CN113735131B - Method for efficiently preparing water glass by using coal gangue - Google Patents
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- CN113735131B CN113735131B CN202111201953.0A CN202111201953A CN113735131B CN 113735131 B CN113735131 B CN 113735131B CN 202111201953 A CN202111201953 A CN 202111201953A CN 113735131 B CN113735131 B CN 113735131B
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
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- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
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- C01D3/02—Fluorides
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Abstract
The invention discloses a method for efficiently preparing water glass by using coal gangue, belonging to the technical field of compound preparation. The water glass is prepared by activating coal gangue, acid leaching, separating and purifying silicon and mixing and heating with alkali liquor, the coal gangue is mixed with potassium carbonate or potassium hydroxide to realize activation under the heating condition, most of silicon in the activated coal gangue in hydrochloric acid with lower concentration can be dissolved out, and potassium fluoride is selected to react with coal gangue acid leaching solution in the separation and purification process of silicon, so that the cyclic utilization of potassium fluoride is realized, and the cost is reduced.
Description
Technical Field
The invention relates to a method for efficiently preparing water glass by utilizing coal gangue, belonging to the technical field of compound preparation.
Background
Coal gangue is waste stone generated in the coal mining washing and dressing process, and at present, the stock of the existing coal gangue reaches five billion tons and is continuously increased. The long-term accumulation of the coal gangue not only needs to occupy a large amount of land and causes the waste of land resources, but also causes the pollution to soil and water resources through long-term weathering and leaching of the coal gangue, and in addition, the coal gangue contains certain combustible substances and is easy to generate nature, and the discharged harmful gas and dust can also cause the pollution to the atmosphere. Therefore, the accumulation of the coal gangue not only causes environmental pollution and damages ecological balance, but also influences the physical health of residents in mining areas, so that the reduction and resource utilization of the coal gangue are necessary.
The water glass is widely applied to various aspects such as a washing agent, a settling agent, a refractory material, a soil curing agent and the like, and the market demand is large, so if the water glass prepared by utilizing the coal gangue can not only solve the problem of coal gangue resource waste, but also realize reasonable utilization of resources. At present, most of coal gangue is used for making bricks, generating electricity, repairing roads, preparing heat insulation materials, adsorbing materials and the like, wherein the coal gangue is prepared into water glass and then applied, the existing method for preparing the coal gangue into the water glass is many, for example, people such as Qiu home and the like calcine and activate the coal gangue, extract aluminum by acid dissolution and then react with caustic soda to prepare the water glass, the process is simple and rapid, but after the aluminum is extracted by acid leaching, acid leaching slag still contains more aluminum oxide, during the second step of alkali melting, the aluminum oxide and a sodium hydroxide solution generate sodium metaaluminate, the sodium metaaluminate is easy to dissolve in water, and the prepared water glass contains more impurities; the Zhumingsan et al utilizes the coal gangue fluoride salt sintering method reaction to separate aluminum and silicon, and SiO in the sample coal gangue 2 The recovery rate of the fluoride is up to 75.25 percent, but the fluosilicate is easy to decompose at high temperature to generate toxic gas of silicon tetrafluoride, and the recovery rate of the fluoride is not high, thus causing secondary pollution to the environment; the white carbon black is prepared by melting waste residues obtained by extracting aluminum from coal gangue with sodium carbonate and adopting a carbon separation method at a high temperature and a high pressure of 200 ℃, the technical process needs to react at a high temperature and a high pressure, higher requirements on equipment are provided, an organic solvent is used in the process, and the waste liquid can cause secondary pollution to the environment. It can be seen that the water glass prepared by coal gangue has high impurity content and unstable property,and the recovery rate of chemical raw materials used in the preparation process is low, so that the method for producing the high-purity water glass by using the coal gangue is provided, the consumption of the raw materials in the preparation process is reduced, and the method has important significance for reducing environmental pollution and realizing reasonable utilization of resources.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for efficiently preparing water glass by using coal gangue. The process can save energy consumption, reduce the pollution of production wastes to the environment and water, reduce the production cost to a great extent, and realize the basic requirements of energy conservation, consumption reduction, emission reduction and the like.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a method for efficiently preparing water glass by utilizing coal gangue, which comprises the following steps:
(1) Preparing activated coal gangue: grinding the coal gangue, mixing the ground coal gangue with potassium carbonate or potassium hydroxide, uniformly mixing, grinding and activating to obtain activated coal gangue; the reaction equation is as follows:
Al 2 O 3 ·2SiO 2 ·2H 2 O-AL 2 O 3 ·2SiO 2 +2H 2 O
AL 2 O 3 ·2SiO 2 -AL 2 O 3 +2SiO 2
AL 2 O 3 +2SiO 2 +K 2 CO 3 -2KAlSiO 4 +CO 2
(2) Acid leaching: mixing the activated coal gangue prepared in the step (1) with hydrochloric acid, stirring and reacting at room temperature, diluting and stirring, and performing solid-liquid separation to obtain coal gangue pickle liquor;
(3) Separation and purification of silicon: mixing potassium fluoride with the gangue acid leaching solution prepared in the step (2) to generate potassium fluosilicate precipitate, washing and drying to obtain pure potassium fluosilicate, adding the potassium fluosilicate into a potassium hydroxide solution to generate a potassium fluoride solution and silicon dioxide precipitate, and washing and drying the silicon dioxide precipitate to obtain pure silicon dioxide;
(4) Preparing water glass: mixing the silicon dioxide prepared in the step (3) with a sodium hydroxide solution, and heating at 80-100 ℃ for 4-8h to prepare water glass; the reaction equation is as follows:
2NaOH+SiO 2 ＝Na 2 SiO 3 +H 2 O
further, in the step (1), the coal gangue is ground to 200 meshes, the activation temperature is 650-900 ℃, and the activation time is 1-2.5h.
Further, the mass ratio of the coal gangue to the potassium carbonate in the step (1) is 10: (6-9).
Further, the concentration of the hydrochloric acid in the step (2) is 4-6mol/L, and the solid-to-liquid ratio of the activated coal gangue to the hydrochloric acid is (3: 20) - (1: 10).
Further, the dilution in the step (2) is diluted to 1-2 times of the volume by deionized water.
Further, the concentration of the potassium fluoride in the step (3) is 5-6mol/L, and the volume ratio of the potassium fluoride to the coal gangue pickle liquor is (1: 1) - (2: 1).
Further, the concentration of the potassium hydroxide in the step (3) is 3-6mol/L, and the solid-to-liquid ratio of the potassium fluosilicate to the potassium hydroxide is (3.
Further, in the step (4), the concentration of the sodium hydroxide solution is 2-3mol/L, and the solid-to-liquid ratio of the silica to the sodium hydroxide solution is (1.
Further, the potassium fluoride solution generated after the potassium fluosilicate in the step (3) is added into the potassium hydroxide solution is reused for mixing with the gangue acid leaching solution prepared in the step (2) to react.
The invention also provides the water glass prepared by the method.
Further, the modulus of the water glass is 2.8.
The invention discloses the following technical effects:
(1) According to the invention, potassium carbonate and coal gangue are mixed, the coal gangue is activated under mild subcritical or supercritical conditions, the activated coal gangue has a fluffy structure, the crystal structure of the coal gangue mainly comprises potassium aluminum silicate and silicon dioxide, the generated potassium aluminum silicate is dissolved in an acid solution, and only a small amount of silicon dioxide cannot be dissolved in the acid solution, so that most of silicon in hydrochloric acid with lower concentration can be dissolved out, and the introduction of impurities is effectively reduced by using the potassium carbonate for activation.
(2) In the invention, potassium fluoride is selected to react with gangue acid leaching solution to generate potassium fluosilicate in the process of separating and purifying silicon, potassium fluosilicate and potassium hydroxide solution in the subsequent steps are mixed to react to generate potassium fluoride solution and silicon dioxide precipitate, and the generated potassium fluoride solution can be continuously reused for the process of reacting with gangue acid leaching solution to generate potassium fluosilicate, thereby realizing the recycling of potassium fluoride. The consumption of potassium fluoride is reduced, the energy consumption is saved, and the production cost is reduced. The circulation rate measured by a titration method reaches over 90 percent.
(3) The method can prepare the water glass with the modulus of 2.8 from the coal gangue by a simple process, has no toxic substance release in the whole preparation process, has good environmental protection property, realizes reasonable utilization of the coal gangue, reduces pollution of the coal gangue to the environment and water, and has practical significance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a process flow diagram for efficiently preparing water glass by using potassium carbonate activated coal gangue;
FIG. 2 is an XRD diffraction intensity pattern of the activated coal gangue prepared in examples 1-5.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but rather as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in the present disclosure, it is understood that each intervening value, to the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in that stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
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 this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated herein by reference to disclose and describe the methods and/or materials in connection with which the documents are cited. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. It is intended that the specification and examples be considered as exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The coal gangue, the potassium hydroxide, the potassium carbonate, the potassium fluoride, the sodium hydroxide and the hydrochloric acid used in the embodiment of the invention are all commercially available, and the potassium hydroxide, the potassium carbonate, the potassium fluoride, the sodium hydroxide and the hydrochloric acid are all of analytical purity, wherein the potassium hydroxide, the potassium carbonate, the potassium fluoride and the sodium hydroxide are solid solids, the hydrochloric acid and deionized water are liquid, and the potassium hydroxide, the potassium carbonate, the potassium fluoride and the sodium hydroxide can be prepared to corresponding concentrations by conventional technical means in the field, and are not described in detail herein.
The solid-liquid ratio of the invention is calculated according to g/mL.
The technical solution of the present invention is further illustrated by the following examples.
Example 1
(1) Preparing activated coal gangue: grinding the coal gangue to 200 meshes, mixing and grinding the coal gangue and potassium carbonate for 10min according to a mass ratio of 10;
(2) Acid leaching: mixing the activated coal gangue prepared in the step (1) with 6mol/L hydrochloric acid according to a solid-to-liquid ratio of 3; the dissolution rate of silicon was 96%.
(3) Separation and purification of silicon: mixing 5mol/L potassium fluoride with the gangue pickle liquor prepared in the step (2) according to the volume ratio of 1;
(4) Preparing water glass: and (4) mixing the silicon dioxide prepared in the step (3) with 2mol/L sodium hydroxide solution according to a solid-to-liquid ratio of 3.
Example 2
The only difference from example 1 is that the activation is carried out at 800 ℃. The leaching rate of silicon in the acid leaching process is 96 percent.
Example 3
The only difference from example 1 is the activation at 750 ℃. The leaching rate of silicon in the acid leaching process is 94%.
Example 4
The only difference from example 1 is the activation at 700 ℃. The leaching rate of silicon during acid leaching was 90%.
Example 5
The only difference from example 1 is the activation at 650 ℃. The leaching rate of silicon in the acid leaching process is 86%.
Example 6
(1) Preparing activated coal gangue: grinding the coal gangue to 200 meshes, mixing and grinding the coal gangue and potassium carbonate for 10min according to a mass ratio of 10;
(2) Acid leaching: mixing the activated coal gangue prepared in the step (1) with 4mol/L hydrochloric acid according to a solid-to-liquid ratio of 1; the dissolution rate of silicon was 96%.
(3) Separation and purification of silicon: mixing 6mol/L potassium fluoride with the gangue pickle liquor prepared in the step (2) according to the volume ratio of 3;
(4) Preparing water glass: and (4) mixing the silicon dioxide prepared in the step (3) with 3mol/L sodium hydroxide solution according to a solid-to-liquid ratio of 1.
Example 7
(1) Preparing activated coal gangue: grinding the coal gangue to 200 meshes, mixing and grinding the coal gangue and potassium carbonate for 10min according to a mass ratio of 10;
(2) Acid leaching: mixing the activated coal gangue prepared in the step (1) with 5mol/L hydrochloric acid according to a solid-liquid ratio of 1; the dissolution rate of silicon was 98%.
(3) Separation and purification of silicon: mixing 5mol/L potassium fluoride with the gangue pickle liquor prepared in the step (2) according to a volume ratio of 1;
(4) Preparing water glass: and (3) mixing the silicon dioxide prepared in the step (3) with 3mol/L sodium hydroxide solution according to a solid-liquid ratio of 1.
Example 8
(1) Preparing activated coal gangue: grinding the coal gangue to 200 meshes, mixing and grinding the coal gangue and potassium hydroxide for 10min according to a mass ratio of 10;
(2) Acid leaching: mixing the activated coal gangue prepared in the step (1) with 6mol/L hydrochloric acid according to a solid-liquid ratio of 1; the dissolution rate of silicon was 91%.
(3) Separation and purification of silicon: mixing 6mol/L potassium fluoride with the gangue pickle liquor prepared in the step (2) according to a volume ratio of 2;
(4) Preparing water glass: mixing the silicon dioxide prepared in the step (3) with 2mol/L sodium hydroxide solution according to a solid-liquid ratio of 1:5, mixing, and heating at 90 ℃ for 8 hours to obtain the water glass.
Comparative example 1
The only difference from example 1 is that potassium carbonate is replaced by potassium hydroxide. The leaching rate of silicon during acid leaching was 61%.
Comparative example 2
The difference from example 1 is only that the preparation process of the activated coal gangue is as follows: grinding the coal gangue to 200 meshes, then placing the coal gangue in a muffle furnace, roasting and activating for 1h at 750 ℃, and continuously grinding and screening to obtain the activated coal gangue. The leaching rate of silicon in the acid leaching process is 31 percent.
Comparative example 3
The difference is only that the volume ratio of the potassium fluoride to the coal gangue pickle liquor is 1:3. the modulus of the obtained water glass is 1.2.
Comparative example 4
The difference from example 1 is only that the solid-to-liquid ratio of silica to sodium hydroxide solution is 1. The modulus of the obtained water glass is 1.6.
The XRD diffraction intensity patterns of the activated coal gangue prepared in the examples 1-5 are shown in figure 2. In fig. 2, the ordinate is diffraction intensity, the abscissa is diffraction angle 2 θ (°), and the diffraction angles at 23.24 °, 28.68 °, 34.40 °, and 42.00 ° are characteristic diffraction peaks of potassium aluminum silicate, which indicates that the main component of the gangue after activation is potassium aluminum silicate and contains a small amount of silicon dioxide.
Determination of the modulus of Water glass
The water glasses prepared in examples 1 to 8 and comparative examples 1 to 4 were subjected to modulus measurement using a constant temperature water glass modulus tester DA-300WG-T, and the measurement results are shown in Table 1.
TABLE 1
| modulus/M | |
| Example 1 | 2.8 |
| Example 2 | 2.6 |
| Example 3 | 2.5 |
| Example 4 | 2.3 |
| Example 5 | 2.2 |
| Example 6 | 2.6 |
| Example 7 | 2.7 |
| Example 8 | 2.3 |
| Comparative example 1 | 1.5 |
| Comparative example 2 | 0.9 |
| Comparative example 3 | 1.2 |
| Comparative example 4 | 1.6 |
As can be seen from the data in Table 1, the modulus of the water glass prepared in the examples 1-8 of the invention is between 2.2 and 2.8, which is higher than that of the water glass prepared in the comparative examples 1-4, and meets the regulation of GB/T4209-2008 (the modulus is between 2.2 and 2.5), which indicates that the water glass prepared by the method of the invention has higher modulus.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (5)
1. A method for efficiently preparing water glass by using coal gangue is characterized by comprising the following steps:
(1) Preparing activated coal gangue: grinding the coal gangue, mixing the ground coal gangue with potassium carbonate, and activating to obtain activated coal gangue;
(2) Acid leaching: mixing the activated coal gangue prepared in the step (1) with hydrochloric acid, stirring for 30s at room temperature, diluting, stirring for 3min, and performing solid-liquid separation to obtain coal gangue pickle liquor;
(3) Separation and purification of silicon: mixing potassium fluoride with the gangue pickle liquor prepared in the step (2), washing and drying to obtain potassium fluosilicate, adding the potassium fluosilicate into a potassium hydroxide solution, stirring for 10min at room temperature, taking the precipitate, washing and drying to obtain silicon dioxide;
(4) Preparing water glass: mixing the silicon dioxide prepared in the step (3) with a sodium hydroxide solution, and heating to prepare water glass;
in the step (1), the mass ratio of the coal gangue to the potassium carbonate is 10: (6-9);
in the step (3), the concentration of the potassium fluoride is 5-6mol/L, and the volume ratio of the potassium fluoride to the gangue acid leaching solution is (1;
in the step (3), the concentration of the potassium hydroxide is 3-6mol/L, and the solid-to-liquid ratio of the potassium fluosilicate to the potassium hydroxide is (3;
in the step (4), the concentration of the sodium hydroxide solution is 2-3mol/L, and the solid-to-liquid ratio of the silicon dioxide to the sodium hydroxide solution is (1;
and (4) adding the potassium fluosilicate in the step (3) into the potassium hydroxide solution to generate a potassium fluoride solution, and mixing the potassium fluoride solution with the gangue acid leaching solution prepared in the step (2) for reaction.
2. The method for efficiently preparing the water glass by using the coal gangue as recited in claim 1, wherein the activation temperature in the step (1) is 650-900 ℃, and the activation time is 1-2.5h.
3. The method for efficiently preparing water glass by using the coal gangue as claimed in claim 1, wherein the concentration of the hydrochloric acid in the step (2) is 4-6mol/L, and the solid-to-liquid ratio of the activated coal gangue to the hydrochloric acid is (3.
4. The method for efficiently preparing the water glass by using the coal gangue as claimed in the claim 1, wherein the dilution in the step (2) is diluted to 1-2 times of the volume by using deionized water.
5. A water glass produced by the method of any one of claims 1 to 4.
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