CN106586992A - Comprehensive fluorine and phosphorous recovery technology for liquid caustic soda decomposition of mixed rare earth concentrate - Google Patents
Comprehensive fluorine and phosphorous recovery technology for liquid caustic soda decomposition of mixed rare earth concentrate Download PDFInfo
- Publication number
- CN106586992A CN106586992A CN201611134251.4A CN201611134251A CN106586992A CN 106586992 A CN106586992 A CN 106586992A CN 201611134251 A CN201611134251 A CN 201611134251A CN 106586992 A CN106586992 A CN 106586992A
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- caustic soda
- fluorine
- liquid
- rare earth
- mixed rare
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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
- C01D3/02—Fluorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/305—Preparation from phosphorus-containing compounds by alkaline treatment
-
- 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
- C01D3/14—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention relates to a comprehensive fluorine and phosphorous recovery technology for liquid caustic soda decomposition of mixed rare earth concentrate. The comprehensive fluorine and phosphorous recovery technology is characterized by including mixing the high-grade mixed rare earth concentrate with a 60wt% sodium hydroxide solution according to a weight ratio of 1:3.5-7.5, reacting for 0.2-1 hour at 150-160 DEG C, conducting hot filtration at 80 DEG C to obtain strong liquid caustic soda and caustic soda cakes, cooling the strong liquid caustic soda to 30-70 DEG C and filtering so as to obtain a sodium phosphate product; mixing the caustic soda cakes into paste prior to washing, and filtering so as to obtain primary caustic soda washed liquid; continuing washing the caustic soda cakes until the caustic soda cakes become neutral, dissolving the neutral caustic soda cakes with 6-10 mol/L hydrochloric acid, and controlling a pH value to be 4-5 so as to obtain a rare earth chloride solution; concentrating the primary caustic soda washed liquid, and filtering so as to obtain a sodium fluoride product. The comprehensive fluorine and phosphorous recovery technology has the advantages that the comprehensive fluorine and phosphorous recovery technology is short in technological process and low in production energy consumption; fluorine and phosphorous recovery and cyclic utilization of liquid caustic soda are achieved, wastewater discharge is avoided, and clean production and comprehensive resource utilization are achieved.
Description
Technical field
The present invention relates to a kind of mixed rare earth concentrates liquid caustic soda Decomposition-Synthesis reclaim the technique of fluorine and phosphorus, particularly rare-earth smelting
During sodium phosphate, the separation and recovery of sodium fluoride, belong to hydrometallurgy and comprehensive utilization of resources field.
Background technology
Mixed rare earth concentrates account for more than 60% that China smelts rare earth ore concentrate, are the primary raw materials of Extraction of rare earth element, concentrate
In also have the scarce resource such as fluorine, phosphorus in addition to rare earth.Decompose the acid technological process of mixed rare earth concentrates at present, fluorine is from high-temperature roasting tail gas
Middle discharge, is not easily recycled；Phosphorus is entered in radioactivity leached mud, it is impossible to recycled.
In decomposing the alkali process of mixed rare earth concentrates, concentrate washes excess base and the fluorination for generating Jing after liquid caustic soda decomposition
The soluble salts such as sodium, sodium phosphate, fluorine and phosphorus are entered in soda liquid.Soda liquid or with lime " causticization " reclaim NaOH, fluorine and
Phosphorus becomes waste residue.Or soda liquid directly also becomes waste sludge discharge with acid neutralization to neutral discharge, fluorine and phosphorus.Chinese patent is " mixed
Close sodium phosphate, the separation and recovery method of sodium fluoride in rare earth ore concentrate alkaline process smelting process "（CN 102277484 A）Invent one
Plant acid and alkali combination method to process in mixed rare earth concentrates technique, the method that sodium fluoride and sodium phosphate are reclaimed from soda liquid.The method
Mainly the mineral after caustic digestion are carried out with adverse current washing, 4 ~ 6 grades of countercurrent washing, 50～90 DEG C of water temperature, the matter of water lotion
Measure as 3 ~ 10 times of mixed rare earth concentrates quality., there is crystallization and filtration and returns in the water lotion heating evaporation gone out to countercurrent washing
Receipts crystal is sodium fluoride；Carry out cooling to temperature to the filtrate after filtration for 10～55 DEG C so as to crystallization occur, filter back
The crystal is received for sodium phosphate.
The content of the invention
It is an object of the invention to solve rare earth ore concentrate liquid caustic soda and decompose the separation of sodium fluoride and sodium phosphate in industrial production, return
Receipts problem, shortened process simultaneously realizes the high efficiente callback of the resources such as fluorine and phosphorus, there is provided a kind of technological process is simple, production cost
The technique that low, free of contamination mixed rare earth concentrates liquid caustic soda Decomposition-Synthesis reclaim fluorine and phosphorus.
To realize the purpose of the present invention, a kind of mixed rare earth concentrates liquid caustic soda Decomposition-Synthesis that the present invention is provided reclaim fluorine and phosphorus
Technique comprise the following steps：
[1] the high-grade mixed rare earth concentrates and concentration by REO more than 60 wt %>60wt% sodium hydroxide solutions press mischmetal
Concentrate and NaOH weight compare 1：3.5 ~ 7.5 ratio is mixed, and mixed slurry reacts 0.2 ~ 1 at 150 DEG C ~ 160 DEG C
Hour；
[2] heat filtering is carried out at a temperature of more than 80 DEG C after the completion of reacting, high alkali liquid and alkali cake is filtrated to get, high alkali liquid is cooled to
30 DEG C ~ 70 DEG C, then carry out being filtrated to get sodium phosphate product；
[3] the alkali cake water pulp washing that step [2] is obtained, solid-to-liquid ratio is controlled 1:1 ~ 3, it is filtrated to get a soda liquid；Alkali
Cake continues to wash to neutrality, and the alkali cake for washing neutrality is dissolved with the hydrochloric acid of 6 ~ 10mol/L, controls pH 4 ~ 5, obtains pure
Re chloride；
[4] the soda liquid that step [3] is obtained is concentrated, and is concentrated to the 1/5 ~ 1/10 of original volume, is filtrated to get sodium fluoride
Product.
Above-mentioned steps（1）In, high-grade mischmetal ore deposit is preferably 1 with the mixed proportion of NaOH：4.0~6.0.Carry
High ore deposit alkali ratio can improve system mobility, change system alkali concn little, and reaction temperature is easily controllable, and the reaction time is short.Hydrogen
The concentration of sodium hydroxide solution is 60 wt % ~ 70 wt %, and improving concentration of sodium hydroxide solution can improve the decomposition temperature of system
Degree, reduces the reaction time, obtains high rare-earth mineral resolution ratio.Described decomposition reaction can be continuous in reactor or pipeline
Carry out, it is also possible to intermittently carry out in reactor.
Above-mentioned steps（2）In, heat filtering temperature is not less than 60 DEG C preferably, preferably 80 DEG C ~ 110 DEG C.The too low hydroxide of temperature
Sodium easily crystallizes precipitation, makes filtration difficulty and concentration of lye is reduced being unfavorable for the recovery of alkali and recycled, and temperature is crossed high filtration and set
Standby service life is reduced.Described heat filtering can be carried out continuously on the equipment such as disk filter, it is also possible in plate-frame filtering
Intermittently carry out on machine.
Above-mentioned steps（2）In, high alkali liquid preferably cools to 40 DEG C ~ 50 DEG C and carries out being filtrated to get sodium phosphate product again.
Above-mentioned steps（3）In, alkali cake uses water pulp washing, solid-to-liquid ratio to be preferably controlled in 1:1.5 ~ 2.0, it is filtrated to get once
Soda liquid is used to reclaim sodium fluoride.
Above-mentioned steps（2）In, the alkali lye and water after filtration is configured to sodium hydroxide solution and is back to use circulation in step [1] to make
With the supplementary NaOH for consuming.
Above-mentioned steps（4）In, the mother liquor being filtrated to get is back to use in [1] and recycles.
It is an advantage of the invention that：The present invention is anti-using the high-concentration caustic soda liquid that rare earth ore concentrate is carried out under the conditions of high alkali ore deposit ratio
Should, heat filtering is directly carried out after the completion of reaction and realizes that fluorine and phosphorus are separated, the isolated sodium phosphate of high alkali liquid cooling；Alkali cake is with little
Solid-to-liquid ratio is washed, and then condensing crystallizing obtains sodium fluoride, is realized the separation of sodium fluoride and sodium phosphate in alkali decomposition process, is returned
Receive, technological process is short, and energy consumption is substantially reduced, be a real efficient resource comprehensive utilization process.
Description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Specific embodiment
Technical scheme provided by the present invention is explained in detail with reference to embodiment, but not as to the claims in the present invention
The restriction of protection domain.
Embodiment 1：
Take 500g NaOH and be made into 65wt% solution, add 100g mischmetal ore deposits（REO 65wt%）, in reactor after mixing
In be heated to 155 DEG C, insulation reaction stops cooling to 110 DEG C of temperature after reaction, and heat filtering obtains high alkali liquid and alkali cake, then
With a small amount of hot water drip washing, it is ensured that system temperature is more than 80 DEG C after filtration.High alkali liquid continues to cool to 45 DEG C, refilters and obtains phosphoric acid
Sodium product.Alkali lye is added to be followed after the NaOH for consuming and badly used after filtration, adds 100g mischmetal ore deposits（REO 65wt%）
Carry out second cyclic test.Alkali cake adds 150mL water agitator treatings, is filtrated to get a soda liquid.Alkali cake is further continued for washing
To neutral, then with the dissolving with hydrochloric acid of 9M, control pH value of solution=4 ~ 5 obtain re chloride.Soda liquid heating is concentrated to
About 30mL, is cooled to room temperature and is filtrated to get sodium fluoride product.5 cyclic tests the results are shown in Table 1.
。
Embodiment 2：
Take 450g NaOH and be made into 65wt% solution, add 100g mischmetal ore deposits（REO 65wt%）, in reactor after mixing
In be heated to 150 DEG C, then insulation reaction stops reaction and cools to 110 DEG C of temperature, filters while hot, obtains high alkali liquid and alkali cake,
Then with a small amount of hot water drip washing, it is ensured that system temperature is more than 80 DEG C after filtration.High alkali liquid continues to cool to 50 DEG C, refilters and obtains
Sodium phosphate product.Alkali lye is added to be followed after the NaOH for consuming and badly used after filtration, adds 100g mischmetal ore deposits（REO
65wt%）Carry out second cyclic test.Alkali cake adds 200mL water agitator treatings, is filtrated to get a soda liquid.Alkali cake followed by
Continuous to be washed to neutrality, then with the dissolving with hydrochloric acid of 9M, control pH value of solution=4 ~ 5 obtain re chloride.Soda liquid heating
About 30mL is concentrated to, room temperature is cooled to and is filtrated to get sodium fluoride product.5 cyclic tests the results are shown in Table 2.
。
Claims (7)
1. a kind of mixed rare earth concentrates liquid caustic soda Decomposition-Synthesis reclaim the technique of fluorine and phosphorus, it is characterized in that：Comprise the following steps：
[1] the high-grade mixed rare earth concentrates and concentration by REO more than 60 wt %>60wt% sodium hydroxide solutions press mischmetal
Concentrate and NaOH weight compare 1：3.5 ~ 7.5 ratio is mixed, and mixed slurry reacts 0.2 ~ 1 at 150 DEG C ~ 160 DEG C
Hour；
[2] heat filtering is carried out at a temperature of more than 80 DEG C after the completion of reacting, high alkali liquid and alkali cake is filtrated to get, high alkali liquid is cooled to
30 DEG C ~ 70 DEG C, then carry out being filtrated to get sodium phosphate product；
[3] the alkali cake water pulp washing that step [2] is obtained, solid-to-liquid ratio is controlled 1:1 ~ 3, it is filtrated to get a soda liquid；Alkali
Cake continues to wash to neutrality, and the alkali cake for washing neutrality is dissolved with the hydrochloric acid of 6 ~ 10mol/L, controls pH 4 ~ 5, obtains pure
Re chloride；
[4] the soda liquid that step [3] is obtained is concentrated, and is concentrated to the 1/5 ~ 1/10 of original volume, is filtrated to get sodium fluoride
Product.
2. mixed rare earth concentrates liquid caustic soda Decomposition-Synthesis according to claim 1 reclaim the technique of fluorine and phosphorus, it is characterized in that：Step
Suddenly（1）In, high-grade mischmetal ore deposit is 1 with the mixed proportion of NaOH：4.0 ~ 6.0, the concentration of sodium hydroxide solution is
60 wt %~70 wt % 。
3. mixed rare earth concentrates liquid caustic soda Decomposition-Synthesis according to claim 1 reclaim the technique of fluorine and phosphorus, it is characterized in that：Step
Suddenly（2）In, heat filtering temperature is 80 DEG C ~ 110 DEG C.
4. mixed rare earth concentrates liquid caustic soda Decomposition-Synthesis according to claim 1 reclaim the technique of fluorine and phosphorus, it is characterized in that：Step
Suddenly（2）In, high alkali liquid cools to 40 DEG C ~ 50 DEG C and carries out being filtrated to get sodium phosphate product again.
5. mixed rare earth concentrates liquid caustic soda Decomposition-Synthesis according to claim 1 reclaim the technique of fluorine and phosphorus, it is characterized in that：Step
Suddenly（3）In, alkali cake water pulp washing, solid-to-liquid ratio is controlled 1:1.5 ~ 2.0, being filtrated to get a soda liquid is used to reclaim fluorination
Sodium.
6. mixed rare earth concentrates liquid caustic soda Decomposition-Synthesis according to claim 1 reclaim the technique of fluorine and phosphorus, it is characterized in that：Step
Suddenly（2）In, the alkali lye and water after filtration is configured to sodium hydroxide solution and is back to use recycling in step [1], supplements what is consumed
NaOH.
7. mixed rare earth concentrates liquid caustic soda Decomposition-Synthesis according to claim 1 reclaim the technique of fluorine and phosphorus, it is characterized in that：Step
Suddenly（4）In, the mother liquor being filtrated to get is back to use in [1] and recycles.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108384945A (en) * | 2018-03-05 | 2018-08-10 | 北京矿冶科技集团有限公司 | A method of alkali containing fosfosiderite soaks dephosphorization |
| CN110357126A (en) * | 2019-08-23 | 2019-10-22 | 中国恩菲工程技术有限公司 | The recovery method of fluorine-containing molten-salt electrolysis slag |
| CN111646546A (en) * | 2020-06-16 | 2020-09-11 | 包头稀土研究院 | Treatment method and application of mixed rare earth alkaline wastewater |
| CN112678933A (en) * | 2020-12-11 | 2021-04-20 | 扬州杰嘉工业固废处置有限公司 | Recycling method of magnesium ammonium phosphate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108384945A (en) * | 2018-03-05 | 2018-08-10 | 北京矿冶科技集团有限公司 | A method of alkali containing fosfosiderite soaks dephosphorization |
| CN110357126A (en) * | 2019-08-23 | 2019-10-22 | 中国恩菲工程技术有限公司 | The recovery method of fluorine-containing molten-salt electrolysis slag |
| CN111646546A (en) * | 2020-06-16 | 2020-09-11 | 包头稀土研究院 | Treatment method and application of mixed rare earth alkaline wastewater |
| CN112678933A (en) * | 2020-12-11 | 2021-04-20 | 扬州杰嘉工业固废处置有限公司 | Recycling method of magnesium ammonium phosphate |
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