CN107324438A - A kind of preparation method of lithium slag adsorbent - Google Patents
A kind of preparation method of lithium slag adsorbent Download PDFInfo
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- CN107324438A CN107324438A CN201710741149.9A CN201710741149A CN107324438A CN 107324438 A CN107324438 A CN 107324438A CN 201710741149 A CN201710741149 A CN 201710741149A CN 107324438 A CN107324438 A CN 107324438A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3042—Use of binding agents; addition of materials ameliorating the mechanical properties of the produced sorbent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
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Abstract
The present invention relates to a kind of preparation method of lithium slag adsorbent, purified and refined by lithium ore deposit waste residue, then add 0%~20% coagent, 1%~20% binding agent and 0~20% water, shaping and roasting prepares lithium slag adsorbent.The lithium slag adsorbent is selectively good to extracting the lithium resource in seawater and salt lake bittern.Raw material of the present invention is easy to get, and preparation process is simple, and production cost is low.
Description
Technical field：
The present invention relates to a kind of lithium slag adsorbent preparation method, more particularly to from seawater and the lithium slag of the extracting lithium from salt lake brine containing lithium
The preparation of adsorbent.
Background technology：
Lithium carbonate is the basic material of the secondary lithium salts of production and lithium metal, in global consumer electronics, new-energy automobile demand growth
Drive under, the demand of global lithium carbonate will keep average annual 15%-20% compound speedup.At present, for the exploitation of lithium resource
Using being no longer limited to lithium ore, oneself is on the verge of exhaustion for the exploitation of lithium ore, far can not meet industrial demand.Such as
What turns into the inexorable trend of lithium resource exploitation from now on from seawater, extracting lithium from salt lake brine.
Liquid puies forward lithium method and is broadly divided into three classes：The precipitation method, solvent extraction and absorption method.Wherein, law technology is precipitated
Maturation, has realized industrial applications, but the method carries that lithium technological process is more complicated, and alkali consumption is larger, and environmental pollution is serious, and
And it is only applicable to the bittern of low Mg/Li ratio.China's liquid lithium aboundresources, but develop backward main reason is that bittern so far
The content of middle magnesium is higher, and the critical problem that lithium is this technology how is carried from high Mg/Li ratio bittern.Solvent extraction is applicable
In high Mg/Li than bittern, but bittern need to be concentrated, equipment corrosion is serious, and organic solvent is poisonous and high volatility, thus it is raw
Produce cost high and unfriendly to environment.Adsorption method of separation is particularly suitable for use in the seawater of high Mg/Li ratio bittern and low lithium concentration, and work
Skill process is simple, green high-efficient, production cost is low, is that most prospects for commercial application puies forward lithium method.The key of absorption method is
The adsorbent of function admirable is developed, it requires that adsorbent has excellent Selective adsorption to lithium, it is a large amount of in bittern to exclude
The interference of the alkali metal, alkaline-earth metal ions that coexist.
Lithium ore deposit waste residue is that lithium ore prepares the waste residue produced during lithium carbonate, and its main component is alumino-silicate（H2O·
Al2O3·4Si2O）.At present, lithium slag resource is mainly used in building materials industry, and all outdoor placement of more than 95% lithium slag is not filled
Divide and utilize.Spodumene crystalline phase under high-temperature roasting turns to β types by α types, and many is there is in β-spodumene can allow lithium ion energy
The passage enough moved freely, makes β-spodumene possess cation exchange property.β-spodumene（β-Li2O·Al2O3·4Si2O）
Acidified roasting, one of the product that acidic leaching is obtained is lithium slag.This acidic leaching process is a simple dissolving
Exist that β-Li2O Al2O34Si2O and H2OAl2O34Si2O mutually convert in diffusion process, solution system can
Inverse balance.Therefore, the same to β-spodumene of lithium slag equally has cation exchange property, and has selective exchange adsorption to lithium ion
Ability, especially this reversible balance is beneficial to the direction that reaction adsorbed to lithium ion and carried out in the basic conditions.Lithium slag leads to
Cross purifying, be modified, lithium slag adsorbent made from addition coagent and binding agent can operate with the liquid such as seawater and salt lake bittern
Put forward lithium process.
The content of the invention：
A kind of system for the lithium slag adsorbent that lithium is carried for liquid is provided the invention aims to improve the deficiencies in the prior art
Preparation Method, this method raw material is easy to get, and preparation process is simple, and obtained lithium slag adsorbent can be used for low lithium concentration seawater and containing lithium salts
Lake bittern water puies forward lithium technique, while comprehensively utilizing waste resource lithium slag.
The technical scheme is that：
A kind of preparation method of lithium slag adsorbent, it is comprised the following steps that：The purifying of lithium ore deposit waste residue is obtained into refined lithium slag, with refined
0~20% coagent, 1%~20% binding agent and 0-20% water are added on the basis of lithium slag amount, 10 are stirred in 50~300rpm~
60min, shaping after drying, then at 200~700 DEG C of 2~8h of roasting, prepares lithium slag adsorbent.
It is preferred that above-mentioned lithium slag purification process is the one or two of settling methods or direct acidization.
It is preferred that settling methods is to crush lithium ore deposit waste residue to be screened to 60~200 mesh, add water sedimentation, is removed by medium of water
Quartzy impurity in lithium slag；The pickling that it is 0.1~3mol/L with concentration that direct acidization, which is, wherein described acid is hydrochloric acid, sulphur
One kind in acid or nitric acid.
Described coagent is aluminium hydroxide, titanium dioxide, metatitanic acid, titanium sulfate, manganese dioxide, manganese carbonate, sulfuric acid
One or two kinds of mixing of manganese, LiMn2O4.
Described binding agent is polyethylene glycol, polyvinyl alcohol, polyacrylamide, polyvinyl chloride, excessively chliorinated polyvinyl chloride, chlorine
Change alkene, acetylbutyrylcellulose, one or more kinds of mixing of fluororesin.
Beneficial effect：
The present invention's prepares that adsorbent material is simple and easy to get, is the waste residue produced during lithium ore Production By Sulfuric Acid Process lithium carbonate,
The recycling of lithium slag is realized, is conducive to environmental protection.Lithium slag adsorbent prepares with low cost, and preparation process is simple, lithium slag
Adsorbent carries lithium for liquid lithium resource has selectivity high, the advantage such as adsorption-desorption stability is good.
Embodiment：
With reference to instantiation, the invention will be further described, in order to the understanding of the present invention, does not therefore limit
The present invention.
Embodiment 1：
Take lithium ore deposit waste residue to cross 60 mesh sieves, add water gravitational settling, dry, obtain refined lithium slag.Added on the basis of refined lithium slag amount
Enter 18% high molecular polymer binder acetylbutyrylcellulose, in speed of agitator 50rpm mixing 20min aftershapings, drying,
550 DEG C of roasting 4h, are made lithium slag adsorbent.In the simulation bittern that initial Li+ concentration is 100mg/L, solid-to-liquid ratio 0.5g/
100ml, the lithium slag adsorbent is 6.18mg/g to the static adsorbance of lithium at 25 DEG C.
Embodiment 2：
Take lithium ore deposit waste residue to cross 80 mesh sieves, add water gravitational settling, dry 2h.The activity of addition 16% on the basis of refining lithium slag amount
Auxiliary agent aluminium hydroxide, 2% chliorinated polyvinyl chloride and 3% distilled water, mix 30min aftershapings under speed of agitator 50rpm, dry
Dry, lithium slag adsorbent is made in 550 DEG C of roasting 4h.In the simulation bittern that initial Li+ concentration is 100mg/L, solid-to-liquid ratio 0.5g/
100ml, the lithium slag adsorbent is 9.31mg/g to the static adsorbance of lithium at 30 DEG C.
Embodiment 3：
Lithium ore deposit waste residue is taken to cross 100 mesh sieves, the salt Ore Leaching for being 0.5mol/L with concentration after the gravitational settling that adds water, washing depickling is extremely
PH is 7.2, drying.By refine lithium slag amount on the basis of add 4% coagent metatitanic acid H2TiO3,6% polyethylene glycol and
18% distilled water, mixes 60min aftershapings under speed of agitator 100rpm, and the absorption of lithium slag is made in drying, 350 DEG C of roasting 6h
Agent.In initial Li+ concentration in 100mg/L simulation bittern, solid-to-liquid ratio 0.5g/100ml, the lithium slag adsorbent pair at 30 DEG C
The static adsorbance of lithium is 12.77 mg/g.
Embodiment 4：
Lithium ore deposit waste residue is taken to cross 80 mesh sieves, the salt Ore Leaching for being 3mol/L with concentration after the gravitational settling that adds water, washing depickling is to PH
7.5, drying.By refine lithium slag amount on the basis of add 12% coagent manganese dioxide and 6% acetylbutyrylcellulose and
5% distilled water, mixes 30min aftershapings under speed of agitator 100rpm, and lithium slag adsorbent is made in drying, 700 DEG C of roasting 3h.
In initial Li+ concentration in 500mg/L simulation bittern, solid-to-liquid ratio 0.5g/100ml, the lithium slag adsorbent is to lithium at 50 DEG C
Static adsorbance is 29.59mg/g.
Embodiment 5：
Lithium ore deposit waste residue is taken to cross 80 mesh sieves, the sulfuric acid leaching for being 0.1mol/L with concentration after the gravitational settling that adds water, washing depickling to PH
About 7, drying.The coagent titanium sulfate and 2% aluminium hydroxide of addition 4%, 10% poly- second on the basis of refining lithium slag amount
Glycol, 10% chliorinated polyvinyl chloride and 10% distilled water, mix 40min aftershapings under speed of agitator 300rpm, dry,
450 DEG C of roasting 4h, are made lithium slag adsorbent.In initial Li+ concentration in 50mg/L simulation bittern, solid-to-liquid ratio 1g/L, 30 DEG C
The lower lithium slag adsorbent is 10.39mg/g to the static adsorbance of lithium.
Embodiment 6：
Lithium ore deposit waste residue is taken to cross 80 mesh sieves, the sulfuric acid leaching for being 0.5mol/L with concentration after the gravitational settling that adds water, washing depickling to PH
For 7.5, drying.The coagent titanium dioxide of addition 4%, 16% superchlorination alkene and 5% steaming on the basis of refining lithium slag amount
Distilled water, mixes 10min aftershapings under speed of agitator 300rpm, and lithium slag adsorbent is made in drying, 300 DEG C of roasting 7h.Initial
Li+ concentration is in 100mg/L concentrated seawater, solid-to-liquid ratio 1g/L, and the lithium slag adsorbent is to the static adsorbance of lithium at 30 DEG C
13.87mg/g。
Embodiment 7：
Lithium ore deposit waste residue is taken to cross 80 mesh sieves, the nitric acid for being 1mol/L with concentration after the gravitational settling that adds water is leached, washing depickling to PH is
6.5, drying.The coagent aluminium hydroxide and 6% titanium dioxide of addition 6%, 8% fluorine tree on the basis of refining lithium slag amount
Fat, 3% distilled water mixes 10min aftershapings under speed of agitator 200rpm, and the absorption of lithium slag is made in drying, 650 DEG C of roasting 2h
Agent.In initial Li+ concentration in 107mg/L simulation bittern, solid-to-liquid ratio 0.1g/100ml, the lithium slag adsorbent is to lithium at 50 DEG C
Static adsorbance be 11.38mg/g.
Embodiment 8：
Lithium ore deposit waste residue is taken to cross 80 mesh sieves, add water gravitational settling, the nitric acid for being 2mol/L with concentration is leached, washing depickling to PH is 7,
Drying.The coagent metatitanic acid and 6% manganese dioxide of addition 6%, 4% polyvinyl alcohol, 1% on the basis of refining lithium slag amount
Distilled water, 10min aftershapings are mixed under speed of agitator 200rpm, lithium slag adsorbent is made in drying, 700 DEG C of roasting 3h.
Initial Li+ concentration is in 750mg/L simulation bittern, solid-to-liquid ratio 0.5g/100ml, and the lithium slag adsorbent is to the quiet of lithium at 70 DEG C
State adsorbance is 30.20mg/g.
Embodiment 9：
Lithium ore deposit waste residue is taken to cross 80 mesh sieves, add water gravitational settling, the salt Ore Leaching for being 1mol/L with concentration, washing depickling is to PH
6.8, drying.Manganese carbonate to count addition 10% on the basis of refining the quality of lithium slag, 6% polyacrylamide and 10% distilled water,
20min shapings are mixed under 50rpm speeds of agitator, drying is calcined 8h in 200 DEG C, lithium slag adsorbent is made.In initial concentration
For in 10mg/L seawater, solid-to-liquid ratio 0.1g/100ml, the lithium slag adsorbent is 6.78mg/g to the static adsorbance of lithium at 25 DEG C.
Embodiment 10：
Lithium ore deposit waste residue is taken to cross 80 mesh sieves, the salt Ore Leaching for being 0.5mol/L with concentration, washing depickling to PH=7, drying.With refined
The coagent LiMn2O4 LiMnO2 of addition 18%, 1% polyacrylamide and 20% distilled water, are being stirred on the basis of lithium slag amount
10min aftershapings are mixed under mix rotating speed 50rpm, lithium slag adsorbent is made in drying, 200 DEG C of roasting 7h.It is in initial Li+ concentration
In 903mg/L simulation bittern, solid-to-liquid ratio 0.5g/100ml, the lithium slag adsorbent is to the static adsorbance of lithium at 50 DEG C
25.32mg/g。
Embodiment 11：
Lithium ore deposit waste residue is taken to cross 80 mesh sieves, the salt Ore Leaching for being 2mol/L with concentration after the gravitational settling that adds water, washing depickling is to PH
6.5, drying.10% coagent LiMn2O4 LiMnO2 and 10% aluminium hydroxide is added on the basis of refining lithium slag amount, then
The polyacrylamide and 2% distilled water of addition 2%, mix 20min aftershapings, drying, 500 DEG C under speed of agitator 200rpm
4h is calcined, lithium slag adsorbent is made.In initial Li+ concentration in 500mg/L simulation bittern, adsorbent solid-to-liquid ratio 1g/L, 70
The lithium slag adsorbent is 22.63mg/g to the static adsorbance of lithium at DEG C.
Embodiment 12：
Lithium ore deposit waste residue is taken to cross 200 mesh sieves, the salt Ore Leaching for being 0.5mol/L with concentration, washing depickling to PH is 7, drying.With essence
Meter adds 9% coagent manganese sulfate on the basis of the quality of lithium slag processed, adds 5% acetylbutyrylcellulose and 5% distillation
Water, mixes 20min aftershapings under speed of agitator 150rpm, and lithium slag adsorbent is made in drying, 500 DEG C of roasting 4h.Initial
Li+ concentration is in 350mg/L simulation bittern, adsorbent solid-to-liquid ratio 0.5g/100ml, and the lithium slag adsorbent is to lithium at 30 DEG C
Static adsorbance is 15.29mg/g.
Claims (5)
1. a kind of preparation method of lithium slag adsorbent, it is comprised the following steps that：The purifying of lithium ore deposit waste residue is obtained into refined lithium slag, with essence
0~20% coagent, 1%~20% binding agent and 0-20% water are added on the basis of lithium slag amount processed, 10 are stirred in 50~300rpm
~60min, shaping after drying, then at 200~700 DEG C of 2~8h of roasting, prepares lithium slag adsorbent.
2. preparation method as claimed in claim 1, it is characterised in that described coagent be aluminium hydroxide, titanium dioxide,
Metatitanic acid, titanium sulfate, manganese dioxide, manganese carbonate, one or two kinds of mixing of manganese sulfate or LiMn2O4.
3. a kind of lithium slag adsorbent preparation method as claimed in claim 1, it is characterised in that described binding agent is poly- second two
Alcohol, polyvinyl alcohol, polyacrylamide, polyvinyl chloride, chliorinated polyvinyl chloride, superchlorination alkene, acetylbutyrylcellulose or fluororesin
One or more kinds of mixing.
4. a kind of lithium slag adsorbent preparation method as claimed in claim 1, it is characterised in that lithium ore deposit waste residue purification process is attached most importance to
The one or two of power sedimentation or direct acidization.
5. purification process as claimed in claim 4, it is characterised in that settling methods is to crush lithium ore deposit waste residue to be screened to 60
~200 mesh, add water sedimentation；The pickling that it is 0.1~3mol/L with concentration that direct acidization, which is, wherein described acid is hydrochloric acid, sulphur
One kind in acid or nitric acid.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102059860B1 (en) * | 2018-12-05 | 2019-12-27 | 한국지질자원연구원 | Porous absorbent granule and method for producing the same |
| KR20200023884A (en) * | 2018-08-27 | 2020-03-06 | 주식회사 엘지화학 | Lithium ion adsorbent and a method for recovering lithium ion using the same |
| CN115323195A (en) * | 2022-07-13 | 2022-11-11 | 江西赣锋锂业股份有限公司 | Method for extracting lithium from brine by adsorption of lithium smelting slag |
| CN115814755A (en) * | 2022-12-20 | 2023-03-21 | 江苏容汇通用锂业股份有限公司 | Adsorbent for waste residue of phosphorus-lithium aluminum, preparation method and application thereof |
| CN116199256A (en) * | 2023-01-20 | 2023-06-02 | 北京碧水源膜科技有限公司 | Preparation method of titanium-based lithium adsorbent precursor with high adsorption capacity |
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2017
- 2017-08-25 CN CN201710741149.9A patent/CN107324438A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200023884A (en) * | 2018-08-27 | 2020-03-06 | 주식회사 엘지화학 | Lithium ion adsorbent and a method for recovering lithium ion using the same |
| KR102521570B1 (en) | 2018-08-27 | 2023-04-12 | 주식회사 엘지화학 | Lithium ion adsorbent and a method for recovering lithium ion using the same |
| KR102059860B1 (en) * | 2018-12-05 | 2019-12-27 | 한국지질자원연구원 | Porous absorbent granule and method for producing the same |
| CN115323195A (en) * | 2022-07-13 | 2022-11-11 | 江西赣锋锂业股份有限公司 | Method for extracting lithium from brine by adsorption of lithium smelting slag |
| CN115814755A (en) * | 2022-12-20 | 2023-03-21 | 江苏容汇通用锂业股份有限公司 | Adsorbent for waste residue of phosphorus-lithium aluminum, preparation method and application thereof |
| CN116199256A (en) * | 2023-01-20 | 2023-06-02 | 北京碧水源膜科技有限公司 | Preparation method of titanium-based lithium adsorbent precursor with high adsorption capacity |
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Application publication date: 20171107 |