CN106046264B - A kind of preparation of lithium hydroxide adsorbent - Google Patents
A kind of preparation of lithium hydroxide adsorbent Download PDFInfo
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- CN106046264B CN106046264B CN201610408097.9A CN201610408097A CN106046264B CN 106046264 B CN106046264 B CN 106046264B CN 201610408097 A CN201610408097 A CN 201610408097A CN 106046264 B CN106046264 B CN 106046264B
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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 present invention relates to a kind of preparations of lithium hydroxide adsorbent, and organolithium olefinic monomer, 1 acetoxyl group, 1,3 butadiene are introduced in polymerization（R）T-butyl sulfonamide, vinyl tributyl ketoximyl silane are aggregated to be prepared.
Description
Technical field
The present invention relates to a kind of preparation of adsorbent, especially a kind of preparation of lithium hydroxide adsorbent.
Background technology
High-purity hydrogen lithia is elemental lithium in national defense industry, atomic energy industry, aerospace industry and electronic industrial products
Important sources are widely used in the high-technology fields such as new energy and new material.In recent years, to the research of lithium hydroxide
How emphasis further decreases impurity content if focusing primarily on, obtain that high-purity, the high grade of transparency, granularity be big and uniform lithium hydroxide
On product.
CN104310430 discloses a kind of impurity-removing method in lithium hydroxide preparation process, belongs to lithium hydroxide system
The method field of Ca, Mg are removed in standby technique, including after alkalizing and freezing analysis sodium and convert lithium sulfate to lithium hydroxide, through supercooling
Freezeout sodium detaches the freezing liquid after sodium sulfate crystal, it is characterised in that further comprising the steps of：To the freezing liquid directly at it
Under cryogenic conditions, after first carrying out the smart filter condition of coarse filtration satisfaction, essence filtering realization removal of impurities is carried out.The present invention is used for lithium hydroxide
In preparation process, Ca/Mg impurity can be simply and efficiently removed, product quality is greatly improved.
CN102491377 provides a kind of method of lithium hydroxide purifying, and this method comprises the following steps：According to containing hydroxide
The raw material of lithium and the mass ratio of water are 1:Raw material containing lithium hydroxide is added to the water dissolving, then removed insoluble by (3.8~11.8)
Property substance, obtains the clear liquid containing lithium hydroxide；The masking that quality is 0.1%~0.3% clear liquid quality is added into the clear liquid of gained
Agent；After to be masked dose of dissolving, it is added with stirring the ethyl alcohol of the mass % of water content≤10, the mass concentration of ethyl alcohol in solution is made to reach
27%~36%, it precipitates crystal, after solution is aged, isolated lithium hydroxide crystal；The water that temperature is 60~80 DEG C is used to drench again
After washing, it is dried in vacuo 2~4 hours at being 60~80 DEG C in temperature, obtains the lithium hydroxide of high-purity.Letter is operated using this method
Single, products obtained therefrom purity is in 99.9% or more and light transmittance 98.9% or more, and impurity content is low and few, and the lithium hydroxide rate of recovery reaches
98% or more, narrow particle size distribution and particle is big.
The lithium hydroxide preparation process reported in document at present is by the way that analysis sodium is alkalized and freezed to lithium sulfate solution
Technique obtain lithium hydroxide, by freezing analysis sodium separation sodium sulfate crystal after freezing liquid.Loss of material can be brought, so needing
It invents a kind of novel sorbing material directly to extract lithium hydroxide from solution, improves the adsorption capacity to lithium hydroxide.
Invention content
For the requirement of the adsorbing and extracting lithium hydroxide from containing lithium hydroxide solution, a kind of lithium hydroxide adsorbent is provided
It prepares, preparation method is realized by following steps：
The preparation of step 1. water phase
By weight, interior in a kettle that 0.5-2 parts of polyvinyl alcohol of 100 parts of pure water are added, it stirs evenly；
The preparation of step 2. oil phase
By weight, by 100 parts of acrylamides, 50-90 parts of organolithium olefinic monomers, 20-50 parts of acetoxyl group -1 1-,
3- butadiene（R）T-butyl sulfonamide, 0.1-0.5 parts of vinyl tributyl ketoximyl silane mixing, adds 0.5-3 parts of mistakes
Benzoyl Oxide stirs evenly；
Step 3. polymerisation
The oil-phase solution prepared is added in step 1 equipped in the reaction kettle for having prepared water phase, 10- is reacted at 80-110 DEG C
24 h, after reaction blowing, drying obtain product.
The organolithium olefinic monomer is tetramethyl-ring pentadiene lithium.
The tetramethyl-ring pentadiene lithium, 1- acetoxyl groups -1,3-butadiene（R）T-butyl sulfonamide, vinyl
Tributanoximo silane is commercial product.
Beneficial effects of the present invention：
The present invention introduces tetramethyl-ring pentadiene lithium as cross-linking comonomer in polymerization, and lithium hydroxide ion is with chemistry
The pattern of key is incorporated in the skeleton of resin, is not easily runed off, and the adsorption capacity of lithium hydroxide ion can be improved；1- acetoxyl groups-
1,3- butadiene（R）The addition of t-butyl sulfonamide, vinyl tributyl ketoximyl silane can also be improved to lithium hydroxide
Adsorption capacity.
Specific implementation mode
Following embodiment is only to further illustrate the present invention, and is not limitation the scope of protection of the invention.
Embodiment 1
The preparation of step 1. water phase
By weight, 100 parts of pure water are added in reaction kettle, 0.5 part of polyvinyl alcohol stirs evenly.
The preparation of step 2. oil phase
The oil phase component of following ratio is mixed evenly；
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. polymerisation
The oil-phase solution prepared in step 2 is added in step 1 equipped in the reaction kettle for having prepared water phase, is reacted at 90 DEG C
14h, after reaction blowing, drying obtain product.Number is W-1.
Embodiment 2
The preparation of step 1. water phase
By weight, 100 parts of pure water are added in reaction kettle, 1.5 parts of polyvinyl alcohol stir evenly.
The preparation of step 2. oil phase
The oil phase component of following ratio is mixed evenly；
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. polymerisation
The oil-phase solution prepared is added in step 1 equipped in the reaction kettle for having prepared water phase, is reacted for 24 hours, instead at 80 DEG C
Blowing after answering, drying, obtains product, number W-2.
Embodiment 3
The preparation of step 1. water phase
By weight, 100 parts of pure water are added in reaction kettle, 2 parts of polyvinyl alcohol stir evenly.
The preparation of step 2. oil phase
The oil phase component of following ratio is mixed evenly；
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. polymerisation
The oil-phase solution prepared is added in step 1 equipped in the reaction kettle for having prepared water phase, 10h is reacted at 110 DEG C, instead
Blowing after answering after drying, obtains product, number 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
Number is W-4.
Comparative example 2
It is added without vinyl tributyl ketoximyl silane, the other the same as in Example 1.Products obtained therefrom number is W-5.
Comparative example 2
It is added without tetramethyl-ring pentadiene lithium, the other the same as in Example 1.Products obtained therefrom number is W-6.
Embodiment 4
Each 5g of adsorbent made from pretreated embodiment 1-3 and comparative example 1-3 is accurately weighed, 250mL tool plugs are placed in
In ground triangular flask, adds the solion containing lithium hydroxide of people's 100mL concentration 50mg/L, triangular flask is vibrated into 5h at room temperature,
Fully after absorption, filtering, the lithium hydroxide ion concentration after detection calculating absorption in solution is shown in Table 1:
Table 1:List after separation material absorption made from this patent
| Product identification | Lithium hydroxide ion concentration mg/L after absorption in solution |
| W-1 | 0.7 |
| W-2 | 0.9 |
| W-3 | 0.2 |
| W-4 | 3.3 |
| W-5 | 3.7 |
| W-6 | 12.1 |
It these are only specific embodiments of the present invention, but the technical characteristic of the present invention is not limited thereto.It is any with this hair
Based on bright, to solve essentially identical technical problem, essentially identical technique effect is realized, made simple change, etc.
With replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (1)
1. a kind of preparation of oximido adsorbent of lithium hydroxide, it is characterised in that include the following steps：
The preparation of step 1. water phase
By weight, interior in a kettle that 0.5-2 parts of polyvinyl alcohol of 100 parts of pure water are added, it stirs evenly；
The preparation of step 2. oil phase
By weight, by 100 parts of acrylamides, 50-90 parts of tetramethyl-ring pentadiene lithiums, 20-50 parts of 1- acetoxyl groups -1,3-
Butadiene（R）T-butyl sulfonamide, 0.1-0.5 parts of vinyl tributyl ketoximyl silane mixing, adds 0.5-3 parts of peroxides
Change benzoyl, stir evenly；
Step 3. polymerisation
The oil-phase solution prepared is added in step 1 equipped in the reaction kettle for having prepared water phase, 10-24 is reacted at 80-110 DEG C
H, after reaction blowing, drying obtain lithium hydroxide oximido adsorbent.
Priority Applications (1)
| 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 |
|---|---|---|---|
| CN201610408097.9A CN106046264B (en) | 2016-06-13 | 2016-06-13 | A kind of preparation of lithium hydroxide adsorbent |
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| CN106046264A CN106046264A (en) | 2016-10-26 |
| CN106046264B true CN106046264B (en) | 2018-09-18 |
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Family Cites Families (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 |
| CN102631897B (en) * | 2012-02-14 | 2015-03-25 | 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 |
| CN105294922B (en) * | 2015-11-30 | 2017-11-28 | 浙江迪特西科技有限公司 | A kind of preparation method of lithium separation material |
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