CN108947156B - Water-saving and efficient circulating red mud dealkalization system and method - Google Patents
Water-saving and efficient circulating red mud dealkalization system and method Download PDFInfo
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- CN108947156B CN108947156B CN201811007835.4A CN201811007835A CN108947156B CN 108947156 B CN108947156 B CN 108947156B CN 201811007835 A CN201811007835 A CN 201811007835A CN 108947156 B CN108947156 B CN 108947156B
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Abstract
The invention relates to a water-saving efficient circulating red mud dealkalization system and a method, and belongs to the technical field of industrial waste treatment. The system comprises an alkali dissolution system, a solid-liquid separation system, an ion exchange system and a detection system, wherein a liquid outlet of the alkali dissolution system is communicated with a liquid inlet of the solid-liquid separation system, a liquid outlet of the solid-liquid separation system is communicated with a liquid inlet of the ion exchange system, a liquid outlet of the ion exchange system is communicated with a liquid inlet of the detection system, and a liquid outlet of the detection system is communicated with a filtrate inlet of the alkali dissolution system. After the raw materials are added, the circulating red mud dealkalization system is treated by the alkali dissolution system, dealkalization liquid of the microwave digestion tank can be automatically conveyed to the solid-liquid separation system, filter residues and filtrate obtained by treatment of the solid-liquid separation system can be automatically returned to the microwave digestion tank, circulation treatment is facilitated, and after dealkalization treatment is finished, the dealkalized red mud can be taken out only by opening the discharge valve, so that the circulating red mud dealkalization system has the characteristics of convenience in operation and high efficiency.
Description
Technical Field
The invention relates to a water-saving efficient circulating red mud dealkalization system and a method, and belongs to the technical field of industrial waste treatment.
Background
In the alumina industry, a large amount of red mud waste residues are generated, complex mineral components are mainly selected from aragonite, calcite, gibbsite and the like, and the mineral components contain a large amount of chemically combined alkali, so that the red mud has strong buffering capacity, and the red mud has higher alkalinity; the common red mud treatment method is to build a red mud disposal site, but the nearby soil and groundwater can be polluted, and the threat to surrounding personnel can be generated, so that the problem of high alkalinity of the red mud is solved, and the method is a key step of harmless and recycling of the red mud.
Wu Yonggui et al, discloses a method for rapidly dealkalizing red mud by phosphogypsum (application number: 201110058514.9), which comprises the steps of grinding phosphogypsum and red mud, and mixing the ground phosphogypsum and red mud with water according to a ratio of 2-3: 4-6: mixing the materials in a weight ratio of 80-150, stirring the materials for reaction, and finally taking out the precipitate and sun-drying the precipitate to achieve the dealkalization effect;
zhang Yihe et al, an invention patent using CO 2 Method for dealkalizing Bayer process red mud by combining waste acid (application number: 201310295802.5) comprises mixing red mud powder with water according to a certain proportion, and introducing CO 2 Acidifying, namely adding waste acid into the solid-liquid mixture, and finally carrying out suction filtration and separation on the mixture;
zhu Xiaobo et al, a red mud citric acid dealkalization process (application number: 201510629907.9) adopts a three-stage cross-flow dealkalization process, so that sodium and potassium in red mud can be effectively removed, and PH of dealkalized slag is 6.5-7.5, and the dealkalized slag can be safely used as stockpiling; the reaction of citric acid and calcium produces calcium citrate fixed in the caustic sludge, which makes the product possible for use in building material.
Qu Yang et al, discloses a red mud alkaloid removing method (application number: 201711229512.5), which uses a method of producing acid by microorganisms to remove the alkali from the red mud. Inoculating Aspergillus niger spore suspension into culture medium, producing acid in fermentation tank, mixing acid liquor separated from strain with red mud powder to obtain dealkalized product,
at present, the common dealkalization methods of red mud mainly comprise washing, leaching, lime dealkalization method, wet carbonization method and the like, and aim to reduce Na ions and OH in the red mud – Each method has different disadvantages, the washing method has huge water consumption, the alkaline removal rate is low, and the CO is removed 2 The operation cost of the acid leaching method is high, and secondary pollution is easy to cause; the lime dealkalization efficiency is low, and rebound is easy to occur; although the biological method is green and environment-friendly, the cost is low, the operation period is longer, the method is not suitable for large-scale treatment, and the dealkalization efficiency is lower.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a water-saving and efficient circulating red mud dealkalization system, after raw materials are added, dealkalization liquid of a microwave digestion tank can be automatically conveyed to a solid-liquid separation system through treatment of an alkali dissolution system, filter residues and filtrate obtained through treatment of the solid-liquid separation system can be automatically returned to the microwave digestion tank, circulation treatment is facilitated, and after dealkalization treatment is finished, the dealkalized red mud can be taken out only by opening a discharge valve, so that the system has the advantages of convenience in operation and high efficiency.
The invention adopts the technical proposal for solving the technical problems that:
the water-saving and efficient circulating red mud dealkalization system comprises an alkali dissolution system, a solid-liquid separation system, an ion exchange system and a detection system, wherein a liquid outlet of the alkali dissolution system is communicated with a liquid inlet of the solid-liquid separation system, a liquid outlet of the solid-liquid separation system is communicated with a liquid inlet of the ion exchange system, a liquid outlet of the ion exchange system is communicated with a liquid inlet of the detection system, and a liquid outlet of the detection system is communicated with a filtrate inlet of the alkali dissolution system;
the alkali dissolution system comprises a shell 1, a microwave digestion tank 2, a microwave generator 20 and a stirrer 3, wherein the microwave digestion tank 2 is fixedly arranged in the shell 1, the microwave generator 20 is arranged on the side wall of the shell 1, the microwave generation end of the microwave generator 20 is communicated with the internal cavity of the microwave digestion tank 2 through a waveguide 21, the stirrer 3 is vertically and fixedly arranged at the top end of the shell 1, a stirring paddle of the stirrer 3 penetrates through the top wall of the microwave digestion tank 2 and downwards extends to the bottom of the microwave digestion tank 2, the top end of the shell 1 is also provided with a feed inlet 4, a water inlet 5, a filter residue inlet 6 and a filtrate outlet 7, the filtrate outlet 7 is a filtrate inlet of the alkali dissolution system, the feed inlet 4, the water inlet 5, the filter residue inlet 6 and the filtrate outlet 7 are respectively communicated with the top of the microwave digestion tank 2 through a feed pipe, a filter residue pipeline and a filter residue conveying pipe 12, the top side wall of the shell 1 is provided with a dealkali removing liquid suction pipe 8, one end of the dealkali removing liquid suction pipe 8 penetrates through the side wall of the microwave digestion tank 2 and downwards extends to the bottom of the microwave digestion tank 2, the bottom of the shell 2 is provided with a discharge pipe 9, and a discharge pipe 9 is arranged on the bottom of the shell 2 is communicated with the bottom of the microwave digestion tank 2, and a discharge pipe 9 is arranged on the vertical bottom of the shell 2;
the bottom of the dealkalized liquid extracting pipe 8 is provided with a peristaltic pump II 18, a liquid flowmeter is arranged on a water inlet pipeline, a solid conveying pump is arranged on a filter residue conveying pipe 12, a pressure relief pipe communicated with the inside of the microwave digestion tank 2 is arranged on the side wall of the shell 1, and a pressure relief valve and a pressure gauge are arranged on the pressure relief pipe;
the dealkalized liquid extracting pipe 8 is a telescopic flexible pipeline;
the solid-liquid separation system is an automatic deslagging filter 11, the bottom end of a dealkalized liquid extracting pipe 8 is communicated with a liquid inlet of the automatic deslagging filter 11, a deslagging port of the dealkalized liquid extracting pipe 8 is communicated with a filter residue conveying pipe 12, and a filtrate outlet of the automatic deslagging filter 11 is communicated with the ion exchange system through a filtrate conveying pipeline I;
a peristaltic pump I17 is arranged on the filtrate conveying pipeline I;
the ion exchange system comprises a liquid main inlet pipe, a reaction column liquid branch inlet pipe, more than 2 reaction columns 13, a reaction column liquid branch outlet pipe and a liquid main outlet pipe, wherein the reaction column liquid branch inlet pipe is vertically arranged, a filtrate conveying pipeline I is communicated with the liquid main inlet pipe, the liquid main inlet pipe is communicated with the top end of the reaction column liquid branch inlet pipe, the reaction column liquid branch inlet pipe is matched with the reaction column 13, the bottom end of the reaction column liquid branch inlet pipe is communicated with the top end of the reaction column 13, strong acid cation exchange resin is filled in the reaction column 13, the bottom end of the reaction column 13 is communicated with a reaction column liquid branch outlet pipe and is matched with the reaction column 13, the reaction column liquid branch outlet pipe is communicated with the liquid main outlet pipe, and the liquid main outlet pipe is communicated with the detection system through a filtrate conveying pipeline II;
the reaction column liquid branch inlet pipes are provided with reaction column electromagnetic valves 14;
the detection system comprises a pH detector 15, a sodium ion detector 16 and a filtrate conveying pipeline III, wherein the pH detector 15 and the sodium ion detector 16 are arranged on the filtrate conveying pipeline III, one end of the filtrate conveying pipeline III is communicated with a filtrate conveying pipeline II, and the other end of the filtrate conveying pipeline III is communicated with a filtrate port 7 of the alkali dissolution system;
and a peristaltic pump III 19 is arranged on the filtrate conveying pipeline III.
A water-saving and efficient circulating red mud dealkalization method adopts a water-saving and efficient circulating red mud dealkalization system, and comprises the following specific steps:
(1) Crushing, grinding and sieving red mud to obtain red mud powder;
(2) Adding the red mud powder obtained in the step (1) into a microwave digestion tank through a charging port of an alkali dissolution system, adding water into the microwave digestion tank through a water inlet of the alkali dissolution system, and uniformly mixing by a stirrer to obtain a mixed material;
(3) Starting a microwave generator, carrying out microwave digestion on the mixed materials in the microwave digestion tank in the step (2) for 20-30 min under the conditions of 80-260 ℃ and stirring, adding a complexing agent into the microwave digestion tank through a feed inlet, reacting for 5-15 min under the conditions of microwaves and stirring, and standing until solid-liquid layering is carried out to obtain supernatant and solid slag;
(4) Starting a peristaltic pump II, pumping the supernatant obtained in the step (3) into a solid-liquid separation system through a lye removal liquid pumping pipe, and filtering through an automatic deslagging filter to obtain filter residues and filtrate; the solid conveying pump conveys filter residues to the top end of the alkali dissolution system through a filter residue conveying pipe and circularly enters the microwave digestion tank through a filter residue port;
(5) The peristaltic pump I conveys the filtrate in the step (4) to a reaction column of an ion exchange system through a filtrate conveying pipeline I, and hydroxide ions in the filtrate react with strong acid cation exchange resin in the reaction column to obtain dealkalized filtrate;
(6) The dealkalized filtrate in the step (5) is conveyed into a filtrate conveying pipeline III of a detection system through a filtrate conveying pipeline II, the pH value of the dealkalized filtrate is detected through a pH detector of the detection system, the sodium ion concentration of the dealkalized filtrate is detected through a sodium ion detector of the detection system, and the flow rate of the filtrate is adjusted through a reaction column electromagnetic valve of a reaction column liquid branch pipe so as to control the reaction time of hydroxyl ions in the filtrate and strong acid cation exchange resin in a reaction column;
(7) The peristaltic pump III conveys the dealkalized filtrate in the step (6) to the top end of an alkali dissolution system through a filtrate conveying pipeline III and circularly enters a microwave digestion tank through a filtrate port;
(8) Performing cyclic operation for more than 7 times in the step (3) to the step (7), when standing treatment is performed in the step (3) until solid-liquid layering is performed to obtain supernatant and solid slag, opening a discharge valve of an alkali dissolution system to discharge and collect dealkalized red mud through a discharge pipe, and then discharging supernatant through the discharge pipe;
preferably, the screening in the step (1) is carried out by a 500-700 mesh screen;
preferably, in the step (2), the mass ratio of the red mud powder to the water is 1:8-12;
preferably, in the step (3), the complexing agent is octahydroxyquinoline, glycine, ethylene diamine tetraacetic acid disodium salt, potassium thiocyanate or malic acid, and the addition amount of the complexing agent is 10-20% of the mass of the mixed material A;
preferably, the height-to-diameter ratio of the reaction column in the step (5) is 20-30:1;
preferably, the strong acid cation exchange resin of step (5) is a 001x7 (732) strong acid cation exchange resin.
The invention has the beneficial effects that:
(1) According to the method, the dissolution of alkaline ions in the red mud can be accelerated by utilizing a mode of matching microwaves with mechanical stirring treatment, filtrate obtained by suction filtration of the dealkalized liquid is subjected to strong acid cation resin exchange treatment and then returned to a microwave digestion step, filter residues are returned to the microwave digestion step at the same time, the cyclic treatment is continuously carried out, the alkali content of the dealkalized red mud is as low as 1-3%, the dealkalized rate is as high as 80%, the dealkalization is high-efficiency, and the water consumption can be greatly reduced;
(2) After microwave digestion treatment, complexing agents (such as octahydroxyquinoline) are added and stirred, so that high-valence metal ions such as Fe and the like in the leaching solution are precipitated, and the exchange resin is prevented from being deactivated in the ion exchange process;
(3) The strong acid cation exchange resin has wide sources, low cost and low reduction cost; the dealkalization rate of the red mud can be greatly improved, and low-cost large-scale operation can be realized;
(4) After the raw materials are added, the method is processed by an alkali dissolution system, the dealkalized liquid of the microwave digestion tank can be automatically conveyed to a solid-liquid separation system, filter residues and filtrate obtained by the treatment of the solid-liquid separation system can be automatically returned to the microwave digestion tank, the cyclic treatment is facilitated, and after the dealkalized treatment is finished, the dealkalized red mud can be taken out only by opening a discharge valve, so that the method has the advantages of convenience in operation and high efficiency;
(2) According to the ion exchange system, the pH of the filtrate can be detected according to the pH detection device, when the pH of the filtrate is more than or equal to 9, the strong acid cation exchange resin of the reaction column is replaced, so that the normal operation of the exchange resin in the cyclic treatment process is ensured, and the problem of failure in the use process of the exchange resin is avoided.
Drawings
FIG. 1 is a schematic diagram of a water-saving and efficient circulating red mud dealkalization system in embodiment 1;
wherein: 1-shell, 2-microwave digestion tank, 3-stirrer, 4-feed inlet, 5-water inlet, 6-filter residue inlet, 7-filtrate inlet, 8-lye extraction pipe, 9-discharge pipe, 10-discharge valve, 11-automatic slag discharge filter, 12-filter residue conveying pipe, 13-reaction column, 14-reaction column electromagnetic valve, 15-pH detector, 16-sodium ion detector, 17-peristaltic pump I, 18-peristaltic pump II, 19-peristaltic pump III, 20-microwave generator and 21-waveguide.
Detailed Description
The invention will be further described with reference to the following specific embodiments.
Example 1: as shown in fig. 1, the water-saving and efficient circulating red mud dealkalization system comprises an alkali dissolution system, a solid-liquid separation system, an ion exchange system and a detection system, wherein a liquid outlet of the alkali dissolution system is communicated with a liquid inlet of the solid-liquid separation system, a liquid outlet of the solid-liquid separation system is communicated with a liquid inlet of the ion exchange system, a liquid outlet of the ion exchange system is communicated with a liquid inlet of the detection system, and a liquid outlet of the detection system is communicated with a filtrate inlet of the alkali dissolution system;
the alkali dissolution system comprises a shell 1, a microwave digestion tank 2, a microwave generator 20 and a stirrer 3, wherein the microwave digestion tank 2 is fixedly arranged in the shell 1, the microwave generator 20 is arranged on the side wall of the shell 1, the microwave generation end of the microwave generator 20 is communicated with the internal cavity of the microwave digestion tank 2 through a waveguide 21, the stirrer 3 is vertically and fixedly arranged at the top end of the shell 1, a stirring paddle of the stirrer 3 penetrates through the top wall of the microwave digestion tank 2 and extends downwards to the bottom of the microwave digestion tank 2, the top end of the shell 1 is also provided with a feed inlet 4, a water inlet 5, a filter residue inlet 6 and a filtrate outlet 7, the filtrate outlet 7 is a filtrate inlet of the alkali dissolution system, the feed inlet 4, the water inlet 5, the filter residue inlet 6 and the filtrate outlet 7 are respectively communicated with the top of the microwave digestion tank 2 through a feed pipe, a filter residue pipe 12 and a solid outlet of a solid-liquid separation system, the top side wall of the shell 1 is provided with a dealkali removal pumping pipe 8, one end of the dealkali removal pumping pipe 8 penetrates through the side wall of the microwave digestion tank 2 and extends downwards to the bottom of the microwave digestion tank 2, the bottom of the shell 2 is provided with a discharge pipe 9, and a discharge pipe 9 is arranged at the bottom of the microwave digestion tank 2 is provided with a vertical discharge pipe 9;
the bottom of the dealkalized liquid extracting pipe 8 is provided with a peristaltic pump II 18, a liquid flowmeter is arranged on a water inlet pipeline, a solid conveying pump is arranged on a filter residue conveying pipe 12, a pressure relief pipe communicated with the inside of the microwave digestion tank 2 is arranged on the side wall of the shell 1, and a pressure relief valve and a pressure gauge are arranged on the pressure relief pipe;
the dealkalized liquid extracting pipe 8 is a telescopic flexible pipeline;
the solid-liquid separation system of the embodiment is an automatic deslagging filter 11, the bottom end of a dealkalization liquid extracting pipe 8 is communicated with a liquid inlet of the automatic deslagging filter 11, a deslagging port of the dealkalization liquid extracting pipe 8 is communicated with a filter residue conveying pipe 12, and a filtrate outlet of the automatic deslagging filter 11 is communicated with an ion exchange system through a filtrate conveying pipeline I;
the peristaltic pump I17 is arranged on the filtrate conveying pipeline I;
the ion exchange system comprises a liquid main inlet pipe, a reaction column liquid branch inlet pipe, 2 reaction columns 13 which are vertically arranged, a reaction column liquid branch outlet pipe and a liquid main outlet pipe, wherein a filtrate conveying pipeline I is communicated with the liquid main inlet pipe, the liquid main inlet pipe is communicated with the top end of the reaction column liquid branch inlet pipe, the reaction column liquid branch inlet pipe is matched with the reaction column 13, the bottom end of the reaction column liquid branch inlet pipe is communicated with the top end of the reaction column 13, strong acid cation exchange resin is filled in the reaction column 13, the bottom end of the reaction column 13 is communicated with a reaction column liquid outlet pipe, the reaction column liquid branch outlet pipe is matched with the reaction column 13, the reaction column liquid branch outlet pipe is communicated with the liquid main outlet pipe, and the liquid main outlet pipe is communicated with a detection system through a filtrate conveying pipeline II;
the reaction column solenoid valves 14 are arranged on the liquid branch inlet pipes of the reaction columns in the embodiment;
the detection system of the embodiment comprises a pH detector 15, a sodium ion detector 16 and a filtrate conveying pipeline III, wherein the pH detector 15 and the sodium ion detector 16 are arranged on the filtrate conveying pipeline III, one end of the filtrate conveying pipeline III is communicated with a filtrate conveying pipeline II, and the other end of the filtrate conveying pipeline III is communicated with a filtrate port 7 of the alkali dissolution system;
the filtrate conveying pipeline III of the embodiment is provided with a peristaltic pump III 19;
a water-saving and efficient circulating red mud dealkalization method adopts a water-saving and efficient circulating red mud dealkalization system, and comprises the following specific steps:
(1) Crushing, grinding and sieving red mud to obtain red mud powder;
(2) Adding the red mud powder obtained in the step (1) into a microwave digestion tank through a charging port of an alkali dissolution system, adding water into the microwave digestion tank through a water inlet of the alkali dissolution system, and uniformly mixing by a stirrer to obtain a mixed material; wherein the mass ratio of the red mud powder to the water is 1:8-12;
(3) Starting a microwave generator, carrying out microwave digestion on the mixed materials in the microwave digestion tank in the step (2) for 20-30 min under the conditions of 80-260 ℃ and stirring, adding a complexing agent into the microwave digestion tank through a feed inlet, reacting for 5-15 min under the conditions of microwaves and stirring, and standing until solid-liquid layering is carried out to obtain supernatant and solid slag; wherein the complexing agent is octahydroxyquinoline, and the addition amount of the complexing agent is 10-20% of the mass of the mixed material A;
(4) Starting a peristaltic pump II, pumping the supernatant obtained in the step (3) into a solid-liquid separation system through a lye removal liquid pumping pipe, and filtering through an automatic deslagging filter to obtain filter residues and filtrate; the solid conveying pump conveys filter residues to the top end of the alkali dissolution system through a filter residue conveying pipe and circularly enters the microwave digestion tank through a filter residue port;
(5) The peristaltic pump I conveys the filtrate in the step (4) to a reaction column of an ion exchange system through a filtrate conveying pipeline I, and hydroxide ions in the filtrate react with strong acid cation exchange resin in the reaction column to obtain dealkalized filtrate;
(6) The dealkalized filtrate in the step (5) is conveyed into a filtrate conveying pipeline III of a detection system through a filtrate conveying pipeline II, the pH value of the dealkalized filtrate is detected through a pH detector of the detection system, the sodium ion concentration of the dealkalized filtrate is detected through a sodium ion detector of the detection system, and the flow rate of the filtrate is adjusted through a reaction column electromagnetic valve of a reaction column liquid branch pipe so as to control the reaction time of hydroxyl ions in the filtrate and strong acid cation exchange resin in a reaction column;
(7) The peristaltic pump III conveys the dealkalized filtrate in the step (6) to the top end of an alkali dissolution system through a filtrate conveying pipeline III and circularly enters a microwave digestion tank through a filtrate port;
(8) And (3) performing cyclic operation for more than 7 times, namely performing standing treatment in the step (3) until solid-liquid layering is performed to obtain supernatant and solid slag, opening a discharge valve of an alkali dissolution system to discharge and collect the dealkalized red mud through a discharge pipe, and then discharging supernatant through the discharge pipe.
Example 2: the structure of the water-saving and efficient circulating red mud dealkalization system in this embodiment is basically the same as that of the water-saving and efficient circulating red mud dealkalization system in embodiment 1, and the difference is that: the number of the reaction columns 13 is 3; the height-diameter ratio of the reaction column is 20:1;
the water-saving and efficient circulating red mud dealkalization method adopts a water-saving and efficient circulating red mud dealkalization system, and comprises the following specific steps:
(1) Crushing, grinding and sieving the red mud with a 500-mesh sieve to obtain red mud powder;
(2) Adding the red mud powder obtained in the step (1) into a microwave digestion tank through a charging port of an alkali dissolution system, adding water into the microwave digestion tank through a water inlet of the alkali dissolution system, and uniformly mixing by a stirrer to obtain a mixed material; wherein the mass ratio of the red mud powder to the water is 1:8;
(3) Starting a microwave generator, carrying out microwave digestion on the mixed material in the microwave digestion tank in the step (2) for 20min under the conditions of 80 ℃ and stirring, adding a complexing agent (the complexing agent is glycine) into the microwave digestion tank through a feed inlet, reacting for 5min under the conditions of microwaves and stirring, and standing until solid-liquid layering is carried out to obtain supernatant and solid slag; wherein the adding amount of the complexing agent (amino acetic acid) is 10% of the mass of the mixed material A;
(4) Starting a peristaltic pump II, pumping the supernatant obtained in the step (3) into a solid-liquid separation system through a lye removal liquid pumping pipe, and filtering through an automatic deslagging filter to obtain filter residues and filtrate; the solid conveying pump conveys filter residues to the top end of the alkali dissolution system through a filter residue conveying pipe and circularly enters the microwave digestion tank through a filter residue port;
(5) The peristaltic pump I conveys the filtrate in the step (4) to a reaction column of an ion exchange system through a filtrate conveying pipeline I, and hydroxide ions in the filtrate react with strong acid cation exchange resin in the reaction column to obtain dealkalized filtrate;
(6) The dealkalized filtrate in the step (5) is conveyed into a filtrate conveying pipeline III of a detection system through a filtrate conveying pipeline II, the pH value of the dealkalized filtrate is detected through a pH detector of the detection system, the sodium ion concentration of the dealkalized filtrate is detected through a sodium ion detector of the detection system, and the flow rate of the filtrate is adjusted through a reaction column electromagnetic valve of a reaction column liquid branch pipe so as to control the reaction time of hydroxyl ions in the filtrate and strong acid cation exchange resin in a reaction column;
(7) The peristaltic pump III conveys the dealkalized filtrate in the step (6) to the top end of an alkali dissolution system through a filtrate conveying pipeline III and circularly enters a microwave digestion tank through a filtrate port;
(8) 7 times of cyclic operation, namely, step (3) to step (7), when standing treatment is carried out in the step (3) until solid-liquid layering is carried out to obtain supernatant and solid slag, a discharge valve of an alkali dissolution system is opened to discharge and collect dealkalized red mud through a discharge pipe, and then supernatant is discharged through the discharge pipe;
the alkaline content of the dealkalized red mud is as low as 3.0% by the determination of the PH of the soil (NY/T1121.2-2006) and the determination of the total amount of calcium, magnesium and sodium in the soil (NY/T296-1995).
Example 2: the structure of the water-saving and efficient circulating red mud dealkalization system in this embodiment is basically the same as that of the water-saving and efficient circulating red mud dealkalization system in embodiment 1, and the difference is that: the number of the reaction columns 13 is 4, and the height-diameter ratio of the reaction columns is 24:1;
the water-saving and efficient circulating red mud dealkalization method adopts a water-saving and efficient circulating red mud dealkalization system, and comprises the following specific steps:
(1) Crushing, grinding and sieving the red mud with a 600-mesh sieve to obtain red mud powder;
(2) Adding the red mud powder obtained in the step (1) into a microwave digestion tank through a charging port of an alkali dissolution system, adding water into the microwave digestion tank through a water inlet of the alkali dissolution system, and uniformly mixing by a stirrer to obtain a mixed material; wherein the mass ratio of the red mud powder to the water is 1:12;
(3) Starting a microwave generator, carrying out microwave digestion on the mixed material in the microwave digestion tank in the step (2) for 30min under the conditions of 140 ℃ and stirring, adding a complexing agent (the complexing agent is disodium ethylenediamine tetraacetate) into the microwave digestion tank through a feed inlet, reacting for 15min under the conditions of microwaves and stirring, and standing until solid-liquid layering is carried out to obtain supernatant and solid slag; wherein the adding amount of the complexing agent (ethylene diamine tetraacetic acid disodium salt) is 20% of the mass of the mixed material A;
(4) Starting a peristaltic pump II, pumping the supernatant obtained in the step (3) into a solid-liquid separation system through a lye removal liquid pumping pipe, and filtering through an automatic deslagging filter to obtain filter residues and filtrate; the solid conveying pump conveys filter residues to the top end of the alkali dissolution system through a filter residue conveying pipe and circularly enters the microwave digestion tank through a filter residue port;
(5) The peristaltic pump I conveys the filtrate in the step (4) to a reaction column of an ion exchange system through a filtrate conveying pipeline I, and hydroxide ions in the filtrate react with strong acid cation exchange resin in the reaction column to obtain dealkalized filtrate;
(6) The dealkalized filtrate in the step (5) is conveyed into a filtrate conveying pipeline III of a detection system through a filtrate conveying pipeline II, the pH value of the dealkalized filtrate is detected through a pH detector of the detection system, the sodium ion concentration of the dealkalized filtrate is detected through a sodium ion detector of the detection system, and the flow rate of the filtrate is adjusted through a reaction column electromagnetic valve of a reaction column liquid branch pipe so as to control the reaction time of hydroxyl ions in the filtrate and strong acid cation exchange resin in a reaction column;
(7) The peristaltic pump III conveys the dealkalized filtrate in the step (6) to the top end of an alkali dissolution system through a filtrate conveying pipeline III and circularly enters a microwave digestion tank through a filtrate port;
(8) Performing cyclic operation for 8 times in the step (3) to the step (7), when standing treatment is performed in the step (3) until solid-liquid layering is performed to obtain supernatant and solid slag, opening a discharge valve of an alkali dissolution system to discharge and collect the dealkalized red mud through a discharge pipe, and then discharging supernatant through the discharge pipe;
the alkaline content of the dealkalized red mud is as low as 2.6% by the determination of the PH of the soil (NY/T1121.2-2006) and the determination of the total amount of calcium, magnesium and sodium in the soil (NY/T296-1995).
Example 3: the structure of the water-saving and efficient circulating red mud dealkalization system in this embodiment is basically the same as that of the water-saving and efficient circulating red mud dealkalization system in embodiment 1, and the difference is that: the number of the reaction columns 13 is 5, and the height-diameter ratio of the reaction columns is 26:1;
the water-saving and efficient circulating red mud dealkalization method adopts a water-saving and efficient circulating red mud dealkalization system, and comprises the following specific steps:
(1) Crushing, grinding and sieving the red mud with a 700-mesh sieve to obtain red mud powder;
(2) Adding the red mud powder obtained in the step (1) into a microwave digestion tank through a charging port of an alkali dissolution system, adding water into the microwave digestion tank through a water inlet of the alkali dissolution system, and uniformly mixing by a stirrer to obtain a mixed material; wherein the mass ratio of the red mud powder to the water is 1:10;
(3) Starting a microwave generator, carrying out microwave digestion on the mixed material in the microwave digestion tank in the step (2) for 25min under the conditions of 180 ℃ and stirring, adding a complexing agent (the complexing agent is potassium thiocyanate) into the microwave digestion tank through a feed inlet, reacting for 10min under the conditions of microwaves and stirring, and standing until solid-liquid layering is carried out to obtain supernatant and solid slag; wherein the adding amount of the complexing agent (potassium thiocyanate) is 15% of the mass of the mixed material A;
(4) Starting a peristaltic pump II, pumping the supernatant obtained in the step (3) into a solid-liquid separation system through a lye removal liquid pumping pipe, and filtering through an automatic deslagging filter to obtain filter residues and filtrate; the solid conveying pump conveys filter residues to the top end of the alkali dissolution system through a filter residue conveying pipe and circularly enters the microwave digestion tank through a filter residue port;
(5) The peristaltic pump I conveys the filtrate in the step (4) to a reaction column of an ion exchange system through a filtrate conveying pipeline I, and hydroxide ions in the filtrate react with strong acid cation exchange resin in the reaction column to obtain dealkalized filtrate;
(6) The dealkalized filtrate in the step (5) is conveyed into a filtrate conveying pipeline III of a detection system through a filtrate conveying pipeline II, the pH value of the dealkalized filtrate is detected through a pH detector of the detection system, the sodium ion concentration of the dealkalized filtrate is detected through a sodium ion detector of the detection system, and the flow rate of the filtrate is adjusted through a reaction column electromagnetic valve of a reaction column liquid branch pipe so as to control the reaction time of hydroxyl ions in the filtrate and strong acid cation exchange resin in a reaction column;
(7) The peristaltic pump III conveys the dealkalized filtrate in the step (6) to the top end of an alkali dissolution system through a filtrate conveying pipeline III and circularly enters a microwave digestion tank through a filtrate port;
(8) Performing cyclic operation for 9 times in the step (3) to the step (7), when standing treatment is performed in the step (3) until solid-liquid layering is performed to obtain supernatant and solid slag, opening a discharge valve of an alkali dissolution system to discharge and collect the dealkalized red mud through a discharge pipe, and then discharging supernatant through the discharge pipe;
the alkaline content of the dealkalized red mud is as low as 2.1% by the determination of the PH of the soil (NY/T1121.2-2006) and the determination of the total amount of calcium, magnesium and sodium in the soil (NY/T296-1995).
Example 4: the structure of the water-saving and efficient circulating red mud dealkalization system in this embodiment is basically the same as that of the water-saving and efficient circulating red mud dealkalization system in embodiment 1, and the difference is that: the number of the reaction columns 13 is 6, and the height-diameter ratio of the reaction columns is 28:1;
the water-saving and efficient circulating red mud dealkalization method adopts a water-saving and efficient circulating red mud dealkalization system, and comprises the following specific steps:
(1) Crushing, grinding and sieving the red mud with a 650-mesh sieve to obtain red mud powder;
(2) Adding the red mud powder obtained in the step (1) into a microwave digestion tank through a charging port of an alkali dissolution system, adding water into the microwave digestion tank through a water inlet of the alkali dissolution system, and uniformly mixing by a stirrer to obtain a mixed material; wherein the mass ratio of the red mud powder to the water is 1:10;
(3) Starting a microwave generator, carrying out microwave digestion on the mixed materials in the microwave digestion tank in the step (2) under the conditions of 220 ℃ and stirring for 25min, adding a complexing agent (malic acid as a complexing agent) into the microwave digestion tank through a feed inlet, reacting for 10min under the conditions of microwaves and stirring, and standing until solid-liquid layering is carried out to obtain supernatant and solid slag; wherein the adding amount of the complexing agent (malic acid) is 15% of the mass of the mixed material A;
(4) Starting a peristaltic pump II, pumping the supernatant obtained in the step (3) into a solid-liquid separation system through a lye removal liquid pumping pipe, and filtering through an automatic deslagging filter to obtain filter residues and filtrate; the solid conveying pump conveys filter residues to the top end of the alkali dissolution system through a filter residue conveying pipe and circularly enters the microwave digestion tank through a filter residue port;
(5) The peristaltic pump I conveys the filtrate in the step (4) to a reaction column of an ion exchange system through a filtrate conveying pipeline I, and hydroxide ions in the filtrate react with strong acid cation exchange resin in the reaction column to obtain dealkalized filtrate;
(6) The dealkalized filtrate in the step (5) is conveyed into a filtrate conveying pipeline III of a detection system through a filtrate conveying pipeline II, the pH value of the dealkalized filtrate is detected through a pH detector of the detection system, the sodium ion concentration of the dealkalized filtrate is detected through a sodium ion detector of the detection system, and the flow rate of the filtrate is adjusted through a reaction column electromagnetic valve of a reaction column liquid branch pipe so as to control the reaction time of hydroxyl ions in the filtrate and strong acid cation exchange resin in a reaction column;
(7) The peristaltic pump III conveys the dealkalized filtrate in the step (6) to the top end of an alkali dissolution system through a filtrate conveying pipeline III and circularly enters a microwave digestion tank through a filtrate port;
(8) Performing cyclic operation for 9 times in the step (3) to the step (7), when standing treatment is performed in the step (3) until solid-liquid layering is performed to obtain supernatant and solid slag, opening a discharge valve of an alkali dissolution system to discharge and collect the dealkalized red mud through a discharge pipe, and then discharging supernatant through the discharge pipe;
the alkaline content of the dealkalized red mud is as low as 1.4% by the determination of the PH of the soil (NY/T1121.2-2006) and the determination of the total amount of calcium, magnesium and sodium in the soil (NY/T296-1995).
Example 5: the structure of the water-saving and efficient circulating red mud dealkalization system in this embodiment is basically the same as that of the water-saving and efficient circulating red mud dealkalization system in embodiment 1, and the difference is that: the number of the reaction columns 13 is 5, and the height-diameter ratio of the reaction columns is 30:1;
the water-saving and efficient circulating red mud dealkalization method adopts a water-saving and efficient circulating red mud dealkalization system, and comprises the following specific steps:
(1) Crushing, grinding and sieving the red mud with a 700-mesh sieve to obtain red mud powder;
(2) Adding the red mud powder obtained in the step (1) into a microwave digestion tank through a charging port of an alkali dissolution system, adding water into the microwave digestion tank through a water inlet of the alkali dissolution system, and uniformly mixing by a stirrer to obtain a mixed material; wherein the mass ratio of the red mud powder to the water is 1:8;
(3) Starting a microwave generator, carrying out microwave digestion on the mixed material in the microwave digestion tank in the step (2) for 20min under the conditions of 260 ℃ and stirring, adding a complexing agent (octahydroxyquinoline as a complexing agent) into the microwave digestion tank through a feed inlet, reacting for 15min under the conditions of microwaves and stirring, and standing until solid-liquid layering is carried out to obtain supernatant and solid slag; wherein the adding amount of the complexing agent (octahydroxyquinoline) is 10% of the mass of the mixed material A;
(4) Starting a peristaltic pump II, pumping the supernatant obtained in the step (3) into a solid-liquid separation system through a lye removal liquid pumping pipe, and filtering through an automatic deslagging filter to obtain filter residues and filtrate; the solid conveying pump conveys filter residues to the top end of the alkali dissolution system through a filter residue conveying pipe and circularly enters the microwave digestion tank through a filter residue port;
(5) The peristaltic pump I conveys the filtrate in the step (4) to a reaction column of an ion exchange system through a filtrate conveying pipeline I, and hydroxide ions in the filtrate react with strong acid cation exchange resin in the reaction column to obtain dealkalized filtrate;
(6) The dealkalized filtrate in the step (5) is conveyed into a filtrate conveying pipeline III of a detection system through a filtrate conveying pipeline II, the pH value of the dealkalized filtrate is detected through a pH detector of the detection system, the sodium ion concentration of the dealkalized filtrate is detected through a sodium ion detector of the detection system, and the flow rate of the filtrate is adjusted through a reaction column electromagnetic valve of a reaction column liquid branch pipe so as to control the reaction time of hydroxyl ions in the filtrate and strong acid cation exchange resin in a reaction column;
(7) The peristaltic pump III conveys the dealkalized filtrate in the step (6) to the top end of an alkali dissolution system through a filtrate conveying pipeline III and circularly enters a microwave digestion tank through a filtrate port;
(8) Performing cyclic operation for 10 times in the step (3) to the step (7), when standing treatment is performed in the step (3) until solid-liquid layering is performed to obtain supernatant and solid slag, opening a discharge valve of an alkali dissolution system to discharge and collect the dealkalized red mud through a discharge pipe, and then discharging supernatant through the discharge pipe;
the alkaline content of the dealkalized red mud is as low as 1.0% by the determination of the PH of the soil (NY/T1121.2-2006) and the determination of the total amount of calcium, magnesium and sodium in the soil (NY/T296-1995).
The specific embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.
Claims (3)
1. A water-saving and efficient circulating red mud dealkalization method is characterized in that a water-saving and efficient circulating red mud dealkalization system is adopted;
the water-saving and efficient circulating red mud dealkalization system comprises an alkali dissolution system, a solid-liquid separation system, an ion exchange system and a detection system, wherein a liquid outlet of the alkali dissolution system is communicated with a liquid inlet of the solid-liquid separation system, a liquid outlet of the solid-liquid separation system is communicated with a liquid inlet of the ion exchange system, a liquid outlet of the ion exchange system is communicated with a liquid inlet of the detection system, and a liquid outlet of the detection system is communicated with a filtrate inlet of the alkali dissolution system;
the alkali dissolution system comprises a shell (1), a microwave digestion tank (2), a microwave generator (20) and a stirrer (3), wherein the microwave digestion tank (2) is fixedly arranged in the shell (1), the microwave generator (20) is arranged on the side wall of the shell (1), the microwave generation end of the microwave generator (20) is communicated with the inner cavity of the microwave digestion tank (2) through a waveguide tube (21), the stirrer (3) is vertically and fixedly arranged at the top end of the shell (1), a stirring paddle of the stirrer (3) penetrates through the top wall of the microwave digestion tank (2) and downwards extends to the bottom of the microwave digestion tank (2), the top end of the shell (1) is also provided with a feed inlet (4), a water inlet (5), a filter residue inlet (6) and a filtrate outlet (7), the filtrate outlet (7) is a filtrate inlet of the alkali dissolution system, the feed inlet (4), the water inlet (5), the filter residue inlet (6), the filtrate outlet (7) are respectively communicated with the top of the microwave digestion tank (2) through a feed pipe, a water inlet pipe, a filter residue pipe and the filtrate pipe are respectively communicated with the top of the solid and liquid separation system (1) through a filter residue conveying pipe (12), the top of the solid and the solid alkali dissolution system is provided with the top of the solid alkali dissolution system, one end of the lye removing liquid suction pipe (8) penetrates through the side wall of the microwave digestion tank (2) and bends downwards to extend to the middle bottom of the microwave digestion tank (2), a discharging pipe (9) is vertically arranged at the bottom of the shell (1), the discharging pipe (9) is communicated with the bottom of the microwave digestion tank (2), and a discharging valve (10) is arranged on the discharging pipe (9);
the bottom of the lye removing liquid extracting pipe (8) is provided with a peristaltic pump II (18), a liquid flowmeter is arranged on a water inlet pipeline, a solid conveying pump is arranged on a filter residue conveying pipe (12), a pressure relief pipe communicated with the inside of the microwave digestion tank (2) is arranged on the side wall of the shell (1), and a pressure relief valve and a pressure gauge are arranged on the pressure relief pipe;
the lye removal liquid suction pipe (8) is a telescopic flexible pipeline;
the solid-liquid separation system is an automatic deslagging filter (11), the bottom end of the dealkalization liquid extracting pipe (8) is communicated with a liquid inlet of the automatic deslagging filter (11), a deslagging port of the dealkalization liquid extracting pipe (8) is communicated with a filter residue conveying pipe (12), and a filtrate outlet of the automatic deslagging filter (11) is communicated with the ion exchange system through a filtrate conveying pipeline I;
a peristaltic pump I (17) is arranged on the filtrate conveying pipeline I;
the ion exchange system comprises a liquid main inlet pipe, a reaction column liquid branch inlet pipe, more than 2 reaction columns (13) which are vertically arranged, a reaction column liquid branch outlet pipe and a liquid main outlet pipe, wherein a filtrate conveying pipeline I is communicated with the liquid main inlet pipe, the liquid main inlet pipe is communicated with the top end of the reaction column liquid branch inlet pipe, the reaction column liquid branch inlet pipe is matched with the reaction column (13) and the bottom end of the reaction column liquid branch inlet pipe is communicated with the top end of the reaction column (13), strong acid cation exchange resin is filled in the reaction column (13), the bottom end of the reaction column (13) is communicated with the reaction column liquid branch outlet pipe, the reaction column liquid branch outlet pipe is matched with the reaction column (13), the liquid main outlet pipe is communicated with the liquid main outlet pipe, and the liquid main outlet pipe is communicated with the detection system through a filtrate conveying pipeline II;
the reaction column liquid branch inlet pipes are provided with reaction column electromagnetic valves (14);
the detection system comprises a pH detector (15), a sodium ion detector (16) and a filtrate conveying pipeline III, wherein the pH detector (15) and the sodium ion detector (16) are arranged on the filtrate conveying pipeline III, one end of the filtrate conveying pipeline III is communicated with the filtrate conveying pipeline II, and the other end of the filtrate conveying pipeline III is communicated with a filtrate port (7) of the alkali dissolution system;
a peristaltic pump III (19) is arranged on the filtrate conveying pipeline III;
the method comprises the following specific steps:
(1) Crushing, grinding and sieving red mud to obtain red mud powder;
(2) Adding the red mud powder obtained in the step (1) into a microwave digestion tank through a charging port of an alkali dissolution system, adding water into the microwave digestion tank through a water inlet of the alkali dissolution system, and uniformly mixing by a stirrer to obtain a mixed material A;
(3) Starting a microwave generator, carrying out microwave digestion on the mixed material in the microwave digestion tank in the step (2) for 20-30 min under the conditions of 80-260 ℃ and stirring, adding a complexing agent into the mixed material A of the microwave digestion tank through a feed inlet, reacting for 5-15 min under the conditions of microwaves and stirring, and standing until solid-liquid layering is carried out to obtain supernatant and digestion slag;
(4) Starting a peristaltic pump II, pumping the supernatant obtained in the step (3) into a solid-liquid separation system through a lye removal liquid pumping pipe, and filtering through an automatic deslagging filter to obtain filter residues and filtrate; the solid conveying pump conveys filter residues to the top end of the alkali dissolution system through a filter residue conveying pipe and circularly enters the microwave digestion tank through a filter residue port;
(5) The peristaltic pump I conveys the filtrate in the step (4) to a reaction column of an ion exchange system through a filtrate conveying pipeline I, and hydroxide ions in the filtrate react with strong acid cation exchange resin in the reaction column to obtain dealkalized filtrate;
(6) The dealkalized filtrate in the step (5) is conveyed into a filtrate conveying pipeline III of a detection system through a filtrate conveying pipeline II, the pH value of the dealkalized filtrate is detected through a pH detector of the detection system, the sodium ion concentration of the dealkalized filtrate is detected through a sodium ion detector of the detection system, and the flow rate of the filtrate is adjusted through a reaction column electromagnetic valve of a reaction column liquid branch pipe so as to control the reaction time of hydroxyl ions in the filtrate and strong acid cation exchange resin in a reaction column;
(7) The peristaltic pump III conveys the dealkalized filtrate in the step (6) to the top end of an alkali dissolution system through a filtrate conveying pipeline III and circularly enters a microwave digestion tank through a filtrate port;
(8) And (3) to (7) of circulating operation for more than 7 times, when standing treatment is carried out in the step (3) until solid-liquid layering is carried out to obtain supernatant and digestion residues, a discharge valve of the alkali dissolution system is opened to discharge and collect digestion residues, namely dealkalized red mud, through a discharge pipe, and then the supernatant is discharged through the discharge pipe.
2. The water-saving and efficient circulating red mud dealkalization method according to claim 1, which is characterized by comprising the following steps: in the step (2), the mass ratio of the red mud powder to the water is 1:8-12.
3. The water-saving and efficient circulating red mud dealkalization method according to claim 1, which is characterized by comprising the following steps: in the step (3), the complexing agent is octahydroxyquinoline, glycine, ethylene diamine tetraacetic acid disodium salt, potassium thiocyanate or malic acid, and the addition amount of the complexing agent is 10-20% of the mass of the mixed material A.
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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 |
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