CN110302764A - A kind of surface improved microballoon of superelevation and its preparation method and application - Google Patents
A kind of surface improved microballoon of superelevation and its preparation method and application Download PDFInfo
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- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
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Abstract
The invention discloses surface improved microballoons of a kind of superelevation and its preparation method and application, comprising the following steps: low cross linked polystyrene microballoon is added in solvent, after being swollen 1h, paraphthaloyl chloride is slowly added to, stirring at normal temperature；Aluminum trichloride solution is added in the above-mentioned solution being prepared, control system temperature is at 10 DEG C ~ 20 DEG C, after addition, is warming up to 35 DEG C ~ 45 DEG C, carries out Friedel-Crafts reaction 2h ~ 4h, adsorbed the superelevation specific surface polystyrene microsphere of alchlor；Obtained superelevation specific surface polystyrene microsphere is slowly added to ammonium hydroxide under mechanical stirring, after addition, pH, normal-temperature reaction 8h ~ 16h is adjusted, obtains the superelevation specific surface polystyrene microsphere of doping aluminium hydroxide.The surface improved microballoon of obtained superelevation is applied to the lithium in adsorbing and extracting liquid.The surface improved microballoon of superelevation of the invention has the advantages that high specific surface area, property stabilization, without molten damage, can keep the ability of higher absorption lithium, can be recycled.
Description
Technical field
The present invention relates to surface improved microballoons of a kind of superelevation and its preparation method and application, belong to high molecular material preparation
And applied technical field.
Background technique
Lithium is the most light alkali metal element of nature, is known as " energy metal of 21 century ".Lithium metal and compound exist
The traditional fields such as metallurgy, manufacture, glass ceramics, petrochemical industry, weaving, synthetic rubber, lubriation material, medical treatment are widely used.Closely
Nian Lai, lithium are also more and more important in fields such as aerospace, nuclear energy, battery power and lithium-aluminium alloys, it has also become in industry very
Important metal.
The main preservation of lithium resource is in salt lake and granite pegmatite deposit, and wherein saline lake lithium resource accounts for global lithium reserves basis
87%.With the growth of the market demand, mineral lithium resource seems that supply falls short of demand, and cost of winning is high, mentions from salt lake bittern
Taking the lithium resource of low cost becomes irresistible trend.Therefore, it has very important significance to the extraction of liquid lithium.
It is existing by high molecular material be rolled into big size particle materials applied to lithium extract method mainly have inorganic salt spray
Comminution granulation, such as silicate；Agarose, polyacrylamide secondary cross-linking are such as used in chemical pack；Chemical polymerization, such as acrylic acid
Ester, divinylbenzene, aluminium-hydroxide powder polymerize balling-up；Absorption method, after porous polymer microsphere surface functionalization, absorption three
Aluminium chloride, hydrolysis obtain the microballoon of aluminium hydroxide.But inorganic spray granulation needs to consume big energy, will cause into
This is excessively high；Chemistry package and chemical crosslinking are all to be carried out by external monomer or macromolecule to existing aluminium-hydroxide powder
Solidify, in solidification process, aluminium hydroxide absorption is insecure, and obtained adsorbent specific surface is not high, hole appearance is lower；Adsorb legal system
Standby material is easy to fall off, and stability is bad.
United States Patent (USP) US4221767 is disclosed LiCl2Al (OH)3·nH2O is carried in anion exchange resin
Method.Specific method is that aluminium ion, then the precipitated aluminium hydroxide in duct are first enriched in resin duct, then uses lithium hydroxide
It is reacted with aluminium hydroxide in resin, is finally transformed into LiCl2Al (OH) again3·nH2O.This method solve active inorganic particles
Loading problem, maintain it and propose lithium activity, but the Kong Rong of anion exchange resin and specific surface area are relatively low.
Patent publication No. be CN106745008A patent disclose preparation high-performance brine mention lithium adsorbent method and
Its adsorbent prepared, preparation high-performance brine propose the method for lithium adsorbent using in situ polymerization method, by active hydrogen-oxygen
Change aluminium powder body to be dispersed in absorption resin duct, then reacted with lithium salt solution, improves reaction efficiency, it is ensured that the work of adsorbent
Property.This method is wound using the crosslinking of resin nano hole inner macromolecule chain, effectively inhibits the loss of reactive nanoparticles, it is ensured that
The service life of adsorbent.But the preparation method that the high-performance brine of this method mentions lithium adsorbent is complicated, specific surface area is low, living
It is difficult to control to change efficiency, full porous structure cannot be formed.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies of existing technologies, it is surface improved micro- to provide a kind of superelevation
Ball and its preparation method and application is prepared into the surface improved microballoon of superelevation by will be microsphere modified, have specific surface area it is high,
The advantages of property is stable, without molten damage can keep the ability of higher absorption lithium, can be recycled.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of preparation method of the surface improved microballoon of superelevation, comprising the following steps:
(1) low cross linked polystyrene microballoon is added in solvent, after being swollen 1h, paraphthaloyl chloride is slowly added to,
Stirring at normal temperature；
(2) aluminum trichloride solution is added in the solution that step (1) is prepared, control system temperature is 10 DEG C~20
DEG C, after addition, 35 DEG C~45 DEG C are warming up to, Friedel-Crafts reaction 2h~4h is carried out, has been adsorbed the superelevation ratio of alchlor
Surface polystyrene microsphere；
(3) the superelevation specific surface polystyrene microsphere that step (2) obtains is slowly added to ammonium hydroxide under mechanical stirring, is added
After, pH, normal-temperature reaction 8h~16h are adjusted, the superelevation specific surface polystyrene microsphere of doping aluminium hydroxide is obtained.
By using above-mentioned technical proposal, the modified microballoon of superhigh specific surface area, preparation side are prepared by three-step reaction
Method is simple, and the material of formation is a kind of full porous structure, and the spacing of molecule interchain only has 10 nanometers, can be effectively by hydrogen-oxygen
Change aluminium powder to be fixed between strand, to increase stability.
Preferably, the solvent in the step (1) is one of methylene chloride, dichloroethanes or chloroform.
Preferably, the aluminum trichloride solution in the step (2) the preparation method comprises the following steps: alchlor is added to nitrobenzene
Or in nitromethane, stirring and dissolving obtains clear solution.
It is anti-to carry out Fu Ke so that alchlor and paraphthaloyl chloride form complex by using above-mentioned technical proposal
It answers, so that polystyrene microsphere adsorbs alchlor.
Preferably, the ammonia concn in the step (3) is 1mol/L~3mol/L.
Preferably, the pH in the step (3) is 9~11.
It is obtained by using above-mentioned technical proposal by the aluminium reaction for being adsorbed in polystyrene microsphere at aluminium hydroxide
Adulterate the superelevation specific surface polystyrene microsphere of aluminium hydroxide.
Meanwhile the present invention provides a kind of surface improved microballoons of superelevation, it is surface improved micro- by a kind of above-mentioned superelevation
The preparation method of ball is prepared.
Preferably, the microspherulite diameter is 200 μm~400 μm.
By using above-mentioned technical proposal, the microballoon with a certain range partial size is obtained, so that its adsorption capacity is stablized.
The present invention also provides a kind of applications of the surface improved microballoon of superelevation lithium in adsorbing and extracting liquid.
Preferably, the application method is the surface improved microballoon of superelevation to be added in brine containing lithium to adsorb, then use water
The lithium ion of absorption is eluted, lithium adsorbance is measured.
By using above-mentioned technical proposal, the surface improved microballoon of superelevation lithium in adsorbing and extracting brine is effectively realized
Using operating method is simple.
In conclusion the invention has the following advantages:
(1) the modified microballoon of superhigh specific surface area is prepared by three-step reaction in the present invention, first makes the low friendship of polymer microsphere
Polystyrene microspheres swell, then with superelevation specific surface microballoon is formed after alchlor, paraphthaloyl chloride reaction, finally by three
Aluminium chloride is directly translated into that aluminium hydroxide is immobilized in microballoon, and preparation method is simple with aqueous slkali, and the microballoon property of formation is stablized,
Not easily to fall off and collapsing；
(2) the modified microballoon of the superhigh specific surface area that the present invention is prepared is a kind of full porous structure, and in strand
Between also will form the cage structure that spacing only has 10 nanosizeds, aluminium-hydroxide powder effectively can be fixed on strand
Between, to increase stability；
(3) the modified microballoon of superhigh specific surface area of the invention has good property in the application of lithium in adsorbing and extracting liquid
Can, lithium adsorbance average value can reach 38mg/g, and not have any molten damage after repeatedly adsorbing and eluting absorption, keep higher
The ability of lithium is adsorbed, can be recycled.
Detailed description of the invention
Fig. 1 is the microscope figure of the surface improved microballoon of superelevation of the invention；
Fig. 2 is the graph of pore diameter distribution of the surface improved microballoon of superelevation of the invention.
Specific embodiment
The invention will be further described below in conjunction with the accompanying drawings.Following embodiment is only used for clearly illustrating the present invention
Technical solution, and not intended to limit the protection scope of the present invention.
A kind of preparation method of the surface improved microballoon of superelevation, comprising the following steps:
(1) low cross linked polystyrene microballoon is added in solvent, after being swollen 1h, paraphthaloyl chloride is slowly added to,
Stirring at normal temperature；
(2) aluminum trichloride solution is added in the solution that step (1) is prepared, control system temperature is 10 DEG C~20
DEG C, after addition, 35 DEG C~45 DEG C are warming up to, Friedel-Crafts reaction 2h~4h is carried out, has been adsorbed the superelevation ratio of alchlor
Surface polystyrene microsphere；
(3) the superelevation specific surface polystyrene microsphere that step (2) obtains is slowly added to ammonium hydroxide under mechanical stirring, is added
After, pH, normal-temperature reaction 8h~16h are adjusted, the superelevation specific surface polystyrene microsphere of doping aluminium hydroxide is obtained.
As shown in Figure 1, a kind of microscope figure of the surface improved microballoon of superelevation of the invention, by a kind of above-mentioned superelevation ratio
The preparation method of surface modified microballons is prepared, as can be seen from the figure microsphere features smooth surface, the aluminium hydroxide and height of generation
The good hydridization of molecule microballoon is together.
As shown in Fig. 2, a kind of pore-size distribution master for the superelevation specific surface lithium adsorption microspheres being prepared by above-mentioned method
20nm is concentrated on hereinafter, pore-size distribution is reasonable, is not easy to collapse.
The surface improved microballoon of a kind of superelevation of the invention applies the lithium in adsorbing and extracting liquid.
Embodiment 1
A kind of preparation method of the surface improved microballoon of superelevation, comprising the following steps:
(1) 100g low cross linked polystyrene microballoon is added in 500mL methylene chloride, after being swollen 1h, by 100g to benzene
Dimethyl chloride is slowly added to, stirring at normal temperature；
(2) 100g aluminum trichloride solution is added in the solution that step (1) is prepared, control system temperature is 10
DEG C, after addition, 35 DEG C are warming up to, Friedel-Crafts reaction 2h is carried out, has been adsorbed the superelevation specific surface polyphenyl second of alchlor
Alkene microballoon；
(3) the superelevation specific surface polystyrene microsphere that step (2) obtains is slowly added to 500mL concentration under mechanical stirring
For the ammonium hydroxide of 1mol/L, after addition, adjusting pH is 9, normal-temperature reaction 8h, and the superelevation specific surface for obtaining doping aluminium hydroxide is poly-
Phenylethylene micro ball.
The partial size of the surface improved microballoon of obtained superelevation is 200 μm~400 μm.
It takes 10 grams of micro-sphere materials to adsorb 15min in brine containing lithium, is washed with water the lithium ion of De contamination, measurement lithium absorption
Amount, is repeated 20 times experiment, is averaged, and obtained microballoon lithium adsorbance is as shown in table 1 below, and there is no any molten damages.
Table 1
Embodiment 2
A kind of preparation method of the surface improved microballoon of superelevation, comprising the following steps:
(1) 100g low cross linked polystyrene microballoon is added in 500mL methylene chloride, after being swollen 1h, by 100g to benzene
Dimethyl chloride is slowly added to, stirring at normal temperature；
(2) 100g aluminum trichloride solution is added in the solution that step (1) is prepared, control system temperature is 15
DEG C, after addition, 40 DEG C are warming up to, Friedel-Crafts reaction 3h is carried out, has been adsorbed the superelevation specific surface polyphenyl second of alchlor
Alkene microballoon；
(3) the superelevation specific surface polystyrene microsphere that step (2) obtains is slowly added to 500mL concentration under mechanical stirring
For the ammonium hydroxide of 2mol/L, after addition, adjusting pH is 10, normal-temperature reaction 12h, obtains the superelevation specific surface of doping aluminium hydroxide
Polystyrene microsphere.
The partial size of the surface improved microballoon of obtained superelevation is 200 μm~400 μm.
It takes 10 grams of micro-sphere materials to adsorb 15min in brine containing lithium, is washed with water the lithium ion of De contamination, measurement lithium absorption
Amount, is repeated 20 times experiment, is averaged, and obtained microballoon lithium adsorbance is as shown in table 2 below, and there is no any molten damages.
Table 2
Embodiment 3
A kind of preparation method of the surface improved microballoon of superelevation, comprising the following steps:
(1) 100g low cross linked polystyrene microballoon is added in 500mL methylene chloride, after being swollen 1h, by 100g to benzene
Dimethyl chloride is slowly added to, stirring at normal temperature；
(2) 100g aluminum trichloride solution is added in the solution that step (1) is prepared, control system temperature is 20
DEG C, after addition, 45 DEG C are warming up to, Friedel-Crafts reaction 4h is carried out, has been adsorbed the superelevation specific surface polyphenyl second of alchlor
Alkene microballoon；
(3) the superelevation specific surface polystyrene microsphere that step (2) obtains is slowly added to 500mL concentration under mechanical stirring
For the ammonium hydroxide of 3mol/L, after addition, adjusting pH is 11, normal-temperature reaction 16h, obtains the superelevation specific surface of doping aluminium hydroxide
Polystyrene microsphere.
The partial size of the surface improved microballoon of obtained superelevation is 200 μm~400 μm.
It takes 10 grams of micro-sphere materials to adsorb 15min in brine containing lithium, is washed with water the lithium ion of De contamination, measurement lithium absorption
Amount, is repeated 20 times experiment, is averaged, and obtained microballoon lithium adsorbance is as shown in table 3 below, and there is no any molten damages.
Table 3
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of the surface improved microballoon of superelevation, characterized in that the following steps are included:
(1) low cross linked polystyrene microballoon is added in solvent, after being swollen 1h, paraphthaloyl chloride is slowly added to, room temperature
Stirring；
(2) aluminum trichloride solution is added in the solution that step (1) is prepared, control system temperature adds at 10 DEG C ~ 20 DEG C
After entering, 35 DEG C ~ 45 DEG C are warming up to, Friedel-Crafts reaction 2h ~ 4h is carried out, has been adsorbed the superelevation specific surface polyphenyl of alchlor
Ethylene microballoon；
(3) the superelevation specific surface polystyrene microsphere that step (2) obtains is slowly added to ammonium hydroxide under mechanical stirring, addition finishes
Afterwards, pH, normal-temperature reaction 8h ~ 16h are adjusted, the superelevation specific surface polystyrene microsphere of doping aluminium hydroxide is obtained.
2. a kind of preparation method of the surface improved microballoon of superelevation according to claim 1, characterized in that the step
(1) solvent in is one of methylene chloride, dichloroethanes or chloroform.
3. a kind of preparation method of the surface improved microballoon of superelevation according to claim 1, characterized in that the step
(2) aluminum trichloride solution in the preparation method comprises the following steps: alchlor is added in nitrobenzene or nitromethane, stirring and dissolving,
Obtain clear solution.
4. a kind of preparation method of the surface improved microballoon of superelevation according to claim 1, characterized in that the step
(3) ammonia concn in is 1mol/L ~ 3mol/L.
5. a kind of preparation method of the surface improved microballoon of superelevation according to claim 1, characterized in that the step
(3) pH in is 9 ~ 11.
6. a kind of surface improved microballoon of superelevation, characterized in that a kind of superelevation as described in any one of claim 1 ~ 5 compares table
The preparation method of the modified microballoon in face is prepared.
7. the surface improved microballoon of a kind of superelevation according to claim 6, characterized in that the microspherulite diameter be 200 μm ~
400μm。
8. a kind of application of the surface improved microballoon of superelevation lithium in adsorbing and extracting liquid.
9. a kind of application of the surface improved microballoon of superelevation lithium in adsorbing and extracting liquid according to claim 8, described
Application method is that the surface improved microballoon of superelevation is added in brine containing lithium to adsorb, and is washed with water the lithium ion of De contamination, surveys
Determine lithium adsorbance.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113509912A (en) * | 2020-11-25 | 2021-10-19 | 中国科学院青海盐湖研究所 | Preparation method of lithium ion sieve adsorbent particles for extracting liquid lithium resources |
| CN114210370A (en) * | 2021-12-20 | 2022-03-22 | 南京亘闪生物科技有限公司 | Preparation method of catalyst microspheres for preparing ethyl acetate |
| CN116899525A (en) * | 2023-09-01 | 2023-10-20 | 江苏海普功能材料有限公司 | Lithium extraction adsorbent and preparation method and application thereof |
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| CN113509912A (en) * | 2020-11-25 | 2021-10-19 | 中国科学院青海盐湖研究所 | Preparation method of lithium ion sieve adsorbent particles for extracting liquid lithium resources |
| CN114210370A (en) * | 2021-12-20 | 2022-03-22 | 南京亘闪生物科技有限公司 | Preparation method of catalyst microspheres for preparing ethyl acetate |
| CN116899525A (en) * | 2023-09-01 | 2023-10-20 | 江苏海普功能材料有限公司 | Lithium extraction adsorbent and preparation method and application thereof |
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