CN107175085A - A kind of material of purifying lithium - Google Patents
A kind of material of purifying lithium Download PDFInfo
- Publication number
- CN107175085A CN107175085A CN201710415736.9A CN201710415736A CN107175085A CN 107175085 A CN107175085 A CN 107175085A CN 201710415736 A CN201710415736 A CN 201710415736A CN 107175085 A CN107175085 A CN 107175085A
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- Prior art keywords
- crosslinked polystyrene
- lithium hydroxide
- lithium
- chlorine ball
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
- C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Medicinal Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a kind of material of purifying lithium：Crosslinked polystyrene chlorine ball dichloroethanes is made into sweller, at a temperature of 20 50 DEG C, 5,10,15,20 four are added by a certain percentage（4 pyridine radicals）Porphyrin reacts, and adds functional amido ionic liquid, and the material applied to foreign ion in removing lithium hydroxide can be made.
Description
Technical field
The present invention relates to a kind of auxiliary agent of purifying lithium, particularly a kind of material of purifying lithium.
Background technology
In recent years, the research emphasis to lithium hydroxide focuses primarily on how further to reduce impurity content, obtain high-purity,
The high grade of transparency, granularity be big and uniform lithium hydroxide product on.It is currently used primarily in production single crystalline chip (such as boron of high pure and high clear four
Sour lithium monocrystalline, the lithium borate monocrystalline of high pure and high clear three etc.), superelevation net product (such as ultra-pure lithium carbonate, purity be 59, i.e.,
More than 99.999%), each side such as green novel energy source (such as high-capacity lithium battery, lithium power vehicle) and nanometer new material,
Microelectronics, digital technology, photoelectron science and technology, novel computer, national defense construction, video transmission, Aero-Space, military science and technology, defend
The various fields such as star communication have extensive and important application, as modern high technology industry is constantly to " ultrapure, ultra-fine, super
Essence, super appearance, ultra micro " direction is developed, and increasingly strong to high-purity, high definition new material demand, its application prospect is very huge.
CN104310430 discloses a kind of impurity-removing method being used in lithium hydroxide preparation technology, belongs to lithium hydroxide system
Ca, Mg method field are removed in standby technique, including after alkalizing and lithium sulfate is converted into lithium hydroxide by freezing analysis sodium, through supercooling
Freezing liquid after freezeout sodium fractional crystallization sodium sulphate, it is characterised in that further comprising the steps of：To the freezing liquid directly at it
Under cryogenic conditions, first carry out coarse filtration and meet after smart filter condition, carry out essence filtering and realize removal of impurities.
CN1312040 provides a kind of method of purification of producing high pure and high clear lithium hydroxide from lithium hydroxide in industrial grade, belongs to hydrogen
Lithia purification technique field, it comprises the steps：(1) industrial raw material lithium hydroxide is filled in a low temperature of 20~30 DEG C
Divide dissolving and fast filtering must remove silicon liquid；(2) when 40~50 DEG C will be heated in reactor except silicon liquid, carbonating purification is added
Reagent, continues to be heated to partial carbonating, the coprecipitation reaction of boiling progress, then carries out filtering to obtain scavenging solution；(3) scavenging solution is added
Heat is concentrated into after 1/3 or visible crystals precipitation, and solid-liquor separation is carried out in time and obtains lithium hydroxide crystallization；(4) by gained lithium hydroxide
Crystallization is purified, bakes dehydration and produce high pure and high clear lithium hydroxide.
The lithium hydroxide preparation technology reported in current document is by the way that analysis sodium is alkalized and freezed to lithium sulfate solution
Technique obtain lithium hydroxide, by freezing analysis sodium fractional crystallization sodium sulphate after freezing liquid.Loss of material can be brought, so needing
Invent a kind of new sorbing material directly to extract impurity in lithium hydroxide from solution, improve the absorption to lithium hydroxide
Ability.
The content of the invention
For the requirement from adsorbing and extracting lithium hydroxide there is provided a kind of material of purifying lithium, its preparation method passes through following
Step is realized：
Crosslinked polystyrene chlorine ball dichloroethanes is made into sweller, consumption is the 200-500% of crosslinked polystyrene chlorine ball weight
(wt)；At a temperature of 20-50 DEG C, 5,10,15,20- tetra- are added（4- pyridine radicals）Porphyrin reacts, and consumption is crosslinked polystyrene
The 1-10% (wt) of chlorine ball weight, adds functional amido ionic liquid, is the 0.1-0.5% of crosslinked polystyrene chlorine ball weight
(wt) 5-15h, is incubated, the adsorbent applied to foreign ion in removing lithium hydroxide can be made.
The crosslinked polystyrene chlorine ball, 5,10,15,20- tetra-（4- pyridine radicals）Porphyrin is commercially available prod.
Described functional amido ionic liquid is 1- amine propyl group -3- methyl imidazolium tetrafluoroborates, 1- amine propyl group -3- first
The product of commercially available prod, such as Chinese Academy of Sciences Lanzhou Chemical Physics Research Institute can be used in base tetrafluoroborate.
Beneficial effects of the present invention：
The present invention has aldehyde functions using crosslinked polystyrene chlorine spherical zone, by 5,10,15,20- tetra-（4- pyridine radicals）Porphyrin,
The structure of 1- amine propyl group -3- methyl imidazolium tetrafluoroborate aminations, porphyrin and imidazoles is complexed with foreign ion, can be improved pair
Foreign ion absorption property in lithium hydroxide, can prepare the Lithium hydroxide of mass percentage content 99.99.
Embodiment
Following examples are only to further illustrate the present invention, are not limitation the scope of protection of the invention.
Embodiment 1
In 1000L reactors, 100Kg crosslinked polystyrene chlorine balls are added, 300Kg dichloroethanes is added；At a temperature of 30 DEG C,
Add 5,10,15,20- tetra-（4- pyridine radicals）Porphyrin reacts, and consumption is 5Kg, adds 0.2Kg1- amine propyl group -3- methylimidazoles four
Borofluoride, is incubated 8h, filters, and drying numbering is SX-1.
Embodiment 2
In 1000L reactors, 100Kg crosslinked polystyrene chlorine balls are added, 200Kg dichloroethanes is added；At a temperature of 20 DEG C,
Add 5,10,15,20- tetra-（4- pyridine radicals）Porphyrin reacts, and consumption is 1Kg, adds 0.1Kg1- amine propyl group -3- methylimidazoles four
Borofluoride, is incubated 5h, filters, drying, and production code member is SX-2.
Embodiment 3
In 1000L reactors, 100Kg crosslinked polystyrene chlorine balls are added, 500Kg dichloroethanes is added；At a temperature of 50 DEG C,
Add 5,10,15,20- tetra-（4- pyridine radicals）Porphyrin reacts, and consumption is 10Kg, adds 20Kg ferric trichlorides, adds 0.5Kg1- amine
Propyl group -3- methyl imidazolium tetrafluoroborates, are incubated 15h, filter, drying, and production code member is SX-3.
Comparative example 1
It is added without 5,10,15,20- tetra-（4- pyridine radicals）Porphyrin, the other the same as in Example 1.Products obtained therefrom numbering is SX-4.
Comparative example 2
It is added without 1- amine propyl group -3- methyl imidazolium tetrafluoroborates, the other the same as in Example 1.Products obtained therefrom numbering is SX-5.
Comparative example 3
It is added without 1- amine propyl group -3- methyl imidazolium tetrafluoroborates, 5,10,15,20- tetra-（4- pyridine radicals）Porphyrin, it is other with real
Apply example 1.Products obtained therefrom numbering is SX-6.
Embodiment 4
Each 5g of material of purifying lithium made from pretreated embodiment 1-3 and comparative example 1-3 is accurately weighed, 250mL tools are placed in
Fill in ground triangular flask in, plus people's 100mL concentration 50mg/L lithium hydroxide in industrial grade, mass percentage content 99.37, by triangle
Bottle vibrates 5h at room temperature, fully after absorption, and filtering, detection calculates the lithium hydroxide concentration in solution after absorption, is shown in Table 1:
Table 1:List after separation material absorption made from this patent
Claims (2)
1. a kind of material of purifying lithium, it is characterised in that its preparation method is to comprise the following steps：
Crosslinked polystyrene chlorine ball dichloroethanes is made into sweller, consumption is the 200-500% of crosslinked polystyrene chlorine ball weight
(wt)；At a temperature of 20-50 DEG C, 5,10,15,20- tetra- are added（4- pyridine radicals）Porphyrin reacts, and consumption is crosslinked polystyrene
The 1-10% (wt) of chlorine ball weight, adds functional amido ionic liquid, is the 0.1-0.5% of crosslinked polystyrene chlorine ball weight
(wt) 5-15h, is incubated, the material applied to foreign ion in removing lithium hydroxide can be made.
2. a kind of sorbing material of purifying lithium according to claim 1, it is characterised in that described functional amido ionic liquid
For 1- amine propyl group -3- methyl imidazolium tetrafluoroborates.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2016104172010 | 2016-06-13 | ||
| CN201610417201.0A CN106084095A (en) | 2016-06-13 | 2016-06-13 | A kind of adsorbing material of purifying lithium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107175085A true CN107175085A (en) | 2017-09-19 |
Family
ID=57846352
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610417201.0A Withdrawn CN106084095A (en) | 2016-06-13 | 2016-06-13 | A kind of adsorbing material of purifying lithium |
| CN201710415736.9A Withdrawn CN107175085A (en) | 2016-06-13 | 2017-06-06 | A kind of material of purifying lithium |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610417201.0A Withdrawn CN106084095A (en) | 2016-06-13 | 2016-06-13 | A kind of adsorbing material of purifying lithium |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115487777B (en) * | 2022-11-18 | 2023-03-07 | 江苏金杉新材料有限公司 | Preparation method of porous particle lithium adsorbent with high adsorption capacity |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225176A (en) * | 2007-12-18 | 2008-07-23 | 南京大学 | Imidazolyl modified complex functional high-crosslinked adsorption resin and preparation method thereof |
| CN102272113A (en) * | 2008-12-30 | 2011-12-07 | 陶氏环球技术有限责任公司 | Process for preparing divinylarene dioxides |
| CN103706325A (en) * | 2013-12-17 | 2014-04-09 | 南京工业大学 | Preparation method of lithium slag adsorbent for liquid extraction of lithium |
| CN103772575A (en) * | 2014-01-22 | 2014-05-07 | 王金明 | Method for preparing parting material for extracting lithium |
-
2016
- 2016-06-13 CN CN201610417201.0A patent/CN106084095A/en not_active Withdrawn
-
2017
- 2017-06-06 CN CN201710415736.9A patent/CN107175085A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225176A (en) * | 2007-12-18 | 2008-07-23 | 南京大学 | Imidazolyl modified complex functional high-crosslinked adsorption resin and preparation method thereof |
| CN102272113A (en) * | 2008-12-30 | 2011-12-07 | 陶氏环球技术有限责任公司 | Process for preparing divinylarene dioxides |
| CN103706325A (en) * | 2013-12-17 | 2014-04-09 | 南京工业大学 | Preparation method of lithium slag adsorbent for liquid extraction of lithium |
| CN103772575A (en) * | 2014-01-22 | 2014-05-07 | 王金明 | Method for preparing parting material for extracting lithium |
Non-Patent Citations (1)
| Title |
|---|
| 曹婉明: ""吸附树脂在工业废水处理中的应用"", 《全国高浓度有机废水处理及工程应用新技术、新设备交流研讨会论文集》 * |
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| Publication number | Publication date |
|---|---|
| CN106084095A (en) | 2016-11-09 |
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Application publication date: 20170919 |
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