CN102277484A - Method for separating and recovering sodium phosphate and sodium fluoride in mixed rare earth concentrate smelting process through alkaline method - Google Patents
Method for separating and recovering sodium phosphate and sodium fluoride in mixed rare earth concentrate smelting process through alkaline method Download PDFInfo
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Abstract
The invention relates to a method for separating and recovering sodium phosphate and sodium fluoride in a mixed rare earth concentrate smelting process through an alkaline method. The method is characterized in that after calcining, acid leaching and alkaline decomposition of mixed rare earth concentrate, the product after alkaline decomposition is washed to obtained a washing liquid, sodium phosphate and sodium fluoride are separated and recovered from the washing liquid, and the efficient utilization of sodium hydroxide is realized. The countercurrent washing manner is adopted for washing, and the crystals of sodium phosphate and sodium fluoride and excessive sodium hydroxide solution or crystals are successively obtained after three steps of heating crystallization, cooling crystallization and concentration. No other impurity is added in the whole process, the production of three wastes does not occur, the recovery cost is low, less water is used, the waste is changed into the valuable, the stability is extremely high, and the recovery of phosphorus and fluorine in the mixed rare earth concentrate smelting process is thoroughly realized.
Description
Technical field
The present invention relates to the Separation and Recovery of sodium phosphate, Sodium Fluoride in the separation and recovery method, particularly rare-earth smelting process of sodium phosphate, Sodium Fluoride in a kind of mixed rare earth concentrates alkaline process smelting technology, belong to hydrometallurgy and comprehensive utilization of waste materials field.
Background technology
At present rare earth is as China's important strategic resource very, more and more important roles of aspect performer such as aerospace, military affairs, material, machinery, chemical industry.From the rare earth reserve distribution, the rare-earth mineral of China mainly is distributed in the Bayan Obo ore body of packet header, and this rare-earth mineral mainly is that the form with hamartite and monazite mixing ore deposit exists, and belongs to typical difficult choosing, the difficult mineral of smelting.In ore dressing and smelting process, there are problems such as rare earth yield is low, other valuable element is difficult to recycle, three-waste pollution is serious always.Yet these problems are along with rare earth resources is fewer and feweri, and environmental protection requirement and consciousness more and more higher has been subjected to that people are increasing to be paid attention to and pay close attention to.
Concentrated sulfuric acid roasting is the topmost method of mishmetal mining and metallurgy refining, this method is stronger to the adaptability of rare-earth mineral, can stably produce rare earth compound, but this technology also exists serious problem: 1, three-waste pollution is too serious, the ecotope around having had a strong impact on; 2, produce the tailings of a large amount of thorium pyrophosphates, this slag radioactivity height also is difficult to utilize again, seals up for safekeeping so can only transfer to environmental administration's appointment, and must pay high storage cost; 3, a lot of useful elements lose in vain with the form of the three wastes in the mineral, but also have increased the expense that is used for environmental protection.
Reason for environment protection and utilization of resources; we have researched and developed out a kind of new mixed rare earth concentrates ore dressing, have smelted process integration; use this technology to produce rare earth compound stability and high efficiency, and in the middle of the very fast production practice with the mishmetal ore deposit, packet header that uses of this technology.
The present invention is just on the basis of this novel process, the water lotion of alkali decomposition mineral in this technology is carried out the Separation and Recovery of useful element, Separation and Recovery has obtained Sodium Fluoride and two kinds of products of sodium phosphate, reduced the cost of rare-earth smelting process, realized the comprehensive utilization of resource, the more important thing is the thorough three-waste pollution problem of having improved, for a new road has been opened up in the thorough reform of mishmetal smelting technology.
Summary of the invention
The object of the present invention is to provide the separation and recovery method of sodium phosphate, Sodium Fluoride in a kind of mixed rare earth concentrates alkaline process smelting technology, this method is Separation and Recovery sodium phosphate, Sodium Fluoride and sodium hydroxide effectively, and having realized the comprehensive reutilization of resource, technical process is simple, production cost is low, pollution-free.
Purpose of the present invention is realized by following processing step.
(1) roasting: at first to the mixed rare earth concentrates roasting, 450～550 ℃ of maturing temperatures, roasting time 30～120 minutes.
(2) acidleach: adopt concentrated hydrochloric acid to leach roasted ore, concentration of hydrochloric acid 5～12mol/L, the consumption of hydrochloric acid: mixed rare earth concentrates quality: concentrated hydrochloric acid quality=1: 1.8～2.8, extraction temperature are 60～95 ℃, 0.5～2.5 hour time, obtain acid leaching residue and pickling liquor.In the leaching process, adopt thiocarbamide to make reductive agent, the adding quality of thiocarbamide is 0.05～0.1 times of ore quality.
(3) alkali decomposes: the hydro-oxidation sodium solution carries out the alkali decomposition in the acid leaching residue after hydrochloric acid leaches, and the sodium hydroxide solution mass concentration is 40～90%, and the alkali decomposition temperature is 130～230 ℃, 0.5～1.5 hour time.
(4) washing: the mineral after the alkali decomposition are washed, and the washing slag is used for the recovery of rare earth, and water lotion is used for Separation and Recovery sodium phosphate and Sodium Fluoride, and realizes effective utilization of sodium hydroxide.The mode of adverse current washing is adopted in washing, 4～6 grades of countercurrent washings, 50～90 ℃ of water temperatures, the quality of water lotion are 3～10 times of mixed rare earth concentrates quality, clear water drip washing is adopted in the last step washing, to the pH of water lotion be 7～9.
(5) evaporative crystallization: the first step water lotion heating evaporation during to countercurrent washing, Heating temperature is 60～100 ℃, when the quality that is evaporated to water lotion is 0.7～6.5 times of mixed rare earth concentrates quality, crystallization occurs, filtered and recycled crystallisate, this crystallisate are Sodium Fluoride.
(6) condensation-crystallization: the evaporative crystallization filtrate filtered is lowered the temperature, and temperature is 10～55 ℃, makes it crystallization occur, and this crystallisate of filtered and recycled, this crystallisate are sodium phosphate.
(7) concentrate: the liquid after condensation-crystallization is filtered further heating concentrates, and thickening temperature is at 65 ℃-100 ℃, and the quality that is concentrated into concentrated solution is below 1 times of mixed rare earth concentrates quality.Spissated liquid is sodium hydroxide solution, the diluent of sodium hydroxide when decomposing mineral as alkali, condensation or further evaporation prepare solid hydroxide.
Notable feature of the present invention is: a kind of technology of alkaline process decomposing Baotou rare earth ore concentrate and from the water lotion of the alkali decomposition step of this technology Separation and Recovery obtain sodium phosphate and Sodium Fluoride, realize effective utilization of sodium hydroxide, the two kinds of elements of phosphorus, fluorine that utilize the present invention to reclaim effectively to produce in the mixed rare earth concentrates smelting process; The technology stability height, stably Separation and Recovery goes out Sodium Fluoride, two kinds of materials of sodium phosphate; The most important thing is that whole technology do not introduce other impurity, also do not have three wastes problem.
The present invention is suitable for the Separation and Recovery of sodium phosphate, Sodium Fluoride in the mixed rare earth concentrates alkaline process smelting technology, also is suitable for the sodium phosphate in the alkaline process process, the Separation and Recovery of Sodium Fluoride in other smelting technology of mixed rare earth concentrates.
Embodiment
Below by specific embodiment technical scheme of the present invention is described in detail, but content of the present invention not only is confined to the following examples.
Embodiment 1
(1) to the REO grade is 65.42% mixed rare earth concentrates roasting, 500 ℃ of maturing temperatures, roasting time 60 minutes.
(2) roasted ore is adopted hydrochloric acid leach, concentration of hydrochloric acid 7mol/L, the consumption of hydrochloric acid: mixed rare earth concentrates quality: concentrated hydrochloric acid quality=1: 2.0, extraction temperature are 95 ℃, 1.5 hours time, get acid leaching residue and pickling liquor.In the leaching process, adopt thiocarbamide to make reductive agent, the adding quality of thiocarbamide is 0.055 times of mixed rare earth concentrates quality.
(3) the hydro-oxidation sodium solution carries out the alkali decomposition in the acid leaching residue after hydrochloric acid leaches, and the sodium hydroxide solution mass concentration is 50%, and the alkali decomposition temperature is 150 ℃, 1.5 hours time.
(4) repeat to do 7 batch mixings continuously by above-mentioned steps and close rare earth ore concentrate, obtain 7 batches of alkali and decompose mineral, these 7 batches of alkali are decomposed mineral carry out the continuous countercurrent washing, the adverse current washing progression of every batch of alkali decomposition mineral is 5 times, and the concrete steps of adverse current washing are:
1) first alkali is decomposed mineral and adopt general industry water continuous washing 5 times, respectively the 1st water lotion, the 2nd water lotion, the 3rd water lotion, the 4th water lotion, the 5th water lotion, the 1st water lotion preserved be used for Separation and Recovery Sodium Fluoride, sodium phosphate;
2) decompose 1st water lotion of the 2nd water lotion of mineral with first alkali as second batch of alkali decomposition mineral, the 3rd water lotion that decomposes mineral with first alkali decomposes the 2nd water lotion of mineral as second batch of alkali, by that analogy, the 5th water lotion of second batch of alkali decomposition mineral adopts the general industry water;
3) continuously all the other five batches of alkali are decomposed mineral by above-mentioned counter-flow water washing method and wash, obtain the water lotion first time that seven batches of alkali decompose mineral.
The volume of water lotion is 10 times that alkali decomposes mineral, and temperature is 75 ℃, and the pH of the last step water lotion of every batch of alkali decomposition mineral is 8.5, then these 7 batches of alkali is decomposed first step water lotion merging the carrying out Separation and Recovery Sodium Fluoride and the sodium phosphate operation of mineral.At first heating evaporation crystallization, temperature is 90 ℃, is evaporated to volume and is when alkali decomposes 2.2 times of mineral to filter immediately, the filtrate that obtains is the crystallisate of Sodium Fluoride.And then carry out condensation-crystallization, temperature is 25 ℃, filters the crystallisate that obtains sodium phosphate, at last the liquid of condensation-crystallization after-filtration is dried the solids that obtains based on sodium hydroxide.
The purity of the Sodium Fluoride that obtains by analysis is 96.1%, and its rate of recovery is 92.2%; The purity of sodium phosphate is 95.7%, and the rate of recovery is 94.5%.
Embodiment 2
(1) to REO is 55.20% mixed rare earth concentrates roasting, 540 ℃ of maturing temperatures, roasting time 30 minutes.
(2) roasted ore is adopted hydrochloric acid leach, concentration of hydrochloric acid 7mol/L, the consumption of hydrochloric acid: mixed rare earth concentrates quality: concentrated hydrochloric acid quality=1: 2.8, extraction temperature are 75 ℃, 1 hour time.In the leaching process, adopt thiocarbamide to make reductive agent, the adding quality of thiocarbamide is 0.075 times of ore quality.
(3) the hydro-oxidation sodium solution carries out the alkali decomposition in the acid leaching residue after hydrochloric acid leaches, and the sodium hydroxide solution mass concentration is 75%, and the alkali decomposition temperature is 200 ℃, 1.2 hours time.
(4) repeat to do 9 batch mixings continuously by above-mentioned steps and close rare earth ore concentrate, obtain 9 batches of alkali and decompose mineral, these 9 batches of alkali are decomposed mineral carried out the continuous countercurrent washing, the method for adverse current washing is identical with embodiment's 1.The adverse current washing progression of every batch of alkali decomposition mineral is 4 grades, the volume of water lotion is 4 times that alkali decomposes mineral, temperature is 88 ℃, the pH of the last step water lotion of every batch of alkali decomposition mineral is 7.2, then these 9 batches of alkali is decomposed first step water lotion merging the carrying out Separation and Recovery Sodium Fluoride and the sodium phosphate operation of mineral.At first heating evaporation crystallization, temperature is 78 ℃, is evaporated to volume and is when alkali decomposes 3.4 times of mineral to filter immediately, the filtrate that obtains is the crystallisate of Sodium Fluoride.And then carry out condensation-crystallization, temperature is 18 ℃, filters the crystallisate that obtains sodium phosphate, at last the liquid of condensation-crystallization after-filtration is dried the solids that obtains based on sodium hydroxide.The purity of the Sodium Fluoride that obtains by analysis is 95.4%, and its rate of recovery is 93.6%; The purity of sodium phosphate is 94.8%, and the rate of recovery is 96.8%.
Embodiment 3
(1) to REO is 67.75% mixed rare earth concentrates roasting, 480 ℃ of maturing temperatures, roasting time 90 minutes.
(2) roasted ore is adopted hydrochloric acid leach, concentration of hydrochloric acid 10mol/L, the consumption of hydrochloric acid: mixed rare earth concentrates quality: concentrated hydrochloric acid quality=1: 2.2, extraction temperature are 80 ℃, 2.5 hours time.In the leaching process, adopt thiocarbamide to make reductive agent, the adding quality of thiocarbamide is 0.095 times of ore quality.
(3) the hydro-oxidation sodium solution carries out the alkali decomposition in the acid leaching residue after hydrochloric acid leaches, and the sodium hydroxide solution mass concentration is 50%, and the alkali decomposition temperature is 230 ℃, 0.5 hour time.
(4) repeat to do 11 batch mixings continuously by above-mentioned steps and close rare earth ore concentrate, obtain 11 batches of alkali and decompose mineral, these 11 batches of alkali are decomposed mineral carried out the washing of successive adverse current, the method for adverse current washing is identical with embodiment's 1.The adverse current washing progression of every batch of alkali decomposition mineral is 6 grades, and the volume of water lotion is 6 times that alkali decomposes mineral, 78 ℃ of temperature, and the pH of the last step water lotion of every batch of alkali decomposition mineral is 7.5.First step water lotion to every batch of alkali decomposition mineral carries out evaporative crystallization, condensation-crystallization and spissated operation successively then, and the temperature of every batch of evaporative crystallization and liquor capacity and alkali decompose the multiple such as the following table 1 of mineral quality.
Table 1
The Sodium Fluoride that obtains of these 11 batches of evaporative crystallization after-filtration merges the most at last, and recording its purity is 96.2%, and the rate of recovery is 93.8%.
And then carry out condensation and tie the temperature of every batch of condensation-crystallization such as following table 2.
Table 2
The sodium phosphate that obtains of these 11 batches of condensation-crystallization after-filtration merges the most at last, and recording its purity is 94.5%, and the rate of recovery is 94.6%.
In enrichment step, every batch of spissated volume is 0.5 times that alkali decomposes mineral quality, the diluent of sodium hydroxide when this concentrated solution decomposes mineral as alkali successively.
Embodiment 4
(1) to REO is 63.02% mixed rare earth concentrates roasting, 460 ℃ of maturing temperatures, roasting time 120 minutes.
(2) roasted ore is adopted hydrochloric acid leach, concentration of hydrochloric acid 9mol/L, the consumption of hydrochloric acid: mixed rare earth concentrates quality: concentrated hydrochloric acid quality=1: 2.4, extraction temperature are 85 ℃, 1 hour time.In the leaching process, adopt thiocarbamide to make reductive agent, the adding quality of thiocarbamide is 0.065 times of ore quality.
(3) the hydro-oxidation sodium solution carries out the alkali decomposition in the acid leaching residue after hydrochloric acid leaches, and the sodium hydroxide solution mass concentration is 80%, and the alkali decomposition temperature is 190 ℃, 0.8 hour time.
(4) repeat to do 6 batch mixings continuously by above-mentioned steps and close rare earth ore concentrate, obtain 6 batches of alkali and decompose mineral, these 6 batches of alkali are decomposed mineral carried out the washing of successive adverse current, the method for adverse current washing is identical with embodiment's 1.The adverse current washing progression of every batch of alkali decomposition mineral is 5 grades, and the volume of every grade of water lotion is 9 times that alkali decomposes mineral, 80 ℃ of temperature, and the pH of the last step water lotion of every batch of alkali decomposition mineral is 7.8.First step water lotion to every batch of alkali decomposition mineral carries out evaporative crystallization, condensation-crystallization and spissated operation successively then, and the temperature of every batch of evaporative crystallization and liquor capacity and alkali decompose the multiple such as the following table 3 of mineral quality.
Table 3
The Sodium Fluoride that obtains of these 6 batches of evaporative crystallization after-filtration merges the most at last, and recording its purity is 93.1%, and the rate of recovery is 91.5%.And then carry out condensation and tie the temperature of every batch of condensation-crystallization such as following table 4.
Table 4
The sodium phosphate that obtains of these 6 batches of condensation-crystallization after-filtration merges the most at last, and recording its purity is 93.7%, and the rate of recovery is 92.4%.
In enrichment step, the liquid after all condensation-crystallization filtrations is merged, dry, obtain the solids of sodium hydroxide.
Claims (1)
1. the separation and recovery method of sodium phosphate, Sodium Fluoride in the mixed rare earth concentrates alkaline process smelting technology is characterized in that method steps is as follows:
(1) roasting: at first to the mixed rare earth concentrates roasting, 450～600 ℃ of maturing temperatures, roasting time 30～120 minutes;
(2) acidleach: adopt hydrochloric acid to leach roasted ore, concentration of hydrochloric acid 5～12mol/L, the consumption of hydrochloric acid are the mixed rare earth concentrates quality: concentrated hydrochloric acid quality=1: 1.8～2.8, extraction temperature are 60～95 ℃, 0.5～2.5 hour time, obtain acid leaching residue and pickling liquor; In the leaching process, adopt thiocarbamide to make reductive agent, the adding quality of thiocarbamide is 0.05～0.1 times of mixed rare earth concentrates quality;
(3) alkali decomposes: the hydro-oxidation sodium solution carries out the alkali decomposition in the acid leaching residue after hydrochloric acid leaches, and the sodium hydroxide solution mass concentration is 40～90%, and the alkali decomposition temperature is 150～250 ℃, 0.5～1.5 hour time;
(4) washing: the mineral after the alkali decomposition are washed, the washing slag is used for the recovery of rare earth, water lotion is used for Separation and Recovery sodium phosphate and Sodium Fluoride, the mode of adverse current washing is adopted in washing, 4～6 grades of countercurrent washings, 50～90 ℃ of water temperatures, the quality of water lotion are 3～10 times of mixed rare earth concentrates quality, clear water drip washing is adopted in last step washing, to the pH of water lotion be 7～9;
(5) evaporative crystallization: the first step water lotion heating evaporation during to countercurrent washing, Heating temperature is 60～100 ℃, when the quality that is evaporated to water lotion is 0.7～6.5 times of mixed rare earth concentrates quality, crystallization occurs, filtered and recycled crystallisate, this crystallisate are Sodium Fluoride;
(6) condensation-crystallization: the evaporative crystallization filtrate filtered is lowered the temperature, and temperature is 10～55 ℃, makes it crystallization occur, and this crystallisate of filtered and recycled, this crystallisate are sodium phosphate;
(7) concentrate: the liquid after condensation-crystallization is filtered further heating concentrates, thickening temperature is at 65～100 ℃, the quality that is concentrated into concentrated solution is below 1 times of mixed rare earth concentrates quality, spissated liquid is sodium hydroxide solution, the diluent of sodium hydroxide when decomposing mineral as alkali, or condensation or further evaporation prepare solid hydroxide.
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Cited By (12)
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| CN102643992A (en) * | 2012-04-19 | 2012-08-22 | 五矿（北京）稀土研究院有限公司 | Method for recovering rare-earth waste material |
| CN103045851A (en) * | 2013-01-17 | 2013-04-17 | 中国科学院长春应用化学研究所 | Technique for decomposing Baotou rare-earth ores |
| CN104404243A (en) * | 2014-12-12 | 2015-03-11 | 钢研集团稀土科技有限公司 | Method for low-temperature decomposition of low-grade Weishan rare earth ore concentrate through acid-alkali combination |
| CN104593622A (en) * | 2014-12-29 | 2015-05-06 | 乐山盛和稀土股份有限公司 | Technology for obtaining cerium enrichment with a partition larger than 99% by optimal extraction of fluoride carbonate rare earths by hydrochloric acid |
| CN104591247A (en) * | 2015-01-09 | 2015-05-06 | 东北大学 | Method for fluorine recovery from bastnaesite by alkali pulp countercurrent washing |
| WO2016090742A1 (en) * | 2014-12-09 | 2016-06-16 | 化工部长沙设计研究院 | Method for producing dense soda ash by removing fluorine from fluorine-containing trona |
| CN106586992A (en) * | 2016-12-10 | 2017-04-26 | 包头稀土研究院 | Comprehensive fluorine and phosphorous recovery technology for liquid caustic soda decomposition of mixed rare earth concentrate |
| CN110512098A (en) * | 2019-08-29 | 2019-11-29 | 包头钢铁（集团）有限责任公司 | A kind of method that bastnaesite wet process prepares rare earth chloride |
| CN111540973A (en) * | 2020-04-14 | 2020-08-14 | 安徽南都华铂新材料科技有限公司 | Resource utilization method of waste gas in waste lithium ion battery recovery process |
| CN112725642A (en) * | 2020-12-18 | 2021-04-30 | 四川省乐山锐丰冶金有限公司 | Method for recycling sodium hydroxide and co-producing sodium fluoride from fluorine carbon cerium alkali conversion process |
| CN112941304A (en) * | 2021-01-27 | 2021-06-11 | 赣州求真科技有限公司 | Rare earth roasting method |
| CN114162796A (en) * | 2021-12-09 | 2022-03-11 | 宁波行殊新能源科技有限公司 | Method for recycling and regenerating phosphate waste |
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| CN102643992A (en) * | 2012-04-19 | 2012-08-22 | 五矿（北京）稀土研究院有限公司 | Method for recovering rare-earth waste material |
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| CN103045851A (en) * | 2013-01-17 | 2013-04-17 | 中国科学院长春应用化学研究所 | Technique for decomposing Baotou rare-earth ores |
| WO2016090742A1 (en) * | 2014-12-09 | 2016-06-16 | 化工部长沙设计研究院 | Method for producing dense soda ash by removing fluorine from fluorine-containing trona |
| CN104404243A (en) * | 2014-12-12 | 2015-03-11 | 钢研集团稀土科技有限公司 | Method for low-temperature decomposition of low-grade Weishan rare earth ore concentrate through acid-alkali combination |
| CN104404243B (en) * | 2014-12-12 | 2016-07-20 | 钢研集团稀土科技有限公司 | A kind of method of soda acid associating low-temperature decomposition low-grade Weishan rare earth ore concentrate |
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| CN104591247A (en) * | 2015-01-09 | 2015-05-06 | 东北大学 | Method for fluorine recovery from bastnaesite by alkali pulp countercurrent washing |
| CN106586992A (en) * | 2016-12-10 | 2017-04-26 | 包头稀土研究院 | Comprehensive fluorine and phosphorous recovery technology for liquid caustic soda decomposition of mixed rare earth concentrate |
| CN106586992B (en) * | 2016-12-10 | 2019-01-15 | 包头稀土研究院 | A kind of technique of the recycling of mixed rare earth concentrates liquid alkaline Decomposition-Synthesis fluorine and phosphorus |
| CN110512098A (en) * | 2019-08-29 | 2019-11-29 | 包头钢铁（集团）有限责任公司 | A kind of method that bastnaesite wet process prepares rare earth chloride |
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| CN112725642A (en) * | 2020-12-18 | 2021-04-30 | 四川省乐山锐丰冶金有限公司 | Method for recycling sodium hydroxide and co-producing sodium fluoride from fluorine carbon cerium alkali conversion process |
| CN112941304A (en) * | 2021-01-27 | 2021-06-11 | 赣州求真科技有限公司 | Rare earth roasting method |
| CN112941304B (en) * | 2021-01-27 | 2022-07-15 | 赣州求真科技有限公司 | Rare earth roasting method |
| CN114162796A (en) * | 2021-12-09 | 2022-03-11 | 宁波行殊新能源科技有限公司 | Method for recycling and regenerating phosphate waste |
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