CN111017974A - Mineral processing technology for resource utilization of low-grade celestite - Google Patents
Mineral processing technology for resource utilization of low-grade celestite Download PDFInfo
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- CN111017974A CN111017974A CN201911310671.7A CN201911310671A CN111017974A CN 111017974 A CN111017974 A CN 111017974A CN 201911310671 A CN201911310671 A CN 201911310671A CN 111017974 A CN111017974 A CN 111017974A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/186—Strontium or barium carbonate
- C01F11/187—Strontium carbonate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/185—After-treatment, e.g. grinding, purification, conversion of crystal morphology
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/28—Chlorides by chlorination of alkaline-earth metal compounds
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
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Abstract
The invention relates to the technical field of beneficiation processes, and particularly discloses a beneficiation process for resource utilization of low-grade celestite, which comprises the following steps: step one, crushing raw ores: crushing raw ores to obtain fine particles with the diameter of less than 4 mm; step two, acid washing: pickling the fine particles obtained in the step one by using hydrochloric acid; step three, tail gas absorption: introducing gas generated in the acid washing process into an alkaline solution for absorption; step four, primary separation: separating solid and liquid generated after acid washing; step five, neutralizing; step six, heating and removing impurities: heating the solution in the fifth step, and adding quicklime; step seven, secondary separation: separating the solid and liquid after the step six; step eight, cleaning celestite; and step nine, cleaning the silt. The scheme is used for solving the problem that in the prior art, the environment is polluted by waste water, waste gas and waste residues in the process of carrying out ore dressing on low-grade celestite.
Description
Technical Field
The invention relates to the technical field of beneficiation processes, in particular to a beneficiation process for resource utilization of low-grade celestite.
Background
Strontium carbonate is an important strontium compound, is widely used in the fields of electronics, military industry, metallurgy, medicine, optics and the like due to the strong X-ray shielding function and the unique physical and chemical properties, is an inorganic chemical material which is developed rapidly in the world at present, and is mainly produced by celestite at present.
Celestite resources in China are relatively rich, but ores are low in grade and high in impurity content, and can be used as raw materials for producing strontium carbonate after ore dressing and impurity removal; the existing celestite subjected to mineral separation has fine granularity, the ore powder obtained by the existing mineral separation is generally below 200 meshes, and the existing process for producing industrial strontium carbonate by adopting celestite is not suitable (when strontium carbonate is produced by adopting a carbon reduction method (dry method), the ore powder obtained by the mineral separation of low-grade celestite cannot be directly sent into a rotary kiln for reduction roasting by adopting the same treatment process as high-grade lump ore, so the existing production process is not suitable), and the ore powder obtained by low-grade celestite needs to be subjected to flotation and agglomeration by adopting other methods, and then is subjected to reduction roasting to prepare strontium carbonate.
In the prior art, low-grade celestite is subjected to mineral separation by a flotation method to obtain ore particles smaller than 6 meshes for producing strontium carbonate, but waste water and waste residues generated in the mineral separation process are not reliably removed, so that waste gas, waste water and waste residues are increased, and the environment is polluted.
Disclosure of Invention
The invention aims to provide a beneficiation process for resource utilization of low-grade celestite, and aims to solve the problem that in the prior art, waste water, waste gas and waste residues pollute the environment in the beneficiation process of the low-grade celestite.
In order to achieve the above object, the basic scheme of the invention is as follows:
a mineral processing technology for resource utilization of low-grade celestite comprises the following steps:
step one, crushing raw ores: crushing the raw ore to obtain fine particles with the diameter of less than 4 mm.
Step two, acid washing: and (4) carrying out acid washing on the fine particles obtained in the step one by using hydrochloric acid.
Step three, tail gas absorption: and introducing gas generated in the acid washing process into an alkaline solution for absorption.
Step four, primary separation: and separating solid and liquid generated after acid washing to obtain celestite, silt and solution.
Step five, neutralizing: and (4) neutralizing the solution obtained by the separation in the step four until the solution is neutral.
Step six, heating and removing impurities: and heating the solution in the fifth step, and adding quicklime.
Step seven, secondary separation: and separating the solid and the liquid after the step six is completed.
Step eight, cleaning celestite: and cleaning the celestite obtained by the separation in the fourth step to obtain the celestite without an acidic solution.
Step nine, washing silt: and D, washing the silt obtained by the separation in the step four to obtain the silt without acid solution.
Compared with the technical principle and the beneficial effects in the prior art:
when this scheme of adoption, except containing about 30% strontium sulfate in the low-grade celestite raw ore, still contain other impurity like: calcite, dolomite, gypsum, silt and the like are washed by acid, non-silt impurities such as the calcite, the dolomite, the gypsum and the like are changed into a solution, the solution is separated for one time to obtain silt, the solution and celestite rich in strontium sulfate (wherein the celestite rich in strontium sulfate can be separated from the celestite due to small density of the silt), the celestite rich in strontium sulfate is subjected to step eight to obtain celestite free of acid solution, the content of strontium sulfate in the celestite is increased to about 78%, and the particles of the celestite are fine particles with the diameter smaller than 4mm, so that the process requirement of producing industrial strontium carbonate by the celestite can be met.
When tail gas is absorbed, gas generated by chemical reaction in acid washing or residual volatile hydrochloric acid reacts with alkaline solution to obtain industrial chlorine salt, so that the environment is prevented from being polluted by waste gas, and the condition that the waste gas is dispersed into the air and is absorbed by human bodies to cause harm to the human bodies is also avoided.
In the scheme, after the solution obtained in the fourth step is processed, magnesium, aluminum and iron in the solution can be changed into solid phases, the magnesium, aluminum and iron which are changed into the solid phases can be used as building material raw materials, and calcium in the solution is changed into industrial calcium chloride for industrial production.
In the whole process of the scheme, the existing low-grade celestite which is difficult to utilize is utilized, the process of the scheme is simple and feasible, the popularization is easy, and the celestite concentrate obtained by the scheme can meet the process requirement of producing industrial strontium carbonate from celestite; in addition, this scheme has all been retrieved to waste water, waste gas and the waste residue that produces among the low-grade celestite ore dressing process, has avoided waste water, waste gas and waste residue to the pollution of environment and the injury of human body, and the material that retrieves and obtain all can be used to industrial production for other materials all can utilize in the low-grade celestite raw ore.
Further, the step eight specifically includes a step a1 and a step a2, which are specifically as follows:
step a1, filter pressing after primary cleaning: and (4) adding water to the celestite obtained by the separation in the step four, cleaning, and then carrying out filter pressing, wherein the liquid obtained by the filter pressing is called primary washing water.
Step a2, pressure filtration after secondary cleaning: and c, adding water to clean the celestite obtained by the separation in the step a1 again, and then performing filter pressing, wherein the liquid obtained by the filter pressing is called secondary washing water, and the solid obtained by the filter pressing is celestite concentrate.
Has the advantages that: and cleaning celestite separated after acid washing to obtain celestite without acid solution, and further improving the purity of concentrate after low-grade celestite beneficiation.
Further, the first washing water is used for pickling the fine particles in the second step; the washing water is recycled, and the utilization rate of resources is improved.
Further, the second washing water is used for washing the celestite in the step a 1; the secondary washing water is recycled, and the utilization rate of resources is improved.
Further, the step nine specifically includes a step b1 and a step b2, and specifically includes the following steps:
step b1, washing silt and performing pressure filtration: and D, adding water to the silt obtained by separation in the step four, cleaning, then performing filter pressing, and using the liquid obtained by filter pressing for acid washing of the fine particles in the step two.
Step b2, washing silt II and performing pressure filtration: and c, adding water to wash the silt separated in the step b1 again, then performing filter pressing, using the liquid obtained by filter pressing for washing celestite in the step a1, and collecting the solid obtained by filter pressing.
Has the advantages that: and (3) washing the separated silt after acid washing to obtain the silt without the acid solution, and recycling the acid solution left by washing the silt, so that the utilization rate of resources is improved.
Further, the first step specifically comprises: crushing the raw ore by a crusher to obtain coarse particles with the diameter of 3-7cm, and then crushing the coarse particles by a crusher until fine particles with the diameter of less than 4mm are obtained.
Has the advantages that: the raw ore is crushed by a crusher and a crusher in a grading way, so that the difficulty of crushing the raw ore by equipment is reduced.
Further, the pH value of the solution washed by the acid in the second step is in the range of 0.5-1.5; strong acidity, and is beneficial to removing impurities in low-grade celestite.
Further, the mass concentration of the hydrochloric acid in the second step is not less than 25%; the hydrochloric acid has proper concentration, so that the hydrochloric acid can be fully contacted with the raw ore under the stirring action.
Further, the alkaline solution in the third step is a sodium hydroxide solution or a sodium carbonate solution; has good absorption effect on volatile hydrochloric acid and other gases.
Further, in the fifth step, calcium carbonate is adopted to neutralize the solution; the method is simple and easy to realize, and the calcium chloride generated after the calcium carbonate is adopted can be used for industrial production.
Drawings
Fig. 1 is a process flow diagram of a first embodiment of the invention.
Detailed Description
The following is further detailed by way of specific embodiments:
example one
An embodiment substantially as shown in figure 1:
a mineral processing technology for resource utilization of low-grade celestite comprises the following steps:
step one, crushing raw ores: taking raw ore which mainly contains about 30 percent of strontium sulfate and other impurities such as calcite, dolomite, gypsum, silt and a small amount of iron, aluminum and the like, crushing the raw ore by using a jaw crusher to obtain coarse particles with the diameter of 3-7cm, and crushing the coarse particles by using a crusher until fine particles with the diameter of less than 4mm are obtained.
Step two, acid washing: adding the fine particles obtained in the step one into an acid tank, adding hydrochloric acid with the mass concentration of 30% into the acid tank, and fully contacting and reacting the hydrochloric acid with the fine particles in a stirring manner to realize the acid washing of the fine particles, wherein the PH of the solution is kept to be 1 in the whole acid washing process; the gas after the acid washing comprises carbon dioxide and gaseous hydrochloric acid volatilized in an acid tank, and the liquid phase after the acid washing comprises magnesium chloride, calcium chloride, unreacted hydrochloric acid solution, a small amount of strontium chloride, iron ions, aluminum ions and the like; the solid phase after acid washing has celestite with high density and silt with low density.
Step three, tail gas absorption: and (2) introducing gas (carbon dioxide and gaseous hydrochloric acid volatilized in an acid tank) generated in the acid washing process into a secondary absorption tower, wherein the secondary absorption tower contains a sodium hydroxide solution, the gas is absorbed by the sodium hydroxide solution, and a sodium chloride solution is obtained after absorption and can be recycled.
Step four, primary separation: and (3) separating the solid and the liquid generated after the acid washing in the step (II) by using a filter press to obtain acid-containing celestite, silt and solution (the solution is the liquid phase after the acid washing recorded in the step (II), and the silt can be separated from the celestite through the filter press due to the low density of the silt).
Step five, neutralizing: and (4) neutralizing the solution obtained by the separation in the fourth step by using calcium carbonate until the solution is neutral.
Step six, heating and removing impurities: and (4) heating the solution after the fifth step to above 60 ℃, adding quicklime to perform chemical reaction with the solution to obtain a mixture of solid and liquid (the solid contains a solid phase containing iron, magnesium and aluminum, and the liquid contains a calcium chloride solution).
Step seven, secondary separation: and D, performing solid-liquid separation on the solid and the liquid which are subjected to the step six by adopting a filter press.
Step eight, cleaning celestite: cleaning the acid-containing celestite obtained by the separation in the step four to obtain celestite without acid solution; the method specifically comprises the following steps:
step a1, filter pressing after primary cleaning: and (4) adding water to clean the celestite obtained by separation in the step four, and then performing filter pressing by using a filter press, wherein the liquid obtained by the filter pressing is called first washing water, and the first washing water is used for performing acid washing on the fine particles in the step two.
Step a2, pressure filtration after secondary cleaning: adding water to the celestite obtained by separation in the step a1 again for cleaning, then carrying out filter pressing again by using a filter press, wherein the liquid obtained by the filter pressing is called secondary washing water, and the solid obtained by the filter pressing is celestite (namely celestite concentrate) without acid solution; the resulting two wash waters were used to wash the celestite in step a 1.
Step nine, washing silt: and (b) cleaning the acid-containing silt separated in the fourth step to obtain silt without acid solution, wherein the method specifically comprises the following steps of b1 and b 2:
step b1, washing silt and performing pressure filtration: and D, adding water to wash the silt obtained by separation in the step four, then performing filter pressing by using a filter press, and using the liquid obtained by filter pressing and the washing water in the step two to perform acid washing on the fine particles.
Step b2, washing silt II and performing pressure filtration: and c, adding water to the silt separated in the step b1 for cleaning again, then performing filter pressing, using the liquid obtained by filter pressing and the secondary cleaning water for cleaning celestite in the step a1, collecting the solid obtained by filter pressing, wherein the solid obtained by filter pressing is silt without acid solution, and the silt is used as a building material raw material.
The specific implementation process is as follows:
three tests were carried out according to the first example, and the test data are as follows (only the materials with higher contents were tested in the following table, and the small contents of iron, aluminum, etc. contained in the crude celestite are not disclosed):
according to the data, the low-grade celestite raw ore contains 30% of strontium sulfate and other impurities such as: calcite (the main component is calcium carbonate), dolomite (the main component is magnesium carbonate), gypsum (the main component is calcium sulfate), silt and a small amount of iron, aluminum and the like, after acid washing, non-silt impurities such as calcite, dolomite, gypsum and the like are changed into solution, and are separated once to obtain silt, solution and celestite rich in strontium sulfate (wherein the silt is used as silt and can be separated from the celestite due to small density), the celestite rich in strontium sulfate is subjected to the step eight to obtain celestite without acid solution, and the content of strontium sulfate in the celestite is increased to about 78 percent because the non-silt impurities such as calcite, dolomite, gypsum and the like except the strontium sulfate in the raw ore are changed into solution and are separated and the silt is also separated, and the particles of the celestite are fine particles with the diameter less than 4mm, so that the process requirement of producing industrial strontium carbonate from the celestite can be met.
When tail gas is absorbed, gas generated by chemical reaction in acid washing or residual volatile hydrochloric acid reacts with alkaline solution to obtain industrial chlorine salt, so that the environment is prevented from being polluted by waste gas, and the condition that the waste gas is dispersed into the air and is absorbed by human bodies to cause harm to the human bodies is also avoided.
In the first embodiment, after the solution (magnesium chloride, calcium chloride, unreacted hydrochloric acid solution, and a small amount of strontium chloride, iron ions, aluminum ions, and the like) obtained in the fourth step is processed, magnesium, aluminum, and iron in the solution can all be changed from a liquid phase to a solid phase, and the magnesium, aluminum, and iron changed into the solid phase can be used as building material materials, while calcium in the solution is changed into industrial calcium chloride for industrial production, so as to avoid the situation that waste liquid cannot be processed; the silt can be used as a building material after being separated and cleaned, and the waste residue is treated and recycled.
In the whole process of the first embodiment, the existing low-grade celestite which is difficult to utilize is utilized, the process of the first embodiment is simple and feasible, and easy to popularize, and the celeste blue concentrate obtained by the first embodiment can meet the process requirements of producing industrial strontium carbonate from celestite.
In the first embodiment, the first washing water and the second washing water generated by washing the acid-containing celestite and the acid-containing silt are recycled, so that energy is saved.
To sum up, waste water, waste gas and waste residue that produce in this embodiment pair low-grade celestite ore dressing process have all been retrieved, have avoided waste water, waste gas and waste residue to the pollution of environment and the injury of human body, and the material that obtains of retrieving all can be used to industrial production for other materials all can utilize in the low-grade celestite raw ore.
Example two
The difference between the second embodiment and the first embodiment is that in the second embodiment, the solution used for absorbing the tail gas is a sodium carbonate solution, which can achieve the same effect as sodium hydroxide.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (10)
1. A mineral processing technology for resource utilization of low-grade celestite is characterized by comprising the following steps:
step one, crushing raw ores: crushing raw ores to obtain fine particles with the diameter of less than 4 mm;
step two, acid washing: pickling the fine particles obtained in the step one by using hydrochloric acid;
step three, tail gas absorption: introducing gas generated in the acid washing process into an alkaline solution for absorption;
step four, primary separation: separating solid and liquid generated after acid washing to obtain celestite, silt and solution;
step five, neutralizing: neutralizing the solution obtained by the separation in the step four until the solution is neutral;
step six, heating and removing impurities: heating the solution in the fifth step, and adding quicklime;
step seven, secondary separation: separating the solid and liquid after the step six;
step eight, cleaning celestite: cleaning celestite obtained by separation in the fourth step to obtain celestite without acid solution;
step nine, washing silt: and D, washing the silt obtained by the separation in the step four to obtain the silt without acid solution.
2. The beneficiation process for resource utilization of low-grade celestite according to claim 1, wherein the step eight specifically comprises a step a1 and a step a2, and specifically comprises the following steps:
step a1, filter pressing after primary cleaning: adding water to the celestite obtained by the separation in the step four, cleaning, and then performing filter pressing to obtain liquid called primary washing water;
step a2, pressure filtration after secondary cleaning: and c, adding water to clean the celestite obtained by the separation in the step a1 again, and then performing filter pressing, wherein the liquid obtained by the filter pressing is called secondary washing water, and the solid obtained by the filter pressing is the celestite without acid solution.
3. The mineral processing process for resource utilization of low-grade celestite according to claim 2, wherein the first washing water is used for acid washing of fine particles in the second step.
4. The beneficiation process for resource utilization of low-grade celestite according to claim 3, wherein the second washing water is used for washing celestite in the step a 1.
5. The beneficiation process for resource utilization of low-grade celestite according to claim 4, wherein the step nine specifically comprises a step b1 and a step b2, and specifically comprises the following steps:
step b1, washing silt and performing pressure filtration: washing the silt separated in the fourth step with water, then performing filter pressing, and using the liquid obtained by filter pressing for pickling the fine particles in the second step;
step b2, washing silt II and performing pressure filtration: and c, adding water to wash the silt separated in the step b1 again, then performing filter pressing, using the liquid obtained by filter pressing for washing celestite in the step a1, and collecting the solid obtained by filter pressing.
6. The mineral processing technology for resource utilization of low-grade celestite according to claim 1, wherein the first step is specifically: crushing the raw ore by a crusher to obtain coarse particles with the diameter of 3-7cm, and then crushing the coarse particles by a crusher until fine particles with the diameter of less than 4mm are obtained.
7. The beneficiation process for resource utilization of low-grade celestite according to claim 1, wherein the pH of the solution after acid washing in the second step is in a range of 0.5 to 1.5.
8. The mineral processing process for resource utilization of low-grade celestite according to claim 1, wherein the mass concentration of hydrochloric acid in the second step is not less than 25%.
9. The mineral processing process for resource utilization of low-grade celestite according to claim 1, wherein the alkaline solution in the third step is a sodium hydroxide solution or a sodium carbonate solution.
10. The beneficiation process for resource utilization of low-grade celestite according to claim 1, wherein in the fifth step, calcium carbonate is used for neutralizing the solution.
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| CN113666407A (en) * | 2021-08-20 | 2021-11-19 | 中山大学 | Comprehensive utilization process for extracting calcium ions in south sea calcareous sand and treating algae sewage and application thereof |
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| CN113666407A (en) * | 2021-08-20 | 2021-11-19 | 中山大学 | Comprehensive utilization process for extracting calcium ions in south sea calcareous sand and treating algae sewage and application thereof |
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Application publication date: 20200417 |