CN113319096B - Method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry method red mud solid alkali and red mud solid alkali enhancer - Google Patents

Method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry method red mud solid alkali and red mud solid alkali enhancer Download PDF

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CN113319096B
CN113319096B CN202110442665.8A CN202110442665A CN113319096B CN 113319096 B CN113319096 B CN 113319096B CN 202110442665 A CN202110442665 A CN 202110442665A CN 113319096 B CN113319096 B CN 113319096B
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red mud
alkali
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CN113319096A (en
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田野
刘中凯
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Aluminum Corp of China Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
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Abstract

The invention discloses a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry red mud solid alkali, and a red mud solid alkali enhancer, wherein the method comprises the following steps: uniformly mixing 80-90 parts of red mud and 10-20 parts of a solid caustic soda enhancer by weight to obtain a red mud solid caustic soda raw material; carrying out ultrasonic dispersion on the red mud alkali-fixing raw material to obtain a dispersion mixture; drying the dispersed mixture to obtain a dried mixture; performing ball milling and screening on the dried mixture to obtain a mixture with a fine particle size; and carrying out modification reaction on the fine-particle-size mixture by adopting microwaves to obtain the low-alkali red mud. According to the invention, the mineral dispersion pretreatment is carried out by using ultrasonic waves, and the rapid alkali fixation is carried out on the mixture of the red mud and the alkali fixation enhancer by using microwaves, so that the problem of overhigh alkali degree of the red mud leaching solution is solved, the pH value of the red mud leaching solution is remarkably reduced from 10.88 to 8.07, the alkali fixation rate reaches 92.50%, and the alkali fixation performance is greatly improved.

Description

Method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry method red mud solid alkali and red mud solid alkali enhancer
Technical Field
The invention relates to the technical field of non-ferrous metal metallurgy waste residue treatment, in particular to a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry red mud alkali fixation and a red mud alkali fixation enhancer.
Background
Bauxite residue-red mud is often generated in the production process of alumina, belongs to strong alkaline waste, has strong corrosivity on various animals, plants, oceans and soil, and generates great damage to the ecological environment. An average of 1.0 to 1.5 tons of red mud is produced per ton of alumina produced. Due to the increasing global demand for alumina, the cumulative amount of red mud is estimated to be about 50 million tons by 2025 years according to the current productivity, and varies with the bauxite source and the alumina extraction efficiency. At present, the main disposal mode of red mud is dam building and stockpiling, and the warehouse is closed after the stockpiling is fully sealed. However, when the dam is released due to improper disposal, the surrounding ecological environment is seriously affected. Therefore, the alkalinity reduction of red mud is always a hot spot of solid waste research in aluminum industry.
At present, the red mud dealkalization is commonly carried out by acid washing, water washing and lime method, for example, the red mud dealkalization of column leaching method disclosed in CN111330943A and modifier is added to fully dealkalize the red mud. The water-saving and efficient circulating red mud dealkalization system disclosed in CN108947156A utilizes the recycling of filtrate to achieve the dealkalization effect. The principle of red mud dealkalization coupled with the calcium method flue gas desulfurization process disclosed in CN110841463A is acid method neutralization dealkalization, and sodium ions, combined alkali and other components in the red mud are deeply replaced and neutralized under the combined action of calcium, sulfate radicals and sulfite radicals in the desulfurization liquid slurry. Microwave technology has been widely used in the field of metallurgy in recent years, and among them, the microwave red mud is widely used for recovering iron-containing substances by carbothermic reduction and for pore-forming. For example, in the method disclosed in CN108866318A, recovery rate can reach more than 85% by magnetic separation recovery after hydrothermal reaction by microwave heating. In CN107140718A, the microwave is used for the pretreatment of carbothermic reduction, so that the excess iron in the red mud can be effectively extracted in the carbothermic reduction-magnetic separation process. Research on the preparation of the porous adsorption material from the microwave low-temperature pore-forming activated granular red mud disclosed in CN102908983A shows that the adsorption pore volume and the specific surface area are greatly improved.
However, the methods such as the red mud alkali reduction technology and the ultrasonic microwave reduction technology disclosed in these documents all have the precondition that the reaction is performed in the acid leaching or water leaching environment, and these methods must introduce new corrosive chemical substances or generate secondary pollutants, which causes the occurrence of the forms of treatment or recycling plus new pollutants.
Therefore, how to develop a red mud alkali reduction technology with low cost, environmental protection and resource saving to solve the problem of overhigh alkali degree of red mud leaching liquid becomes a technical problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry red mud alkali fixation and a red mud alkali fixation enhancer, which solve the problem of overhigh alkali degree of red mud leaching liquid, remarkably reduce the pH value of the red mud leaching liquid from 10.88 to 8.07, ensure that the alkali fixation rate reaches 92.50 percent and greatly improve the alkali fixation performance.
In order to achieve the purpose, the invention provides a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry red mud alkali fixation, which comprises the following steps:
uniformly mixing 80-90 parts of red mud and 10-20 parts of a solid caustic soda enhancer by weight to obtain a red mud solid caustic soda raw material;
carrying out ultrasonic dispersion on the red mud solid caustic soda raw material to obtain a dispersion mixture;
drying the dispersed mixture to obtain a dried mixture;
performing ball milling and screening on the dried mixture to obtain a mixture with a fine particle size;
and carrying out modification reaction on the fine-particle-size mixture by adopting microwaves to obtain the low-alkali red mud.
Further, the alkali-fixing enhancer comprises, by weight, 2-10 parts of n-dodecyl trimethoxy silane, 2-5 parts of dodecyl dimethyl amine oxide, 1-3 parts of polyethylene glycol succinate, 1-4 parts of saponin powder, 1-3 parts of coal gangue, 1-5 parts of cullet and 1-4 parts of silica fume.
Further, the frequency of the ultrasonic wave is 28-80 KHz.
Further, the ultrasound adopts a one-time ultrasound mode or a multiple-time ultrasound mode; in the multiple ultrasonic mode, interval time exists between two adjacent ultrasonic waves, wherein the single ultrasonic time is 3-10 s, the single interval time is 3-10 s, and the total ultrasonic time is 3-30 min.
Furthermore, the drying temperature is 50-100 ℃, and the drying time is 0.5-3 h.
Further, the water content of the dried mixture is 2-5% by mass.
Furthermore, the grain diameter of the fine grain diameter mixture is 355-500 mu m.
Furthermore, a screen with 35-45 meshes is adopted for screening.
Further, the modification reaction is carried out in a rotary tube of a microwave rotary furnace, the temperature of the modification reaction is more than or equal to 796 ℃, the time of the modification reaction is 20-60 min, and the rotating speed of a cylinder of the rotary tube of the microwave rotary furnace is 0.2-2.0 r/min.
The invention also provides a red mud solid alkali enhancer which comprises, by weight, 80-90 parts of red mud and 10-20 parts of a solid alkali enhancer, wherein the solid alkali enhancer comprises, by weight, 2-10 parts of n-dodecyl trimethoxy silane, 2-5 parts of dodecyl dimethyl amine oxide prepared by using ultrasonic wave and microwave synergistic dry method red mud solid alkali, 1-3 parts of polyethylene glycol succinate, 1-4 parts of saponin powder, 1-3 parts of coal gangue, 1-5 parts of cullet and 1-4 parts of silica fume.
One or more technical solutions in the embodiments of the present invention at least have the following technical effects or advantages:
the invention provides a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry red mud solid alkali, and a red mud solid alkali enhancer, wherein the method comprises the following steps: uniformly mixing 80-90 parts of red mud and 10-20 parts of a solid caustic soda enhancer by weight to obtain a red mud solid caustic soda raw material; carrying out ultrasonic dispersion on the red mud alkali-fixing raw material to obtain a dispersion mixture; drying the dispersed mixture to obtain a dried mixture; performing ball milling and screening on the dried mixture to obtain a mixture with a fine particle size; and carrying out modification reaction on the fine-particle-size mixture by adopting microwaves to obtain the low-alkali red mud. The invention utilizes ultrasonic waves (mechanical waves) to cooperate with microwaves (electromagnetic waves) for pretreatment and modification, adds the solid alkali reinforcer to play roles of reducing the melting point and exciting the reaction, forms a molten glass state at higher temperature, enables the solid alkali reaction to be in a solid state and a molten state reaction, has more sufficient reaction, plays a role of early-stage excitation and promotion of reinforcement for the dry-process solid alkali, and simultaneously provides more binding sites for free alkali and attached alkali. The red mud components after pretreatment and modification are reduced, the properties of the residual components are stable, the specific surface area is obviously increased, and the surface is rougher. Through the dry alkali fixation, the pH value of the red mud leachate is remarkably reduced from 10.88 to 8.07, the alkali fixation rate reaches 92.50%, and the alkali fixation performance is greatly improved; the invention utilizes ultrasonic waves to carry out mineral dispersion pretreatment, uniformly disperses red mud minerals, and utilizes microwaves to carry out rapid alkali fixation on the red mud by adding alkali fixation enhancer mixture. The method not only greatly reduces the alkali fixation time, but also realizes the green and environment-friendly alkali fixation process, does not generate any secondary pollution, especially waste liquid and waste acid, and provides a rapid and efficient treatment method for subsequent safe disposal or resource utilization of red mud.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic diagram of microwave alkali fixation;
FIG. 2 is an XRD analysis chart of red mud microwave at 0, 20 and 40 min;
FIG. 3 is SEM images before and after microwave irradiation;
fig. 4 is a flowchart of a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry method for fixing alkali in red mud according to an embodiment of the present invention.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the embodiments of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that the present embodiments and examples are illustrative of the present invention and are not to be construed as limiting the present invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood in accordance with the meanings commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which embodiments of the invention belong. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the examples of the present invention are commercially available or can be prepared by an existing method.
In order to solve the technical problems, the embodiment of the invention provides a technical scheme, and the general idea is as follows:
according to a typical implementation manner of the embodiment of the present invention, there is provided a method for preparing low-alkali red mud by using ultrasonic wave and microwave in cooperation with dry-process red mud solid alkali, as shown in fig. 4, the method includes:
s1, uniformly mixing 80-90 parts by weight of red mud and 10-20 parts by weight of a solid alkali enhancer to obtain a red mud solid alkali raw material;
the addition proportion of the red mud is too much, the alkali fixation effect is insufficient, and the alkalinity of the modified red mud is still higher; the addition proportion of the red mud is too small, the red mud treated by the method is less under the same quality, the alkali fixation effect is improved, but the cost is increased due to too many additives;
as a preferable embodiment, the solid alkali enhancer comprises, by weight, 2-10 parts of n-dodecyl trimethoxy silane, 2-5 parts of dodecyl dimethyl amine oxide, 1-3 parts of polyethylene glycol succinate, 1-4 parts of saponin powder, 1-3 parts of coal gangue, 1-5 parts of cullet and 1-4 parts of silica fume.
The reason for selecting the raw materials of the solid caustic soda enhancer according to the proportion is as follows:
2-10 parts of n-dodecyl trimethoxy silane: the function is as follows: firstly, n-dodecyl trimethoxy silane can form a hydrophobic layer, can be temporarily stored in a mixture system when water absorbs energy to diffuse, provides energy for a solid alkali process, is a polar high molecular organic matter, can reduce activation energy required by a chemical reaction when electromagnetic waves continuously provide energy, provides a substance for exciting the solid alkali reaction together with water, and finally can be decomposed into nontoxic and harmless products of carbon dioxide and water. The n-dodecyl trimethoxy silane can improve the compatibility among all components of the solid alkali reinforcer and the compatibility between the solid alkali reinforcer and the red mud, and the addition is too little, so that the compatibility among the solid alkali reinforcers is weakened and the excitation energy is not sufficiently provided; too much addition, increased cost and increased energy consumption;
2-5 parts of dodecyl dimethyl amine oxide: the function is as follows: firstly, dodecyl dimethyl amine oxide can promote thickening, bulking and stability among all components, secondly, the activation energy of solid-alkali chemical reaction of the mixed material can be reduced, the solid-alkali reaction is promoted, and the bulking and thickening among solid-alkali reinforcers and the stability of all the components can be reduced if the addition amount is too small; too much addition, increased cost and increased energy consumption;
1-3 parts of polyethylene glycol succinate: the function is as follows: promoting the crystallization of solid alkali reaction, promoting the formation of glass-transition phase of red mud, finally forming a stable substance to reduce the alkalinity, and causing low glass-transition degree of a mixed material system and insufficient solid alkali reaction due to too little addition; too much addition, increased cost and increased energy consumption;
1-4 parts of saponin powder: the function is as follows: the saponin powder has good dispersion, wetting and other effects on the wettable hydrous red mud, is added into the hydrous red mud to be beneficial to the dispersion and wetting of various substances, the substance components can be fully excited after the moisture absorbs energy, the reaction process is promoted to be carried out, the addition is too little, the substance components are not sufficiently dispersed and wetted, the reaction of a mixed material system is not uniform, the reaction part is unbalanced, and partial reaction is not sufficient; too much addition, increased cost and increased energy consumption;
1-3 parts of coal gangue: the function is as follows: supplement of Al 2 O 3 、SiO 2 Part of minerals provide framework binding sites and an ore energy excitation foundation for subsequent solid caustic soda reaction, and the addition is too little, the solid caustic soda binding sites are less, and the solid caustic soda is insufficient; excessive addition of other minerals can cause excessive addition of other minerals, energy is dispersed, and red mud components are more complicated;
1-5 parts of cullet: the function is as follows: supplement of Al 2 O 3 、SiO 2 Providing a skeleton binding site for subsequent solid caustic soda reaction, wherein the addition is too little, the solid caustic soda binding sites are less, and the solid caustic soda is insufficient; the cost is increased due to excessive addition, and most of the main components of the cullet are inorganic non-metallic materials, which are not beneficial to microwave absorption and promotion of solid alkali reaction;
1-4 parts of silica fume: the function is as follows: the silicon ash has large specific surface area and high activity, can provide amorphous silicon binding sites for solid-base reaction, can prevent energy dissipation of a mixed material system, can better store the energy in the system, has the function of heat preservation energy, can greatly prolong the service life of a product material and resist corrosion of acid and base, and is easy to cause insufficient solid-base reaction due to less addition; excessive addition easily causes cost increase and energy consumption improvement;
s2, performing ultrasonic dispersion on the red mud solid alkali raw material to obtain a dispersion mixture;
as an optional implementation mode, the frequency of the ultrasonic wave is 28-80 KHz. The ultrasonic frequency range is favorable for fully dispersing the red mud solid caustic soda raw material; the ultrasonic frequency is above 20KHz, and has the advantages of good directivity, strong penetrating power, concentrated energy, cavitation, and the like during propagation. The ultrasonic waves are subjected to mechanical vibration propagation in the ore, and in the propagation process, due to different inherent frequencies of various liquid and ore solid particles, the vibration acceleration and the vibration amplitude generated by the liquid and the ore solid particles are different, so that the interfaces of various forms of substances generate relative motion, the ore is loosened, and the permeability is improved. The longer the microwave power and time are, the more thoroughly the mineral structure changes and the more stable it tends to be.
The ultrasound adopts a one-time ultrasound mode or a multi-time ultrasound mode; in the multiple ultrasonic mode, interval time exists between two adjacent ultrasonic waves, wherein the single ultrasonic time is 3-10 s, the single interval time is 3-10 s, and the total ultrasonic time is 3-30 min. The dispersion can be realized by adopting a one-time ultrasonic mode, and the multiple ultrasonic mode has the following possible advantages: the particles are dispersed more uniformly, gaps among the particles are reduced, contact is more dense and sufficient, multiple times of stronger sound wave intensity can be generated, a plurality of substances which cannot be penetrated by electromagnetic waves are penetrated, high-energy density and high-frequency stress and waves with bunching, orientation and reflection are converted into energy absorbed by the ore, and a foundation is laid for the energy stored in advance by the ore and subsequent excitation.
S3, drying the dispersed mixture to obtain a dried mixture;
as an optional embodiment, the drying temperature is 50-100 ℃, and the drying time is 0.5-3 h. The drying condition is favorable for obtaining a dried mixture with proper moisture content;
the moisture content of the dried mixture is 2-5% by mass. If the moisture content of the dried mixture is lower than 2%, the reaction is insufficient, because water is a polar molecule, the absorption of electromagnetic waves is very quick and sensitive, the premise of energy excitation is provided for the quick reaction of the mixture, and if the moisture content is lower, the reaction of the whole mixed system is slowed down; if the moisture content of the dried mixture is higher than 5%, partial energy loss of electromagnetic waves exists, because water is polar molecules, the early energy provided by the electromagnetic waves is absorbed by the water, if the microwave time is short, most energy is consumed on the water, the solid-alkali reaction may not occur or is not fully completed, and part of minerals in the red mud also contain crystal water, so that the energy loss is serious due to excessive free water. In addition, if the water content is too high, the mix system may burst in a small closed space;
the red mud is dried to a level with lower water content, free water still exists in the red mud, water molecules are of a typical polar molecule covalent bond structure, original disordered water molecule arrangement tends to be ordered in an externally-applied electromagnetic field, when the direction of the externally-applied electric field is changed, the water molecules also turn, the direction of the water molecules continuously changes and swings in a rapidly-changing microwave electromagnetic field, and huge heat is rapidly generated by the aid of thermal motion of the molecules and interaction between adjacent molecules. By subsequent microwave internal radiation, free water and crystal water are quickly evaporated, so that larger vacancies of Na can be generated in mineral crystal lattices 2 O/K 2 O, etc. into the stationary phase mineral structure providing a site for bonding.
S4, performing ball milling and screening on the dried mixture to obtain a mixture with a fine particle size;
as an alternative embodiment, the ball milling can be carried out by a vertical planetary high-energy ball mill, and a screen with 35-45 meshes is adopted for screening. The screening mesh number is mainly used for regulating and controlling the average particle size of the red mud, crystal water is removed during microwave alkali fixation, and the particle size is small and dispersed, so that a higher specific surface area can be generated, and more binding sites are provided for free alkali and attached alkali.
The grain diameter of the fine grain diameter mixture is 355-500 mu m. If the particle size of the fine-particle-size mixture is too small, the microstructure of the mineral and all components is damaged, the characteristics of the material are changed, and the adverse effect of insufficient solid alkali reaction is caused; if the particle size is too large, all the components are not fully contacted, and the particles are easy to agglomerate;
and S5, performing modification reaction on the fine-particle-size mixture by using microwaves to obtain the low-alkali red mud. The alkalinity of the low-alkali red mud is between 8 and 9.
The modification reaction is carried out in a rotary tube of a microwave rotary furnace, the temperature of the modification reaction is more than or equal to 796 ℃, the time of the modification reaction is 20-60 min, and the rotating speed of a cylinder of the rotary tube of the microwave rotary furnace is 0.2-2.0 r/min.
If the temperature of the modification reaction is less than 796 ℃, the adverse effect of insufficient energy provided for the solid alkali reaction is caused; if the time of the modification reaction is less than 20min, the solid caustic soda time is short, the solid caustic soda reaction is not sufficient, if the time is more than 60min, the reaction is basically complete, and if the reaction time after the reaction is prolonged, the consumed energy consumption is higher, the cost is higher, but the obtained solid caustic soda effect is not obvious, so that waste is caused;
if the rotating speed of the cylinder body is less than 0.2 r/min, glass phase is easy to agglomerate and adhere to the wall of the container during alkali fixation, so that the full reaction during alkali fixation is influenced, and if the rotating speed is more than 2.0 r/min, the rotating speed is too high, so that centrifugal force is easy to form, different components cannot be well contacted, and the full reaction during alkali fixation is influenced;
to sum up, the method for preparing the low-alkali red mud by using the ultrasonic wave and the microwave for the dry process of the red mud alkali fixation provided by the embodiment of the invention utilizes the ultrasonic wave (mechanical wave) and the microwave (electromagnetic wave) for pretreatment and modification, and the alkali fixation enhancer is added to play a role in lowering the melting point and form a molten glass state at a higher temperature, so that the solid-solid reaction can be in a solid-molten state reaction, the reaction is more sufficient, the enhancement promotion effect is played for the dry process of the alkali fixation, and more binding sites are provided for the alkali fixation. The components of the red mud after pretreatment and modification are reduced, the properties of the residual components are stable, the specific surface area is obviously increased, and the surface is rougher. By adopting the dry alkali fixation method, the pH value of the red mud leachate is obviously reduced from 10.88 to 8.07, the alkali fixation rate reaches 92.50 percent, and the alkali fixation performance is greatly improved. The invention utilizes ultrasonic waves to carry out mineral dispersion pretreatment, uniformly disperses red mud minerals, and utilizes microwaves to carry out rapid alkali fixation on the mixture of the red mud added with the alkali fixation enhancer. The method not only greatly reduces the alkali fixation time, but also realizes the green and environment-friendly alkali fixation process, does not generate any secondary pollution, especially waste liquid and waste acid, and provides a quick and efficient treatment method for subsequent safe disposal or resource utilization of red mud.
According to another typical embodiment of the invention, the red mud alkali consolidating agent comprises 80-90 parts by weight of red mud and 10-20 parts by weight of alkali consolidating agent, wherein the alkali consolidating agent comprises 2-10 parts by weight of n-dodecyl trimethoxy silane, 2-5 parts by weight of dodecyl dimethyl amine oxide, 1-3 parts by weight of polyethylene glycol succinate, 1-4 parts by weight of saponin powder, 1-3 parts by weight of coal gangue, 1-5 parts by weight of cullet and 1-4 parts by weight of silica fume.
The red mud alkali fixing agent is prepared by the method, so that the problem of overhigh alkali degree of the red mud leaching solution can be solved, the pH value of the red mud leaching solution is remarkably reduced and is reduced to 8.07 from 10.88, the alkali fixing rate is up to 92.50%, and the alkali fixing performance is greatly improved.
The method for preparing low-alkali red mud by using ultrasonic wave and microwave dry method red mud alkali fixation and the red mud alkali fixation agent of the present application will be described in detail below with reference to examples, comparative examples and experimental data.
Example 1
The embodiment provides a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry red mud solid alkali, which comprises the following specific operations:
adding 10 parts of solid alkali enhancer (comprising 2 parts of n-dodecyl trimethoxy silane, 3 parts of dodecyl dimethyl amine oxide, 1 part of polyethylene glycol succinate, 1 part of Chinese honeylocust fruit powder, 1 part of coal gangue, 1 part of cullet and 1 part of silica fume) into 90 parts of red mud, uniformly stirring in stirring equipment to form a raw material mixture, and then putting the raw material mixture into an ultrasonic generator for ultrasonic dispersion, loosening and energy storage, wherein the frequency is 28KHz; then, placing the red mud in a drying oven for drying, wherein the drying temperature is 100 ℃, and the drying time is 3 hours, so as to obtain a raw material mixture with the water content of 0.5%; ball-milling the raw material mixture by a vertical planetary high-energy ball mill, and then sieving by a 40-mesh sieve; placing the screened red mud in a microwave rotary furnace to carry out microwave dry alkali fixation for 60min, wherein the reaction temperature can reach 1556 ℃, and the rotating speed of a cylinder body is 0.2 r/min.
Example 2
The embodiment provides a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry red mud solid alkali, which comprises the following specific operations:
adding 13 parts of solid caustic soda reinforcer (comprising 3 parts of n-dodecyl trimethoxy silane, 3 parts of dodecyl dimethyl amine oxide, 2 parts of polyethylene glycol succinate, 2 parts of saponin powder, 1 part of coal gangue, 1 part of cullet and 1 part of silica fume) into 87 parts of red mud, uniformly stirring in a stirring device to form a raw material mixture, and then putting the raw material mixture into an ultrasonic generator for ultrasonic dispersion, loosening and energy storage, wherein the frequency is 40KHz; then, placing the red mud in a drying oven for drying, wherein the drying temperature is 100 ℃, and the drying time is 3 hours, so as to obtain a raw material mixture with the water content of 0.5%; ball-milling the raw material mixture by a vertical planetary high-energy ball mill, and then sieving by a 40-mesh sieve; and (3) placing the screened red mud into a microwave rotary furnace to carry out microwave dry alkali fixation for 30min, wherein the reaction temperature can reach 1053 ℃, and the rotating speed of the cylinder body is 0.5 r/min.
Example 3
The embodiment provides a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry red mud solid alkali, which comprises the following specific operations:
adding 15 parts of solid alkali enhancer (comprising 2 parts of n-dodecyl trimethoxy silane, 3 parts of dodecyl dimethyl amine oxide, 2 parts of polyethylene glycol succinate, 2 parts of Chinese honeylocust fruit powder, 2 parts of coal gangue, 2 parts of cullet and 2 parts of silica fume) into 85 parts of red mud, uniformly stirring in stirring equipment to form a raw material mixture, and then putting the raw material mixture into an ultrasonic generator for ultrasonic dispersion, loosening and energy storage, wherein the frequency is 60KHz; then, placing the red mud in a drying box for drying, wherein the drying temperature is 60 ℃, and the drying time is 1h, so as to obtain a raw material mixture with the water content of 2%; ball-milling the raw material mixture by a vertical planetary high-energy ball mill, and then sieving by a 40-mesh sieve; and (3) placing the screened red mud into a microwave rotary furnace to carry out microwave dry alkali fixation for 20min, wherein the reaction temperature can reach 796 ℃, and the rotating speed of the cylinder body is 1.5 r/min.
Example 4
The embodiment provides a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry method for solid alkali of red mud, which comprises the following specific operations:
adding 17 parts of a solid alkali enhancer (comprising 6 parts of n-dodecyl trimethoxy silane, 2 parts of dodecyl dimethyl amine oxide, 1 part of polyethylene glycol succinate, 2 parts of Chinese honeylocust fruit powder, 1 part of coal gangue, 3 parts of cullet and 2 parts of silica fume) into 83 parts of red mud, uniformly stirring in stirring equipment to form a raw material mixture, and then putting the raw material mixture into an ultrasonic generator for ultrasonic dispersion, loosening and energy storage, wherein the frequency is 80KHz; then, placing the red mud in a drying box for drying, wherein the drying temperature is 80 ℃, and the drying time is 1h, so as to obtain a raw material mixture with the water content of 1.5%; ball-milling the raw material mixture by a vertical planetary high-energy ball mill, and then sieving by a 40-mesh sieve; and (3) placing the screened red mud into a microwave rotary furnace to carry out microwave dry alkali fixation for 40min, wherein the reaction temperature can reach 1164 ℃, and the rotating speed of the cylinder body is 1.0 r/min.
Example 5
The embodiment provides a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry method for solid alkali of red mud, which comprises the following specific operations:
adding 18 parts of solid caustic soda reinforcer (comprising 5 parts of n-dodecyl trimethoxy silane, 5 parts of dodecyl dimethyl amine oxide, 1 part of polyethylene glycol succinate, 1 part of saponin powder, 3 parts of coal gangue, 1 part of cullet and 2 parts of silica fume) into 82 parts of red mud, uniformly stirring in a stirring device to form a raw material mixture, and then putting the raw material mixture into an ultrasonic generator for ultrasonic dispersion, loosening and energy storage, wherein the frequency is 28-80KHz; then, placing the red mud in a drying oven for drying, wherein the drying temperature is 100 ℃, and the drying time is 2 hours, so as to obtain a raw material mixture with the water content of 0.9%; ball-milling the raw material mixture by a vertical planetary high-energy ball mill, and then sieving by a 40-mesh sieve; and (3) placing the screened red mud into a microwave rotary furnace for carrying out microwave dry alkali fixation for 50min, wherein the reaction temperature can reach 1373 ℃, and the rotating speed of the cylinder body is 1.8 r/min.
Example 6
The embodiment provides a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry red mud solid alkali, which comprises the following specific operations:
adding 20 parts of solid caustic soda reinforcer (comprising 7 parts of n-dodecyl trimethoxy silane, 3 parts of dodecyl dimethyl amine oxide, 3 parts of polyethylene glycol succinate, 2 parts of saponin powder, 2 parts of coal gangue, 2 parts of cullet and 1 part of silica fume) into 80 parts of red mud, uniformly stirring in a stirring device to form a raw material mixture, and then putting the raw material mixture into an ultrasonic generator for ultrasonic dispersion, loosening and energy storage, wherein the frequency is 40KHz; then, placing the red mud in a drying oven for drying, wherein the drying temperature is 50 ℃, and the drying time is 0.5h, so as to obtain a raw material mixture with the water content of 2%; ball-milling the raw material mixture by a vertical planetary high-energy ball mill, and then sieving by a 40-mesh sieve; and (3) placing the screened red mud into a microwave rotary furnace to carry out microwave dry alkali fixation for 40min, wherein the reaction temperature can reach 1164 ℃, and the rotating speed of the cylinder body is 1.2 r/min.
Example 7
The embodiment provides a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry red mud solid alkali, which comprises the following specific operations:
adding 15 parts of solid caustic soda reinforcer (comprising 5 parts of n-dodecyl trimethoxy silane, 2 parts of dodecyl dimethyl amine oxide, 2 parts of polyethylene glycol succinate, 1 part of saponin powder, 2 parts of coal gangue, 1 part of cullet and 2 parts of silica fume) into 85 parts of red mud, uniformly stirring in a stirring device to form a raw material mixture, and then putting the raw material mixture into an ultrasonic generator for ultrasonic dispersion, loosening and energy storage, wherein the frequency is 40KHz; then, placing the red mud in a drying oven for drying, wherein the drying temperature is 70 ℃, and the drying time is 1h, so as to obtain a raw material mixture with the water content of 1.7%; ball-milling the raw material mixture by a vertical planetary high-energy ball mill, and then sieving by a 40-mesh sieve; and (3) placing the screened red mud into a microwave rotary furnace to carry out microwave dry alkali fixation for 30min, wherein the reaction temperature can reach 1053 ℃, and the rotating speed of the cylinder body is 0.5 r/min.
Example 8
The embodiment provides a method for preparing low-alkali red mud by using ultrasonic wave and microwave synergistic dry red mud solid alkali, which comprises the following specific operations:
adding 20 parts of solid alkali enhancer (comprising 8 parts of n-dodecyl trimethoxy silane, 5 parts of dodecyl dimethyl amine oxide, 3 parts of polyethylene glycol succinate, 1 part of Chinese honeylocust fruit powder, 1 part of coal gangue, 1 part of cullet and 1 part of silica fume) into 80 parts of red mud, uniformly stirring in stirring equipment to form a raw material mixture, and then putting the raw material mixture into an ultrasonic generator for ultrasonic dispersion, loosening and energy storage, wherein the frequency is 80KHz; then, placing the red mud in a drying oven for drying, wherein the drying temperature is 50-100 ℃, and the drying time is 0.5h, so as to obtain a raw material mixture with the water content of 2%; ball-milling the raw material mixture by a vertical planetary high-energy ball mill, and then sieving by a 40-mesh sieve; placing the screened red mud in a microwave rotary furnace to carry out microwave dry alkali fixation for 60min, wherein the reaction temperature can reach 1556 ℃, and the rotating speed of a cylinder body is 2.0 r/min.
Comparative example 1
This comparative example differs from example 7 in that the microwave treatment was not carried out, and the remaining steps were the same as in example 7.
Comparative example 2
This comparative example differs from example 8 in that no drying was performed and the remaining steps were the same as example 8.
Comparative example 3
This comparative example differs from example 8 in that sintering was carried out in a muffle furnace without using microwaves, and the remaining steps were the same as in example 8.
Comparative example 4
In this comparative example, the microwaving time was 10min, and the remaining steps were the same as in example 8.
Comparative example 5
In this comparative example, the microwaving time was 80min, and the remaining steps were the same as in example 8.
Comparative example 6
The comparative example uses a conventional silica powder reagent as a solid caustic strengthening agent, and the remaining steps are the same as in example 8.
Experimental example 1
The determination was carried out according to the standard of GBT15555.12-1995 method for determining the corrosivity of solid wastes by the pH glass electrode method. And (3) measuring the pH value of the leaching solution: weighing 100.00g of red mud mixture, 1L of deionized water, and the solid-to-liquid ratio is 1:10, oscillating for 8 hours on an oscillator, the frequency is 120 times/min, the amplitude is 40mm, and standing for 16 hours after oscillation is finished. The pH of the filtrate was immediately measured by a solid-liquid separator. And observing the appearance color of the sample by naked eyes after the microwave is applied. The pH and appearance color of the leach solution are shown in table 1 below:
TABLE 1
Figure BDA0003035560540000111
From the data in table 1:
in the comparative example 1, the microwave treatment is not carried out, only the independent drying is carried out, the pH value of the leaching solution is not obviously changed, and the color appearance shows that the minerals in the red mud are not obviously changed;
in comparative example 2, no drying pretreatment is carried out, the water content is high, a large amount of energy is consumed by the microwave in evaporating water molecules, so that the internal minerals cannot absorb electromagnetic waves quickly, the minerals do not change obviously in a short time, and the minerals start to change after the water molecules are completely evaporated, so that the solid caustic ratio is low;
in comparative example 3, the microwave is an electromagnetic wave mainly radiating from the inside of the mineral, while the high temperature muffle heating is from the surface, the energy loss is large. The heating and heat-generating sources are different, so that the alkali fixing effect has obvious difference;
in comparative example 4, the microwave time is 10min, which is less than the range of 20-60 min in the embodiment of the invention, the alkali fixing effect is poor, the time is short, and the components of each substance are stopped when beginning to react with each other, so that the stored energy is not completely excited, and the alkali fixing process is not reacted or the reaction is not complete;
in the comparative example 5, the microwave time is 80min, which is larger than the range of 20-60 min in the embodiment of the invention, the alkali fixation effect is not obviously improved, and large energy consumption is wasted;
in comparative example 6, the conventional solid caustic soda enhancer is adopted, the components are single, the effect is single, and sufficient microwave modification time is provided, so that the solid caustic soda is not sufficient. The reason is that the single solid caustic hardening agent only provides silicon binding sites for solid caustic reaction, and cannot provide early-stage excitation substances, energy storage substances and binding substances for the reaction, so that the alkalinity cannot be sufficiently reduced;
in the embodiments 1 to 8, the pH value of the red mud leaching solution is obviously reduced from 10.88 to 8.07 through dry alkali fixation, the alkali fixation rate reaches 92.50%, and the alkali fixation performance is greatly improved;
in conclusion, the invention utilizes ultrasonic waves to carry out mineral dispersion pretreatment, uniformly disperses red mud minerals, and utilizes microwaves to add alkali fixation reinforcer mixture into the red mud to carry out quick alkali fixation, so that the whole process is short of all; and the pH value and the solid caustic soda rate of the leachate are known, the most important influencing factors are a solid caustic soda enhancer and microwave time, and the parameters of the solid caustic soda enhancer and the microwave time are selected within the range of the embodiment of the invention, so that the rapid and sufficient reaction in the solid caustic soda process is facilitated, the solid caustic soda efficiency is improved, the time cost is controlled within a reasonable interval, and the energy consumption can be reduced. The drying temperature, the drying time and the screening mesh number have small influence, but the red mud can be dried to the level with lower water content through fine regulation and control, free water still exists in the red mud, water molecules are typical polar molecule covalent bond structures, original disordered water molecule arrangement tends to be ordered in an external electromagnetic field, when the direction of an external electric field is changed, the water molecules also turn, the direction of the water molecules is continuously changed and swings in a rapidly changed microwave electromagnetic field, and huge heat is rapidly generated through the thermal motion of the molecules and the interaction between adjacent molecules. By microwave internal radiation, free water is quickly evaporated, so that larger vacancies of Na can be generated in mineral crystal lattices 2 O/K 2 O, etc. into the stationary phase provides binding sites.
Description of the attached drawings 1-3:
fig. 1 is a schematic diagram of microwave dry method red mud solid alkali, wherein after ultrasonic dispersion, the appearance is more uniformly dispersed, and water molecules are more easily evaporated and are not blocked by impurities. Meanwhile, unstable minerals in the red mud are decomposed more easily, and the energy for dispersing or decomposing the minerals by subsequent microwaves can be reduced. The microwave mineral quickly raises the temperature, so that the phenomenon of isomorphism replacement occurs in the red mud, and partial mineral crystal lattices are easy to distort, thereby changing the unit cell parameters and the atomic bond force. The mass of minerals decreases with increasing microwave time and power due to the rapid removal of free water and crystal water from the minerals, which crystal water removal also produces atomic dislocations, voids, etc. that provide binding sites.
Fig. 2 microscopically shows that the red mud undergoes microwave material structure change, impurities are reduced, a stable crystal structure is formed finally, and free alkali or attached alkali is fixed in a stable state mineral form. The surface is in a glass phase state and is in an adhesive bonding state, because the solid alkali reinforcer reduces the melting point and forms a molten glass state at a higher temperature, the solid-solid reaction can be in a solid-molten state reaction, the reaction is more sufficient, the strengthening effect is promoted for the dry-process solid alkali, and simultaneously more bonding sites are provided for the solid alkali. The microwave front main component is one or more of hydrated garnet, nepheline, chlorite, calcite, illite, hematite, perovskite and diaspore. The microwave has less components and is stable, and the microwave contains garnet, perovskite, aluminosilicate with a stable skeleton structure, glass and other minerals.
Fig. 3 shows that the color change before and after the microwave also shows that the minerals in the red mud change before and after the microwave, the gray brown color mainly evaporates free water and removes crystal water, the main process of the change into light red and brick red color is the decomposition and removal of crystal water containing carbonate minerals, hydrated garnet minerals and the like, and partial decomposed minerals are recombined into garnet, and the color of the garnet is generally red. The final color of the microwave red mud alkali fixation is changed into black, and the fact that part of ferric oxide is converted into ferroferric oxide is also proved; fig. 3 also shows that when the internal temperature is very high, the alkali-containing substance portion becomes molten and thus enters into the voids created in the mineral lattice more easily.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications of those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the embodiments of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made in the embodiments of the present invention without departing from the spirit or scope of the embodiments of the invention. Thus, provided that such modifications and variations of the embodiments of the present invention fall within the scope of the claims of the embodiments of the present invention and their equivalents, the embodiments of the present invention are intended to include such modifications and variations as well.

Claims (9)

1. A method for preparing low-alkali red mud by utilizing ultrasonic wave and microwave in a dry method for solid alkali of red mud is characterized by comprising the following steps:
uniformly mixing 80-90 parts by weight of red mud and 10-20 parts by weight of solid caustic soda enhancer to obtain a red mud solid caustic soda raw material;
carrying out ultrasonic dispersion on the red mud solid caustic soda raw material to obtain a dispersion mixture;
drying the dispersed mixture to obtain a dried mixture;
performing ball milling and screening on the dried mixture to obtain a mixture with a fine particle size;
carrying out modification reaction on the fine-particle-size mixture by adopting microwaves to obtain low-alkali red mud;
the alkali-fixing reinforcer comprises, by weight, 2-10 parts of n-dodecyl trimethoxy silane, 2-5 parts of dodecyl dimethyl amine oxide, 1-3 parts of polyethylene glycol succinate, 1-4 parts of saponin powder, 1-3 parts of coal gangue, 1-5 parts of cullet and 1-4 parts of silica fume.
2. The method for preparing low-alkali red mud by using the dry method of red mud solid alkali by using the ultrasonic wave and the microwave as claimed in claim 1, wherein the frequency of the ultrasonic wave is 28-80 KHz.
3. The method for preparing low-alkali red mud by using the dry method of red mud solid alkali by using ultrasonic wave and microwave according to claim 1, wherein the ultrasonic treatment adopts a one-time ultrasonic treatment mode or a multiple ultrasonic treatment mode; in the multiple ultrasonic mode, interval time exists between two adjacent ultrasonic waves, wherein the single ultrasonic time is 3-10 s, the single interval time is 3-10 s, and the total ultrasonic time is 3-30 min.
4. The method for preparing low-alkali red mud by utilizing the dry method of the red mud solid alkali by utilizing the ultrasonic wave and the microwave as claimed in claim 1, wherein the drying temperature is 50-100 ℃, and the drying time is 0.5-3 h.
5. The method for preparing low-alkali red mud by utilizing the ultrasonic wave and microwave synergistic dry method for the solid alkali of the red mud as claimed in claim 1, wherein the moisture content of the drying mixture is 2-5% by mass.
6. The method for preparing low-alkali red mud by using the dry method of the red mud solid alkali by using the ultrasonic wave and the microwave as claimed in claim 1, wherein the particle size of the fine particle size mixture is 355-500 μm.
7. The method for preparing low-alkali red mud by utilizing the dry process of the solid alkali of the red mud by the combination of the ultrasonic wave and the microwave according to claim 1, wherein the temperature of the modification reaction is not less than 796 ℃, and the time of the modification reaction is 20-60 min.
8. The method for preparing low-alkali red mud by utilizing the dry process of fixing alkali of red mud by utilizing the combination of ultrasonic waves and microwaves as claimed in claim 1, wherein the modification reaction is carried out in a rotary microwave oven tube, and the rotating speed of the rotary microwave oven tube is 0.2-2.0 r/min.
9. The red mud alkali-fixing reinforcer is characterized by comprising, by weight, 80-90 parts of red mud and 10-20 parts of alkali-fixing reinforcer, wherein the alkali-fixing reinforcer comprises, by weight, 2-10 parts of n-dodecyl trimethoxy silane, 2-5 parts of dodecyl dimethyl amine oxide, 1-3 parts of polyethylene glycol succinate, 1-4 parts of saponin powder, 1-3 parts of coal gangue, 1-5 parts of cullet and 1-4 parts of silica fume.
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