CN108947156A - A kind of circulating red mud dealkalization system and method for water-saving efficient - Google Patents

A kind of circulating red mud dealkalization system and method for water-saving efficient Download PDF

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Publication number
CN108947156A
CN108947156A CN201811007835.4A CN201811007835A CN108947156A CN 108947156 A CN108947156 A CN 108947156A CN 201811007835 A CN201811007835 A CN 201811007835A CN 108947156 A CN108947156 A CN 108947156A
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liquid
filtrate
red mud
micro
reaction column
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CN108947156B (en
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黄建洪
张利祥
高强
高一强
田森林
胡学伟
李英杰
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/10Treatment of sludge; Devices therefor by pyrolysis

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  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The present invention relates to a kind of circulating red mud dealkalization system and methods of water-saving efficient, belong to trade waste processing technology field.The system includes alkali digestion series, solid-liquid separation system, ion exchange system, detection system, the liquid outlet of alkali digestion series is connected to the liquid inlet of solid-liquid separation system, the liquid outlet of solid-liquid separation system is connected to the liquid inlet of ion exchange system, the liquid outlet of ion exchange system is connected to the liquid inlet of detection system, and the liquid outlet of detection system is connected to the filtrate inlet of alkali digestion series.The circulating red mud dealkalization system of the present invention is after raw material addition, it is handled through alkali digestion series, the dealkalize liquid of micro-wave diminishing pot can be delivered to solid-liquid separation system automatically, filter residue that solid-liquid separation system is handled, filtrate can automatically return in micro-wave diminishing pot, conducive to circular treatment, after dealkalize is disposed, it is only necessary to open blow-off valve, it can be taken off dealkalize treated red mud, have the characteristics that easy to operate, efficient.

Description

A kind of circulating red mud dealkalization system and method for water-saving efficient
Technical field
The present invention relates to a kind of circulating red mud dealkalization system and methods of water-saving efficient, belong to trade waste processing skill Art field.
Background technique
A large amount of waste red mud residues can be generated in aluminum oxide industry, complicated mineral constituent, main mineral constituent be text Stone, calcite, gibbsite etc., containing a large amount of chemical bonding alkali in mineralogical composition, so have very strong buffer capacity, this Red mud alkalinity with higher is allowed for,;Common red mud treating method is the soil built red mud dump, but can pollute neighbouring Earth and underground water, it is also possible to threat can be generated to the personnel of surrounding, therefore, solve the problems, such as the high alkalinity of red mud, be that red mud is harmless Change, one step of key of resource utilization.
A kind of Wu Yong expensive et al. ardealite of patent of invention red mud is carried out quick dealkalize method (application number: 201110058514.9) it, by after ardealite and red mud grinding, is stirred after mixing with water by 2 ~ 3:4 ~ 6:80 ~ 150 weight ratio Reaction is mixed, precipitating is finally taken out and shines height, achieve the effect that dealkalize;
The patent of invention of Zhang Yihe et al. is a kind of to utilize CO2With the method for spent acid Combined Treatment Bayer process red mud dealkalize (application number: 201310295802.5) after, red mud powder and water are mixed in a certain ratio, it is passed through CO2It is acidified, is added into solidliquid mixture Enter spent acid, suction filtration separation finally is carried out to mixture;
A kind of patent of invention of Zhu Xiaobo et al. red mud citric acid dealkalize technique (application number: 201510629907.9), using three Grade cross-flow dealkalize technique, can effectively remove the sodium and potassium in red mud, and PH6.5 ~ 7.5 of dealkalize slag safe can be used as Stockpiling;It since citric acid is reacted with calcium generates calcium citrate and is fixed in alkaline residue, have product and utilized in terms of building materials Possibility.
A kind of biological dealkalization method of red mud of the patent of invention of Qu Yang et al. (application number: 201711229512.5), utilizes The method that microorganism produces acid carries out red mud dealkalization.By aspergillus niger spore inoculation of suspension liquid in culture medium, acid is produced in fermentor, so It will be mixed afterwards with the acid solution of strain separating and red mud powder and achieve the purpose that dealkalize,
Currently, the common dealkalization method of red mud mainly has washing, leach, lime dealkalize method, wet process carbonizatin method etc., in order to Reduce the Na ion and OH in red mud, all there are different disadvantages in every kind of method, washing method water consumption is huge, and alkalinity is gone Except rate is low, CO2It is high with the operating cost of the acid-hatching of young eggs, it be easy to cause secondary pollution;The inefficient of lime dealkalize be easy to cause instead Bullet;Bioanalysis is although environmentally protective, at low cost, but the cycle of operation is longer, be not suitable for large scale processing, and dealkalize efficiency compared with It is low.
Summary of the invention
The present invention is in view of the above-mentioned problems of the prior art, provide a kind of circulating red mud dealkalization system of water-saving efficient System, the present invention are handled after raw material addition through alkali digestion series, the dealkalize liquid of micro-wave diminishing pot can be delivered to solid-liquid point automatically From system, filter residue that solid-liquid separation system is handled, filtrate can be automatically returned in micro-wave diminishing pot, be conducive at circulation Reason, after dealkalize is disposed, it is only necessary to open blow-off valve, that is, can be taken off dealkalize treated red mud, have easy to operate, efficient The advantages of.
The present invention be solve its technical problem and the technical solution adopted is that:
A kind of circulating red mud dealkalization system of water-saving efficient, including alkali digestion series, solid-liquid separation system, ion exchange system System, detection system, the liquid outlet of alkali digestion series are connected to the liquid inlet of solid-liquid separation system, the liquid of solid-liquid separation system Body outlet is connected to the liquid inlet of ion exchange system, the liquid outlet of ion exchange system and the liquid inlet of detection system Connection, the liquid outlet of detection system are connected to the filtrate inlet of alkali digestion series;
The alkali digestion series include shell 1, micro-wave diminishing pot 2, microwave generator 20, blender 3, and micro-wave diminishing pot 2 is fixed It is arranged in shell 1, the side wall of shell 1 is arranged in microwave generator 20, and the microwave of microwave generator 20 occurs end and passes through waveguide Pipe 21 is connected to the internal cavity of micro-wave diminishing pot 2, and blender 3 is fixed at 1 top of shell, the stirring of blender 3 vertically Paddle passes through the roof of micro-wave diminishing pot 2 and extends downward into the bottom of micro-wave diminishing pot 2, and 1 top of shell is additionally provided with feed opening 4, water inlet 5, filter residue entrance 6, filtrate port 7, filtrate port 7 are the filtrate inlet of alkali digestion series, feed opening 4, water inlet 5, filter Slag entrance 6, filtrate port 7 pass through the top of feeding tube, water inlet line, filter residue pipeline, filtrate conduit and micro-wave diminishing pot 2 respectively Connection, filter residue entrance 6 are connected to by filter residue delivery pipe 12 with the solid outlet of solid-liquid separation system, the setting of 1 top sidewall of shell There is dealkalize liquid liquid suction pipe 8, one end of dealkalize liquid liquid suction pipe 8, which passes through the side wall of micro-wave diminishing pot 2 and bends downward, extends to microwave The middle bottom of counteracting tank 2,1 bottom of shell are vertically arranged with drainage conduit 9, and drainage conduit 9 is connected to the bottom of micro-wave diminishing pot 2, row Blow-off valve 10 is provided in expects pipe 9;
The bottom of the dealkalize liquid liquid suction pipe 8 is provided with peristaltic pump II 18, fluid flowmeter is provided on water inlet line, filter residue is defeated It send and is provided with solid pump on pipe 12,1 side wall of shell is provided with the relief tube inside connection micro-wave diminishing pot 2, on relief tube It is provided with relief valve and pressure gauge;
The dealkalize liquid liquid suction pipe 8 is scalable flexible duct;
The solid-liquid separation system is automatic discharge filter 11, the bottom end of dealkalize liquid liquid suction pipe 8 and automatic discharge filter 11 Liquid inlet connection, the slag-drip opening of dealkalize liquid liquid suction pipe 8 is connected to filter residue delivery pipe 12, the filtrate of automatic discharge filter 11 Outlet is connected to by filtrate conveyance conduit I with ion exchange system;
Peristaltic pump I 17 is provided on the filtrate conveyance conduit I;
The ion exchange system includes that liquid master enters pipe, reaction column liquid branch enters pipe, 2 or more the reaction columns being vertically arranged 13, the main outlet pipe of reaction column liquid payout tube, liquid, filtrate conveyance conduit I enter pipe with liquid master and are connected to, liquid master enter pipe with react Column liquid branch enters the top connection of pipe, and reaction column liquid branch enters pipe and reaction column 13 matches and reaction column liquid branch enters the bottom of pipe End be connected to the top of reaction column 13, is filled with strong-acid cation-exchange resin in reaction column 13, the bottom end of reaction column 13 with instead It answers the connection of column liquid payout tube and reaction column liquid payout tube matches with reaction column 13, reaction column liquid payout tube and liquid master Outlet pipe connection, the main outlet pipe of liquid are connected to by filtrate conveyance conduit II with detection system;
The reaction column liquid branch enters to be provided with reaction column solenoid valve 14 on pipe;
The detection system includes pH detector 15, sodium ion detector 16, filtrate conveyance conduit III, pH detector 15, sodium from Sub- detector 16 is arranged on filtrate conveyance conduit III, and one end of filtrate conveyance conduit III is connected to filtrate conveyance conduit II, The other end of filtrate conveyance conduit III is connected to the filtrate port 7 of alkali digestion series;
Peristaltic pump III 19 is provided on the filtrate conveyance conduit III.
A kind of circulating red mud dealkalization method of water-saving efficient, using the circulating red mud dealkalization system of water-saving efficient, tool Steps are as follows for body:
(1) by red mud, broken, grinding, sieving obtain red mud powder;
(2) red mud powder of step (1) is added in micro-wave diminishing pot by the feed opening of alkali digestion series, water is passed through into alkali soluble The water inlet of system is added in micro-wave diminishing pot out, is uniformly mixed by blender and is obtained mixed material;
(3) microwave generator is opened, is 80 ~ 260 DEG C, under stirring condition in temperature, the mixture in step (2) micro-wave diminishing pot Material carries out 20 ~ 30min of micro-wave digestion, complexing agent is added in micro-wave diminishing pot by feed opening, under microwave, stirring condition 5 ~ 15min is reacted, stewing process is layered to obtain supernatant and solid slag to solid-liquid;
(4) peristaltic pump II is opened, the supernatant extraction of step (3) is transported to by solid-liquid separation system by dealkalize liquid liquid suction pipe In, filter residue and filtrate are obtained by filtration by automatic discharge filter;Filter residue is delivered to by solid pump by filter residue delivery pipe Alkali digestion series top is simultaneously recycled into micro-wave diminishing pot by filter residue mouth;
(5) filtrate of step (4) is transported in the reaction column of ion exchange system by peristaltic pump I by filtrate conveyance conduit I, is filtered Hydroxide ion in liquid reacts to obtain dealkalize filtrate with the strong-acid cation-exchange resin in reaction column;
(6) the dealkalize filtrate of step (5) is delivered in the filtrate conveyance conduit III of detection system by filtrate conveyance conduit II, is led to The pH value for crossing the pH detector test dealkalize filtrate of detection system passes through the sodium ion detector test dealkalize filtrate of detection system Na ion concentration, and by reaction column liquid branch enter pipe reaction column solenoid valve adjust filtrate flow velocity to control in filtrate The strong-acid cation-exchange resin reaction time in hydroxide ion and reaction column;
(7) the dealkalize filtrate of step (6) is delivered to alkali digestion series top by filtrate conveyance conduit III and led to by peristaltic pump III Filtered fluid mouth is recycled into micro-wave diminishing pot;
(8) 7 above steps (3) of circulate operation ~ step (7), when stewing process is layered to obtain supernatant to solid-liquid in step (3) And solid slag, dealkalize red mud is discharged the blow-off valve for opening alkali digestion series by drainage conduit collects, and then passes through drainage conduit again Supernatant liquor is discharged;
Preferably, sieving was 500 ~ 700 meshes in the step (1);
Preferably, the mass ratio of red mud powder and water is 1:8 ~ 12 in the step (2);
Preferably, complexing agent is 8-hydroxy-quinoline, amion acetic acid, disodium EDTA, thiocyanation in the step (3) Potassium or malic acid, the additional amount of complexing agent are the 10 ~ 20% of mixed material A mass;
Preferably, 20 ~ 30:1 of ratio of height to diameter of step (5) reaction column;
Preferably, step (5) strong-acid cation-exchange resin is 001x7 (732) strong-acid cation-exchange resin.
Beneficial effects of the present invention:
(1) the method for the present invention can speed up the dissolution of red mud neutral and alkali ion in the way of microwave cooperative mechanical stir process, The filtrate filtered to dealkalize liquid returns to micro-wave digestion step, while filter residue after strong acid cation resin exchange processing Micro-wave digestion step is also returned to, continuous circular treatment, down to 1 ~ 3%, dealkalize rate not only takes off the red mud alkalinity after dealkalize up to 80% Alkali high-efficiency, and water consumption can be greatly decreased;
(2) after microwave digestion complexing agent (8-hydroxy-quinoline etc.) and stir process is added, to precipitate in the method for the present invention The high volence metal ions such as the Fe in leachate can prevent the exchanger resin in ion exchange process from inactivating;
(3) strong-acid cation-exchange resin of the invention is from a wealth of sources cheap, restores at low cost;Red mud can be greatly improved Low-coat scale operation may be implemented in dealkalize rate;
(4) present invention is handled after raw material addition through alkali digestion series, can be automatically delivered to the dealkalize liquid of micro-wave diminishing pot solid Liquid separation system, filter residue that solid-liquid separation system is handled, filtrate can automatically return in micro-wave diminishing pot, be conducive to circulation Processing, after dealkalize is disposed, it is only necessary to open blow-off valve, that is, can be taken off dealkalize treated red mud, have easy to operate, high The advantages of effect;
(2) ion exchange system of the invention can detect the pH of filtrate according to pH detection device, and when the pH >=9 of filtrate, replacement is anti- The strong-acid cation-exchange resin of Ying Zhu ensures in circulating treatment procedure that exchanger resin works normally, to avoid exchanger resin The problem of failing in use process.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the circulating red mud dealkalization system of the water-saving efficient of embodiment 1;
Wherein: 1- shell, 2- micro-wave diminishing pot, 3- blender, 4- feed opening, 5- water inlet, 6- filter residue entrance, 7- filtrate port, 8- dealkalize liquid liquid suction pipe, 9- drainage conduit, 10- blow-off valve, 11- automatic discharge filter, 12- filter residue delivery pipe, 13- reaction column, 14- reaction column solenoid valve, 15-pH detector, 16- sodium ion detector, 17- peristaltic pump I, 18- peristaltic pump II, 19- peristaltic pump III, 20- microwave generator, 21- waveguide.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1: as shown in Figure 1, as shown in Figure 1, a kind of circulating red mud dealkalization system of water-saving efficient, including alkali soluble System, solid-liquid separation system, ion exchange system, detection system out, the liquid outlet and solid-liquid separation system of alkali digestion series Liquid inlet connection, the liquid outlet of solid-liquid separation system is connected to the liquid inlet of ion exchange system, ion exchange system The liquid outlet of system is connected to the liquid inlet of detection system, the liquid outlet of detection system and the filtrate inlet of alkali digestion series Connection;
The present embodiment alkali digestion series include shell 1, micro-wave diminishing pot 2, microwave generator 20, blender 3, micro-wave diminishing pot 2 It is fixed in shell 1, the side wall of shell 1 is arranged in microwave generator 20, and the microwave of microwave generator 20 occurs end and passes through Waveguide 21 is connected to the internal cavity of micro-wave diminishing pot 2, and blender 3 is fixed at 1 top of shell vertically, blender 3 Agitating paddle passes through the roof of micro-wave diminishing pot 2 and extends downward into the bottom of micro-wave diminishing pot 2, and 1 top of shell, which is additionally provided with, to be added Material mouth 4, water inlet 5, filter residue entrance 6, filtrate port 7, filtrate port 7 are the filtrate inlet of alkali digestion series, feed opening 4, water inlet 5, filter residue entrance 6, filtrate port 7 pass through feeding tube, water inlet line, filter residue pipeline, filtrate conduit and micro-wave diminishing pot 2 respectively Top connection, filter residue entrance 6 are connected to by filter residue delivery pipe 12 with the solid outlet of solid-liquid separation system, 1 top sidewall of shell It is provided with dealkalize liquid liquid suction pipe 8, one end of dealkalize liquid liquid suction pipe 8 passes through the side wall of micro-wave diminishing pot 2 and bends downward and extends to The middle bottom of micro-wave diminishing pot 2,1 bottom of shell are vertically arranged with drainage conduit 9, the bottom company of drainage conduit 9 and micro-wave diminishing pot 2 It is logical, blow-off valve 10 is provided in drainage conduit 9;
The bottom of the present embodiment dealkalize liquid liquid suction pipe 8 is provided with peristaltic pump II 18, and fluid flowmeter is provided on water inlet line, filter Solid pump is provided in slag delivery pipe 12,1 side wall of shell is provided with the relief tube inside connection micro-wave diminishing pot 2, pressure release Relief valve and pressure gauge are provided on pipe;
The present embodiment dealkalize liquid liquid suction pipe 8 is scalable flexible duct;
The present embodiment solid-liquid separation system is automatic discharge filter 11, and the bottom end of dealkalize liquid liquid suction pipe 8 and automatic discharge filter The liquid inlet of machine 11 is connected to, and the slag-drip opening of dealkalize liquid liquid suction pipe 8 is connected to filter residue delivery pipe 12, automatic discharge filter 11 Filtrate (liquid is connected to by filtrate conveyance conduit I with ion exchange system;
Peristaltic pump I 17 is provided on the present embodiment filtrate conveyance conduit I;
The present embodiment ion exchange system includes that liquid master enters pipe, reaction column liquid branch enters pipe, 2 reaction columns being vertically arranged 13, the main outlet pipe of reaction column liquid payout tube, liquid, filtrate conveyance conduit I enter pipe with liquid master and are connected to, liquid master enter pipe with react Column liquid branch enters the top connection of pipe, and reaction column liquid branch enters pipe and reaction column 13 matches and reaction column liquid branch enters the bottom of pipe End be connected to the top of reaction column 13, is filled with strong-acid cation-exchange resin in reaction column 13, the bottom end of reaction column 13 with instead It answers the connection of column liquid payout tube and reaction column liquid payout tube matches with reaction column 13, reaction column liquid payout tube and liquid master Outlet pipe connection, the main outlet pipe of liquid are connected to by filtrate conveyance conduit II with detection system;
The present embodiment reaction column liquid branch enters to be provided with reaction column solenoid valve 14 on pipe;
The present embodiment detection system includes pH detector 15, sodium ion detector 16, filtrate conveyance conduit III, pH detector 15, Sodium ion detector 16 is arranged on filtrate conveyance conduit III, and one end of filtrate conveyance conduit III and filtrate conveyance conduit II connect Logical, the other end of filtrate conveyance conduit III is connected to the filtrate port 7 of alkali digestion series;
Peristaltic pump III 19 is provided on the present embodiment filtrate conveyance conduit III;
A kind of circulating red mud dealkalization method of water-saving efficient is specific to walk using the circulating red mud dealkalization system of water-saving efficient It is rapid as follows:
(1) by red mud, broken, grinding, sieving obtain red mud powder;
(2) red mud powder of step (1) is added in micro-wave diminishing pot by the feed opening of alkali digestion series, water is passed through into alkali soluble The water inlet of system is added in micro-wave diminishing pot out, is uniformly mixed by blender and is obtained mixed material;Wherein red mud powder with The mass ratio of water is 1:8 ~ 12;
(3) microwave generator is opened, is 80 ~ 260 DEG C, under stirring condition in temperature, the mixture in step (2) micro-wave diminishing pot Material carries out 20 ~ 30min of micro-wave digestion, complexing agent is added in micro-wave diminishing pot by feed opening, under microwave, stirring condition 5 ~ 15min is reacted, stewing process is layered to obtain supernatant and solid slag to solid-liquid;Wherein complexing agent is 8-hydroxy-quinoline, complexing The additional amount of agent is the 10 ~ 20% of mixed material A mass;
(4) peristaltic pump II is opened, the supernatant extraction of step (3) is transported to by solid-liquid separation system by dealkalize liquid liquid suction pipe In, filter residue and filtrate are obtained by filtration by automatic discharge filter;Filter residue is delivered to by solid pump by filter residue delivery pipe Alkali digestion series top is simultaneously recycled into micro-wave diminishing pot by filter residue mouth;
(5) filtrate of step (4) is transported in the reaction column of ion exchange system by peristaltic pump I by filtrate conveyance conduit I, is filtered Hydroxide ion in liquid reacts to obtain dealkalize filtrate with the strong-acid cation-exchange resin in reaction column;
(6) the dealkalize filtrate of step (5) is delivered in the filtrate conveyance conduit III of detection system by filtrate conveyance conduit II, is led to The pH value for crossing the pH detector test dealkalize filtrate of detection system passes through the sodium ion detector test dealkalize filtrate of detection system Na ion concentration, and by reaction column liquid branch enter pipe reaction column solenoid valve adjust filtrate flow velocity to control in filtrate The strong-acid cation-exchange resin reaction time in hydroxide ion and reaction column;
(7) the dealkalize filtrate of step (6) is delivered to alkali digestion series top by filtrate conveyance conduit III and led to by peristaltic pump III Filtered fluid mouth is recycled into micro-wave diminishing pot;
(8) 7 above steps (3) of circulate operation ~ step (7), when stewing process is layered to obtain supernatant to solid-liquid in step (3) And solid slag, dealkalize red mud is discharged the blow-off valve for opening alkali digestion series by drainage conduit collects, and then passes through drainage conduit again Supernatant liquor is discharged.
Embodiment 2: the structure of the circulating red mud dealkalization system of the present embodiment water-saving efficient and 1 water-saving efficient of embodiment The structure of circulating red mud dealkalization system is essentially identical, the difference is that: reaction column 13 is 3;The ratio of height to diameter 20 of reaction column: 1;
The circulating red mud dealkalization method of the present embodiment water-saving efficient, using the circulating red mud dealkalization system of water-saving efficient, tool Steps are as follows for body:
(1) by red mud, broken, grinding, 500 meshes excessively obtain red mud powder;
(2) red mud powder of step (1) is added in micro-wave diminishing pot by the feed opening of alkali digestion series, water is passed through into alkali soluble The water inlet of system is added in micro-wave diminishing pot out, is uniformly mixed by blender and is obtained mixed material;Wherein red mud powder with The mass ratio of water is 1:8;
(3) open microwave generator, be 80 DEG C, under stirring condition in temperature, the mixed material in step (2) micro-wave diminishing pot into Complexing agent (complexing agent is amion acetic acid) is added in micro-wave diminishing pot, micro- by row micro-wave digestion 20min by feed opening 5min is reacted under wave, stirring condition, stewing process is layered to obtain supernatant and solid slag to solid-liquid;Wherein complexing agent (amino second Acid) additional amount be mixed material A mass 10%;
(4) peristaltic pump II is opened, the supernatant extraction of step (3) is transported to by solid-liquid separation system by dealkalize liquid liquid suction pipe In, filter residue and filtrate are obtained by filtration by automatic discharge filter;Filter residue is delivered to by solid pump by filter residue delivery pipe Alkali digestion series top is simultaneously recycled into micro-wave diminishing pot by filter residue mouth;
(5) filtrate of step (4) is transported in the reaction column of ion exchange system by peristaltic pump I by filtrate conveyance conduit I, is filtered Hydroxide ion in liquid reacts to obtain dealkalize filtrate with the strong-acid cation-exchange resin in reaction column;
(6) the dealkalize filtrate of step (5) is delivered in the filtrate conveyance conduit III of detection system by filtrate conveyance conduit II, is led to The pH value for crossing the pH detector test dealkalize filtrate of detection system passes through the sodium ion detector test dealkalize filtrate of detection system Na ion concentration, and by reaction column liquid branch enter pipe reaction column solenoid valve adjust filtrate flow velocity to control in filtrate The strong-acid cation-exchange resin reaction time in hydroxide ion and reaction column;
(7) the dealkalize filtrate of step (6) is delivered to alkali digestion series top by filtrate conveyance conduit III and led to by peristaltic pump III Filtered fluid mouth is recycled into micro-wave diminishing pot;
(8) 7 steps (3) of circulate operation ~ step (7), when stewing process to solid-liquid is layered to obtain supernatant and consolidate in step (3) Body slag, dealkalize red mud is discharged the blow-off valve for opening alkali digestion series by drainage conduit collects, and is then discharged again by drainage conduit Supernatant liquor;
By the measurement (NY/T 1121.2-2006) of P in soil H, soil total calcium, magnesium, sodium measurement (NY/T 296- 1995) method detects, and alkalinity is down to 3.0% in the present embodiment dealkalize red mud.
Embodiment 2: the structure of the circulating red mud dealkalization system of the present embodiment water-saving efficient and 1 water-saving efficient of embodiment The structure of circulating red mud dealkalization system is essentially identical, the difference is that: reaction column 13 is 4, the ratio of height to diameter 24 of reaction column: 1;
The circulating red mud dealkalization method of the present embodiment water-saving efficient, using the circulating red mud dealkalization system of water-saving efficient, tool Steps are as follows for body:
(1) by red mud, broken, grinding, 600 meshes excessively obtain red mud powder;
(2) red mud powder of step (1) is added in micro-wave diminishing pot by the feed opening of alkali digestion series, water is passed through into alkali soluble The water inlet of system is added in micro-wave diminishing pot out, is uniformly mixed by blender and is obtained mixed material;Wherein red mud powder with The mass ratio of water is 1:12;
(3) microwave generator is opened, is 140 DEG C, under stirring condition in temperature, the mixed material in step (2) micro-wave diminishing pot Micro-wave digestion 30min is carried out, complexing agent (complexing agent is disodium EDTA) is added to microwave by feed opening and is disappeared It solves in tank, 15min is reacted under microwave, stirring condition, stewing process is layered to obtain supernatant and solid slag to solid-liquid;Wherein network The additional amount of mixture (disodium EDTA) is the 20% of mixed material A mass;
(4) peristaltic pump II is opened, the supernatant extraction of step (3) is transported to by solid-liquid separation system by dealkalize liquid liquid suction pipe In, filter residue and filtrate are obtained by filtration by automatic discharge filter;Filter residue is delivered to by solid pump by filter residue delivery pipe Alkali digestion series top is simultaneously recycled into micro-wave diminishing pot by filter residue mouth;
(5) filtrate of step (4) is transported in the reaction column of ion exchange system by peristaltic pump I by filtrate conveyance conduit I, is filtered Hydroxide ion in liquid reacts to obtain dealkalize filtrate with the strong-acid cation-exchange resin in reaction column;
(6) the dealkalize filtrate of step (5) is delivered in the filtrate conveyance conduit III of detection system by filtrate conveyance conduit II, is led to The pH value for crossing the pH detector test dealkalize filtrate of detection system passes through the sodium ion detector test dealkalize filtrate of detection system Na ion concentration, and by reaction column liquid branch enter pipe reaction column solenoid valve adjust filtrate flow velocity to control in filtrate The strong-acid cation-exchange resin reaction time in hydroxide ion and reaction column;
(7) the dealkalize filtrate of step (6) is delivered to alkali digestion series top by filtrate conveyance conduit III and led to by peristaltic pump III Filtered fluid mouth is recycled into micro-wave diminishing pot;
(8) 8 steps (3) of circulate operation ~ step (7), when stewing process to solid-liquid is layered to obtain supernatant and consolidate in step (3) Body slag, dealkalize red mud is discharged the blow-off valve for opening alkali digestion series by drainage conduit collects, and is then discharged again by drainage conduit Supernatant liquor;
By the measurement (NY/T 1121.2-2006) of P in soil H, soil total calcium, magnesium, sodium measurement (NY/T 296- 1995) method detects, and alkalinity is down to 2.6% in the present embodiment dealkalize red mud.
Embodiment 3: the structure of the circulating red mud dealkalization system of the present embodiment water-saving efficient and 1 water-saving efficient of embodiment The structure of circulating red mud dealkalization system is essentially identical, the difference is that: reaction column 13 is 5, the ratio of height to diameter 26 of reaction column: 1;
The circulating red mud dealkalization method of the present embodiment water-saving efficient, using the circulating red mud dealkalization system of water-saving efficient, tool Steps are as follows for body:
(1) by red mud, broken, grinding, 700 meshes excessively obtain red mud powder;
(2) red mud powder of step (1) is added in micro-wave diminishing pot by the feed opening of alkali digestion series, water is passed through into alkali soluble The water inlet of system is added in micro-wave diminishing pot out, is uniformly mixed by blender and is obtained mixed material;Wherein red mud powder with The mass ratio of water is 1:10;
(3) microwave generator is opened, is 180 DEG C, under stirring condition in temperature, the mixed material in step (2) micro-wave diminishing pot Micro-wave digestion 25min is carried out, complexing agent (complexing agent is potassium rhodanate) is added in micro-wave diminishing pot by feed opening, micro- 10min is reacted under wave, stirring condition, stewing process is layered to obtain supernatant and solid slag to solid-liquid;Wherein complexing agent (thiocyanation Potassium) additional amount be mixed material A mass 15%;
(4) peristaltic pump II is opened, the supernatant extraction of step (3) is transported to by solid-liquid separation system by dealkalize liquid liquid suction pipe In, filter residue and filtrate are obtained by filtration by automatic discharge filter;Filter residue is delivered to by solid pump by filter residue delivery pipe Alkali digestion series top is simultaneously recycled into micro-wave diminishing pot by filter residue mouth;
(5) filtrate of step (4) is transported in the reaction column of ion exchange system by peristaltic pump I by filtrate conveyance conduit I, is filtered Hydroxide ion in liquid reacts to obtain dealkalize filtrate with the strong-acid cation-exchange resin in reaction column;
(6) the dealkalize filtrate of step (5) is delivered in the filtrate conveyance conduit III of detection system by filtrate conveyance conduit II, is led to The pH value for crossing the pH detector test dealkalize filtrate of detection system passes through the sodium ion detector test dealkalize filtrate of detection system Na ion concentration, and by reaction column liquid branch enter pipe reaction column solenoid valve adjust filtrate flow velocity to control in filtrate The strong-acid cation-exchange resin reaction time in hydroxide ion and reaction column;
(7) the dealkalize filtrate of step (6) is delivered to alkali digestion series top by filtrate conveyance conduit III and led to by peristaltic pump III Filtered fluid mouth is recycled into micro-wave diminishing pot;
(8) 9 steps (3) of circulate operation ~ step (7), when stewing process to solid-liquid is layered to obtain supernatant and consolidate in step (3) Body slag, dealkalize red mud is discharged the blow-off valve for opening alkali digestion series by drainage conduit collects, and is then discharged again by drainage conduit Supernatant liquor;
By the measurement (NY/T 1121.2-2006) of P in soil H, soil total calcium, magnesium, sodium measurement (NY/T 296- 1995) method detects, and alkalinity is down to 2.1% in the present embodiment dealkalize red mud.
Embodiment 4: the structure of the circulating red mud dealkalization system of the present embodiment water-saving efficient and 1 water-saving efficient of embodiment The structure of circulating red mud dealkalization system is essentially identical, the difference is that: reaction column 13 is 6, the ratio of height to diameter 28 of reaction column: 1;
The circulating red mud dealkalization method of the present embodiment water-saving efficient, using the circulating red mud dealkalization system of water-saving efficient, tool Steps are as follows for body:
(1) by red mud, broken, grinding, 650 meshes excessively obtain red mud powder;
(2) red mud powder of step (1) is added in micro-wave diminishing pot by the feed opening of alkali digestion series, water is passed through into alkali soluble The water inlet of system is added in micro-wave diminishing pot out, is uniformly mixed by blender and is obtained mixed material;Wherein red mud powder with The mass ratio of water is 1:10;
(3) microwave generator is opened, is 220 DEG C, under stirring condition in temperature, the mixed material in step (2) micro-wave diminishing pot Micro-wave digestion 25min is carried out, complexing agent (complexing agent is malic acid) is added in micro-wave diminishing pot by feed opening, micro- 10min is reacted under wave, stirring condition, stewing process is layered to obtain supernatant and solid slag to solid-liquid;Wherein complexing agent (apple Acid) additional amount be mixed material A mass 15%;
(4) peristaltic pump II is opened, the supernatant extraction of step (3) is transported to by solid-liquid separation system by dealkalize liquid liquid suction pipe In, filter residue and filtrate are obtained by filtration by automatic discharge filter;Filter residue is delivered to by solid pump by filter residue delivery pipe Alkali digestion series top is simultaneously recycled into micro-wave diminishing pot by filter residue mouth;
(5) filtrate of step (4) is transported in the reaction column of ion exchange system by peristaltic pump I by filtrate conveyance conduit I, is filtered Hydroxide ion in liquid reacts to obtain dealkalize filtrate with the strong-acid cation-exchange resin in reaction column;
(6) the dealkalize filtrate of step (5) is delivered in the filtrate conveyance conduit III of detection system by filtrate conveyance conduit II, is led to The pH value for crossing the pH detector test dealkalize filtrate of detection system passes through the sodium ion detector test dealkalize filtrate of detection system Na ion concentration, and by reaction column liquid branch enter pipe reaction column solenoid valve adjust filtrate flow velocity to control in filtrate The strong-acid cation-exchange resin reaction time in hydroxide ion and reaction column;
(7) the dealkalize filtrate of step (6) is delivered to alkali digestion series top by filtrate conveyance conduit III and led to by peristaltic pump III Filtered fluid mouth is recycled into micro-wave diminishing pot;
(8) 9 steps (3) of circulate operation ~ step (7), when stewing process to solid-liquid is layered to obtain supernatant and consolidate in step (3) Body slag, dealkalize red mud is discharged the blow-off valve for opening alkali digestion series by drainage conduit collects, and is then discharged again by drainage conduit Supernatant liquor;
By the measurement (NY/T 1121.2-2006) of P in soil H, soil total calcium, magnesium, sodium measurement (NY/T 296- 1995) method detects, and alkalinity is down to 1.4% in the present embodiment dealkalize red mud.
Embodiment 5: the structure of the circulating red mud dealkalization system of the present embodiment water-saving efficient and 1 water-saving efficient of embodiment The structure of circulating red mud dealkalization system is essentially identical, the difference is that: reaction column 13 is 5, the ratio of height to diameter 30 of reaction column: 1;
The circulating red mud dealkalization method of the present embodiment water-saving efficient, using the circulating red mud dealkalization system of water-saving efficient, tool Steps are as follows for body:
(1) by red mud, broken, grinding, 700 meshes excessively obtain red mud powder;
(2) red mud powder of step (1) is added in micro-wave diminishing pot by the feed opening of alkali digestion series, water is passed through into alkali soluble The water inlet of system is added in micro-wave diminishing pot out, is uniformly mixed by blender and is obtained mixed material;Wherein red mud powder with The mass ratio of water is 1:8;
(3) microwave generator is opened, is 260 DEG C, under stirring condition in temperature, the mixed material in step (2) micro-wave diminishing pot Micro-wave digestion 20min is carried out, complexing agent (complexing agent is 8-hydroxy-quinoline) is added in micro-wave diminishing pot by feed opening, 15min is reacted under microwave, stirring condition, stewing process is layered to obtain supernatant and solid slag to solid-liquid;Wherein complexing agent (eight hydroxyls Base quinoline) additional amount be mixed material A mass 10%;
(4) peristaltic pump II is opened, the supernatant extraction of step (3) is transported to by solid-liquid separation system by dealkalize liquid liquid suction pipe In, filter residue and filtrate are obtained by filtration by automatic discharge filter;Filter residue is delivered to by solid pump by filter residue delivery pipe Alkali digestion series top is simultaneously recycled into micro-wave diminishing pot by filter residue mouth;
(5) filtrate of step (4) is transported in the reaction column of ion exchange system by peristaltic pump I by filtrate conveyance conduit I, is filtered Hydroxide ion in liquid reacts to obtain dealkalize filtrate with the strong-acid cation-exchange resin in reaction column;
(6) the dealkalize filtrate of step (5) is delivered in the filtrate conveyance conduit III of detection system by filtrate conveyance conduit II, is led to The pH value for crossing the pH detector test dealkalize filtrate of detection system passes through the sodium ion detector test dealkalize filtrate of detection system Na ion concentration, and by reaction column liquid branch enter pipe reaction column solenoid valve adjust filtrate flow velocity to control in filtrate The strong-acid cation-exchange resin reaction time in hydroxide ion and reaction column;
(7) the dealkalize filtrate of step (6) is delivered to alkali digestion series top by filtrate conveyance conduit III and led to by peristaltic pump III Filtered fluid mouth is recycled into micro-wave diminishing pot;
(8) 10 steps (3) of circulate operation ~ step (7), when in step (3) stewing process to solid-liquid be layered to obtain supernatant and Solid slag, dealkalize red mud is discharged the blow-off valve for opening alkali digestion series by drainage conduit collects, and is then arranged again by drainage conduit Supernatant liquor out;
By the measurement (NY/T 1121.2-2006) of P in soil H, soil total calcium, magnesium, sodium measurement (NY/T 296- 1995) method detects, and alkalinity is down to 1.0% in the present embodiment dealkalize red mud.
Specific embodiments of the present invention are explained in detail above in conjunction with attached drawing, but the present invention is not limited to above-mentioned realities Example is applied, it within the knowledge of a person skilled in the art, can also be without departing from the purpose of the present invention Various changes can be made.

Claims (13)

1. a kind of circulating red mud dealkalization system of water-saving efficient, it is characterised in that: including alkali digestion series, be separated by solid-liquid separation system System, ion exchange system, detection system, the liquid outlet of alkali digestion series are connected to the liquid inlet of solid-liquid separation system, Gu The liquid outlet of liquid separation system is connected to the liquid inlet of ion exchange system, the liquid outlet of ion exchange system and detection The liquid inlet of system is connected to, and the liquid outlet of detection system is connected to the filtrate inlet of alkali digestion series.
2. the circulating red mud dealkalization system of water-saving efficient according to claim 1, it is characterised in that: alkali digestion series include Shell (1), micro-wave diminishing pot (2), microwave generator (20), blender (3), micro-wave diminishing pot (2) are fixed at shell (1) Interior, the side wall in shell (1) is arranged in microwave generator (20), and the microwave of microwave generator (20) occurs end and passes through waveguide (21) It is connected to the internal cavity of micro-wave diminishing pot (2), blender (3) is fixed at shell (1) top vertically, blender (3) Agitating paddle passes through the roof of micro-wave diminishing pot (2) and extends downward into the bottom of micro-wave diminishing pot (2), and shell (1) top is also set It is equipped with feed opening (4), water inlet (5), filter residue entrance (6), filtrate port (7), filtrate port (7) is that the filtrate of alkali digestion series enters Mouthful, feed opening (4), water inlet (5), filter residue entrance (6), filtrate port (7) pass through feeding tube, water inlet line, filter residue pipe respectively Road, filtrate conduit are connected to the top of micro-wave diminishing pot (2), and filter residue entrance (6) is by filter residue delivery pipe (12) and is separated by solid-liquid separation The solid outlet of system is connected to, and shell (1) top sidewall is provided with dealkalize liquid liquid suction pipe (8), one end of dealkalize liquid liquid suction pipe (8) The middle bottom of micro-wave diminishing pot (2) is extended to across the side wall and bending downward of micro-wave diminishing pot (2), shell (1) bottom is vertical It is provided with drainage conduit (9), drainage conduit (9) is connected to the bottom of micro-wave diminishing pot (2), and drainage conduit is provided with blow-off valve on (9) (10).
3. the circulating red mud dealkalization system of water-saving efficient according to claim 2, it is characterised in that: dealkalize liquid liquid suction pipe (8) bottom is provided with peristaltic pump II (18), and fluid flowmeter is provided on water inlet line, and filter residue delivery pipe is provided on (12) Solid pump, shell (1) side wall are provided with the internal relief tube of connection micro-wave diminishing pot (2), are provided with pressure release on relief tube Valve and pressure gauge.
4. the circulating red mud dealkalization system of water-saving efficient according to claim 2, it is characterised in that: dealkalize liquid liquid suction pipe It (8) is scalable flexible duct.
5. the circulating red mud dealkalization system of water-saving efficient according to claim 2, it is characterised in that: solid-liquid separation system is The bottom end of automatic discharge filter (11), dealkalize liquid liquid suction pipe (8) is connected to the liquid inlet of automatic discharge filter (11), is taken off The slag-drip opening of lye liquid suction pipe (8) is connected to filter residue delivery pipe (12), and the filtrate (liquid of automatic discharge filter (11) passes through filter Liquid conveyance conduit I is connected to ion exchange system.
6. the circulating red mud dealkalization system of water-saving efficient according to claim 5, it is characterised in that: filtrate conveyance conduit I On be provided with peristaltic pump I (17).
7. the circulating red mud dealkalization system of water-saving efficient according to claim 5, it is characterised in that: ion exchange system packet Include that liquid master enters pipe, reaction column liquid branch enters pipe, 2 or more reaction column (13), the reaction column liquid payout tubes, liquid being vertically arranged The main outlet pipe of body, filtrate conveyance conduit I enter pipe with liquid master and are connected to, and liquid master enters pipe and reaction column liquid branch enters the top company of pipe Logical, reaction column liquid branch enters pipe and reaction column (13) match and reaction column liquid branch enters the bottom end of pipe and the top of reaction column (13) End connection, reaction column (13) is interior to be filled with strong-acid cation-exchange resin, and the bottom end of reaction column (13) and reaction column liquid are paid Pipe is connected to and reaction column liquid payout tube matches with reaction column (13), and reaction column liquid payout tube is connected to the main outlet pipe of liquid, The main outlet pipe of liquid is connected to by filtrate conveyance conduit II with detection system.
8. the circulating red mud dealkalization system of water-saving efficient according to claim 7, it is characterised in that: reaction column liquid branch enters Reaction column solenoid valve (14) are provided on pipe.
9. the circulating red mud dealkalization system of water-saving efficient according to claim 7, it is characterised in that: detection system includes pH Detector (15), sodium ion detector (16), filtrate conveyance conduit III, pH detector (15), sodium ion detector (16) are all provided with It sets on filtrate conveyance conduit III, one end of filtrate conveyance conduit III is connected to filtrate conveyance conduit II, filtrate conveyance conduit III The other end be connected to the filtrate port (7) of alkali digestion series.
10. the circulating red mud dealkalization system of water-saving efficient according to claim 9, it is characterised in that: filtrate conveyance conduit Peristaltic pump III (19) is provided on III.
11. a kind of circulating red mud dealkalization method of water-saving efficient, which is characterized in that de- using the circulating red mud of water-saving efficient Alkali system, the specific steps are as follows:
(1) by red mud, broken, grinding, sieving obtain red mud powder;
(2) red mud powder of step (1) is added in micro-wave diminishing pot by the feed opening of alkali digestion series, water is passed through into alkali soluble The water inlet of system is added in micro-wave diminishing pot out, is uniformly mixed by blender and is obtained mixed material A;
(3) microwave generator is opened, is 80 ~ 260 DEG C, under stirring condition in temperature, the mixture in step (2) micro-wave diminishing pot Material carries out 20 ~ 30min of micro-wave digestion, complexing agent is added in the mixed material A of micro-wave diminishing pot by feed opening, micro- 5 ~ 15min is reacted under wave, stirring condition, stewing process to solid-liquid is layered to obtain supernatant and resolution slag;
(4) peristaltic pump II is opened, the supernatant extraction of step (3) is transported to by solid-liquid separation system by dealkalize liquid liquid suction pipe In, filter residue and filtrate are obtained by filtration by automatic discharge filter;Filter residue is delivered to by solid pump by filter residue delivery pipe Alkali digestion series top is simultaneously recycled into micro-wave diminishing pot by filter residue mouth;
(5) filtrate of step (4) is transported in the reaction column of ion exchange system by peristaltic pump I by filtrate conveyance conduit I, is filtered Hydroxide ion in liquid reacts to obtain dealkalize filtrate with the strong-acid cation-exchange resin in reaction column;
(6) the dealkalize filtrate of step (5) is delivered in the filtrate conveyance conduit III of detection system by filtrate conveyance conduit II, is led to The pH value for crossing the pH detector test dealkalize filtrate of detection system passes through the sodium ion detector test dealkalize filtrate of detection system Na ion concentration, and by reaction column liquid branch enter pipe reaction column solenoid valve adjust filtrate flow velocity to control in filtrate The strong-acid cation-exchange resin reaction time in hydroxide ion and reaction column;
(7) the dealkalize filtrate of step (6) is delivered to alkali digestion series top by filtrate conveyance conduit III and led to by peristaltic pump III Filtered fluid mouth is recycled into micro-wave diminishing pot;
(8) 7 above steps (3) of circulate operation ~ step (7), when stewing process is layered to obtain supernatant to solid-liquid in step (3) With resolution slag, the blow-off valve for opening alkali digestion series will clear up slag, that is, dealkalize red mud and be collected by drainage conduit discharge, then be led to again Cross drainage conduit discharge supernatant liquor.
12. the circulating red mud dealkalization method of water-saving efficient according to claim 11, it is characterised in that: red in step (2) The mass ratio of mud powder and water is 1:8 ~ 12.
13. the circulating red mud dealkalization method of water-saving efficient according to claim 11, it is characterised in that: network in step (3) Mixture is that complexing agent is 8-hydroxy-quinoline, amion acetic acid, disodium EDTA, potassium rhodanate or malic acid, complexing agent Additional amount be mixed material A mass 10 ~ 20%.
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CN110482821A (en) * 2019-08-13 2019-11-22 昆明理工大学 The circulating water type dealkalize system and dealkalization method of a kind of sulfur-bearing tailing to red mud

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CN106267882A (en) * 2016-08-30 2017-01-04 李斌 A kind of microwave coupling leach extraction method and device
CN106809863A (en) * 2017-02-10 2017-06-09 河南理工大学 A kind of method that red mud reclaims NaOH
CN106865923A (en) * 2017-02-14 2017-06-20 同济大学 The red mud dealkalization and recovery process of a kind of electrodialysis coupled ion exchanger resin
CN208995357U (en) * 2018-08-31 2019-06-18 昆明理工大学 A kind of circulating red mud dealkalization system of water-saving efficient

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Publication number Priority date Publication date Assignee Title
CN104071995A (en) * 2014-07-18 2014-10-01 河南理工大学 Red mud on-line comprehensive treatment method
CN106267882A (en) * 2016-08-30 2017-01-04 李斌 A kind of microwave coupling leach extraction method and device
CN106809863A (en) * 2017-02-10 2017-06-09 河南理工大学 A kind of method that red mud reclaims NaOH
CN106865923A (en) * 2017-02-14 2017-06-20 同济大学 The red mud dealkalization and recovery process of a kind of electrodialysis coupled ion exchanger resin
CN208995357U (en) * 2018-08-31 2019-06-18 昆明理工大学 A kind of circulating red mud dealkalization system of water-saving efficient

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110482821A (en) * 2019-08-13 2019-11-22 昆明理工大学 The circulating water type dealkalize system and dealkalization method of a kind of sulfur-bearing tailing to red mud

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