CN107381605A - A kind of NaOH decomposes the method that spodumene prepares lithium carbonate by-product analcime - Google Patents
A kind of NaOH decomposes the method that spodumene prepares lithium carbonate by-product analcime Download PDFInfo
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- CN107381605A CN107381605A CN201710589395.7A CN201710589395A CN107381605A CN 107381605 A CN107381605 A CN 107381605A CN 201710589395 A CN201710589395 A CN 201710589395A CN 107381605 A CN107381605 A CN 107381605A
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- spodumene
- analcime
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
- C01B33/28—Base exchange silicates, e.g. zeolites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
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- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses the method that a kind of NaOH decomposition spodumenes prepare lithium carbonate by-product analcime.The technique is by spodumene ore reduction, is ground to 74 μm of particle diameter ＜ powder, after spodumene powder is well mixed with sodium hydroxide and water again, the hydro-thermal reaction 60min 240min under conditions of 240 280 DEG C, analcime and lithium-containing solution is prepared, gained mixture is filtered, washed and dried, analcime product is made, filtrate obtains lithium carbonate by carbonating and precipitated, filtered, washing and dry as lithium carbonate product.The technique is discharged without " three wastes ", efficiently utilizes spodumene resource, and cycling of elements is lithium carbonate in making wherein, and sial cycling of elements is analcime, while most of Li in spodumene2O dissolutions, the cost implementation easy to spread for preparing lithium salts can be reduced.
Description
Technical field
Prepared the invention belongs to lithium salts and molecular sieve water heat synthetic technology, more specifically a kind of NaOH decompose spodumene
The method for preparing lithium carbonate by-product analcime.
Background technology
Spodumene is also known as α-spodumene, can be changed into higher active β-spodumene when more than 720 DEG C, and have
Hot tearing property, it is one of the most frequently used resource containing lithium minerals in the world at present, as lithium chemicals raw material, is widely used in lithium
Chemical industry, glass, ceramic industry, enjoy the good reputation of " industrial monosodium glutamate ".Lithium chemicals raw material mainly for the production of lithium carbonate, but with
It is high compared to technical process cost that lithium is carried in bittern, is unfavorable for industrial production.Analcime is a kind of good material of absorption property, extensively
It is general to be applied to the fields such as sewage disposal, environmental protection, slow release fertilizer, there is higher added value.
Lithium carbonate can be used for compound, lithium metal and its isotope for preparing various lithiums, be additionally operable to prepare chemical reaction
Catalyst etc..Lithium carbonate also has application in semiconductor, ceramics, TV, medicine and atomic energy industry.Due to producing the master of lithium carbonate
It is salt lake bittern (ore method is because cost height is in global production capacity very little) to want raw material, therefore the enterprise of large-scale production lithium carbonate must
Salt lake resources right to mine of the lithium resource reserves compared with horn of plenty must be possessed, this causes the sector to possess higher resource barrier；It is another
Aspect, because global salt lake overwhelming majority resource is all the low lithium type of high magnesium, and the purification ＆ isolation lithium carbonate from the low lithium of high magnesium old halogen
Technological difficulty it is very big.
The content of the invention
It is an object of the invention to provide the method that a kind of NaOH decomposition spodumenes prepare lithium carbonate by-product analcime, analcime
It can be used as person's slow-release fertilizer carrier, can act also as sorbing material, it is widely used.The invention provides a kind of simple and efficient
The method that analcime is prepared using spodumene, lithium carbonate lithium and analcime directly are prepared by raw material of spodumene, is carried for spodumene
For a kind of new purposes, improve spodumene utilization rate, solve the problems, such as spodumene prepare lithium salts during cost it is high.The technique without
" three wastes " discharge, implementation easy to spread.
To achieve the above object, the present invention takes following technical scheme：
A kind of NaOH decomposes the method that spodumene prepares lithium carbonate by-product analcime, and this method comprises the following steps：
(1) spodumene ore treatment：By spodumene ore through broken, ore grinding, ore dressing processing, Li is obtained2O >=6.5%
Powder material；
(2) prepared by analcime：Carried out after the spodumene powder that step (1) obtains is sufficiently mixed with sodium hydrate aqueous solution
Hydro-thermal process, the hydrothermal crystallizing 60-240min under conditions of 240-280 DEG C, by washing, filtering, gained filter cake is through drying
For analcime powder；
(3) prepared by lithium carbonate：Into step (2), gained filtrate is passed through CO2Carbonation reaction is carried out, after reaction terminates, warp
Filtering, washing, gained filter cake are lithium carbonate product through drying.
NaOH as described above decomposes the method that spodumene prepares lithium carbonate by-product analcime, it is preferable that lithium in step (1)
75 μm of pyroxene powder granularity ＜.
NaOH as described above decomposes the method that spodumene prepares lithium carbonate by-product analcime, it is preferable that lithium in step (2)
Pyroxene, sodium hydroxide and water quality ratio are 4: (1-2): (40-80).
NaOH as described above decomposes the method that spodumene prepares lithium carbonate by-product analcime, it is preferable that carbon in step (3)
Souring temperature is 40-80 DEG C, time 20-90min, CO2Ventilation flow rate is (2-5) L/Lmin.
NaOH as described above decomposes the method that spodumene prepares lithium carbonate by-product analcime, it is preferable that step (2) reclaimed water
Reaction product after heat treatment, is first filtered, then is washed, and cleaning solution is incorporated into filtrate.
The beneficial effects of the present invention are：
1. low raw-material cost, technical process is simple, is calcined without spodumene, is directly by hydrothermal reaction process
It can be achieved, technical process is discharged without " three wastes ", and clean manufacturing, popularization convenient to carry out can be achieved；
2. efficiently utilizing spodumene resource, wherein elemental lithium is set to be converted into lithium carbonate, sial cycling of elements is analcime.Fill
Divide the analcime powder for the sial component direct hydrothermal synthesis high added value that make use of in spodumene powder, while in spodumene
Most of Li2O dissolutions, the lithium carbonate product of high concentration is obtained, the cost for preparing lithium salts can be reduced.
3. Li in this method spodumene2O dissolution rates are more than 95%；Analcime yield more than 90%, lithium carbonate product it is pure
Degree is more than 99%.
Brief description of the drawings
Fig. 1 is that a kind of NaOH of the present invention decomposes the method flow diagram that spodumene prepares lithium carbonate by-product analcime；
Fig. 2 is the X ray powder diffraction pattern of analcime synthesized by embodiment 1.
Embodiment
The invention provides a kind of method that spodumene prepares lithium carbonate by-product potassium type zeolite, below in fact with reference to accompanying drawing and reality
Applying example, the present invention is described in detail.
As shown in figure 1, present invention process is that spodumene ore reduction, grinding be made into powder, then by spodumene powder with
After sodium hydroxide and water are well mixed, react under hydrothermal conditions, analcime and lithium-containing solution is prepared, by gained mixture
It is filtered, washed and dried, that is, analcime product is made.This technical process is simple, makes full use of spodumene resource, improves money
Source utilization rate.Experimental raw：Li in spodumene powder2O=7.0%, the main thing of spodumene powder are mutually：α spodumenes, quartz.
Experimental raw：Li in spodumene powder2O=7.0%, the main thing of spodumene powder are mutually：α spodumenes, quartz.
Embodiment 1
By spodumene ore by broken, ball milling, ore dressing processing make 75 μm of its granularity ＜, Li in spodumene powder2O=
7.0%；8g spodumenes are weighed, 2g sodium hydroxides, 80mL water, sodium hydroxide and water are first mixed into sodium hydroxide solution,
Spodumene is added in sodium hydroxide solution again, mixed slurry is made in stirring；It is put into autoclave, heats, at 240 DEG C
Under the conditions of hydro-thermal reaction 240min, naturally cool to room temperature, it is filtered, when washing 4-5 times is to pH value of solution=7~8, filter cake is put
Enter baking oven, in 110 ± 5 DEG C of dry 12h, obtain analcime product；CO is passed through to gained filtrate2, CO2Ventilation flow rate is 0.2L/
Min, carbonation temperature are 40 DEG C, carbonation time 90min, gained filter cake by washing, in 110 ± 5 DEG C of dry 12h, i.e.,
For lithium carbonate product.It is 91% to synthesize analcime yield, and its product composition is shown in Table 1, XRD powder diffractions result (Fig. 2) and is shown to be
Analcime；The yield of lithium carbonate is 90%, and its product is shown in component list 2.
Table 1 synthesizes the main chemical compositions (w of analcimeB%)
Chemical composition analysis result (the w of the lithium carbonate product of table 2B%)
Embodiment 2
By spodumene ore by broken, ball milling, ore dressing processing make 75 μm of its granularity ＜, Li in spodumene powder2O=
7.0%；8g spodumenes are weighed, 3g sodium hydroxides, 120mL water, sodium hydroxide and water are first mixed into sodium hydroxide solution,
Spodumene is added in sodium hydroxide solution again, mixed slurry is made in stirring；It is put into autoclave, heats, at 260 DEG C
Under the conditions of hydro-thermal reaction 120min, naturally cool to room temperature, it is filtered, when washing 4-5 times is to pH value of solution=7~8, filter cake is put
Enter baking oven, in 110 ± 5 DEG C of dry 12h, obtain analcime product.CO is passed through to above-mentioned gained filtrate2, CO2Ventilation flow rate is
0.4L/min, carbonation temperature are 60 DEG C, carbonation time 60min, and gained filter cake passes through washing, in 110 ± 5 DEG C of dryings
12h, as lithium carbonate product.It is 90% to synthesize analcime yield, and its product composition is shown in Table 3, and the yield of lithium carbonate is 90%, its
Product is shown in component list 4.
Table 3 synthesizes the main chemical compositions (w of analcimeB%)
Chemical composition analysis result (the w of the lithium carbonate product of table 4B%)
Embodiment 3
By spodumene ore by broken, ball milling, ore dressing processing make 75 μm of its granularity ＜, Li in spodumene powder2O=
7.0%；8g spodumenes are weighed, 4g sodium hydroxides, 160mL water, sodium hydroxide and water are first mixed into sodium hydroxide solution,
Spodumene powder is added in sodium hydroxide solution again, mixed slurry is made in stirring；It is put into autoclave, heats, 280
Hydro-thermal reaction 60min under conditions of DEG C, room temperature is naturally cooled to, it is filtered, when washing 4-5 times is to pH value of solution=7~8, it will filter
Cake is put into baking oven, in 110 ± 5 DEG C of dry 12h, obtains analcime product.CO is passed through to above-mentioned gained filtrate2, CO2Ventilation flow rate
For 0.5L/min.Carbonation temperature is 80 DEG C, carbonation time 20min, and gained filter cake passes through washing, in 110 ± 5 DEG C of dryings
12h, as lithium carbonate product.It is 92% to synthesize analcime yield, and its product composition is shown in Table 5, and the yield of lithium carbonate is 91%, its
Component list 6.
Table 5 synthesizes the main chemical compositions (w of analcimeB%)
Chemical composition analysis result (the w of the lithium carbonate product of table 6B%)
Claims (5)
1. a kind of NaOH decomposes the method that spodumene prepares lithium carbonate by-product analcime, it is characterised in that：This method includes following
Step：
(1) spodumene ore treatment：By spodumene ore through broken, ore grinding, ore dressing processing, Li is obtained2The powder thing of O >=6.5%
Material；
(2) prepared by analcime：The spodumene powder that step (1) obtains and sodium hydrate aqueous solution are sufficiently mixed laggard water-filling heat
Processing, the hydrothermal crystallizing 60-240min under conditions of 240-280 DEG C, by washing, filtering, gained filter cake is side through drying
Zeolite powder；
(3) prepared by lithium carbonate：Into step (2), gained filtrate is passed through CO2Carbonation reaction is carried out, after reaction terminates, filtered,
Washing, gained filter cake are lithium carbonate product through drying.
2. NaOH as claimed in claim 1 decomposes the method that spodumene prepares lithium carbonate by-product analcime, it is characterised in that：Step
Suddenly 75 μm of spodumene powder granularity ＜ in (1).
3. NaOH as claimed in claim 1 decomposes the method that spodumene prepares lithium carbonate by-product analcime, it is characterised in that：Step
Suddenly spodumene, sodium hydroxide and water quality ratio are 4 in (2): (1-2): (40-80).
4. NaOH as claimed in claim 1 decomposes the method that spodumene prepares lithium carbonate by-product analcime, it is characterised in that：Step
Suddenly carbonation temperature is 40-80 DEG C in (3), time 20-90min, CO2Ventilation flow rate is (2-5) L/Lmin.
5. the NaOH as any one of claim 1-4 decomposes the method that spodumene prepares lithium carbonate by-product analcime, its
It is characterised by：Reaction product in step (2) after hydro-thermal process, is first filtered, then is washed, and cleaning solution is incorporated into filtrate.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108017415A (en) * | 2017-12-08 | 2018-05-11 | 昊青薪材（北京）技术有限公司 | A kind of method that ammonium type zeolite is prepared using analcime powder |
| CN108046289A (en) * | 2017-12-08 | 2018-05-18 | 昊青薪材（北京）技术有限公司 | A kind of method that potassium type zeolite is prepared using analcime powder |
| CN109321748A (en) * | 2018-11-12 | 2019-02-12 | 北京科技大学 | A method of extracting lithium, rubidium and by-product zeolite or kaliophilite from lepidolite ore |
| CN109399672A (en) * | 2018-11-12 | 2019-03-01 | 北京科技大学 | Lithium is extracted from spodumene mine and the method for by-product zeolite or kaliophilite |
| CN110526264A (en) * | 2019-09-27 | 2019-12-03 | 福州大学 | A kind of method that natural α spodumene directly mentions lithium by-product zeolite |
| CN112703259A (en) * | 2018-07-24 | 2021-04-23 | 澳大利亚锂公司 | Caustic conversion process |
| CN116786078A (en) * | 2023-05-25 | 2023-09-22 | 苏州博睿特环保科技有限公司 | Lithium iron silicate modified spodumene slag lithium ion sieve, precursor thereof and preparation method thereof |
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| CN104291350A (en) * | 2014-09-29 | 2015-01-21 | 中国地质大学（北京） | Process for synthesizing analcite from potassium feldspar powder by virtue of hydro-thermal alkaline method |
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| CN101948124A (en) * | 2010-09-09 | 2011-01-19 | 江西赣锋锂业股份有限公司 | Method for extracting lithium salt from spodumene |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108017415A (en) * | 2017-12-08 | 2018-05-11 | 昊青薪材（北京）技术有限公司 | A kind of method that ammonium type zeolite is prepared using analcime powder |
| CN108046289A (en) * | 2017-12-08 | 2018-05-18 | 昊青薪材（北京）技术有限公司 | A kind of method that potassium type zeolite is prepared using analcime powder |
| CN108046289B (en) * | 2017-12-08 | 2020-10-16 | 昊青薪材（北京）技术有限公司 | Method for preparing potassium zeolite by using analcime powder |
| CN108017415B (en) * | 2017-12-08 | 2021-04-27 | 昊青薪材（北京）技术有限公司 | Method for preparing ammonium zeolite by using analcime powder |
| CN112703259A (en) * | 2018-07-24 | 2021-04-23 | 澳大利亚锂公司 | Caustic conversion process |
| CN112703259B (en) * | 2018-07-24 | 2023-06-09 | 澳大利亚锂公司 | Caustic conversion process |
| CN109321748A (en) * | 2018-11-12 | 2019-02-12 | 北京科技大学 | A method of extracting lithium, rubidium and by-product zeolite or kaliophilite from lepidolite ore |
| CN109399672A (en) * | 2018-11-12 | 2019-03-01 | 北京科技大学 | Lithium is extracted from spodumene mine and the method for by-product zeolite or kaliophilite |
| CN109399672B (en) * | 2018-11-12 | 2020-08-07 | 北京科技大学 | Method for extracting lithium from spodumene ore and by-producing zeolite or kaliophilite |
| CN110526264A (en) * | 2019-09-27 | 2019-12-03 | 福州大学 | A kind of method that natural α spodumene directly mentions lithium by-product zeolite |
| CN116786078A (en) * | 2023-05-25 | 2023-09-22 | 苏州博睿特环保科技有限公司 | Lithium iron silicate modified spodumene slag lithium ion sieve, precursor thereof and preparation method thereof |
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Application publication date: 20171124 |