CN105256156B - Process for decomposing fluorine-containing rare earth molten salt waste residues - Google Patents
Process for decomposing fluorine-containing rare earth molten salt waste residues Download PDFInfo
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- CN105256156B CN105256156B CN201510706337.9A CN201510706337A CN105256156B CN 105256156 B CN105256156 B CN 105256156B CN 201510706337 A CN201510706337 A CN 201510706337A CN 105256156 B CN105256156 B CN 105256156B
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Abstract
The invention belongs to the field of resource recycling, and particularly relates to a method for recovering rare earth elements by treating fused salt electrolysis waste residues containing rare earth fluoride through sodium hydroxide alkali conversion and hydrochloric acid dissolution. The invention comprises the following steps: drying and pulverizing fluorine-containing rare earth fused salt electrolysis waste residue raw materials, roasting, carrying out alkali conversion, washing alkali melt with water to remove fluorine, obtaining calcium fluoride, dissolving with hydrochloric acid, and adjusting back acid solution; the invention is characterized in that low-temperature alkali conversion, calcium fluoride recovery and liquid alkali recovery are carried out in the production process, so that compared with other processes, the invention has the outstanding advantages of simple working procedures, energy saving, environmental protection, high one-time recovery rate of rare earth (finally the leaching rate of rare earth elements reaches more than 98 percent) and the like.
Description
Technical field
Field is recycled the invention belongs to resources circulation, and in particular to turn by sodium hydroxide alkali and dissolving with hydrochloric acid processing contains
The method of rare earth fluoride molten-salt electrolysis waste residue recovering rare earth element.
Background technology
Current single rare earth metal and function rare earth alloy are all mainly to be electrolysed fused salt by fluoride system rare earth oxide
Technique is produced.A certain amount of fused salt waste residue will be produced during Rare Earth Electrolysis, these fused salt waste residues contain 20%-70%'s
Rare earth (is calculated) with REO, wherein most rare earth element exists in the form of fluoride.At present, molten-salt electrolysis waste residue is handled
Most extensive method is that have concentrated sulfuric acid high temperature roast fluorine removal, after go out sulfuric acid rare earth with water logging, then reclaimed through subsequent treatment and obtain rare earth
Product.This technique consumption acid is high, have making for 60% or so and the concentrated sulfuric acid of special requirement, rare earth primary recovery in total amount to equipment
With and roasting process in produce hydrogen fluoride gas processing have special technical requirements, it is easy to produce accident.Chinese patent
(application number:201010505807.2) a kind of method of the recovering rare earth element from molten salt electrolysis wastes is disclosed, use
Will electrolysis waste material and calcium hydroxide by weight 1：0.5 mixing 950-1000 DEG C roasting, then again with 30% dissolving with hydrochloric acid.This
Kind of method is improved the leaching rate of rare earth, but sintering temperature too high energy consumption is big, calcination when earthen bowl loss it is big, during acid dissolving because
Containing non-rare earths such as a large amount of Ca, Ba in the solution that calcium hydroxide excessively causes acid consumption big and obtained, later stage extraction point is caused
It is high from cost.
The content of the invention
It is an object of the invention to provide a kind of technique for decomposing fluorine-containing rare earth molten salt waste residue, its more efficient, energy-saving and environmental protection.
Technical scheme：A kind of technique for decomposing fluorine-containing rare earth molten salt waste residue, comprises the following steps：
A, the drying of fluorine-containing rare earth molten-salt electrolysis raw slag material, powder processed：First it should be dried for wet feed at 150-200 DEG C, then
Powder is broken into Raymond machine；
B, roasting alkali turn：By powder in step A and piece alkali by weight 1：0.6-0.8 is well mixed, and fashionable dress alms bowl,
It is calcined 2-6 hours at 500-600 DEG C, rare earth fluoride is converted into corresponding oxide and sodium fluoride, obtained after block alkali fusion thing again
Crushed in time with Raymond machine；
C, alkali fusion thing washing fluorine removal：Alkali fusion thing is with water by weight 1：10 be added in Water washing bucket wash 3-5 times to pH value be 7-9
After squeeze, obtain washery slag；
D, acquisition calcirm-fluoride：Milk of lime is added in the washing clear liquid of step C and is adjusted to neutrality, is squeezed, slag is washed with watery hydrochloric acid
Wash holding neutral, squeezing, 150-200 DEG C of drying, obtain calcirm-fluoride of the content more than 90% again；
E, dissolving with hydrochloric acid：The washery slag of step C is stirred 1 hour at 70-90 DEG C in proportion with concentrated hydrochloric acid, it is rear carefully to add
Enter appropriate NaClO31 hour is stirred for without Fe2+, then remove Fe with liquid caustic soda readjustment pH value to 3.53+, then add 2mol/L's
Na2SO4Solution removes Ca to without white precipitate generation2+And Ba2+；Squeezing, washing, drying, the main graphitiferous of pressure slag, hydroxide
Iron, barium sulfate；Obtain REO contents and treat that follow-up extract and separate obtains high-purity rare-earth product in 50-120g/L rare earth chloride liquid
(extraction process is prior art)；
F, sour molten feed liquid readjustment：Liquid caustic soda is added in the water lotion of E steps adjusts pH value to 12 precipitation to extract out for 24 hours
Layer clear liquid, lower floor's turbid solution is that rare earth hydrate can replace readjustment of the liquid caustic soda as sour molten feed liquid in E steps；
Washery slag weight and concentrated hydrochloric acid volume ratio are 1 in step E：1.5 tons/cubic metre, concentrated hydrochloric acid concentration is 10mol/L work
Industry hydrochloric acid；
NaClO in step E3Consumption solution in production Fe2+Content determines that its actual amount is theoretical amount
1.2 again, i.e.,：1.2×6n(NaClO3)=n (Fe2+), n represents amount of substance.
Fluorine-containing weight ratio is determined the weight ratio of powder and piece alkali in electrolytic waste slag in step B, is pressed if fluorine-containing 0-10%
1：0.6,1 is pressed if fluorine-containing 10-15%：0.7,1 is pressed if fluorine-containing more than 15%：0.8.
Described liquid caustic soda is industrial lye, and concentration is 10mol/L.
Described watery hydrochloric acid concentration is 0.1mol/L.
Calcination temperature is relevant with mixing alkali number in step B, and temperature can be reduced suitably the time if same raw material mixes alkali number height
Extension, temperature is low to be unfavorable for fluorine conversion, the high fluorine of temperature and changes but alms bowl easy to stick.
The chemical reaction process of the present invention is as follows：
Electrolytic waste slag alkali turns：2REF3+ 6NaOH=RE2O3+6NaF3+H2O
BaF2+ 2NaOH=BaO+2NaF+H2O
4RE+3O2=2RE2O3
3Fe+2O2=Fe3O4
Dissolving with hydrochloric acid：RE2O3+6H+=2RE3+
Fe3O4+8H+=2Fe3++Fe2++4H2O
Oxidation：6Fe2++ClO3-+6H+=6Fe3++Cl-+3H2O
Deliming barium：Ca2++S04 2-=CaS04
Ba2++S04 2-=BaS04
PH value is adjusted to remove iron：Fe3++3H2O=Fe (OH)3+3H+
The present invention is turned using sodium hydroxide alkali, the advantage of dissolving with hydrochloric acid is：(1) rare earth leaching efficiency is higher, once soaks
Extracting rate is up to more than 98%；(2) calcination alkali turns that temperature is relatively low, consumption sour low, acid-soluble ratio height, an overall energy consumption is small；(3) rare earth member
Element is efficiently separated with non-rare earth, facilitates follow-up extract and separate；(4) simple to operate, more environmentally-friendly, calcirm-fluoride can be returned
Receive.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Embodiment
With reference to embodiment, the invention will be further described, but the present invention is not limited solely to following examples.
(washery slag and concentrated hydrochloric acid ratio in embodiment：1：1.5 tons/cubic metre, concentrated hydrochloric acid concentration is 10mol/L technical hydrochloric acid；Liquid caustic soda is work
Industry liquid caustic soda, concentration is 10mol/L；Watery hydrochloric acid concentration is 0.1mol/L.)
Embodiment 1：The rare earth molten salt waste residue 1000Kg 471Kg of REO containing rare earth, single rare earth percentage composition and non-rare earth contain
Measure examination and be shown in Table one；
Table one：The partition table of raw material one
| Project | La2O3 | CeO2 | Pr6O11 | Nd2O3 | Sm2O3 | Eu2O3 | Gd2O3 | Tb4O7 | Dy2O3 |
| Quality (%) | 2.94 | 0.07 | 19.18 | 76.84 | 0.07 | <0.01 | 0.53 | <0.01 | 0.22 |
| Project | Ho2O3 | Er2O3 | Tm2O3 | Yb2O3 | Lu2O3 | Y2O3 | REO | Fe2O3 | F |
| Quality (%) | 0.10 | <0.01 | <0.01 | <0.01 | <0.01 | <0.01 | 47.10 | 7.58 | 16.57 |
Production stage：
(1) fused salt raw slag material is broken into the mesh of Powder Particle Size about 100 with Raymond machine；
(2) roasting alkali turns：By powder in step (1) and piece alkali by weight 1：0.8 is well mixed, and fashionable dress alms bowl, 550 DEG C
Under in no good roasting in kilns 4 hours；Obtain block alkali fusion thing and be crushed to about 100 mesh in time with Raymond machine；
(3) alkali fusion product is washed：Alkali fusion thing is with water by weight 1：10 are added in Water washing bucket, stir 1 hour, and squeezing is obtained
Washery slag, is repeated 2 times to wash water pH=8 and obtains washery slag；
(4) calcirm-fluoride is obtained：Wash addition milk of lime in clear liquid for the first time in step (3) and be adjusted to neutrality, squeeze, slag is used
Watery hydrochloric acid washing keeps neutral, and squeezing, 200 DEG C of drying, obtain the calcirm-fluoride 260Kg that content is about 90% again；
(5) dissolving with hydrochloric acid：1 is pressed with concentrated hydrochloric acid to washery slag in step (3)：1.5 stir 1 hour at 80 DEG C, with survey ferron
Detection contains Fe2+3.5Kg NaClO is carefully added into afterwards3Be stirred for 1 hour, after with liquid caustic soda adjust back pH value to 3.5, then while survey while
Add 2mol/L Na2SO4Solution about 4L removes Ca to without white precipitate generation2+And Ba2+；Squeezing, washing, drying, obtain wet pressing
Slag 265.5Kg, it is 92.50g/L to obtain rare earth chloride liquid 5000L containing REO, treats that follow-up extract and separate obtains high-purity rare-earth product；
(6) liquid caustic soda is added in second of water lotion of step (5) adjusts pH value to extract supernatant liquor out within 24 hours to 12 precipitation,
Lower floor's turbid solution is mainly that rare earth hydrate can replace readjustment of the liquid caustic soda as sour molten feed liquid in step (5).
Production interpretation of result is shown in Table two, table three：
Table two：Acid dissolution slag and sour molten feed liquid main project analysis test table
Table three：Acid-soluble ratio analytical table
Embodiment 2：The rare earth molten salt waste residue 850Kg 360Kg of REO containing rare earth, single rare earth percentage composition and non-content of rare earth
Test is shown in Table four.
Table four：The partition table of raw material two
Production stage：
(1) fused salt raw slag material is broken into the mesh of Powder Particle Size about 100 with Raymond machine；
(2) roasting alkali turns：By powder in step (1) and piece alkali by weight 1：0.7 is well mixed, and fashionable dress alms bowl, 600 DEG C
Under in no good roasting in kilns 4 hours.Obtain block alkali fusion thing and be crushed to about 100 mesh in time with Raymond machine；
(3) alkali fusion product is washed：Alkali fusion thing is with water by weight 1：10 are added in Water washing bucket, stir 1 hour, and squeezing is obtained
Washery slag.It is repeated 2 times to wash water pH=9 and obtains washery slag.
(4) calcirm-fluoride is obtained：Wash addition milk of lime in clear liquid for the first time in step (3) and be adjusted to neutrality, squeeze, slag is used
Watery hydrochloric acid washing keeps neutral, and squeezing, 200 DEG C of drying, obtain the calcirm-fluoride 141Kg that content is about 91% again.
(5) dissolving with hydrochloric acid：1 is pressed with concentrated hydrochloric acid to washery slag in step (3)：1.5 stir 1 hour at 90 DEG C, with survey ferron
Detection is without Fe2+, pH value is adjusted back to 3.5 with liquid caustic soda, then adds 2mol/L Na when surveying2SO4Solution about 3L is to without white precipitate
Generation removes Ca2+And Ba2+.Squeezing, washing, drying, obtain wet pressing slag 123.5Kg.Obtain rare earth chloride liquid 4500L and contain REO about
78.48g/L, treats that follow-up extract and separate obtains high-purity rare-earth product.
(6) liquid caustic soda is added in second of water lotion of step (5) adjusts pH value to extract supernatant liquor out within 24 hours to 12 precipitation,
Lower floor's turbid solution is mainly that rare earth hydrate can replace readjustment of the liquid caustic soda as sour molten feed liquid in step (5).
Produce interpretation of result as follows：
Table five：Acid dissolution slag and sour molten feed liquid main project analysis test table
Table six：Acid-soluble ratio analytical table
Note：During raw slag material, acid dissolution slag, sour molten feed liquid analysis test table data are tested both from Ganzhou research institute
Heart test result.
Claims (4)
1. a kind of technique for decomposing fluorine-containing rare earth molten salt waste residue, it is characterized in that：Comprise the following steps：
A, the drying of fluorine-containing rare earth molten-salt electrolysis raw slag material, powder processed：Thunder should be then used for wet feed first in 150-200 DEG C of drying
Illiteracy machine is broken into powder；
B, roasting alkali turn：By powder in step A and piece alkali by weight 1：0.6-0.8 is well mixed, and fashionable dress alms bowl, 500-
It is calcined 2-6 hours at 600 DEG C, rare earth fluoride is converted into corresponding oxide and sodium fluoride, thunder is used again after obtaining block alkali fusion thing
Illiteracy machine is crushed in time；
C, alkali fusion thing washing fluorine removal：Alkali fusion thing is with water by weight 1：10 be added in Water washing bucket wash 3-5 times to pH value be 7-9 after
Squeezing, obtains washery slag；
D, acquisition calcirm-fluoride：Milk of lime is added in the washing clear liquid of step C and is adjusted to neutrality, is squeezed, slag washs guarantor with watery hydrochloric acid
Neutrality is held, squeezing, 150-200 DEG C of drying, obtain calcirm-fluoride of the content more than 90% again；
E, dissolving with hydrochloric acid：The washery slag of step C is stirred 1 hour at 70-90 DEG C in proportion with concentrated hydrochloric acid, after be carefully added into it is suitable
Measure NaClO31 hour is stirred for without Fe2+, then remove Fe with liquid caustic soda readjustment pH value to 3.53+, then add 2mol/L Na2SO4
Solution removes Ca to without white precipitate generation2+And Ba2+；Squeezing, washing, drying, obtain chlorine of the REO contents in 50-120g/L
Change rare earth feed liquid and treat that follow-up extract and separate obtains high-purity rare-earth product；
F, sour molten feed liquid readjustment：Liquid caustic soda is added in the water lotion of E steps adjusts pH value clear to 12 precipitation, 24 hours extraction upper stratas
Liquid, lower floor's turbid solution is that rare earth hydrate can replace readjustment of the liquid caustic soda as sour molten feed liquid in E steps；
Washery slag weight and concentrated hydrochloric acid volume ratio are 1 in step E：1.5 tons/cubic metre, concentrated hydrochloric acid concentration is 10mol/L Nacl
Acid；
NaClO in step E3Consumption solution in production Fe2+Content determines that its actual amount is 1.2 times of theoretical amount,
I.e.：1.2×6n(NaClO3)=n (Fe2+), n represents amount of substance.
2. a kind of technique for decomposing fluorine-containing rare earth molten salt waste residue according to claim 1, it is characterized in that：Powder in step B
Fluorine-containing weight ratio is determined in electrolytic waste slag with the weight ratio of piece alkali, and 1 is pressed if fluorine-containing 0-10%：0.6, if fluorine-containing 10-
15% is pressed 1：0.7,1 is pressed if fluorine-containing more than 15%：0.8.
3. a kind of technique for decomposing fluorine-containing rare earth molten salt waste residue according to claim 1, it is characterized in that：Described liquid caustic soda is
Industrial lye, concentration is 10mol/l.
4. a kind of technique for decomposing fluorine-containing rare earth molten salt waste residue according to claim 1, it is characterized in that：Described watery hydrochloric acid
Concentration is 0.1mol/L.
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| CN106044833B (en) * | 2016-06-07 | 2017-10-27 | 福建省长汀金龙稀土有限公司 | A kind of method of the recovering rare earth fluoride from rare earth electrode scrap reclaimed materials and clinker |
| CN106745340B (en) * | 2016-12-31 | 2018-12-28 | 山东飞源科技有限公司 | The method of heavy metal nickel is recycled from high fluorine-containing electrolysis fused salt |
| CN106636654B (en) * | 2016-12-31 | 2019-04-26 | 山东飞源科技有限公司 | The method of metallic nickel is recycled from fluorine-containing electrolysis fused salt |
| CN107630143B (en) * | 2017-09-26 | 2019-10-25 | 赣南师范大学 | Method for extracting rare earth from rare earth fluorescent powder waste and fluorine-containing rare earth electrolysis waste residue |
| CN110387474B (en) * | 2019-08-23 | 2021-05-07 | 中国恩菲工程技术有限公司 | Method for treating electrolytic slag generated in process of producing aluminum-scandium alloy by molten salt electrolysis method |
| 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 |
| CN112981146A (en) * | 2021-02-07 | 2021-06-18 | 中国科学院过程工程研究所 | Method for recovering rare earth molten salt electrolytic slag through fluorine fixation transformation roasting |
| CN113652560B (en) * | 2021-07-14 | 2022-11-08 | 四川省冕宁县方兴稀土有限公司 | Method for efficiently recovering rare earth from rare earth molten salt waste residues |
| CN114934201A (en) * | 2022-06-20 | 2022-08-23 | 淄博灵芝化工有限公司 | Method for recovering rare earth from rare earth tempering slag |
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| CN101956078B (en) * | 2010-10-13 | 2012-07-04 | 赣州鑫磊稀土新材料有限公司 | Method for separating and recycling rare-earth elements from molten salt electrolysis wastes of rare-earth metals |
| CN104843761A (en) * | 2015-03-31 | 2015-08-19 | 福建省长汀金龙稀土有限公司 | Method for recovering rare earth from rare earth fluoride fused salt electrolysis waste with effects of environmental protection and low cost |
| CN104818390B (en) * | 2015-05-14 | 2016-09-28 | 孙东江 | Rare earth metal metallurgy slag environment-friendly treating process |
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Address after: No.1, Shiyuan South Road, Rongjiang New District, Ganzhou City, Jiangxi Province Patentee after: GANNAN NORMAL University Address before: 341000 No. 1, Shiyuan South Road, Ganzhou economic and Technological Development Zone, Jiangxi Province Patentee before: GANNAN NORMAL University |
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Effective date of registration: 20220524 Address after: 341401 Long Hua Xiang Sha Tian Yu Cun, Nankang District, Ganzhou City, Jiangxi Province Patentee after: GANZHOU JISHENG TECHNOLOGY Co.,Ltd. Address before: No.1, Shiyuan South Road, Rongjiang New District, Ganzhou City, Jiangxi Province Patentee before: GANNAN NORMAL University |
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Denomination of invention: A Process for Decomposing Fluorinated Rare Earth Molten Salt Waste Effective date of registration: 20230908 Granted publication date: 20170905 Pledgee: Ganzhou Branch of Bank of Communications Co.,Ltd. Pledgor: GANZHOU JISHENG TECHNOLOGY Co.,Ltd. Registration number: Y2023980055960 |