluorine silicon
Acid and oxalic acid, which can be fed again into the Pickling-shop of quartz sand, to be recycled, and the calcium sulfate of generation can make byproduct sale；In treating
After the acid solution in portion space 6 precipitates completely, the second flashboard 4 is opened, acid solution is imported in lower space 7, the second shower nozzle 11 is thereto
Sodium hydrate aqueous solution is added, adjusts pH to 8.5~9, the iron ion in acid solution forms ferric hydroxide precipitate in the basic conditions,
The iron ion in acid solution is removed, acid solution discharges anhydride recovery plant eventually through leakage fluid dram 2, adds careless acid for adjusting pH to 6~7,
By the calcium ions precipitate in acid solution, filter clear water can be sent into workshop recycling, as far as possible by acid solution in whole process
Utility reclaim and recycle, be finally reached zero-emission, no pollution.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, it is of the invention and unlimited
In specific details and shown here as the legend and embodiment with description.
Claims (9)
1. a kind of method that acid-washed quartz sand is quickly cleaned, it is characterised in that comprise the following steps：
Step 1: the quartz sand for treating pickling is put into pickling purifying plant, pickle is added, by the temperature in pickling purifying plant
Degree is heated to 60~85 DEG C, and ON cycle system makes the pickle circulation dynamic acid-washed quartz sand of heat, deviates from after 3~6h of pickling
And collect pickle；
Step 2: the quartz sand after pickling is delivered in water washing device, multiple absorbent packets, 10~20min are buried into quartz sand
After take out all absorbent packets, into water washing device add clear water soak 10~20min, then agitator treating, cleaning solution is discharged,
Absorbent packet absorption, clear water immersion, agitator treating are placed again into repeatedly to quartz sand surface in neutrality, merges the cleaning solution；Will
Clean quartz sand, which is gone to, dries 3~4h in drier, obtain the quartz sand of purifying；
Wherein, the absorbent packet is NACF material, and the particle diameter equipped with 1~5g is 0.2~0.5mm inside the absorbent packet
Green stone, the absorbent packet is fitted into after green stone before being put into quartz sand, have passed through pretreatment：By equipped with green stone
Absorbent packet is put into 10~20min of immersion in the limewash of clarification, then takes out drying, stand-by；
Step 3: the pickle of collection and the cleaning solution merged are gone in anhydride recovery plant, the place of spent acid and waste water is carried out
Reason.
2. the method that acid-washed quartz sand as claimed in claim 1 is quickly cleaned, it is characterised in that the anhydride recovery plant bag
Include：
Tank body, it is the hollow structure closed up and down, and the top of the tank body is provided with inlet, and bottom is provided with leakage fluid dram, described
The inside of tank body is horizontal from top to bottom to be provided with the first flashboard and the second flashboard, by the tank interior be separated into it is mutual it is disconnected on
Portion space, central space and lower space, the tank wall of the upper space are provided with heating mantle, first flashboard and described
The top of second flashboard is respectively equipped with the first screen pack and the second screen pack；The upper space, the central space and described
Agitator is equipped with lower space；
Acid mist recovering mechanism, it is arranged in the upper space and is located at the inlet top, the acid mist recovering mechanism
The pipe group set including at least two row of horizontal, the pipe group include hollow pipe that is multiple horizontal and being parallel to each other, the hollow pipe
Both ends be detachably connected respectively with the inner tank wall, the tube wall of the hollow pipe is provided with multiple through holes, the hollow pipe
Anion-cation exchange resin of the inside filled with absorption acid mist；
First shower nozzle, it is arranged in the central space, and the inlet of first shower nozzle passes through the first flexible pipe and the tank
Milk of lime holding vessel connection outside body, the middle part of first flexible pipe is provided with the first valve；
Second shower nozzle, it is arranged on the lower space, and the inlet of second shower nozzle passes through the second flexible pipe and the tank body
The sodium hydrate aqueous solution holding vessel that outside mass fraction is 2.5% connects, and the middle part of second flexible pipe is provided with the second valve
Door；
First pH meter, it is arranged in the central space；
Second pH meter, it is arranged in the lower space；
First valve, second valve, first pH meter and second pH meter are electrically connected with the controller, the control
Device processed is arranged to：Receive the first pH value that first pH meter detects liquid in the central space, and second pH meter inspection
Second pH value of liquid in the lower space surveyed, if the first pH value is less than 6, the controller controls first valve
To open, first shower nozzle conveys milk of lime to the central space, if the first pH value is not less than 6, the controller control
First valve is closed；If the second pH value is less than 8.5, the controller controls second valve to open, described second
Shower nozzle conveys sodium hydrate aqueous solution to the lower space, if the second pH value is not less than 8.5, described in the controller control
Second valve is closed.
3. the method that acid-washed quartz sand as claimed in claim 2 is quickly cleaned, it is characterised in that the specific behaviour of the step 3
As：Pickle and cleaning solution are imported into the upper space by the inlet, start the heating mantle heats to 40~
50 DEG C, after stirring 1~2h, stop heating, open first flashboard, liquid is imported into the central space, open described the
One valve, liquid pH to 6~7 is adjusted, after stirring 20~30min, stand 10~20min, second flashboard is opened, by liquid
The lower space is imported, opens second valve, adjusts liquid pH to 8.5~9, after stirring 20~30min, standing 10~
20min, from the leakage fluid dram discharge liquid, and use careless acid for adjusting pH to 6~7, filter off except precipitation, obtain clear water feeding workshop follow
Ring uses.
4. the method that acid-washed quartz sand as claimed in claim 3 is quickly cleaned, it is characterised in that is connected in the leakage fluid dram
Three screen packs.
5. the method that acid-washed quartz sand as claimed in claim 1 is quickly cleaned, it is characterised in that the absorbent packet it is embedded close
Spend for 30g/.
6. the method that acid-washed quartz sand as claimed in claim 2 is quickly cleaned, it is characterised in that the both ends of the hollow pipe with
The position of the inner tank wall contact is provided with sealing gasket.
7. the method that acid-washed quartz sand as claimed in claim 1 is quickly cleaned, it is characterised in that added in the limewash of clarification
There is the hydrogen peroxide that volume fraction is 0.1~0.3%.
8. the method that acid-washed quartz sand as claimed in claim 1 is quickly cleaned, it is characterised in that described pickle by 2~
The hydrofluoric acid of 15 parts by weight, the fluosilicic acid of 5~20 parts by weight, the oxalic acid of 4~25 parts by weight, the hydrochloric acid of 1~8 parts by weight and 50
The water composition of~90 parts by weight.
9. the method that acid-washed quartz sand as claimed in claim 2 is quickly cleaned, it is characterised in that the upper space, described
The height of central space and lower space ratio is 1.5:1:1.
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| CN108190894B (en) * | 2018-01-19 | 2019-12-06 | 徐州市万达石英有限公司 | acid washing circulation process of high-purity quartz sand |
| CN109607550B (en) * | 2019-01-07 | 2022-02-01 | 临沂昊泉硅业科技有限公司 | Deacidifying method for acid-washed quartz sand |
| CN109485050B (en) * | 2019-01-08 | 2021-11-02 | 临沂昊泉硅业科技有限公司 | Circulating pickling method for high-purity quartz sand convenient for removing impurities |
| CN112010316B (en) * | 2020-07-06 | 2022-08-12 | 安徽凤砂矿业集团有限公司 | Quartz sand processing technology |
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| US6277349B1 (en) * | 1998-11-14 | 2001-08-21 | C. Eric Westbrook | Tridymite-based processing for high purity quartz |
| CN103964445A (en) * | 2014-05-05 | 2014-08-06 | 临沂晟泉矿业有限公司 | Quartz sand pickling comprehensive recycle method |
| CN105016348A (en) * | 2015-07-16 | 2015-11-04 | 安徽东阳矿业科技有限公司 | Acidiferous quartz mortar treatment method |
| CN105036404A (en) * | 2015-06-30 | 2015-11-11 | 田辉明 | Zero discharge treatment method for acid wastewater generated by acid pickling and purification of quartz sand powder or feldspar sand powder |
| CN105197939A (en) * | 2015-09-26 | 2015-12-30 | 田辉明 | Acid pickling and waste acid treatment process for improving purity of powdery quartz sand |
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| US6277349B1 (en) * | 1998-11-14 | 2001-08-21 | C. Eric Westbrook | Tridymite-based processing for high purity quartz |
| CN103964445A (en) * | 2014-05-05 | 2014-08-06 | 临沂晟泉矿业有限公司 | Quartz sand pickling comprehensive recycle method |
| CN105036404A (en) * | 2015-06-30 | 2015-11-11 | 田辉明 | Zero discharge treatment method for acid wastewater generated by acid pickling and purification of quartz sand powder or feldspar sand powder |
| CN105016348A (en) * | 2015-07-16 | 2015-11-04 | 安徽东阳矿业科技有限公司 | Acidiferous quartz mortar treatment method |
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