CN108435142A - A kind of granular ion crossover adsorbent, preparation and the application of absorption rubidium or lithium - Google Patents
A kind of granular ion crossover adsorbent, preparation and the application of absorption rubidium or lithium Download PDFInfo
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- CN108435142A CN108435142A CN201810368182.6A CN201810368182A CN108435142A CN 108435142 A CN108435142 A CN 108435142A CN 201810368182 A CN201810368182 A CN 201810368182A CN 108435142 A CN108435142 A CN 108435142A
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- 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
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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—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
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- 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
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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- 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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- 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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
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- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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- B01J2220/00—Aspects relating to sorbent materials
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- B01J2220/48—Sorbents characterised by the starting material used for their preparation
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- 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
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a kind of granular ion crossover adsorbent, preparation and the applications of absorption rubidium or lithium.Powdered lithium ion sieve or rubidium ion exchanger are mixed with water soluble polymer prepolymer, after adding water to be sufficiently stirred heating melting, multi-group crosslink agent is added, increase temperature, heat preservation reflux makes prepolymer that build condensation reaction further occur, and at thick space network polymer, is evaporated under reduced pressure, dehydrating and curing, Mechanical Crushing forming.The sorbent preparation method of the present invention is simple, and operation adjusts mild.Because of the condensation polymer for having selected the stronger polymer monomer of hydrophily to be formed, the adsorption and desorption speed of adsorbent.
Description
Technical field
The invention belongs to adsorbent preparing technical fields, and in particular to a kind of granular ion crossover adsorbent, prepare and
Adsorb the application of rubidium or lithium.
Background technology
Increasing to the demand of lithium in the world, lithium is referred to as " energy metal " " metal of future world "；Rubidium metal is
One of important rare metal is also applied to civil field in addition to applied to military project department and science and technology field.However the world
Upper land lithium resource total amount is provided far from the distant view market demand for meeting lithium, in contrast seawater, brine, well halogen lithium resource and rubidium
Source total amount is very huge.Currently, the method that well known salt lake bittern carries lithium mainly have the precipitation method, solvent extraction, roasting method and
Adsorbent method.Adsorbent method has larger advantage than other methods from the consideration of economical and environmentally friendly angle, especially from low-grade
Lithium or rubidium are carried in brine.The key of this method is to seek that adsorptive selectivity is good, cyclic utilization rate is high and the suction of advantage of lower cost
Attached dose.But no matter adsorbent in the prior art is not also especially to make us full in terms of adsorption effect or recycling rate of waterused
Meaning.
Invention content
For the defect and deficiency of existing technology of preparing, the object of the present invention is to provide a kind of absorption of granular ion crossover
Agent, preparation and the application of absorption rubidium or lithium, it is therefore an objective to it solves in existing rubidium, lithium ion exchanged type adsorbent forming technique, it is hydrophobic
Property material embedding adsorbent bad hydraulic permeability influence performance of the adsorbent, hydrophilic material prepare adsorbent in reuse it is easy because
Material molten causes unstable problem.
To achieve the goals above, the present invention is realised by adopting the following technical scheme：
A kind of preparation method of granular ion crossover adsorbent, by powdery ion-exchanger and water soluble polymer pre-polymerization
After object mixed melting, multi-group crosslink agent is added, increases temperature, it is anti-that heat preservation reflux makes prepolymer that build condensation further occur
It answers, at thick space network polymer, is shaped through reduction vaporization, dehydrating and curing and Mechanical Crushing successively to obtain the final product.
Optionally, the water soluble polymer prepolymer is in pollopas, melmac and water soluble starch
One or more kinds of mixtures.
Optionally, the powdery ion-exchanger is lithium ion sieve or rubidium ion exchanger；
The lithium ion sieve is lithium manganese oxysome lithium ion sieve Li1+xMn2-xO4, 0≤x≤0.33；
The rubidium ion exchanger is ammonium phosphomolybdate or tungsten ammonium molybdate；
The mass ratio of powdery ion-exchanger and water soluble polymer prepolymer is 1~3：1.
Optionally, the temperature of powdery ion-exchanger and water soluble polymer prepolymer mixed melting is 80 DEG C.
Optionally, the multi-group crosslink agent is polyalcohol or polyacid containing ternary or quaternary functional group；
Polyalcohol containing ternary or quaternary functional group is selected from at least one of glycerine and pentaerythrite；
Polyacid containing ternary or quaternary functional group is selected from at least one of oxalic acid, malonic acid, citric acid and acetic anhydride.
Optionally, the addition of the multi-group crosslink agent is the 30% of water soluble polymer pre-polymerization amount of substance；
2~4h of reaction time of the build condensation reaction, reaction temperature are 100~120 DEG C.
Optionally, the negative pressure of the reduction vaporization and dehydrating and curing is 0.1MPa, and temperature is 100 DEG C；
The equipment of Mechanical Crushing is slot type spreading crusher, and the particle size range for being crushed molding adsorbent is 1~3mm.
A kind of granular ion crossover adsorbent, the adsorbent use the preparation of the granular ion crossover adsorbent
Method is prepared.
The adsorbent that the preparation method of the granular ion crossover adsorbent is prepared for adsorbing and extracting rubidium from
The application of son or lithium ion.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) offer of the present invention prepares granular ion crossover adsorbent, has used hydrophilicity prepolymer embedding, build condensation
The method of polymerization crosslinking solidification, Mechanical Crushing forming, it is good that obtained ionic adsorbent maintains hydrophilic polymer material
Good water permeable ability, condition is provided for rubidium, lithium ion exchanged.Efficiently solve current adsorbent forming technique, by PVC or
The hydrophobic polymers such as PVDF coat ion sieve, cause ion sieve that cannot effectively be contacted with water phase and exchange, and influence adsorbent
The problem of absorption property；
(2) ion-exchange type adsorbent provided by the invention, because good hydrogen bond action, water and adsorbent can be generated with water
Content can be exchanged well, and therefore, the rate of adsorption is fast, and parsing rate is fast.Be conducive to improve rubidium/lithium production capacity.
(3) adsorbent preparation process provided by the invention is simple, and operation is flexible, and production efficiency is high, at low cost.For example,
" method that JP2002282684A is used to manufacture porous prilled lithium adsorbent " provides a kind of for producing a kind of lithium adsorbent
Method, the adsorbent of lithium production is by a kind of method containing lithium manganese oxide in the powder, and a kind of powdered water-can
Molten pore former and organic binder is to mix the mixture pelleting, and the particle is to be immersed in water, solvable to elute the water-
Pore former, and contacted with acidic aqueous solution, to elute lithium；Binder used in it is cellular PVC, is had excellent
Lithium selective absorption is stable aqueous solution, it is seen then that the pore former selected in the document is aqueous soluble, but is bonded
Agent, which is still, is not readily dissolved in water, its adsorption efficiency also has the space promoted in actual use, the aqueous pre-polymerization with the present invention
Object is different, and the theory of preparation is also different.
Description of the drawings
Attached drawing is for providing further understanding of the disclosure, and a part for constitution instruction, with following tool
Body embodiment is used to explain the disclosure together, but does not constitute the limitation to the disclosure.In the accompanying drawings：
Fig. 1 is the SEM figures for the granular ion crossover adsorbent that embodiment 1 is prepared, the amplification that figure a is 1000 times
Figure, the enlarged drawing that figure b is 5000 times；
Fig. 2 is the SEM figures for the granular ion crossover adsorbent that embodiment 2 is prepared, and schemes the enlarged drawing that a is 200 times,
Scheme the enlarged drawing that b is 500 times；
Fig. 3 is the SEM figures for the granular ion crossover adsorbent that embodiment 3 is prepared, and schemes the enlarged drawing that a is 500 times,
Scheme the enlarged drawing that b is 5000 times；
The present invention is illustrated below in conjunction with specification drawings and specific embodiments.
Specific implementation mode
The preparation method of the granular ion crossover adsorbent of the present invention is to exchange powdered lithium ion sieve or rubidium ion
Agent is mixed with water soluble polymer prepolymer, and after heating melting, multi-group crosslink agent is added, and increases temperature, and heat preservation reflux makes
Build condensation reaction further occurs for prepolymer, at thick space network polymer, is evaporated under reduced pressure, dehydrating and curing, Mechanical Crushing at
Shape.
The granular ion crossover adsorbent that the present invention is prepared is mainly used for carrying from seawater, brine, lepidolite acidleach
Lithium raffinate, lithium carbonate precipitation carry lithium raffinate etc., adsorbing and extracting rubidium ion or lithium ion.
Specific embodiments of the present invention are given below, it should be noted that the invention is not limited in following specific examples
In, all equivalent transformations made on the basis of the technical solutions of the present application each falls within protection scope of the present invention.
Embodiment 1:
By 20g lithium manganese oxysome lithium ion sieves Li1.6Mn1.6O4The urine aldehyde tree for being 8000 with 5g water soluble starch and 5g molecular weight
Fat mixes, and is heated to 80 DEG C of fully meltings, citric acid 5g, 1/1 mixture of pentaerythrite and glycerine are added in mixed liquor
5g, 100 DEG C of heating reflux reaction 2h in closed container, by the lower 80 DEG C of reduction vaporization of mixture of viscous form 0.1MPa, dehydrating and curing,
With the granular adsorbent that slot type spreading disintegrating apparatus Mechanical Crushing is 1~3mm grain sizes.
The pattern for the adsorbent that the present embodiment is prepared as shown in Figure 1, scheme by the enlarged drawing that the figure a in Fig. 1 is 1000 times
The enlarged drawing that b is 5000 times；
By lithium ion adsorbent 2g (lithium ion sieve powder content is 1g), parsed in the hydrochloric acid solution of 0.5mol/L
48h, until the lithium concentration in parsing eluent no longer changes.It is placed in 200mL and contains Li+A concentration of 200mg/L, Mg2+
A concentration of 23g/L, K+A concentration of 15g/L, Na+In the brine of a concentration of 110g/L, carried out under 300 revs/min of shaking speed from
Sub- exchange adsorption carries lithium.Lithium concentration no longer declines after dropping to 125mg/L in stoste after 6h, and absorption reaches balance, calculates and inhales
Attached dose of adsorbance is 15mg/g (in terms of the powder lithium ion sieve quality in adsorbent).Adsorbent is immersed in 100mL's
In the hydrochloric acid solution of 0.5mol/L, after parsing 3h under 300 revs/min of shaking speed, lithium concentration no longer increases, and measures lithium
Ion concentration is 135mg/L, and resolution factor reaches 90%.K/Li is 4/1, Na/Li 17/1, Mg/Li 6/1 in desorbed solution.Table
Bright adsorbent is maintained to the good selectivity of lithium ion.
Embodiment 2:
Compared with example 1, operating process is identical, wherein lithium manganese oxysome lithium ion sieve LiMn2O4, with 5g water soluble starch and
Pollopas and mixing of the 5g molecular weight 8000 are heated to 80 DEG C of fully meltings, citric acid 5g, season penta are added in mixed liquor
The mixture 5g of the mass ratio 1/1 of tetrol and glycerine, 100 DEG C of heating reflux reaction 2h in closed container, by mixture of viscous form
The lower 80 DEG C of reduction vaporization of 0.1MPa, dehydrating and curing, with the graininess that slot type spreading disintegrating apparatus Mechanical Crushing is 1~3mm grain sizes
Adsorbent.
As shown in Figure 2, the enlarged drawing that the figure a in Fig. 2 is 200 times schemes b to the pattern for the adsorbent that the present embodiment is prepared
For 500 times of enlarged drawing；
By lithium ion adsorbent 2g (lithium ion sieve powder content is 1g), parsed in the hydrochloric acid solution of 0.5mol/L
48h, until the lithium concentration in parsing eluent no longer changes.It is placed in 200mL brine identical with example one,
Ion exchange adsorption is carried out under 300 revs/min of shaking speed carries lithium.Absorption reaches balance after 6h, calculates the adsorbance of adsorbent
For 13.5mg/g (in terms of the powder lithium ion sieve quality in adsorbent).Hydrochloric acid solution of the adsorbent in the 0.5mol/L of 100mL
In, after parsing 4h under 300 revs/min of shaking speed, lithium concentration no longer increases, and measures resolution factor and reaches 90%.
Embodiment 3:
It by 10g ammonium phosphomolybdates, mixes, heats in 12000 melmac with 5g water soluble starch and 5g molecular weight
To 80 DEG C of fully meltings, it is added metaformaldehyde 5g in mixed liquor, the mixture that the mass ratio of pentaerythrite and glycerine is 1/1
5g, 100 DEG C of heating reflux reaction 4h in closed container, by the lower 80 DEG C of reduction vaporization of mixture of viscous form 0.1MPa, dehydrating and curing,
With the granular adsorbent that slot type spreading disintegrating apparatus Mechanical Crushing is 1~3mm grain sizes.
As shown in Figure 3, the enlarged drawing that the figure a in Fig. 3 is 500 times schemes b to the pattern for the adsorbent that the present embodiment is prepared
For 5000 times of enlarged drawing；
By rubidium ion adsorbent 2g (lithium ion sieve powder content is 1g), in 20% ammonium chloride solution, at 40 DEG C
48h is parsed, until the rubidium ion concentration in parsing eluent no longer changes.It is placed in 500mL again and contains Rb+A concentration of 80mg/
L, brine in, under 300 revs/min of shaking speed carry out ion exchange adsorption carry lithium.Rubidium ion concentration drops in stoste after for 24 hours
No longer decline after to 5mg/L, absorption reaches balance, and the adsorbance for calculating adsorbent is 35mg/g (with the powder lithium in adsorbent
Ion sieve quality meter).By adsorbent with 20% ammonium chloride of 200mL at 40 DEG C, on shaking table with 300 revs/min of rotating speed
After lower parsing 12h, rubidium ion concentration no longer increases in solution, and the resolution factor for measuring rubidium reaches 91%.Show that adsorbent maintains
To the good selectivity of rubidium ion.Absorption and parsing rate are compared with the height that document provides.
The preferred embodiment of the disclosure is described in detail above in association with attached drawing, still, the disclosure is not limited to above-mentioned reality
The detail in mode is applied, in the range of the technology design of the disclosure, a variety of letters can be carried out to the technical solution of the disclosure
Monotropic type, these simple variants belong to the protection domain of the disclosure.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the disclosure to it is various can
The combination of energy no longer separately illustrates.
In addition, arbitrary combination can also be carried out between a variety of different embodiments of the disclosure, as long as it is without prejudice to originally
Disclosed thought equally should be considered as disclosure disclosure of that.
Claims (9)
1. a kind of preparation method of granular ion crossover adsorbent, which is characterized in that by powdery ion-exchanger and water solubility
After macromolecule prepolymer mixed melting, multi-group crosslink agent is added, increases temperature, heat preservation reflux makes prepolymer further occur
Build condensation reaction is shaped through reduction vaporization, dehydrating and curing and Mechanical Crushing successively at thick space network polymer to obtain the final product.
2. the preparation method of granular ion crossover adsorbent as described in claim 1, which is characterized in that the water solubility
Macromolecule prepolymer is mixture one or more kinds of in pollopas, melmac and water soluble starch.
3. the preparation method of granular ion crossover adsorbent as described in claim 1, which is characterized in that the powdery from
Sub- exchanger is lithium ion sieve or rubidium ion exchanger；
The lithium ion sieve is lithium manganese oxysome lithium ion sieve Li1+xMn2-xO4, 0≤x≤0.33；
The rubidium ion exchanger is ammonium phosphomolybdate or tungsten ammonium molybdate；
The mass ratio of powdery ion-exchanger and water soluble polymer prepolymer is 1~3：1.
4. the preparation method of granular ion crossover adsorbent as described in claim 1, which is characterized in that powdery ion exchange
The temperature of agent and water soluble polymer prepolymer mixed melting is 80 DEG C.
5. the preparation method of granular ion crossover adsorbent as described in claim 1, which is characterized in that described is multifunctional
Group's crosslinking agent is polyalcohol or polyacid containing ternary or quaternary functional group；
Polyalcohol containing ternary or quaternary functional group is selected from at least one of glycerine and pentaerythrite；
Polyacid containing ternary or quaternary functional group is selected from at least one of oxalic acid, malonic acid, citric acid and acetic anhydride.
6. the preparation method of the granular ion crossover adsorbent as described in claim 1 or 5, which is characterized in that described is more
The addition of functional group's crosslinking agent is the 30% of water soluble polymer pre-polymerization amount of substance；
2~4h of reaction time of the build condensation reaction, reaction temperature are 100~120 DEG C.
7. the preparation method of the granular ion crossover adsorbent as described in claim 1 or 5, which is characterized in that the decompression
The negative pressure of evaporation and dehydrating and curing is 0.1MPa, and temperature is 100 DEG C；
The equipment of Mechanical Crushing is slot type spreading crusher, and the particle size range for being crushed molding adsorbent is 1~3mm.
8. a kind of granular ion crossover adsorbent, which is characterized in that the adsorbent is using any grains of claim 1-7
The preparation method of shape ion-exchange type adsorbent is prepared.
9. the adsorbent that the preparation method of any granular ion crossover adsorbents of claim 1-7 is prepared is used for
The application of adsorbing and extracting rubidium ion or lithium ion.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109225124A (en) * | 2018-11-09 | 2019-01-18 | 华东理工大学 | A kind of preparation method of particle lithium adsorbent |
| CN114259997A (en) * | 2021-12-15 | 2022-04-01 | 淮阴工学院 | High-strength rubidium/cesium special-effect adsorbent and preparation method and application thereof |
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