CN104445342B - Sulfuric acid rare earth Salt And Preparation Method - Google Patents
Sulfuric acid rare earth Salt And Preparation Method Download PDFInfo
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- CN104445342B CN104445342B CN201410678802.8A CN201410678802A CN104445342B CN 104445342 B CN104445342 B CN 104445342B CN 201410678802 A CN201410678802 A CN 201410678802A CN 104445342 B CN104445342 B CN 104445342B
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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
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/282—Sulfates
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Abstract
The invention discloses a kind of sulfuric acid rare earth salt being prepared good water solubility by carbonated rare earth salt, it is characterized in that outward appearance is Powdered odorless crystal, chemical formula is RE
2(SO
4)
3.nH
20, water-soluble and sour, solution is limpid, the rising of the solubility with temperature in water and declining, solubleness in sulphuric acid soln reduces with the rising of acidity, its preparation method is for adding acid-soluble in sulphuric acid soln, filtering and impurity removing, crystallization, rinsing dehydration, baking procedure by carbonated rare earth salt, present invention process flow process is succinct, and acid-soluble acidity is low, spent acid is low, equipment corrosion is little, non-environmental-pollution and product yield is high, and cost is low; The sulfuric acid rare earth water-soluble of preparation is good.
Description
Technical field
The present invention relates to a kind of rare-earth products and preparation method, specifically a kind of sulfuric acid rare earth Salt And Preparation Method, particularly relate to a kind of sulfuric acid rare earth Salt And Preparation Method being prepared good water solubility by carbonated rare earth salt.
Background technology
Rare earth is one group of new function material simultaneously with multifrequency natures such as electricity, magnetic, light, superconduction, catalysis and biologies, it is the important foundation material of the high-tech sectors such as information technology, biotechnology, novel material, new energy technology and national defense construction, simultaneously also to some conventional industries of transformation, as agricultural, chemical industry, building materials etc. play an important role.Rare earth is of many uses, and the functional materials of rare earth can be used of a great variety, is forming a large-scale hi-tech industry group, is having very wide market outlook and very important strategic importance, have the laudatory title of " industrial VITAMIN ".Sulfuric acid rare earth is mainly used in sanitas, laboratory reagent, organic intermediate, fine chemicals, catalyst aid, bio-pharmaceuticals etc.
The preparation of current sulfuric acid rare earth salt, application number is the preparation method that application discloses a kind of anhydrous ceric sulfate of 200810150416.6, and it is with Ce (OH)
4for raw material, with the sulfuric acid dissolution cerous hydroxide of 9.1mol/L ~ 9.2mol/L, controlling solvent temperature is 70 DEG C ~ 80 DEG C, and rare earth concentration is 1.05mol/L ~ 1.16mol/L, spent acid 4.4mol/L ~ 4.6mol/L, start stirring to make it to dissolve completely, filter, get filtrate limit heating in reactor, limit is stirred, make it to be concentrated into and separate out ceric sulfate crystal, centrifugally toast to obtain anhydrous powder shape ceric sulfate.The acid-soluble acidity of this preparation method is high, and spent acid is high, has certain corrodibility to equipment, and ceric sulfate prepared by this technique is water-soluble bad, and yield is low, and cost is higher.
Summary of the invention
The object of this invention is to provide a kind of sulfuric acid rare earth Salt And Preparation Method being prepared good water solubility by carbonated rare earth salt.
The present invention adopts following technical scheme to realize its goal of the invention, a kind of sulfuric acid rare earth salt, and outward appearance is Powdered odorless crystal, and chemical formula is RE
2(SO
4)
3.nH
20, under room temperature, n is 3 ~ 9, and water-soluble and sour, solution is limpid, the rising of the solubility with temperature in water and declining, and the solubleness in sulphuric acid soln reduces with the rising of acidity.
A kind of sulfuric acid rare earth salt, outward appearance is Powdered odorless crystal, and chemical formula is RE
2(SO
4)
3.nH
20, under room temperature, n is less than 0.5, and water-soluble and sour, solution is limpid, the rising of the solubility with temperature in water and declining, and the solubleness in sulphuric acid soln reduces with the rising of acidity.
A preparation method for sulfuric acid rare earth salt, it comprises the following steps:
(1) in enamel reactor, compound concentration is the sulphuric acid soln of 0.5mol/L ~ 2.0mol/L, is cooled to 30 DEG C ~ 35 DEG C; Slowly added by carbonated rare earth salt and carry out acid-soluble in the sulphuric acid soln prepared, solvent temperature 30 DEG C ~ 70 DEG C, obtains rare earth sulfate solution, to the pH value 3.5 ~ 4.0 of described solution;
(2) by step (1) gained rare earth sulfate solution filtering and impurity removing, obtain limpid rare earth sulfate solution, with dilute sulphuric acid adjust pH to 1.5 ~ 2;
(3) the step rare earth sulfate solution stirring heating that (2) gained is limpid is boiled, crystal is separated out, is less than 10g/L to the rare earth concentration in mother liquor;
By step (3) gained crystal mixing solutions be placed in strainer and filter, the gained crystal rinsed with deionized water of closely boiling, vacuum filtration obtains sulfuric acid rare earth salt;
(5) sulfuric acid rare earth salt centrifuge dewatering step (4) obtained, obtains the sulfuric acid rare earth salt containing 3 ~ 9 crystal water.
The present invention step (5) in, toast containing the sulfuric acid rare earth salt of 3 ~ 9 crystal water at 150 DEG C ~ 260 DEG C temperature, obtain anhydrous slufuric acid rare-earth salts.
The present invention step (1) in, the preferred concentration of described sulphuric acid soln is 1.0mol/L ~ 1.5mol/L.
Owing to adopting technique scheme, the present invention achieves goal of the invention preferably, and technical process is succinct, and acid-soluble acidity is low, and spent acid is low, and equipment corrosion is little, non-environmental-pollution and product yield is high, and cost is low; The sulfuric acid rare earth water-soluble of preparation is good.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
A kind of sulfuric acid rare earth salt, outward appearance is Powdered odorless crystal, and chemical formula is RE
2(SO
4)
3.nH
20, under room temperature, n is 3 ~ 9, and water-soluble and sour, solution is limpid, the rising of the solubility with temperature in water and declining, and the solubleness in sulphuric acid soln reduces with the rising of acidity.
A preparation method for sulfuric acid rare earth salt, it comprises the following steps:
(1) in enamel reactor, compound concentration is the sulphuric acid soln of 0.5mol/L ~ 2.0mol/L, is cooled to 30 DEG C ~ 35 DEG C; Slowly added by carbonated rare earth salt and carry out acid-soluble in the sulphuric acid soln prepared, solvent temperature 30 DEG C ~ 70 DEG C, obtains rare earth sulfate solution, to the pH value 3.5 ~ 4.0 of described solution;
(2) by step (1) gained rare earth sulfate solution filtering and impurity removing, obtain limpid rare earth sulfate solution, with dilute sulphuric acid adjust pH to 1.5 ~ 2;
(3) the step rare earth sulfate solution stirring heating that (2) gained is limpid is boiled, crystal is separated out, is less than 10g/L to the rare earth concentration in mother liquor;
By step (3) gained crystal mixing solutions be placed in strainer and filter, the gained crystal rinsed with deionized water of closely boiling, vacuum filtration obtains sulfuric acid rare earth salt;
(5) sulfuric acid rare earth salt centrifuge dewatering step (4) obtained, obtains the sulfuric acid rare earth salt containing 3 ~ 9 crystal water.
The sulphuric acid soln 2000L of the present embodiment preparation 0.6mol/L, be cooled to 30 DEG C, it is complete that the Phosbloc being 43.5 ﹪ by 298 ㎏ TREO while stirring adds dissolving in sulphuric acid soln, dissolution process controls solvent temperature 55 DEG C, to the pH value 3.5 of solution, now, the concentration of solution middle-weight rare earths is 0.37mol/L; By solution filtering and impurity removing, with dilute sulphuric acid adjust pH to 2, obtain limpid rare earth sulfate solution 2150L; Limpid rare earth sulfate solution stirring heating being boiled, crystal is separated out, is 5g/L to the rare earth concentration in mother liquor, obtains 1850L slip; For preventing dissolution of crystals, improve direct yield, by slip fast filtering, by the rinsed with deionized water of closely boiling, vacuum filtration obtains lanthanum sulfat, and filtrate obtains Phosbloc by sodium carbonate precipitation, makes the raw material of other rare-earth salts of preparation or lanthanum trioxide; By lanthanum sulfat centrifuge dewatering, obtain lanthanum sulfat 289.5 ㎏ containing crystal water, TREO=42.5 ﹪, direct yield is 94.91 ﹪.
The lanthanum sulfat outward appearance of preparation is Powdered odorless crystal, and water-soluble and sour, solution is limpid, the rising of the solubility with temperature in water and declining, and the solubleness in sulphuric acid soln reduces with the rising of acidity.
Embodiment 2:
A kind of sulfuric acid rare earth salt, outward appearance is Powdered odorless crystal, and chemical formula is RE
2(SO
4)
3.nH
20, under room temperature, n is less than 0.5, and water-soluble and sour, solution is limpid, the rising of the solubility with temperature in water and declining, and the solubleness in sulphuric acid soln reduces with the rising of acidity.
Step (5) in, toast containing the sulfuric acid rare earth salt of 3 ~ 9 crystal water at 150 DEG C ~ 260 DEG C temperature, obtain anhydrous slufuric acid rare-earth salts.
RE
2(SO
4)
3.nH
20→RE
2(SO
4)
3+nH
20(150℃～260℃)
Anhydrous slufuric acid rare-earth salts decomposes prepared by the present embodiment, controls decomposition temperature and time, can obtain the alkali formula sulfuric acid rare earth salt or the rare earth oxide that are insoluble in water.
RE
2(SO
4)
3→RE
2O
2SO
4+2SO
2↑+0
2↑(855℃～946℃)
RE
2O
2SO
4→RE
2O
3+SO
2↑+1/20
2↑(1090℃～1250℃)
Wherein cerous sulfate is decomposed into the decomposition temperature of cerium oxide is 919 DEG C.
The present embodiment toasts de-crystal water to the lanthanum sulfat containing crystal water prepared by embodiment 1 at 200 DEG C of temperature, obtains anhydrous slufuric acid lanthanum 214.3 ㎏, TREO=57.4 ﹪.
Lanthanum sulfat outward appearance prepared by the present embodiment is Powdered odorless crystal, and water-soluble and sour, solution is limpid, the rising of the solubility with temperature in water and declining, and the solubleness in sulphuric acid soln reduces with the rising of acidity.The solubleness of described lanthanum sulfat in water (unit: g/100gH
2o), being 3.8g when 20 DEG C, is 1.5g when 40 DEG C.
Remaining with embodiment 1.
Embodiment 3:
The present invention step (1) in, the preferred concentration of described sulphuric acid soln is 1.0mol/L ~ 1.5mol/L.
The sulphuric acid soln 2000L of the present embodiment preparation 1.0mol/L, be cooled to 30 DEG C, it is complete that the Phosbloc being 43.5 ﹪ by 500 ㎏ TREO while stirring adds dissolving in sulphuric acid soln, dissolution process controls solvent temperature 65 DEG C, to the pH value 4.0 of solution, now, the concentration of solution middle-weight rare earths is 0.61mol/L; By solution filtering and impurity removing, with dilute sulphuric acid adjust pH to 2, obtain limpid rare earth sulfate solution 2200L; Limpid rare earth sulfate solution stirring heating being boiled, crystal is separated out, is 7g/L to the rare earth concentration in mother liquor, obtains 2000L slip; For preventing dissolution of crystals, improve direct yield, by slip fast filtering, by the rinsed with deionized water of closely boiling, vacuum filtration obtains lanthanum sulfat, and filtrate obtains Phosbloc by sodium carbonate precipitation, makes the raw material of other rare-earth salts of preparation or lanthanum trioxide; By lanthanum sulfat centrifuge dewatering, obtain lanthanum sulfat 460.4 ㎏ containing crystal water, TREO=44.5 ﹪; Then at the de-crystal water of baking at 200 DEG C of temperature, obtain anhydrous slufuric acid lanthanum 357.1 ㎏, TREO=57.37 ﹪, direct yield is 94.19 ﹪.
Remaining with embodiment 1,2.
Embodiment 4:
The sulphuric acid soln 1350L of the present embodiment preparation 1.48mol/L, be cooled to 30 DEG C, it is complete that the Phosbloc being 43.5 ﹪ by 500 ㎏ TREO while stirring adds dissolving in sulphuric acid soln, dissolution process controls solvent temperature 50 DEG C, to the pH value 3.5 of solution, now, the concentration of solution middle-weight rare earths is 0.83mol/L; By solution filtering and impurity removing, with dilute sulphuric acid adjust pH to 2, obtain limpid rare earth sulfate solution 1600L; Limpid rare earth sulfate solution stirring heating being boiled, crystal is separated out, is 8g/L to the rare earth concentration in mother liquor, obtains 1400L slip; For preventing dissolution of crystals, improve direct yield, by slip fast filtering, by the rinsed with deionized water of closely boiling, vacuum filtration obtains lanthanum sulfat, and filtrate obtains Phosbloc by sodium carbonate precipitation, makes the raw material of other rare-earth salts of preparation or lanthanum trioxide; By lanthanum sulfat centrifuge dewatering, obtain lanthanum sulfat 443.2 ㎏ containing crystal water, TREO=46.4 ﹪; Then at the de-crystal water of baking at 200 DEG C of temperature, obtain anhydrous slufuric acid lanthanum 357.6 ㎏, TREO=57.5 ﹪, direct yield is 94.54 ﹪.
Remaining with embodiment 1,2.
Embodiment 5:
The sulphuric acid soln 1000L of the present embodiment preparation 2.0mol/L, is cooled to 30 DEG C, and it is complete that the cerous carbonate being 49.9 ﹪ by 460 ㎏ TREO while stirring adds dissolving in sulphuric acid soln, dissolution process controls solvent temperature 38 DEG C, to the pH value 3.5 of solution, now, the concentration of solution middle-weight rare earths is 1.1mol/L; By solution filtering and impurity removing, with dilute sulphuric acid adjust pH to 2, obtain limpid rare earth sulfate solution 1200L; Limpid rare earth sulfate solution stirring heating being boiled, crystal is separated out, is 10g/L to the rare earth concentration in mother liquor, obtains 950L slip; For preventing dissolution of crystals, improve direct yield, by slip fast filtering, by the rinsed with deionized water of closely boiling, vacuum filtration obtains cerous sulfate, and filtrate obtains cerous carbonate by sodium carbonate precipitation, makes the raw material of other rare-earth salts of preparation or cerium oxide; By cerous sulfate centrifuge dewatering, obtain cerous sulfate 470.1 ㎏ containing crystal water, TREO=46.8 ﹪; Then at the de-crystal water of baking at 180 DEG C of temperature, obtain anhydrous ceric sulfate 382.62 ㎏, TREO=57.5 ﹪, direct yield is 95.85 ﹪.
Cerous sulfate outward appearance prepared by the present embodiment is Powdered odorless crystal, and water-soluble and sour, solution is limpid, the rising of the solubility with temperature in water and declining, and the solubleness in sulphuric acid soln reduces with the rising of acidity.The solubleness of described cerous sulfate in water (unit: g/100gH
2o), being 23.8g when 20 DEG C, is 10.3g when 40 DEG C.
Remaining with embodiment 1.
Embodiment 6:
The sulphuric acid soln 2000L of the present embodiment preparation 1.2mol/L, be cooled to 30 DEG C, it is complete that the gadolinium carbonate being 46.0 ﹪ by 630 ㎏ TREO while stirring adds dissolving in sulphuric acid soln, dissolution process controls solvent temperature 45 DEG C, to the pH value 3.5 of solution, now, the concentration of solution middle-weight rare earths is 0.72mol/L; By solution filtering and impurity removing, with dilute sulphuric acid adjust pH to 2, obtain limpid rare earth sulfate solution 2200L; Limpid rare earth sulfate solution stirring heating being boiled, crystal is separated out, is 6.1g/L to the rare earth concentration in mother liquor, obtains 2000L slip; For preventing dissolution of crystals, improve direct yield, by slip fast filtering, by the rinsed with deionized water of closely boiling, vacuum filtration obtains gadolinium sulphate, and filtrate obtains gadolinium carbonate by sodium carbonate precipitation, makes the raw material of other rare-earth salts of preparation or gadolinium sesquioxide; By gadolinium sulphate centrifuge dewatering, obtain gadolinium sulphate 620 ㎏ containing crystal water, TREO=44.5 ﹪; Then at the de-crystal water of baking at 200 DEG C of temperature, obtain anhydrous slufuric acid gadolinium 459.1 ㎏, TREO=60.1 ﹪, direct yield is 95.21 ﹪.
Gadolinium sulphate outward appearance prepared by the present embodiment is Powdered odorless crystal, and water-soluble and sour, solution is limpid, the rising of the solubility with temperature in water and declining, and the solubleness in sulphuric acid soln reduces with the rising of acidity.The solubleness of described gadolinium sulphate in water (unit: g/100gH
2o), being 2.87g when 20 DEG C, is 2.19g when 40 DEG C.
Remaining with embodiment 1.
Embodiment 7:
The sulphuric acid soln 1500L of the present embodiment preparation 2.0mol/L, be cooled to 30 DEG C, it is complete that the gadolinium carbonate being 46.0 ﹪ by 790 ㎏ TREO while stirring adds dissolving in sulphuric acid soln, dissolution process controls solvent temperature 45 DEG C, to the pH value 3.9 of solution, now, the concentration of solution middle-weight rare earths is 1.14mol/L; By solution filtering and impurity removing, with dilute sulphuric acid adjust pH to 2, obtain limpid rare earth sulfate solution 1750L; Limpid rare earth sulfate solution stirring heating being boiled, crystal is separated out, is 9.5g/L to the rare earth concentration in mother liquor, obtains 1550L slip; For preventing dissolution of crystals, improve direct yield, by slip fast filtering, by the rinsed with deionized water of closely boiling, vacuum filtration obtains gadolinium sulphate, and filtrate obtains gadolinium carbonate by sodium carbonate precipitation, makes the raw material of other rare-earth salts of preparation or gadolinium sesquioxide; By gadolinium sulphate centrifuge dewatering, obtain gadolinium sulphate 755.3 ㎏ containing crystal water, TREO=45.9 ﹪; Then at the de-crystal water of baking at 200 DEG C of temperature, obtain anhydrous slufuric acid gadolinium 576.9 ㎏, TREO=60.09 ﹪, direct yield is 95.39 ﹪.
Remaining with embodiment 1,6.
Embodiment 8:
The sulphuric acid soln 1770L of the present embodiment preparation 1.5mol/L, be cooled to 30 DEG C, it is complete that the yttrium carbonate being 40.0 ﹪ by 500 ㎏ TREO while stirring adds dissolving in sulphuric acid soln, dissolution process controls solvent temperature 40 DEG C, to the pH value 4.0 of solution, now, the concentration of solution middle-weight rare earths is 0.87mol/L; By solution filtering and impurity removing, with dilute sulphuric acid adjust pH to 2, obtain limpid rare earth sulfate solution 2020L; Limpid rare earth sulfate solution stirring heating being boiled, crystal is separated out, is 9.5g/L to the rare earth concentration in mother liquor, obtains 1700L slip; For preventing dissolution of crystals, improve direct yield, by slip fast filtering, by the rinsed with deionized water of closely boiling, vacuum filtration obtains yttrium sulfate, and filtrate obtains yttrium carbonate by sodium carbonate precipitation, makes the raw material of other rare-earth salts of preparation or yttrium oxide; By yttrium sulfate centrifuge dewatering, obtain yttrium sulfate 550.5 ㎏ containing crystal water, TREO=34.33 ﹪; Then at the de-crystal water of baking at 200 DEG C of temperature, anhydrous slufuric acid yttrium 396.98 ㎏ is obtained, TREO=47.51 ﹪.Direct yield is 94.30 ﹪.
Yttrium sulfate outward appearance prepared by the present embodiment is Powdered odorless crystal, and water-soluble and sour, solution is limpid, the rising of the solubility with temperature in water and declining, and the solubleness in sulphuric acid soln reduces with the rising of acidity.The solubleness of described yttrium sulfate in water (unit: g/100gH
2o), being 9.76g when 20 DEG C, is 4.90g when 40 DEG C.
Remaining with embodiment 1.
Claims (3)
1. a preparation method for sulfuric acid rare earth salt, is characterized in that it comprises the following steps:
(1) in enamel reactor, compound concentration is the sulphuric acid soln of 0.5mol/L ~ 2.0mol/L, is cooled to 30 DEG C ~ 35 DEG C; Slowly added by carbonated rare earth salt and carry out acid-soluble in the sulphuric acid soln prepared, solvent temperature 30 DEG C ~ 70 DEG C, obtains rare earth sulfate solution, to the pH value 3.5 ~ 4.0 of described solution;
(2) by step (1) gained rare earth sulfate solution filtering and impurity removing, obtain limpid rare earth sulfate solution, with dilute sulphuric acid adjust pH to 1.5 ~ 2;
(3) the step rare earth sulfate solution stirring heating that (2) gained is limpid is boiled, crystal is separated out, is less than 10g/L to the rare earth concentration in mother liquor;
By step (3) gained crystal mixing solutions be placed in strainer and filter, the gained crystal rinsed with deionized water of closely boiling, vacuum filtration obtains sulfuric acid rare earth salt;
(5) sulfuric acid rare earth salt centrifuge dewatering step (4) obtained, obtains the sulfuric acid rare earth salt containing 3 ~ 9 crystal water.
2. the preparation method of sulfuric acid rare earth salt according to claim 1, it is characterized in that step (5) in, the sulfuric acid rare earth salt containing 3 ~ 9 crystal water is toasted at 150 DEG C ~ 260 DEG C temperature, obtains anhydrous slufuric acid rare-earth salts.
3. the preparation method of sulfuric acid rare earth salt according to claim 1 or 2, it is characterized in that step (1) in, the preferred concentration of described sulphuric acid soln is 1.0mol/L ~ 1.5mol/L.
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| CN113044872A (en) * | 2021-04-14 | 2021-06-29 | 江苏温塑实业有限公司 | Preparation method of lanthanum sulfate |
| CN115321577A (en) * | 2022-08-29 | 2022-11-11 | 焦天棋 | Preparation method of yttrium oxide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1017419B (en) * | 1989-06-13 | 1992-07-15 | 甘肃稀土公司 | Preparation process of europium sulfate |
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| FR2530608A1 (en) * | 1982-07-26 | 1984-01-27 | Rhone Poulenc Spec Chim | VERY SOLUBLE CERIC SULFATE, PROCESS FOR PRODUCING THE SAME AND APPLICATIONS THEREOF |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1017419B (en) * | 1989-06-13 | 1992-07-15 | 甘肃稀土公司 | Preparation process of europium sulfate |
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| Title |
|---|
| 试剂硫酸铈的制备;孙晓白;《湖南化工》;19881231(第3期);31-32 * |
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