CN114058882B - Method for purifying barite and recovering rare earth from barite concentrate - Google Patents
Method for purifying barite and recovering rare earth from barite concentrate Download PDFInfo
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- CN114058882B CN114058882B CN202111338245.1A CN202111338245A CN114058882B CN 114058882 B CN114058882 B CN 114058882B CN 202111338245 A CN202111338245 A CN 202111338245A CN 114058882 B CN114058882 B CN 114058882B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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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
- C01F11/46—Sulfates
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/02—Apparatus therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for purifying barite and recovering rare earth from barite concentrate, which comprises the following steps: s1, acid leaching is carried out on barite concentrate, then, acid leaching liquid is filtered, and a precipitate is obtained; s2, washing the precipitate with hot water until the pH value is not less than 6 to obtain acid leaching ore; s3, carrying out oxidizing roasting on the acid leached ore at the roasting temperature of 400-500 ℃ to obtain roasted ore; s4, acid leaching the roasted ore by using dilute sulfuric acid, and filtering to obtain leaching liquid and leaching ore; s5, recycling the leaching material liquid as a rare earth sulfate material liquid, and washing and drying the leaching ore to obtain the barite product. According to the method, fluorite and rare earth are effectively dissociated in the modes of acid leaching, roasting and acid leaching, the purity of the barite product is improved to be more than 96%, the content of fluorite is lower than 0.5%, the content of rare earth is lower than 0.2%, rare earth resources are effectively recycled, the whole process flow is not complex, the production cost is low, and the profit margin of enterprises is increased.
Description
Technical Field
The invention relates to the technical field of mineral separation, in particular to a method for purifying barite and recovering rare earth from barite concentrate.
Background
The barite is the most common mineral of barium, the component of the barite is barium sulfate, the barite belongs to nonrenewable resources, is one of export mineral products with Chinese advantages, is widely used as a weighting agent for drilling mud of petroleum and natural gas, and the consumption in the fields of barium chemical industry, filling materials and the like is gradually increasingThe annual growth of the barite is that the barite resource of China is quite rich and is distributed in 21 provinces (regions) of the country, 3.6 hundred million tons of ore are always reserved, and the barite resource occupies the 1 st position in the world. Can be used for contrast medium in digestive system. The barite concentrate product produced by the current industrial and mining enterprises has more complex components and low purity, the content of barium sulfate is mostly between 85 and 95 percent (mass fraction), the barite concentrate product contains silicate, fluorite, rare earth and other non-barite element impurities, the content of rare earth is between 1.5 and 6 percent, and CaF 2 The content is between 2 and 8 percent, and the impurities are important factors influencing the purity of the product.
The method is very important for improving the grade of barite, improving the purity of barium sulfate and reducing the content of fluorite and rare earth in the mixed barite ore. The existing enrichment process of barite concentrate usually enriches barite and fluorite in a flotation and reselection mode, but barite and fluorite are mixed and symbiotic, so that the content of fluorite in the barite concentrate is difficult to reduce to below 2%, the content of rare earth is difficult to reduce to below 0.5%, the cost is exponentially increased along with the improvement of purity, enterprises hardly have profit space, and the quality of the barite concentrate in China is difficult to be introduced into the international high-end product market.
Disclosure of Invention
The invention aims to: aiming at the existing problems, the invention provides a method for purifying barite and recovering rare earth from barite concentrate, and the method not only effectively improves the purity of the barite concentrate by the modes of acid leaching, roasting and acid leaching, so that the content of fluorite in the concentrate is lower than 0.5 percent, but also effectively recovers rare earth resources and fluorite resources, has uncomplicated process flow, low production cost and obvious technical advantages, and overcomes the defects of the traditional process.
The technical scheme adopted by the invention is as follows: a method for purifying barite and recovering rare earth from barite concentrate comprises the following steps:
s1, acid leaching is carried out on barite concentrate, then acid leaching liquid is filtered, and a precipitate is obtained:
s2, washing the precipitate with hot water until the pH value is not less than 6 to obtain acid leaching ore;
s3, oxidizing and roasting the acid-leached ore at the roasting temperature of 400-500 ℃ to obtain roasted ore;
s4, acid leaching the roasted ore by using dilute sulfuric acid, and filtering to obtain leaching liquid and leaching ore;
s5, recycling the leaching material liquid as a rare earth sulfate material liquid, and washing and drying the leaching ore to obtain the barite product.
Further, in S1, the mixed barite concentrate is subjected to acid leaching by using hydrochloric acid, wherein the concentration of the hydrochloric acid is 5-7mol/L.
Further, in the S1, when acid leaching is carried out, hydrochloric acid is heated to 80 ℃, and the acid leaching time is not less than 20min.
According to the method, the barite concentrate reacts with hydrochloric acid with a certain concentration under a heating condition, so that calcium fluoride, rare earth and other impurities in the barite concentrate can be dissociated, experiments show that only part of calcium fluoride and rare earth in the barite concentrate can be dissociated in the method, the purity of the barite concentrate subjected to acid leaching cannot meet the requirement of high purity, when the using concentration of the hydrochloric acid is 5-7mol/L, the content of the calcium fluoride in the barite concentrate can be limited to be below 2%, the concentration of the hydrochloric acid is not high or low, if the concentration of the hydrochloric acid is low, the reaction degree of the calcium fluoride and the hydrochloric acid is poor, only a small amount of calcium fluoride in the barite concentrate is dissociated, and at the moment, the content of the calcium fluoride in the barite concentrate is about 2-3%, and the acid leaching effect is poor; if the concentration of the hydrochloric acid is too high, the change of the dissociated calcium fluoride is not obvious, the amount of the dissociated rare earth is obviously increased, the loss of the rare earth is higher, the recovery of the rare earth is not facilitated, and in addition, the acid leaching is carried out at the temperature of 80 ℃, the volatilization of the high-concentration hydrochloric acid is obvious, the pollution is caused to the production environment, and the harm to the body of an operator is larger.
In the invention, the roasting time is 1-3h during oxidizing roasting. Through the roasting mode, firstly, the dissociation degree of the barite concentrate is improved, and secondly, the compound is completely converted into oxide and fluoride, so that the subsequent further purification operation is facilitated, and the interference of carbonate, sulfate and other miscellaneous salts on the subsequent purification is avoided. The oxidizing roasting can not be carried out before the hydrochloric acid leaching, otherwise, the problem of large loss amount of the barite and the rare earth can be caused, and the usage amount of the hydrochloric acid can be multiplied.
Further, in S4, the mass fraction of dilute sulfuric acid is 3-6%, the acid leaching temperature of the dilute sulfuric acid is 70-90 ℃, and the acid leaching time is not less than 20min. Acid leaching is carried out on the calcined barite ore by dilute sulfuric acid at high temperature, and the oxidized rare earth and fluoride in the barite ore can be dissociated out, so that the purity of the barite ore is further improved, after acid leaching by dilute sulfuric acid, the purity of the barite ore reaches over 96 percent, the content of rare earth is lower than 0.2 percent, the leaching rate of rare earth reaches over 99 percent, the content of fluorite is lower than 0.5 percent, the purification effect is obvious, and the high-quality barite product is obtained.
Further, in S1, absorbing the generated white smoke with water to obtain a hydrofluoric acid solution with a certain concentration, mixing the hydrofluoric acid solution with the acid leaching solution generated in S1, filtering to obtain filter residue, and recovering the filter residue as a crude fluorite product. In the acid leaching process, HF gas is generated, HF is absorbed by water to form a hydrofluoric acid solution, the acid leaching solution after acid leaching mainly contains calcium chloride and rare earth chloride, calcium fluoride and rare earth fluoride precipitates are formed by the hydrofluoric acid solution, and therefore, fluorite and rare earth resources are obtained while 'treating waste with waste' is realized, and valuable recovery is realized.
Further, in S4, absorbing the generated white smoke with water to obtain hydrofluoric acid solution with a certain concentration, mixing the hydrofluoric acid solution with the acid leaching solution generated in S1, filtering to obtain filter residue, and recycling the filter residue as a fluorite crude product.
Further, in the obtained barite product, the content of barium sulfate is not less than 96%, and the content of rare earth is less than 0.2%.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that: according to the method, the fluorite and the rare earth mixed in the barite ore are effectively dissociated in the modes of acid leaching, roasting and acid leaching, so that the purity of the barite product is improved and can reach over 96 percent, the content of the fluorite is lower than 0.5 percent, and the content of the rare earth is lower than 0.2 percent; in addition, the dissociated fluorite and rare earth are recycled at a high value in a mode of treating waste by waste and sulfuric acid rare earth feed liquid, so that the profit of an enterprise is increased while the generation amount of solid waste and waste water is reduced, the whole process flow is not complex, the production cost is low, the technical advantage is obvious, and the defects of the traditional process are overcome.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A method for purifying barite and recovering rare earth from barite concentrate comprises the following steps:
s1, preparing hydrochloric acid with the concentration of 5-7mol/L, performing acid leaching on barite concentrate at the temperature of 80 ℃, wherein the acid leaching time is 20-30min, and then filtering acid leaching liquid to obtain a precipitate;
s2, washing the precipitate with hot water until the pH value is not less than 6 to obtain acid leaching ores, and combining a washing liquid and an acid leaching solution to obtain an acid leaching solution mainly containing calcium chloride;
s3, drying the acid-leached ore, and carrying out oxidation roasting on the acid-leached ore, wherein the roasting temperature is 400-500 ℃, and the roasting time is 1-3h, so as to obtain a roasted ore;
s4, performing acid leaching on the roasted ore by using dilute sulfuric acid with the mass fraction of 3-6% at the temperature of 80 ℃, wherein the acid leaching time is 20-30min, and then filtering to obtain leaching material liquid and leaching ore;
s5, recycling the leaching material liquid as a rare earth sulfate material liquid, and washing and drying the leaching ore to obtain a high-purity barite product.
In the method, white smoke generated in the acid leaching process is absorbed by water to obtain a hydrofluoric acid solution with a certain concentration, then the hydrofluoric acid solution and the acid leaching solution are mixed and stirred, filter residue is obtained after filtration, the filter residue is a fluorite product containing rare earth, and the filter liquor is used as wastewater for further treatment.
To better illustrate the technical advantages of the process of the invention, specific production examples are listed below:
example 1
A method for purifying barite and recovering rare earth from barite concentrate comprises the following steps:
s1, 100kg of barite concentrate with the purity of 90.6% (calculated by barium sulfate), wherein the content of fluorite (calculated by calcium fluoride) is 3.3%, the content of rare earth REO is 2.5%, hydrochloric acid with the concentration of 6mol/L is prepared, acid leaching is carried out on the barite concentrate at the temperature of 80 ℃, the acid leaching time is 20min, and then acid leaching solution is filtered to obtain precipitate;
s2, washing the precipitate with hot water until the pH value is not less than 6 to obtain acid leaching ore, and combining washing liquor and acid leaching liquor to obtain acid leaching liquor mainly containing calcium chloride;
s3, drying the acid leaching ore, and oxidizing and roasting the acid leaching ore at the roasting temperature of 500 ℃ for 2 hours to obtain roasted ore;
s4, performing acid leaching on the roasted ore by using dilute sulfuric acid with the mass fraction of 5% at the temperature of 80 ℃, wherein the acid leaching time is 20min, and then filtering to obtain leaching liquid and leaching ore;
s5, recycling the leaching liquid as a rare earth sulfate liquid, and washing and drying the leached ore to obtain a high-purity barite product.
Example 2
A method for purifying barite and recovering rare earth from barite concentrate comprises the following steps:
s1, 100kg of barite concentrate with the purity of 88.4% (calculated by barium sulfate), wherein the content of fluorite (calculated by calcium fluoride) is 2.9%, the content of rare earth REO is 3.1%, hydrochloric acid with the concentration of 6mol/L is prepared, acid leaching is carried out on the barite concentrate at the temperature of 80 ℃, the acid leaching time is 20min, and then acid leaching solution is filtered to obtain precipitate;
s2, washing the precipitate with hot water until the pH value is not less than 6 to obtain acid leaching ore, and combining washing liquor and acid leaching liquor to obtain acid leaching liquor mainly containing calcium chloride;
s3, drying the acid leaching ore, and oxidizing and roasting the acid leaching ore at the roasting temperature of 500 ℃ for 2 hours to obtain roasted ore;
s4, performing acid leaching on the roasted ore by using dilute sulfuric acid with the mass fraction of 5% at the temperature of 80 ℃, wherein the acid leaching time is 20min, and then filtering to obtain leaching liquid and leaching ore;
s5, recycling the leaching material liquid as a rare earth sulfate material liquid, and washing and drying the leaching ore to obtain a high-purity barite product.
Example 3
A method for purifying barite and recovering rare earth from barite concentrate comprises the following steps:
s1, 100kg of barite concentrate with the purity of 92.3 percent (calculated by barium sulfate), wherein the content of fluorite (calculated by calcium fluoride) is 2.6 percent, the content of rare earth REO is 1.8 percent, hydrochloric acid with the concentration of 6mol/L is prepared, the barite concentrate is subjected to acid leaching at the temperature of 80 ℃, the acid leaching time is 20min, and then acid leaching solution is filtered to obtain precipitate;
s2, washing the precipitate with hot water until the pH value is not less than 6 to obtain acid leaching ore, and combining washing liquor and acid leaching liquor to obtain acid leaching liquor mainly containing calcium chloride;
s3, drying the acid leaching ore, and oxidizing and roasting the acid leaching ore at the roasting temperature of 500 ℃ for 2 hours to obtain roasted ore;
s4, performing acid leaching on the roasted ore by using dilute sulfuric acid with the mass fraction of 5% at the temperature of 80 ℃, wherein the acid leaching time is 20min, and then filtering to obtain leaching material liquid and leaching ore;
s5, recycling the leaching material liquid as a rare earth sulfate material liquid, and washing and drying the leaching ore to obtain a high-purity barite product.
Examples 1-3 the results of the tests on the final barite product are shown in table 1:
table 1 examples 1-3 barite product purity test results (% are mass fractions)
| Item | Purity of product (BaSO) 4 Meter) | Fluorite content (CaF) 2 Meter) | Content of rare earth REO |
| Example 1 | 97.5％ | 0.42％ | 0.18％ |
| Example 2 | 96.0％ | 0.50％ | 0.20％ |
| Example 3 | 97.8％ | 0.33％ | 0.16％ |
As shown in Table 1, the method of the invention can ensure that the purity of the barite concentrate is more than 96%, the content of fluorite is less than 0.5%, the content of rare earth is less than 0.2%, the whole process flow is not complex, the production cost is low, the technical advantages are obvious, the requirements of high-end markets are met, and considerable production profits are provided for enterprises.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (4)
1. A method for purifying barite and recovering rare earth from barite concentrate is characterized by comprising the following steps:
s1, acid leaching barite concentrate by using hydrochloric acid, wherein the concentration of the hydrochloric acid is 5-7mol/L, heating the hydrochloric acid to 80 ℃ during acid leaching, wherein the acid leaching time is not less than 20min, and then filtering acid leaching solution to obtain a precipitate;
s2, washing the precipitate with hot water until the pH value is not less than 6 to obtain acid leaching ore;
s3, carrying out oxidizing roasting on the acid leached ore at the roasting temperature of 400-500 ℃ to obtain roasted ore;
s4, acid leaching the roasted ore by using dilute sulfuric acid, wherein the mass fraction of the dilute sulfuric acid is 3-6%, the acid leaching temperature of the dilute sulfuric acid is 70-90 ℃, the acid leaching time is not less than 20min, and then filtering is carried out to obtain leaching material liquid and leaching ore;
s5, recycling the leaching material liquid as rare earth sulfate material liquid, washing and drying the leaching ore to obtain a barite product, wherein the content of barium sulfate in the barite product is not less than 96%, and the content of rare earth is less than 0.2%.
2. The method of purifying barite and recovering rare earths from barite concentrate as claimed in claim 1, wherein the roasting time is 1-3 hours at the time of oxidizing roasting.
3. The method for purifying barite and recovering rare earth from barite concentrate as claimed in claim 1, wherein in S1, the generated white fume is absorbed by water to obtain a hydrofluoric acid solution with a certain concentration, the hydrofluoric acid solution is mixed with the acid leaching solution generated in S1, the filter residue is filtered and recovered as crude fluorite.
4. The method for purifying barite and recovering rare earth from barite concentrate as claimed in claim 1, wherein in S4, the generated white fume is absorbed by water to obtain a hydrofluoric acid solution with a certain concentration, the hydrofluoric acid solution is mixed with the acid leaching solution generated in S1, and the filter residue is filtered and recovered as crude fluorite.
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| CN115821077A (en) * | 2022-11-29 | 2023-03-21 | 包头稀土研究院 | Method for obtaining rare earth chloride by using fluorite concentrate as initial raw material |
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| CN209317889U (en) * | 2018-11-01 | 2019-08-30 | 四川江铜稀土有限责任公司 | A kind of fluorine carbon cerium type rare earth weight magnetic tailing recycling production system |
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Address after: 615600 Rare Earth Industrial Park, Fuxing Town, Mianning County, Liangshan Yi Autonomous Prefecture, Sichuan Province Patentee after: Zhongxi (Liangshan) Rare Earth Co.,Ltd. Address before: 615600 Rare Earth Industrial Park, Fuxing Town, Mianning County, Liangshan Yi Autonomous Prefecture, Sichuan Province Patentee before: SICHUAN JCC RARE EARTH METALS CO.,LTD. |