CN106046264A - Preparation of lithium hydroxide adsorbent - Google Patents
Preparation of lithium hydroxide adsorbent Download PDFInfo
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- CN106046264A CN106046264A CN201610408097.9A CN201610408097A CN106046264A CN 106046264 A CN106046264 A CN 106046264A CN 201610408097 A CN201610408097 A CN 201610408097A CN 106046264 A CN106046264 A CN 106046264A
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- lithium
- lithium hydrate
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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
- C08F261/00—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00
- C08F261/02—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols
- C08F261/04—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols on to polymers of vinyl alcohol
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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
- B01J20/22—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
- B01J20/267—Cross-linked polymers
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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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The invention relates to preparation of a lithium hydroxide adsorbent. Organic lithium olefin monomers, 1-acetoxyl-1,3-butadiene(R)-tert-butanesulfinamide and vinyl tributanoneoxime silane are introduced in polymerization to prepare the lithium hydroxide adsorbent by polymerization.
Description
Technical field
The present invention relates to the preparation of a kind of adsorbent, the preparation of a kind of Lithium hydrate adsorbent.
Background technology
High-purity hydrogen lithium oxide is elemental lithium in national defense industry, atomic energy industry, aerospace industry and electronic industrial products
Important sources, is widely used in the high-technology field such as new forms of energy and new material.In recent years, the research to Lithium hydrate
Emphasis focuses primarily on and reduces impurity content the most further, obtains that high-purity, the high grade of transparency, granularity be big and uniform Lithium hydrate
On product.
CN104310430 discloses a kind of impurity-removing method in Lithium hydrate preparation technology, belongs to Lithium hydrate system
Except the method field of Ca, Mg in standby technique, including after lithium sulfate is converted into Lithium hydrate by alkalization and freezing analysis sodium, through supercool
Freezing liquid after freezeout sodium fractional crystallization sodium sulfate, it is characterised in that further comprising the steps of: to described freezing liquid directly at it
Under cryogenic conditions, after first carrying out coarse filtration satisfied essence filtercondition, carry out essence filtration and realize remove impurity.The present invention is used for Lithium hydrate
In preparation technology, can simply and efficiently remove Ca/Mg impurity, product quality is greatly improved.
CN102491377 provides a kind of method of lithium hydroxide purifying, and the method comprises the steps: according to containing hydroxide
The raw material of lithium and the mass ratio of water are 1:(3.8～11.8), the raw material containing Lithium hydrate is added to the water dissolving, then removes insoluble
Property material, obtains the clear liquid containing Lithium hydrate；Adding quality in the clear liquid of gained is sheltering of 0.1%～0.3% clear liquid quality
Agent；After to be masked dose dissolves, add the ethanol of water content≤10 mass % under stirring, make the mass concentration of ethanol in solution reach
27%～36%, separate out crystal, after solution is aged, isolated Lithium hydrate crystal；Drench with the water that temperature is 60～80 DEG C again
After washing, it is vacuum dried 2～4 hours at temperature is 60～80 DEG C, obtains highly purified Lithium hydrate.Use the method operation letter
Single, products obtained therefrom purity is more than 99.9% and light transmittance is more than 98.9%, and impurity content is low and few, and the Lithium hydrate response rate reaches
More than 98%, narrow particle size distribution and granule are big.
The Lithium hydrate preparation technology reported in document at present is by lithium sulfate solution alkalization and freezing analysis sodium
Technique obtain Lithium hydrate, through freezing analysis sodium fractional crystallization sodium sulfate after freezing liquid.Loss of material can be brought, so needing
Invent a kind of novel adsorbing material directly to be extracted from solution by Lithium hydrate, improve the absorbability to Lithium hydrate.
Summary of the invention
For from containing the requirement of adsorbing and extracting Lithium hydrate in lithium hydroxide solution, it is provided that a kind of Lithium hydrate adsorbent
Preparation, its preparation method is realized by following steps:
The preparation of step 1. aqueous phase
By weight, 100 parts of pure water 0.5-2 part polyvinyl alcohol of interior addition, stir in a kettle.；
The preparation of step 2. oil phase
By weight, by 100 parts of acrylamides, 50-90 part organolithium olefinic monomer, 20-50 part 1-acetoxyl group-1,3-fourth
Diene (R)-t-butyl sulfonamide, 0.1-0.5 part vinyl tributyl ketoximyl silane mixes, adds 0.5-3 part peroxidating
Benzoyl, stir；
Step 3. polyreaction
It is added to the oil-phase solution prepared in step 1, equipped with in the reactor preparing aqueous phase, react 10-24 at 80-110 DEG C
H, reaction terminates rear blowing, dries, obtains product.
Described organolithium olefinic monomer is tetramethyl-ring pentadiene lithium.
Described tetramethyl-ring pentadiene lithium, 1-acetoxyl group-1,3-butadiene (R)-t-butyl sulfonamide, vinyl
Tributanoximo silane is commercially available prod.
Beneficial effects of the present invention:
The present invention introduces tetramethyl-ring pentadiene lithium as cross-linking comonomer in polymerization, and Lithium hydrate ion is with chemical bond
Pattern is combined in the skeleton of resin, not easily runs off, and can improve the absorbability of Lithium hydrate ion；1-acetoxyl group-1,3-
Butadiene (R)-t-butyl sulfonamide, the addition of vinyl tributyl ketoximyl silane can also improve the absorption to Lithium hydrate
Ability.
Detailed description of the invention
Following example only further illustrate the present invention, are not to limit the scope of protection of the invention.
Embodiment 1
The preparation of step 1. aqueous phase
By weight, in reactor, add 100 parts of pure water, 0.5 part of polyvinyl alcohol, stir.
The preparation of step 2. oil phase
By the oil phase component mixing and stirring of following ratio；
Ingredients weight parts
Acrylamide 100
Tetramethyl-ring pentadiene lithium 65
1-acetoxyl group-1,3-butadiene (R)-t-butyl sulfonamide 33
Vinyl tributyl ketoximyl silane 0.3
Benzoyl peroxide 2
Step 3. polyreaction
It is added to the oil-phase solution prepared in step 2 in step 1, equipped with in the reactor preparing aqueous phase, react 14h at 90 DEG C,
Reaction terminates rear blowing, dries, obtains product.Numbered W-1.
Embodiment 2
The preparation of step 1. aqueous phase
By weight, in reactor, add 100 parts of pure water, 1.5 parts of polyvinyl alcohol, stir.
The preparation of step 2. oil phase
By the oil phase component mixing and stirring of following ratio；
Ingredients weight parts
Acrylamide 100
Tetramethyl-ring pentadiene lithium 50
1-acetoxyl group-1,3-butadiene (R)-t-butyl sulfonamide 20
Vinyl tributyl ketoximyl silane 0.1
Benzoyl peroxide 0.5
Step 3. polyreaction
It is added to the oil-phase solution prepared in step 1, equipped with in the reactor preparing aqueous phase, react 24h, reaction knot at 80 DEG C
Blowing after bundle, dries, obtains product, numbered W-2.
Embodiment 3
The preparation of step 1. aqueous phase
By weight, in reactor, add 100 parts of pure water, 2 parts of polyvinyl alcohol, stir.
The preparation of step 2. oil phase
By the oil phase component mixing and stirring of following ratio；
Ingredients weight parts
Acrylamide 100
Tetramethyl-ring pentadiene lithium 90
1-acetoxyl group-1,3-butadiene (R)-t-butyl sulfonamide 50
Vinyl tributyl ketoximyl silane 0.5
Benzoyl peroxide 3
Step 3. polyreaction
It is added to the oil-phase solution prepared in step 1, equipped with in the reactor preparing aqueous phase, react 10h, reaction knot at 110 DEG C
Blowing after bundle, after drying, obtains product, numbered W-3.
Comparative example 1
It is added without 1-acetoxyl group-1,3-butadiene (R)-t-butyl sulfonamide, the other the same as in Example 1.Products obtained therefrom is numbered
For W-4.
Comparative example 2
It is added without vinyl tributyl ketoximyl silane, the other the same as in Example 1.The numbered W-5 of products obtained therefrom.
Comparative example 2
It is added without tetramethyl-ring pentadiene lithium, the other the same as in Example 1.The numbered W-6 of products obtained therefrom.
Embodiment 4
Accurately weigh each 5g of adsorbent that pretreated embodiment 1-3 and comparative example 1-3 prepare, be placed in 250mL tool plug ground
In triangular flask, add people's 100mL concentration 50mg/L containing Lithium hydrate solion, at room temperature vibrate 5h by triangular flask, fully
After absorption, filtering, detection calculates the Lithium hydrate ion concentration after absorption in solution, is shown in Table 1:
Table 1: catalog after the separation material absorption that this patent prepares
| Production code member | Lithium hydrate ion concentration mg/L in solution after absorption |
| W-1 | 0.7 |
| W-2 | 0.9 |
| W-3 | 0.2 |
| W-4 | 3.3 |
| W-5 | 3.7 |
| W-6 | 12.1 |
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.Any with the present invention it is
Basis, for solving essentially identical technical problem, it is achieved essentially identical technique effect, done simple change, equivalent are replaced
Change or modification etc., be all covered by among protection scope of the present invention.
Claims (2)
1. a preparation for Lithium hydrate adsorbent, its feature its preparation method is to comprise the following steps:
The preparation of step 1. aqueous phase
By weight, 100 parts of pure water 0.5-2 part polyvinyl alcohol of interior addition, stir in a kettle.；
The preparation of step 2. oil phase
By weight, by 100 parts of acrylamides, 50-90 part organolithium olefinic monomer, 20-50 part 1-acetoxyl group-1,3-fourth
Diene (R)-t-butyl sulfonamide, 0.1-0.5 part vinyl tributyl ketoximyl silane mixes, adds 0.5-3 part peroxidating
Benzoyl, stir；
Step 3. polyreaction
It is added to the oil-phase solution prepared in step 1, equipped with in the reactor preparing aqueous phase, react 10-24 at 80-110 DEG C
H, reaction terminates rear blowing, dries, obtains product.
The preparation of a kind of Lithium hydrate adsorbent the most according to claim 1, it is characterised in that described organolithium olefinic monomer
For tetramethyl-ring pentadiene lithium.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610408097.9A CN106046264B (en) | 2016-06-13 | 2016-06-13 | A kind of preparation of lithium hydroxide adsorbent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610408097.9A CN106046264B (en) | 2016-06-13 | 2016-06-13 | A kind of preparation of lithium hydroxide adsorbent |
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| CN106046264A true CN106046264A (en) | 2016-10-26 |
| CN106046264B CN106046264B (en) | 2018-09-18 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4221767A (en) * | 1978-09-05 | 1980-09-09 | The Dow Chemical Company | Recovery of lithium from brines |
| CN102631897A (en) * | 2012-02-14 | 2012-08-15 | 西安蓝晓科技新材料股份有限公司 | Method for preparing lithium adsorbent resin |
| CN104310430A (en) * | 2014-09-30 | 2015-01-28 | 甘孜州泸兴锂业有限公司 | Impurity removal method for lithium hydroxide preparation process |
| CN105294922A (en) * | 2015-11-30 | 2016-02-03 | 王金明 | Lithium separation material preparation method |
-
2016
- 2016-06-13 CN CN201610408097.9A patent/CN106046264B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4221767A (en) * | 1978-09-05 | 1980-09-09 | The Dow Chemical Company | Recovery of lithium from brines |
| CN102631897A (en) * | 2012-02-14 | 2012-08-15 | 西安蓝晓科技新材料股份有限公司 | Method for preparing lithium adsorbent resin |
| CN104310430A (en) * | 2014-09-30 | 2015-01-28 | 甘孜州泸兴锂业有限公司 | Impurity removal method for lithium hydroxide preparation process |
| CN105294922A (en) * | 2015-11-30 | 2016-02-03 | 王金明 | Lithium separation material preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 焦剑等: "《功能高分子材料》", 31 August 2007, 化学工业出版社 * |
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Granted publication date: 20180918 |