CN108975412B - Method for preparing iron compound from raw ore vermiculite - Google Patents
Method for preparing iron compound from raw ore vermiculite Download PDFInfo
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- CN108975412B CN108975412B CN201810850474.3A CN201810850474A CN108975412B CN 108975412 B CN108975412 B CN 108975412B CN 201810850474 A CN201810850474 A CN 201810850474A CN 108975412 B CN108975412 B CN 108975412B
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- C01G49/00—Compounds of iron
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- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for preparing an iron compound from raw ore vermiculite, which comprises the following steps: a. performing microwave ultrasonic expansion treatment on raw ore vermiculite; b. carrying out ultrasonic crushing and magnetic washing flotation on the obtained expanded vermiculite; c. performing acid dissolution on the obtained flotation vermiculite, and then performing solid-liquid separation to obtain an acidolysis solution; d. performing alkali precipitation reaction on the obtained acidolysis solution to obtain ferric hydroxide precipitate; e. washing, drying and roasting the obtained ferric hydroxide precipitate; f. carrying out acid dissolution on the obtained ferric oxide product, then carrying out solid-liquid separation, and drying the obtained liquid to obtain a ferric trichloride product; g. and (3) synthesizing the obtained ferric trichloride product at high temperature and high pressure to obtain the magnetic ferroferric oxide microspheres. The method can obtain the magnetic ferroferric oxide microspheres and recycle the iron impurities in the raw ore vermiculite. The invention can obtain ferric hydroxide, ferric chloride, magnetic ferroferric oxide and other products through separating and treating impurities contained in the vermiculite.
Description
Technical Field
The invention relates to the technical field of vermiculite, in particular to a method for preparing an iron compound from raw ore vermiculite.
Background
Vermiculite is one of nonmetallic minerals with better resource prospect and potential advantages in China, is an important nonmetallic mineral, is also a magnesium-containing aluminosilicate secondary metamorphic mineral with a layered structure, belongs to layered silicate, and is cheap and easy to obtain. The vermiculite can resist high temperature, is a poor thermal conductor and has good electrical insulation; expanded vermiculite is prone to water and moisture absorption; it expands at high temperature and is easy to peel. Vermiculite has the characteristics of good interlayer cation exchange capacity, expansion capacity, adsorption capacity, sound insulation, heat insulation, fire resistance, freezing resistance and the like, is stable in chemical property, is insoluble in water, is non-toxic and tasteless, has no side effect, and is mainly used for treating wastewater containing heavy metals and organic cations by utilizing good adsorption performance and ion exchange performance in industry, preparing antibacterial materials and heat insulation materials, vermiculite filter aid, purifying agent, organic vermiculite and the like.
Vermiculite is a layered material, and the key of industrial application is that the vermiculite is expanded to obtain the layered material before being utilized. In fact, as the vermiculite contains iron element, the prepared vermiculite composite material has the color of iron compound and is red, and the practical application of the vermiculite material is seriously hindered. Therefore, how to effectively remove the iron element in the vermiculite is a key problem for expanding the application of the vermiculite. Therefore, the research on the separation of the iron element from the vermiculite has important practical significance.
Disclosure of Invention
The invention aims to provide a method for preparing an iron compound from raw ore vermiculite, which can be used for obtaining magnetic ferroferric oxide microspheres and recycling iron impurities in the raw ore vermiculite.
To achieve the above object, the present invention provides a method for preparing an iron compound from raw ore vermiculite, the method comprising:
a. performing microwave ultrasonic expansion treatment on raw ore vermiculite to obtain expanded vermiculite;
b. carrying out ultrasonic crushing and magnetic washing flotation on the obtained expanded vermiculite to obtain iron particles and flotation vermiculite;
c. performing first acid dissolution on the obtained flotation vermiculite, and then performing solid-liquid separation to obtain an acidolysis solution;
d. performing alkali precipitation reaction on the obtained acidolysis solution to obtain ferric hydroxide precipitate;
e. washing, drying and roasting the obtained ferric hydroxide precipitate to obtain a ferric oxide product;
f. dissolving the obtained ferric oxide product and hydrochloric acid solution with second acid, performing solid-liquid separation, and drying the obtained liquid to obtain a ferric trichloride product;
g. dispersing the obtained ferric trichloride product in an organic alcohol solution of anhydrous sodium acetate for high-temperature high-pressure synthesis to obtain the magnetic ferroferric oxide microspheres.
Optionally, the conditions of the microwave ultrasonic expansion treatment in the step a are 10-20000 hz, the microwave power is 100-.
Optionally, the magnetic water washing flotation in the step b is performed under stirring, the stirring rotation speed is 600-5500Rpm, and the magnetic water washing flotation power is 0.5-1 Tesla.
Optionally, in the step c, the floating vermiculite is crushed to 90-350 meshes and then dissolved in the first acid, the acid used for dissolving the first acid is at least one of nitric acid, phosphoric acid, acetic acid and hydrogen peroxide, the mass concentration of the acid solution is 0.01-35%, the reaction temperature is 80-98 ℃, the reaction time is 0.1-20 hours, and the mass ratio of the acid solution to the floating vermiculite is 1: (0.1-100), the solid-liquid separation method is centrifugation, and the rotating speed is 15000-100000 Rpm.
Optionally, the conditions of the alkaline precipitation reaction in step d are as follows: the alkali solution is ammonia water and/or potassium hydroxide solution, the concentration of the alkali solution is 0.01-5mol/L, the reaction temperature is 50-99 ℃, the reaction time is 0.1-32 hours, and the pH value is 2.5-3.5.
Optionally, in the step e, the washing time is 5-10 times, the drying temperature is 30-120 ℃, the drying time is 1-50 hours, the roasting temperature is 300-.
Optionally, in the step f, the mass concentration of the hydrochloric acid solution is 0.1-36%, and the weight ratio of the hydrochloric acid solution to the ferric oxide product is (0.1-100): 1, the solid-liquid separation is ultrafiltration filtration, the aperture of an ultrafiltration membrane is 0.01-100 microns, and the vacuum degree is 0.01-0.20 MPa.
Optionally, in step g, the organic alcohol is one or more of ethylene glycol, vinyl alcohol, glycerol, polyethylene glycol and polyglycerol, and the mass ratio of sodium acetate, ferric trichloride and organic alcohol is 1: (5-20): (1-1000), the high-temperature high-pressure synthesis temperature is 100-280 ℃, and the synthesis time is 0.5-30 hours.
The invention has the following advantages:
the invention obtains magnetic ferroferric oxide microspheres and iron particles by performing microwave ultrasonic expansion, magnetic water washing flotation, acid dissolution, alkali precipitation, acid dissolution and high-temperature pressure synthesis on raw ore vermiculite, and recycles iron impurities in the raw ore vermiculite.
In addition, the invention has the advantages of simple and effective separation method, quick separation, low energy loss, easy separation, simple equipment, improved production efficiency, less pollutants and obvious economic value.
Drawings
FIG. 1 is an electron microscope image of a magnetic ferroferric oxide microsphere prepared in an embodiment of the invention.
Fig. 2 is a photograph of raw ore vermiculite used in the example of the present invention.
Fig. 3 is a photograph of an exfoliated vermiculite prepared according to an example of the present invention.
Figure 4 is a photograph of a floated vermiculite prepared according to an example of the present invention.
FIG. 5 is a photograph of an acid hydrolysis solution prepared in an example of the present invention.
FIG. 6 is a photograph of an iron hydroxide precipitate prepared in an example of the present invention.
FIG. 7 is a photograph of a product of ferric trichloride made in accordance with an embodiment of the present invention.
FIG. 8 is a photograph of magnetic ferroferric oxide microspheres prepared according to an example of the invention.
FIG. 9 is a graph showing the relationship between the dissolution temperature of the first acid and the amount of extracted iron ions (in terms of ferric oxide) in step c of the example of the present invention.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The invention provides a method for preparing iron compounds from raw ore vermiculite, which comprises the following steps: a. performing microwave ultrasonic expansion treatment on raw ore vermiculite to obtain expanded vermiculite; b. carrying out ultrasonic crushing and magnetic washing flotation on the obtained expanded vermiculite to obtain iron particles and flotation vermiculite; c. performing first acid dissolution on the obtained flotation vermiculite, and then performing solid-liquid separation to obtain an acidolysis solution; d. performing alkali precipitation reaction on the obtained acidolysis solution to obtain ferric hydroxide precipitate; e. washing, drying and roasting the obtained ferric hydroxide precipitate to obtain a ferric oxide product; f. dissolving the obtained ferric oxide product and hydrochloric acid solution with second acid, performing solid-liquid separation, and drying the obtained liquid to obtain a ferric trichloride product; g. dispersing the obtained ferric trichloride product in an organic alcohol solution of anhydrous sodium acetate for high-temperature high-pressure synthesis to obtain the magnetic ferroferric oxide microspheres. The invention obtains iron particles and magnetic ferroferric oxide microspheres by performing microwave ultrasonic expansion, magnetic water washing flotation, acid dissolution, alkali precipitation, acid dissolution and high-temperature high-pressure synthesis on raw vermiculite, and recycles iron impurities in the raw vermiculite.
In the invention, the microwave ultrasonic expansion treatment is used for expanding the raw vermiculite so as to facilitate the falling of iron particles in the raw vermiculite, for example, the conditions of the microwave ultrasonic expansion treatment in the step a are 10-20000 Hz, the microwave power is 100-. Other suitable conditions may be used by those skilled in the art to perform the microwave ultrasonic expansion treatment.
In the invention, the magnetic water washing flotation utilizes the characteristic that the density of expanded vermiculite is reduced and the expanded vermiculite can float on the water surface, and the iron particles can be adsorbed by a magnet to quickly separate the iron particles from the vermiculite, preferably, the magnetic water washing flotation in the step b is carried out under stirring, the stirring rotation speed can be 600-5500Rpm, and the magnetic water washing flotation power can be 0.5-1 Tesla.
In the invention, in order to facilitate the separation of iron particles which are not removed in a particle form from the floating vermiculite, the floating vermiculite is subjected to first acid dissolution, in order to improve the acid dissolution efficiency, in the step c, the floating vermiculite is crushed to 90-350 meshes and then subjected to first acid dissolution, the acid used for first acid dissolution can be at least one of nitric acid, phosphoric acid, acetic acid and hydrogen peroxide, the mass concentration of the acid solution can be 0.01-35%, the reaction temperature can be 80-98 ℃, the reaction time can be 0.1-20 hours, and the mass ratio of the acid solution to the floating vermiculite can be 1: (0.1-100), the solid-liquid separation method can be centrifugation, and the rotating speed can be 15000-100000 Rpm.
In the invention, in order to precipitate the iron element dissolved in the acid solution, adding alkali liquor into the acidolysis solution, wherein the conditions of the alkali precipitation reaction in the step d can be as follows: the alkali solution is ammonia water and/or potassium hydroxide solution, the concentration of the alkali solution is 0.01-5mol/L, the reaction temperature is 50-99 ℃, the reaction time is 0.1-32 hours, and the pH value is 2.5-3.5.
In the invention, in order to remove alkali components in the ferric hydroxide precipitate and obtain ferric oxide, the washing time in the step e can be 5-10 times, the drying temperature can be 30-120 ℃, the drying mode can be vacuum drying, the time can be 1-50 hours, the roasting temperature can be 300-850 ℃, and the time can be 1-50 hours.
In the invention, in order to obtain ferric trichloride for further purifying the iron compound, in the step f, the mass concentration of the hydrochloric acid solution can be 0.1-36%, and the weight ratio of the hydrochloric acid solution to the ferric oxide product can be (0.1-100): 1, the solid-liquid separation can be ultrafiltration filtration, the aperture of the ultrafiltration membrane can be 0.01-100 microns, the vacuum degree can be 0.01-0.20MPa, and high-speed centrifugation can be performed in advance before ultrafiltration.
In the invention, in order to obtain high-purity magnetic ferroferric oxide microspheres, in step g, the organic alcohol may be one or more of ethylene glycol, vinyl alcohol, glycerol, polyethylene glycol and polyglycerol, and the mass ratio of sodium acetate, ferric trichloride and the organic alcohol may be 1: (5-20): (1-1000), the high-temperature high-pressure synthesis temperature is 100-280 ℃, the synthesis time is 0.5-30 hours, and the product synthesized at high temperature and high pressure can be washed and dried to obtain the magnetic ferroferric oxide microspheres.
The invention is further illustrated by the following examples, but is not to be construed as being limited thereto.
Examples
a. Raw vermiculite (containing 5.8% by mass of ferric oxide, the photograph is shown in fig. 2) was subjected to expansion at a microwave power of 900W and an ultrasonic wave of 500 hz for 5 minutes to obtain expanded vermiculite (the photograph is shown in fig. 3).
b. Placing the obtained expanded vermiculite in a container under stirring, and performing ultrasonic magnetic water washing flotation by using an electromagnet, wherein the stirring speed is controlled to be 300Rpm, and the flotation power is controlled to be 0.5 Tesla, so as to obtain separated iron particles and flotation vermiculite (the photo is shown in figure 4).
c. Filtering the obtained flotation vermiculite, and then mixing the filtered flotation vermiculite with the water according to a mass ratio of 1: 10 adding 30 mass percent hydrogen peroxide solution, controlling the pH value to be 3, carrying out first acid dissolution, wherein the reaction time is 1.5 hours, the reaction temperature is 85 ℃ (as shown in figure 9, if the temperature is lower than 85 ℃, the extraction efficiency is reduced, the ordinate is the mass of iron ions (calculated by ferric oxide) extracted by 13 g of vermiculite, centrifuging for 5 minutes at 15000Rpm to obtain acidolysis solution (a picture is shown in figure 5). The step, if the first acid dissolution extraction of iron is carried out by adopting phosphoric acid, the extraction speed is accelerated, and only 0.4 hour is needed for achieving the same extraction amount by 5 mass percent phosphoric acid solution.
d. 0.1mol/L potassium hydroxide lye is added into the acidolysis solution, and then the reaction is carried out for 2.5 hours at 90 ℃, so as to obtain ferric hydroxide precipitate (the photo is shown in figure 6).
e. The resulting iron hydroxide precipitate was washed 5 times with water, then vacuum dried at 75 ℃ for 8 hours, followed by calcination at 450 ℃ for 2 hours to give an iron trioxide product (photograph shown in FIG. 7).
f. Mixing the obtained ferric oxide with 36 mass% of acid salt solution according to the weight ratio of 1: 10, dissolving the second acid, performing high-speed centrifugation and ultrafiltration, wherein the aperture of an ultrafiltration membrane is 0.02 micron, and the vacuum degree is 0.25MPa, and concentrating and drying the solution obtained by ultrafiltration to obtain the ferric trichloride product.
g. And (3) mixing the obtained ferric trichloride product with sodium acetate, ferric trichloride and organic alcohol according to the mass ratio of 1: 9: 30, dispersing in ethylene glycol alcoholic solution of anhydrous sodium acetate, and performing high-temperature high-pressure synthesis at 200 ℃ for 8 hours to obtain the magnetic ferroferric oxide microspheres (the photograph is shown in figure 8).
Through detection, the iron content in the magnetic ferroferric oxide microspheres is 99.2 mass percent, the magnetic ferroferric oxide microspheres have paramagnetic property, and an electron microscopic picture is shown in figure 1. It can be seen from the experiment that the products such as ferric hydroxide, ferric chloride, magnetic ferroferric oxide and the like can be obtained by separating and treating impurities contained in the vermiculite.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (5)
1. A method of producing iron compounds from raw ore vermiculite, the method comprising:
a. performing microwave ultrasonic expansion treatment on raw ore vermiculite to obtain expanded vermiculite;
b. carrying out ultrasonic crushing and magnetic washing flotation on the obtained expanded vermiculite to obtain iron particles and flotation vermiculite; the magnetic washing flotation in the step b is carried out under stirring, the stirring rotating speed is 600-5500Rpm, and the magnetic washing flotation power is 0.5-1 Tesla;
c. performing first acid dissolution on the obtained flotation vermiculite, and then performing solid-liquid separation to obtain an acidolysis solution; in the step c, the flotation vermiculite is crushed to 90-350 meshes and then dissolved by the first acid, the first acid is dissolved by phosphoric acid, the mass concentration of acid liquor is 0.01-35%, the reaction temperature is 85-98 ℃, the reaction time is 0.1-20 hours, and the mass ratio of the acid liquor to the flotation vermiculite is 1: (0.1-100), the solid-liquid separation method is centrifugation, and the rotating speed is 15000-100000 Rpm;
d. performing alkali precipitation reaction on the obtained acidolysis solution to obtain ferric hydroxide precipitate;
e. washing, drying and roasting the obtained ferric hydroxide precipitate to obtain a ferric oxide product;
f. dissolving the obtained ferric oxide product and hydrochloric acid solution with second acid, performing solid-liquid separation, and drying the obtained liquid to obtain a ferric trichloride product;
g. dispersing the obtained ferric trichloride product in an organic alcohol solution of anhydrous sodium acetate for high-temperature high-pressure synthesis to obtain magnetic ferroferric oxide microspheres;
in the step g, the organic alcohol is one or more of ethylene glycol, vinyl alcohol, glycerol, polyethylene glycol and polyglycerol, and the mass ratio of sodium acetate, ferric trichloride and the organic alcohol is 1: (5-20): (1-1000), the high-temperature high-pressure synthesis temperature is 100-280 ℃, and the synthesis time is 0.5-30 hours.
2. The method as claimed in claim 1, wherein the conditions of the microwave ultrasonic expansion treatment in step a are 10-20000 Hz, the microwave power is 100-.
3. The method according to claim 1, wherein the conditions of the alkaline precipitation reaction in step d are as follows: the alkali solution is ammonia water and/or potassium hydroxide solution, the concentration of the alkali solution is 0.01-5mol/L, the reaction temperature is 50-99 ℃, the reaction time is 0.1-32 hours, and the pH value is 2.5-3.5.
4. The method as claimed in claim 1, wherein the number of washing in step e is 5-10, the drying temperature is 30-120 ℃, the drying time is 1-50 hours, the calcination temperature is 300-850 ℃, and the calcination time is 1-50 hours.
5. The method according to claim 1, wherein in step f, the mass concentration of the hydrochloric acid solution is 0.1-36%, and the weight ratio of the hydrochloric acid solution to the ferric oxide product is (0.1-100): 1, the solid-liquid separation is ultrafiltration filtration, the aperture of an ultrafiltration membrane is 0.01-100 microns, and the vacuum degree is 0.01-0.20 MPa.
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| CN111573686A (en) * | 2020-05-19 | 2020-08-25 | 陕西科技大学 | Preparation method of vermiculite ultrafine powder |
| CN113603150A (en) * | 2021-09-23 | 2021-11-05 | 广州大学 | Iron oxide red and preparation method thereof |
| CN115487816B (en) * | 2022-08-16 | 2023-08-04 | 中国地质大学（武汉） | Vermiculite-based ferric molybdate nano enzyme and preparation method and application thereof |
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| CN104292888B (en) * | 2014-10-14 | 2018-03-27 | 塔里木大学 | A kind of method that PVC heat stabilizer is prepared using vermiculite as raw material |
| CN105948135B (en) * | 2016-05-03 | 2018-06-29 | 上海交通大学 | A kind of monodisperse porous magnetic sub-micro ball and preparation method thereof |
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