CN108543521A - A kind of fiber adsorbing substance and preparation method carrying lithium for salt lake bittern - Google Patents
A kind of fiber adsorbing substance and preparation method carrying lithium for salt lake bittern Download PDFInfo
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- CN108543521A CN108543521A CN201810341774.9A CN201810341774A CN108543521A CN 108543521 A CN108543521 A CN 108543521A CN 201810341774 A CN201810341774 A CN 201810341774A CN 108543521 A CN108543521 A CN 108543521A
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/28—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
- B01J20/28023—Fibres or filaments
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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Abstract
The invention belongs to salt lake bittern extractive technique fields, specifically provide a kind of fiber adsorbing substance and preparation method carrying lithium for salt lake bittern.A kind of fiber adsorbing substance and preparation method carrying lithium for salt lake bittern of the present invention, the ceramic fibre loose by preparing inner core, inner core is graphitized, and absorption lithium source, manganese source and roasting obtain complex Li-Mn-oxide, and complex Li-Mn-oxide is in threadiness in the inner core of ceramic fibre, lithium is taken off by pickling, make inner core that there is lithium vacancy, is used for the adsorbing and extracting lithium in brine, not only good cycling stability, and contacted with water fully, adsorption efficiency is high.Complex Li-Mn-oxide crystal structure flimsy defect when adsorbing deintercalation repeatedly is effectively overcome, bulky grain is prepared without bonding.
Description
Technical field
The invention belongs to salt lake bittern extractive technique fields, specifically provide a kind of fiber suction carrying lithium for salt lake bittern
Attached dose and preparation method.
Background technology
As New-energy electric vehicle and mobile IT product continue to introduce new, the demand to lithium battery is also drastically increasing
Add, has thus driven the continuous soaring of core material lithium valence.Mainstream electric vehicle is all using lithium battery as driving on the market at present
Battery, therefore, sufficient lithium resource are most important for the development of new-energy automobile industry.Lithium is the pass for producing serondary lithium battery
Key raw material.Either anode, electrolyte, lithium is essential raw material.
The lithium of early stage is extracted from containing lithium ore, but with the increasingly reduction containing lithium ore, under grade is gradual
Drop, with the continuous discovery in the lake containing lithium salts, then the sight for carrying lithium has gradually been turned to salt lake and has carried lithium by people.Salt lake contains at present
Lithium amount has accounted for the 91% of earth lithium resource, Li in salt lake bittern+Often in the form of micro with a large amount of alkali metal, alkaline-earth metal ions
It coexists.Since their chemical property is very close so that therefrom separation and Extraction lithium is very difficult, especially high-content Mg2+
Presence, make separation Li+Technology it is increasingly complex, therefore separating magnesium and lithium is the bottleneck that brine carries lithium.
According to it has been reported that absorption method is to put forward the preferable method of lithium in high Mg/Li ratio brine at present.Absorption method is profit
Eluted to adsorb lithium ion, then by lithium ion with the adsorbent to the selective absorption of lithium ion, reach lithium ion with
The purpose of other foreign ion separation.This method is simple for process, and the rate of recovery is high, and selectivity is good, not only can compared with other methods
It is enough to detach lithium with magnesium and at low cost, low energy consumption, pollution-free.The key of absorption method is adsorbent, it requires adsorbent to lithium
There is excellent Selective adsorption, is suitble to fairly large operate with repeatedly.According to the prior art, adsorbent be mainly some from
Sub- sieve-type metal oxide, principle are that target lithium ion is first imported in metal oxide, generate metal composite oxide,
Under the premise of maintaining metal oxide structures, target lithium ion is removed, obtains that there is the pore structure that can accommodate lithium ion, from
And it is used to adsorb lithium ion.It is attritive powder to be limited to compound metal oxide, is needed when in use as adsorbent continuous
It adsorbs lithium, be detached from, not only operating difficulties, and its crystal structure is fragile when adsorbing deintercalation repeatedly, and adsorption is caused to drop
It is low.And powdered fine metal oxide is prepared into large grained by granulations such as adhesives, and although easy to use, ratio
Surface area substantially reduces, and adsorption efficiency reduces.
Chinese invention patent application number 02145583.X discloses a kind of method of extracting lithium from salt lake brine by adsorption.
Be related to a kind of method of absorption method from extracting lithium from salt lake brine, be suitable for Qinghai lake bittern water containing lithium salts and salt pan concentration to contain lithium old
Halogen, and produce from Qinghai Salt Lake Bittern the technical process of lithium carbonate and lithium chloride；Wherein being directed to salt pan solar evaporation must contain
Lithium concentrated brine adsorbs Li with aluminium salt type adsorbent+, Li is eluted with water+Eluent is obtained, eluent is refined, concentrates, and satisfaction is produced
Qualified raw material needed for lithium carbonate or lithium chloride.
Chinese invention patent application number 201410353274.9 discloses a kind of side of absorption method extraction Lithium from Salt Lake Brine
Method discloses a kind of method of absorption method extraction Lithium from Salt Lake Brine, includes the following steps：Adsorbent, halogen are added in brine
Lithium ion absorption in water is on the sorbent；Using ceramic film process, adsorbent is trapped in concentrate, concentrate passes through again
Plate compression obtains adsorbent filter cake, removes most of impurity and water in brine, and filter cake is desorbed through washing and eluant, eluent, obtained
Stripping liquid, stripping liquid removes the magnesium in stripping liquid through weak-type cation exchange resin, then is concentrated through reverse osmosis membrane, is prepared
The refined lithium solution of lithium carbonate.This method has simple for process, and operation is easy, and adsorbent utilization ratio is high, carries lithium process cycle
It is short, the advantages of high-content refines lithium solution is made.
Chinese invention patent application number 201710248598.X discloses a kind of method for extracting lithium from salt lake bittern, relates to
And the method that lithium is extracted from salt lake bittern, belong to brine and puies forward lithium technical field.The technical problem to be solved by the present invention is to provide from
The method that lithium is extracted in the lower salt lake bittern of lithium concentration.This method comprises the following steps：A, it adsorbs：In salt lake bittern successively
Aluminium salt and calcium hydroxide solid is added, is stirred to react, the reaction time >=1h takes precipitation, obtains lithium adsorbed product；B, it is desorbed：It will
Lithium adsorbed product De contamination, obtains lithium solution.The method of the present invention, can be relatively low from lithium concentration, straight in the higher brine of Mg/Li ratio
It connects absorption and carries lithium, concentrated without being evaporated, need not also reduce Mg/Li ratio in advance, it is easy to operate.The formation of adsorbent and lithium
Absorption be carried out at the same time, eliminate and adsorbent this link be prepared separately, and raw material is cheap and easy to get, process route is simple.
From the point of view of the above-mentioned prior art, the adsorbent that synthesizes at present for carried from brine lithium there are it is of high cost, carry lithium and follow
The defects such as ring poor performance, adsorption efficiency be low, have seriously affected the scale application in industrial abstract lithium.
Invention content
In view of the deficienciess of the prior art, the present invention proposes a kind of at low cost, carry that lithium cyclicity is good, and adsorption efficiency is high
The fiber adsorbing substance and preparation method of lithium are carried for salt lake bittern.
To solve the above problems, the present invention uses following technical scheme：
A kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern, includes the following steps：
A, by the nano oxidized sodium of 5~12 parts by weight, the zinc oxide of 3~10 parts by weight, the silica of 5~20 parts by weight, 1~
The aluminium oxide of 8 parts by weight, the yttria of 0.5~2 parts by weight, 20~40 parts by weight kaolin be ground to nanoscale, so
Afterwards slurry is configured to water, polyvinyl alcohol；
B, superfine bacteria cellulose fiber is obtained using a point comb micronization processes；
C, slurry prepared by a steps is mixed into spinneret with the superfine bacteria cellulose fiber that b step obtains, obtains surface and uniformly wraps up in
Cover the superfine bacteria cellulose fiber of slurry；
D, the surface that step c obtains uniformly is wrapped to the superfine bacteria cellulose fiber of slurry with the heating speed of 50~80 DEG C/min
Rate is warming up to 1200~1800 DEG C, and heat preservation fires 3~8h and carries out porcelain, and the superfine bacteria cellulose of inner core is through pyrolysis carbonization and stone
Mo Hua forms the loose ceramic fibre of inner core；
E, the loose ceramic fibre of the inner core that Step d is prepared immerses in manganese salt solution, and lithium hydroxide is then added, and heats
To 70 DEG C, lithia solution and manganese salt solution precipitation reaction generation colloid, dry, roasting in the loose inner core of ceramic fibre
It burns, obtains the complex Li-Mn-oxide of threadiness；
F, the complex Li-Mn-oxide for the threadiness that step e is prepared carries out pickling, lithium ion is removed, in ceramic fibre
Core forms lithium gap, obtains the fiber adsorbing substance that lithium is carried for salt lake bittern.
Further, the preparation method of above-mentioned a kind of fiber adsorbing substance carrying lithium for salt lake bittern, wherein in a steps
It is vertical lapping machine, valve body grinder, horizontal mill or disc type grinding that the grinding, which uses nano-level grinder, the grinder,
The grain size of one kind in machine, the mixing nanometer powder after grinding is 50~200nm.
Bacteria cellulose（Bacterial cellulose, BC）Refer at different conditions, by acetic acid Pseudomonas
（Acetobacter）, Agrobacterium（Agrobacterium）, rhizobium（Rhizobium）And Sarcina
（Sarcina）The general designation of the cellulose of certain Microbe synthesis in.Wherein compare the glucose in typically acetic acid Pseudomonas
Acetobacter（Glucoacetobacterxylinum,Old name acetobacter xylinumAcetobacter xylinum）, it has highest
Cellulose production capacity is confirmed to be the model bacterial strain of research cellulosic electrode, crystallization process and structural property.Bacteria cellulose
Synthesis be one by a large amount of multienzyme complex systems（Cellulose-synthesizing enzyme, cellulose synthase, CS）Accuracy controlling
Multistep reaction process, be cellulose precursor uridine diphosphoglucose (uridine diphoglucose, UDPGlu) first
Synthesis, then oligomerization CS compounds be also known as end compound (terminal complexe, TC) continuously by pyranoid form grape
Saccharide residue is transferred to from UDPGlu on newly-generated polysaccharide chain, forms dextran chain, and most pass through afterwards to extracellular across outer membrane secretion
Multiple dextran chain assembly crystallize to form supermolecular texture with combining.
Bacteria cellulose has higher purity and crystallinity；Compared with plant cellulose, bacteria cellulose is free of half fiber
The impurity such as element, lignin are tieed up, are existed with 100% Cellulosed molded article；With fine network structure；Modulatory character when synthesis；Carefully
Cellulose degradation can be the sugar of small molecule by the degradability and reusing of fungin, under field conditions (factors), microorganism,
It will not cause the pollution of environment.Bacteria cellulose is renewable and degradable biological resource, and extraction process is simple；Also have good
Hydrophily and gas permeability well, high-tensile and Young's modulus etc., and diameter is thinner, and the bacterium by acetobacter xylinum production is fine
The diameter of element is tieed up between 0.01nm~0.1 μm, is natural nanometer materials, and about 10 μm of the diameter of plant cellulose,
It is hundred times or more of bacteria cellulose.
Further, a kind of above-mentioned fiber adsorbing substance and preparation method carrying lithium for salt lake bittern, wherein b step institute
Stating superfine bacteria cellulose fiber is prepared by following methods：
I, the bacteria cellulose original film being prepared using acetobacter xylinum, it is wet after NaOH solution is handled to obtain bacteria cellulose
Film；
II, cellulose wet-coating that step I is prepared punctured through licker-in surface needle thorn high speed, isolated and combing effect, made
Bacterial cellulose wet-coating becomes superfine bacteria cellulose fiber.
Further, a kind of above-mentioned fiber adsorbing substance and preparation method carrying lithium for salt lake bittern, wherein the licker-in
Including central shaft, it being cased with roller on central shaft, the outer wall of roller is pierced equipped with needle-shaped teasing needle, and diameter of cylinder is 300~
600mm, needle pierce 0.5~3cm of length, a diameter of 0.01~2mm in needle thorn stick portion, a diameter of 10~80um in needle puncture tip portion, needle thorn
Tip length is 1~10mm, 20~800/cm of needling density2。
Further, a kind of above-mentioned fiber adsorbing substance and preparation method carrying lithium for salt lake bittern, wherein the bacterium
The moisture content of cellulose fibre is 150~10000%, 50~300nm of fibre diameter, fibre length 500nm~100000nm.
Further, a kind of above-mentioned fiber adsorbing substance and preparation method carrying lithium for salt lake bittern, wherein the spinneret
Temperature be 120~200 DEG C, spin rate be 2~9m/s, spinneret a diameter of 1 × 10-5~3 × 10-5m。
Further, above-mentioned a kind of fiber adsorbing substance and preparation method carrying lithium for salt lake bittern, wherein in step e
The manganese salt solution is at least one of manganese sulfate solution, manganese chloride or manganese nitrate, and wherein manganese containing solution is a concentration of
0.1mol/L~0.2mol/ L.Lithium hydroxide is excessive, preferably lithium：Manganese molar ratio is 3:1.
Further, above-mentioned a kind of fiber adsorbing substance and preparation method carrying lithium for salt lake bittern, wherein in step e
100~300 DEG C of the calcination temperature, roasting time are 3~5h.
Further, a kind of above-mentioned fiber adsorbing substance and preparation method carrying lithium for salt lake bittern, wherein the pickling
Use mass concentration for 1~10% H2SO4Solution, liquid-solid ratio be 2.5~3, under the conditions of 50~90 DEG C pickling 15~
60min。
The present invention also provides a kind of fibers adsorptions carrying lithium for salt lake bittern that a kind of above-mentioned preparation method is prepared
Agent.Mainly by the way that nano oxidized sodium, zinc oxide, silica, aluminium oxide, yttria, kaolin are ground to micron order,
Then it is configured to slurry with water, polyvinyl alcohol；A point superfine bacteria cellulose fiber for comb micronization processes is added；Spinneret makes slurry
Uniformly wrap in superfine bacteria cellulose fiber surface；The superfine bacteria cellulose of high-temperature firing porcelain, inner core is carbonized through pyrolysis
Or graphitization, formation inner core is loose, and outer layer is the fiber of ceramics；The loose ceramic fibre of inner core is immersed into manganese salt solution, then
Lithium hydroxide is added, colloid is generated in the loose inner core lithia solution of ceramic fibre and manganese salt solution precipitation reaction, it is dry,
Roasting obtains the complex Li-Mn-oxide of threadiness；Further pickling removes lithium ionic insertion/deinsertion, and it is empty to form lithium in ceramic fibre inner core
Gap obtains the fiber adsorbing substance that lithium is carried for salt lake bittern.
A kind of fiber adsorbing substance and preparation method carrying lithium for salt lake bittern of the present invention, the pottery loose by preparing inner core
Porcelain fiber, inner core be carbonized or be graphitized it is loose, have good capillary absorption, ensure that good adsorptivity；In capillary
Inner core, there is a large amount of lithium vacancy, for the adsorbing and extracting lithium in brine, not only good cycling stability, and contacted with water
Fully, adsorption efficiency is high.Complex Li-Mn-oxide crystal structure flimsy defect when adsorbing deintercalation repeatedly is effectively overcome,
Bulky grain is prepared without bonding.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern of the present invention, includes the following steps：
A, by the nano oxidized sodium of 5 parts by weight, the zinc oxide of 3 parts by weight, 6 parts by weight silica, 4 parts by weight oxidation
Aluminium, the yttria of 0.8 parts by weight, 25 parts by weight kaolin be ground to nanoscale, be then configured to water, polyvinyl alcohol
Slurry；The grinder is vertical lapping machine, and the grain size of the mixing nanometer powder after grinding is 70nm；
B, superfine bacteria cellulose fiber is obtained using a point comb micronization processes；The superfine bacteria cellulose fiber is by with lower section
Method is prepared：
I, the bacteria cellulose original film being prepared using acetobacter xylinum, it is wet after NaOH solution is handled to obtain bacteria cellulose
Film；
II, cellulose wet-coating that step I is prepared punctured through licker-in surface needle thorn high speed, isolated and combing effect, made
Bacterial cellulose wet-coating becomes superfine bacteria cellulose fiber；The licker-in includes central shaft, and roller, roller are cased on central shaft
Outer wall pierced equipped with needle-shaped teasing needle, diameter of cylinder 400mm, needle pierces length 0.9cm, and needle thorn stick portion is a diameter of
0.05mm, a diameter of 60um in needle puncture tip portion, needle puncture tip minister's degree are 5mm, 110/cm of needling density2；
C, slurry prepared by a steps is mixed into spinneret with the superfine bacteria cellulose fiber that b step obtains, obtains surface and uniformly wraps up in
Cover the superfine bacteria cellulose fiber of slurry；The moisture content of the bacteria cellulose fibre is 200%, fibre diameter 76nm, fibre
Tie up length 800nm；The temperature of the spinneret is 160 DEG C, spin rate 5m/s, spinneret a diameter of 2 × 10-5m；
D, the surface that step c obtains uniformly is wrapped into the superfine bacteria cellulose fiber of slurry with the heating rate liter of 60 DEG C/min
Temperature is to 1500 DEG C, and heat preservation fires 5h and carries out porcelain, and the superfine bacteria cellulose of inner core is carbonized through pyrolysis or graphitization, forms inner core
Loose ceramic fibre；
E, the loose ceramic fibre of the inner core that Step d is prepared immerses in manganese salt solution, and lithium hydroxide is then added, and heats
To 70 DEG C, lithia solution and manganese salt solution precipitation reaction generation colloid, dry, roasting in the loose inner core of ceramic fibre
It burns, obtains the complex Li-Mn-oxide of threadiness；The manganese salt solution is manganese sulfate solution, and wherein manganese containing solution is a concentration of
0.1mol/L；Lithium hydroxide dosage is according to lithium：Manganese molar ratio is 3:1 is added.130 DEG C of the calcination temperature, roasting time 4h；
F, the complex Li-Mn-oxide for the threadiness that step e is prepared carries out pickling, lithium ion is removed, in ceramic fibre
Core forms lithium gap, obtains the fiber adsorbing substance that lithium is carried for salt lake bittern；The pickling use mass concentration for 6% H2SO4
Solution, liquid-solid ratio 2.5, pickling 20min under the conditions of 60 DEG C.
It is 120g/L, lithium that the fiber adsorbing substance 800g for carrying lithium that embodiment 1 is prepared, which is added to 8000mL content of magnesium,
Be stirred under state in the high Mg/Li ratio aqueous salt brine that content is 4g/L and adsorb lithium, when adsorbing small up to 2 after stop stirring into
Row is separated by solid-liquid separation, and it is 120g/L, lithium content 0.15g/L to measure content of magnesium in the aqueous salt brine after absorption, and isolating
Adsorbent filter cake sulfuric acid deviates from lithium, the lithium solution 1200mL deviate from, and the lithium concentration for measuring the lithium solution is 25.67g/L.
It is above-mentioned deviate from lithium after adsorbent 760g put into that 8000mL content of magnesium is 120g/L, lithium content is again
Be stirred in the high Mg/Li ratio aqueous salt brine of 4g/L under state and adsorb lithium, when adsorb it is small up to 2 when after stop stirring carry out solid-liquid
Separation, measure content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content 0.18g/L, and the adsorbent isolated
Filter cake sulfuric acid deviates from lithium, the lithium solution 1200mL deviate from, and the lithium concentration for measuring the lithium solution is 25.47g/L.
Embodiment 2
A kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern of the present invention, includes the following steps：
A, by the nano oxidized sodium of 7 parts by weight, the zinc oxide of 7 parts by weight, 7 parts by weight silica, 7 parts by weight oxidation
Aluminium, the yttria of 0.7 parts by weight, 27 parts by weight kaolin be ground to nanoscale, be then configured to water, polyvinyl alcohol
Slurry；The grinder is valve body grinder, and the grain size of the mixing nanometer powder after grinding is 55nm；
B, superfine bacteria cellulose fiber is obtained using a point comb micronization processes；The superfine bacteria cellulose fiber is by with lower section
Method is prepared：
I, the bacteria cellulose original film being prepared using acetobacter xylinum, it is wet after NaOH solution is handled to obtain bacteria cellulose
Film；
II, cellulose wet-coating that step I is prepared punctured through licker-in surface needle thorn high speed, isolated and combing effect, made
Bacterial cellulose wet-coating becomes superfine bacteria cellulose fiber；The licker-in includes central shaft, and roller, roller are cased on central shaft
Outer wall equipped with needle-shaped teasing needle pierce, diameter of cylinder 600mm, needle pierce length 3cm, a diameter of 0.09mm in needle thorn stick portion,
The a diameter of 80um in needle puncture tip portion, needle puncture tip minister's degree are 6mm, 600/cm of needling density2；
C, slurry prepared by a steps is mixed into spinneret with the superfine bacteria cellulose fiber that b step obtains, obtains surface and uniformly wraps up in
Cover the superfine bacteria cellulose fiber of slurry；The moisture content of the bacteria cellulose fibre is 400%, fibre diameter 250nm, fibre
Tie up length 900nm；The temperature of the spinneret is 180 DEG C, spin rate 6m/s, spinneret a diameter of 3 × 10-5m；
D, the surface that step c obtains uniformly is wrapped into the superfine bacteria cellulose fiber of slurry with the heating rate liter of 60 DEG C/min
Temperature is to 1500 DEG C, and heat preservation fires 5h and carries out porcelain, and the superfine bacteria cellulose of inner core is carbonized through pyrolysis or graphitization, forms inner core
Loose ceramic fibre；
E, the loose ceramic fibre of the inner core that Step d is prepared immerses in manganese salt solution, and lithium hydroxide is then added, and heats
To 70 DEG C, lithia solution and manganese salt solution precipitation reaction generation colloid, dry, roasting in the loose inner core of ceramic fibre
It burns, obtains the complex Li-Mn-oxide of threadiness；The manganese salt solution is manganese nitrate, and wherein manganese containing solution is a concentration of
0.1mol/ L；Lithium hydroxide dosage is according to lithium：Manganese molar ratio is 3:1 is added.170 DEG C of the calcination temperature, roasting time are
4h；
F, the complex Li-Mn-oxide for the threadiness that step e is prepared carries out pickling, lithium ion is removed, in ceramic fibre
Core forms lithium gap, obtains the fiber adsorbing substance that lithium is carried for salt lake bittern.The pickling use mass concentration for 5% H2SO4
Solution, liquid-solid ratio 2.8, pickling 50min under the conditions of 60 DEG C；
It is 120g/L, lithium content that the fiber adsorbing substance 800g for carrying lithium that embodiment 2 is prepared, which is added to 8000mL content of magnesium,
Adsorb lithium to be stirred under state in the high Mg/Li ratio aqueous salt brine of 4g/L, when adsorb it is small up to 2 when after stop stirring being consolidated
Liquid detaches, and it is 120g/L, lithium content 0.5g/L to measure content of magnesium in the aqueous salt brine after absorption, and the adsorbent isolated
Filter cake sulfuric acid deviates from lithium, the lithium solution 1200mL deviate from, and the lithium concentration for measuring the lithium solution is 23.33g/L.
It is above-mentioned deviate from lithium after adsorbent 760g put into that 8000mL content of magnesium is 120g/L, lithium content is again
Be stirred in the high Mg/Li ratio aqueous salt brine of 4g/L under state and adsorb lithium, when adsorb it is small up to 2 when after stop stirring carry out solid-liquid
Separation, measure content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content 0.75g/L, and the adsorbent isolated
Filter cake sulfuric acid deviates from lithium, the lithium solution 1200mL deviate from, and the lithium concentration for measuring the lithium solution is 21.67g/L.
Embodiment 3
A kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern of the present invention, includes the following steps：
A, by the nano oxidized sodium of 8 parts by weight, the zinc oxide of 5 parts by weight, 7 parts by weight silica, 3 parts by weight oxidation
Aluminium, the yttria of 0.8 parts by weight, 28 parts by weight kaolin be ground to nanoscale, be then configured to water, polyvinyl alcohol
Slurry；The grinder is horizontal mill, and the grain size of the mixing nanometer powder after grinding is 100nm；
B, superfine bacteria cellulose fiber is obtained using a point comb micronization processes；The superfine bacteria cellulose fiber is by with lower section
Method is prepared：
I, the bacteria cellulose original film being prepared using acetobacter xylinum, it is wet after NaOH solution is handled to obtain bacteria cellulose
Film；
II, cellulose wet-coating that step I is prepared punctured through licker-in surface needle thorn high speed, isolated and combing effect, made
Bacterial cellulose wet-coating becomes superfine bacteria cellulose fiber；The licker-in includes central shaft, and roller, roller are cased on central shaft
Outer wall equipped with needle-shaped teasing needle pierce, diameter of cylinder 500mm, needle pierce length 2cm, a diameter of 1mm in needle thorn stick portion, needle
The a diameter of 40um in puncture tip portion, needle puncture tip minister's degree are 4mm, 300/cm of needling density2；
C, slurry prepared by a steps is mixed into spinneret with the superfine bacteria cellulose fiber that b step obtains, obtains surface and uniformly wraps up in
Cover the superfine bacteria cellulose fiber of slurry；The moisture content of the bacteria cellulose fibre be 1000%, fibre diameter 240nm,
Fibre length 10000nm；The temperature of the spinneret is 160 DEG C, spin rate 4m/s, spinneret a diameter of 1.6 × 10-5m；
D, the surface that step c obtains uniformly is wrapped into the superfine bacteria cellulose fiber of slurry with the heating rate liter of 60 DEG C/min
Temperature is to 1600 DEG C, and heat preservation fires 5h and carries out porcelain, and the superfine bacteria cellulose of inner core is carbonized through pyrolysis or graphitization, forms inner core
Loose ceramic fibre；
E, the loose ceramic fibre of the inner core that Step d is prepared immerses in manganese salt solution, and lithium hydroxide is then added, and heats
To 70 DEG C, lithia solution and manganese salt solution precipitation reaction generation colloid, dry, roasting in the loose inner core of ceramic fibre
It burns, obtains the complex Li-Mn-oxide of threadiness；The manganese salt solution is manganese sulfate solution, and wherein manganese containing solution is a concentration of
0.15mol/ L；Lithium hydroxide dosage is according to lithium：Manganese molar ratio is 3:1 is added.200 DEG C of the calcination temperature, roasting time are
4h；
F, the complex Li-Mn-oxide for the threadiness that step e is prepared carries out pickling, lithium ion is removed, in ceramic fibre
Core forms lithium gap, obtains the fiber adsorbing substance that lithium is carried for salt lake bittern.The pickling use mass concentration for 4% H2SO4
Solution, liquid-solid ratio 2.8, pickling 40min under the conditions of 70 DEG C.
It is 120g/L, lithium that the fiber adsorbing substance 800g for carrying lithium that embodiment 3 is prepared, which is added to 8000mL content of magnesium,
Be stirred under state in the high Mg/Li ratio aqueous salt brine that content is 4g/L and adsorb lithium, when adsorbing small up to 2 after stop stirring into
Row is separated by solid-liquid separation, and it is 117g/L, lithium content 0.40g/L to measure content of magnesium in the aqueous salt brine after absorption, and isolating
Adsorbent filter cake sulfuric acid deviates from lithium, the lithium solution 1200mL deviate from, and the lithium concentration for measuring the lithium solution is 24g/L.
It is above-mentioned deviate from lithium after adsorbent 780g put into that 8000mL content of magnesium is 120g/L, lithium content is again
Be stirred in the high Mg/Li ratio aqueous salt brine of 4g/L under state and adsorb lithium, when adsorb it is small up to 2 when after stop stirring carry out solid-liquid
Separation, measure content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content 0.45g/L, and the adsorbent isolated
Filter cake sulfuric acid deviates from lithium, the lithium solution 1200mL deviate from, and the lithium concentration for measuring the lithium solution is 23.67g/L.
Embodiment 4
A kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern of the present invention, includes the following steps：
A, by the nano oxidized sodium of 6 parts by weight, the zinc oxide of 7 parts by weight, 6 parts by weight silica, 3 parts by weight oxidation
Aluminium, the yttria of 0.9 parts by weight, 38 parts by weight kaolin be ground to nanoscale, be then configured to water, polyvinyl alcohol
Slurry；The grinder is vertical lapping machine, and the grain size of the mixing nanometer powder after grinding is 150nm；
B, superfine bacteria cellulose fiber is obtained using a point comb micronization processes；The superfine bacteria cellulose fiber is by with lower section
Method is prepared：
I, the bacteria cellulose original film being prepared using acetobacter xylinum, it is wet after NaOH solution is handled to obtain bacteria cellulose
Film；
II, cellulose wet-coating that step I is prepared punctured through licker-in surface needle thorn high speed, isolated and combing effect, made
Bacterial cellulose wet-coating becomes superfine bacteria cellulose fiber；The licker-in includes central shaft, and roller, roller are cased on central shaft
Outer wall pierced equipped with needle-shaped teasing needle, diameter of cylinder 500mm, needle pierces length 2.5cm, and needle thorn stick portion is a diameter of
0.15mm, a diameter of 70um in needle puncture tip portion, needle puncture tip minister's degree are 8mm, 700/cm of needling density2；
C, slurry prepared by a steps is mixed into spinneret with the superfine bacteria cellulose fiber that b step obtains, obtains surface and uniformly wraps up in
Cover the superfine bacteria cellulose fiber of slurry；The moisture content of the bacteria cellulose fibre be 2000%, fibre diameter 280nm,
Fibre length 20000nm；The temperature of the spinneret is 180 DEG C, spin rate 9m/s, spinneret a diameter of 3 × 10-5m；
D, the surface that step c obtains uniformly is wrapped into the superfine bacteria cellulose fiber of slurry with the heating rate liter of 70 DEG C/min
Temperature is to 1700 DEG C, and heat preservation fires 7h and carries out porcelain, and the superfine bacteria cellulose of inner core is carbonized through pyrolysis or graphitization, forms inner core
Loose ceramic fibre；
E, the loose ceramic fibre of the inner core that Step d is prepared immerses in manganese salt solution, and lithium hydroxide is then added, and heats
To 70 DEG C, lithia solution and manganese salt solution precipitation reaction generation colloid, dry, roasting in the loose inner core of ceramic fibre
It burns, obtains the complex Li-Mn-oxide of threadiness；The manganese salt solution is manganese nitrate, and wherein manganese containing solution is a concentration of
0.16mol/ L；Lithium hydroxide dosage is according to lithium：Manganese molar ratio is 3:1 is added.176 DEG C of the calcination temperature, roasting time are
4.4h；
F, the complex Li-Mn-oxide for the threadiness that step e is prepared carries out pickling, lithium ion is removed, in ceramic fibre
Core forms lithium gap, obtains the fiber adsorbing substance that lithium is carried for salt lake bittern.The pickling use mass concentration for 7% H2SO4
Solution, liquid-solid ratio 2.7, pickling 55min under the conditions of 60 DEG C.
It is 120g/L, lithium that the fiber adsorbing substance 800g for carrying lithium that embodiment 4 is prepared, which is added to 8000mL content of magnesium,
Be stirred under state in the high Mg/Li ratio aqueous salt brine that content is 4g/L and adsorb lithium, when adsorbing small up to 2 after stop stirring into
Row is separated by solid-liquid separation, and it is 120g/L, lithium content 0.30g/L to measure content of magnesium in the aqueous salt brine after absorption, and isolating
Adsorbent filter cake sulfuric acid deviates from lithium, the lithium solution 1200mL deviate from, and the lithium concentration for measuring the lithium solution is 24.67g/L.
It is above-mentioned deviate from lithium after adsorbent 760g put into that 8000mL content of magnesium is 120g/L, lithium content is again
Be stirred in the high Mg/Li ratio aqueous salt brine of 4g/L under state and adsorb lithium, when adsorb it is small up to 2 when after stop stirring carry out solid-liquid
Separation, measure content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content 0.45g/L, and the adsorbent isolated
Filter cake sulfuric acid deviates from lithium, the lithium solution 1200mL deviate from, and the lithium concentration for measuring the lithium solution is 23.67g/L.
Embodiment 5
A kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern of the present invention, includes the following steps：
A, by the nano oxidized sodium of 6 parts by weight, the zinc oxide of 9 parts by weight, 12 parts by weight silica, 5 parts by weight oxidation
Aluminium, the yttria of 0.6 parts by weight, 29 parts by weight kaolin be ground to nanoscale, be then configured to water, polyvinyl alcohol
Slurry；The grinder is valve body grinder, and the grain size of the mixing nanometer powder after grinding is 180nm；
B, superfine bacteria cellulose fiber is obtained using a point comb micronization processes；The superfine bacteria cellulose fiber is by with lower section
Method is prepared：
I, the bacteria cellulose original film being prepared using acetobacter xylinum, it is wet after NaOH solution is handled to obtain bacteria cellulose
Film；
II, cellulose wet-coating that step I is prepared punctured through licker-in surface needle thorn high speed, isolated and combing effect, made
Bacterial cellulose wet-coating becomes superfine bacteria cellulose fiber；The licker-in includes central shaft, and roller, roller are cased on central shaft
Outer wall equipped with needle-shaped teasing needle pierce, diameter of cylinder 400mm, needle pierce length 2cm, a diameter of 0.2mm in needle thorn stick portion,
The a diameter of 60um in needle puncture tip portion, needle puncture tip minister's degree are 3mm, 400/cm of needling density2；
C, slurry prepared by a steps is mixed into spinneret with the superfine bacteria cellulose fiber that b step obtains, obtains surface and uniformly wraps up in
Cover the superfine bacteria cellulose fiber of slurry；The moisture content of the bacteria cellulose fibre is 8000%, fibre diameter 80nm, fibre
Tie up length 60000nm；The temperature of the spinneret is 190 DEG C, spin rate 5m/s, spinneret a diameter of 1 × 10-5m；
D, the surface that step c obtains uniformly is wrapped into the superfine bacteria cellulose fiber of slurry with the heating rate liter of 77 DEG C/min
Temperature is to 1700 DEG C, and heat preservation fires 6h and carries out porcelain, and the superfine bacteria cellulose of inner core is carbonized through pyrolysis and graphitization, forms inner core
Loose ceramic fibre；
E, the loose ceramic fibre of the inner core that Step d is prepared immerses in manganese salt solution, and lithium hydroxide is then added, and heats
To 70 DEG C, lithia solution and manganese salt solution precipitation reaction generation colloid, dry, roasting in the loose inner core of ceramic fibre
It burns, obtains the complex Li-Mn-oxide of threadiness；The manganese salt solution is manganese sulfate solution, and wherein manganese containing solution is a concentration of
0.2mol/ L；Lithium hydroxide dosage is according to lithium：Manganese molar ratio is 3:1 is added.170 DEG C of the calcination temperature, roasting time are
4h；
F, the complex Li-Mn-oxide for the threadiness that step e is prepared carries out pickling, lithium ion is removed, in ceramic fibre
Core forms lithium gap, obtains the fiber adsorbing substance that lithium is carried for salt lake bittern.The pickling use mass concentration for 6% H2SO4
Solution, liquid-solid ratio 2.7, pickling 45min under the conditions of 80 DEG C.
It is 120g/L, lithium that the fiber adsorbing substance 800g for carrying lithium that embodiment 5 is prepared, which is added to 8000mL content of magnesium,
Be stirred under state in the high Mg/Li ratio aqueous salt brine that content is 4g/L and adsorb lithium, when adsorbing small up to 2 after stop stirring into
Row is separated by solid-liquid separation, and it is 120g/L, lithium content 0.12g/L to measure content of magnesium in the aqueous salt brine after absorption, and isolating
Adsorbent filter cake sulfuric acid deviates from lithium, the lithium solution 1200mL deviate from, and the lithium concentration for measuring the lithium solution is 25.87g/L.
It is above-mentioned deviate from lithium after adsorbent 780g put into that 8000mL content of magnesium is 120g/L, lithium content is again
Be stirred in the high Mg/Li ratio aqueous salt brine of 4g/L under state and adsorb lithium, when adsorb it is small up to 2 when after stop stirring carry out solid-liquid
Separation, measure content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content 0.15g/L, and the adsorbent isolated
Filter cake sulfuric acid deviates from lithium, the lithium solution 1200mL deviate from, and the lithium concentration for measuring the lithium solution is 25g/L.
Comparative example 1
Lithium hydroxide is added in manganese salt solution, lithium hydroxide dosage is according to lithium：Manganese molar ratio is 3:1 is heated to 70 DEG C, hydrogen
Lithia solution and manganese salt solution precipitation reaction generate colloid, dry, and roasting obtains complex Li-Mn-oxide；The manganese salt
Solution is manganese sulfate solution, wherein a concentration of 0.1mol/L of manganese containing solution.130 DEG C of the calcination temperature, roasting time 4h；
Pickling is carried out to the complex Li-Mn-oxide being prepared, removes lithium ion, lithium gap is formed in ceramic fibre inner core, obtains
To the fiber adsorbing substance for carrying lithium for salt lake bittern；The pickling use mass concentration for 6% H2SO4Solution, liquid-solid ratio are
2.5, pickling 20min under the conditions of 60 DEG C.
By the lithium adsorbent 800g that comparative example 1 is prepared be added to 8000mL content of magnesium be 120g/L, lithium content 4g/
Be stirred in the high Mg/Li ratio aqueous salt brine of L under state and adsorb lithium, when adsorbing small up to 2 after stop stirring and carry out solid-liquid point
From it is 120g/L, lithium content 0.80g/L to measure content of magnesium in the aqueous salt brine after absorption, and the adsorbent isolated is filtered
Cake sulfuric acid deviates from lithium, the lithium solution 1200mL deviate from, and the lithium concentration for measuring the lithium solution is 21.33g/L.
It is above-mentioned deviate from lithium after adsorbent 620g put into that 8000mL content of magnesium is 120g/L, lithium content is again
Be stirred in the high Mg/Li ratio aqueous salt brine of 4g/L under state and adsorb lithium, when adsorb it is small up to 2 when after stop stirring carry out solid-liquid
Separation, measure content of magnesium in the aqueous salt brine after absorption be 120g/L, lithium content 1.05g/L, and the adsorbent isolated
Filter cake sulfuric acid deviates from lithium, the lithium solution 1200mL deviate from, and the lithium concentration for measuring the lithium solution is 19.67g/L.
By using comparative example 1 is not preloaded using fiber, and one side adsorbance is relatively low, and on the other hand molten loss rate is higher.
Claims (10)
1. a kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern, which is characterized in that include the following steps：
A, by the nano oxidized sodium of 5~12 parts by weight, the zinc oxide of 3~10 parts by weight, the silica of 5~20 parts by weight, 1~
The aluminium oxide of 8 parts by weight, the yttria of 0.5~2 parts by weight, 20~40 parts by weight kaolin be ground to nanoscale, so
Afterwards slurry is configured to water, polyvinyl alcohol；
B, superfine bacteria cellulose fiber is obtained using a point comb micronization processes；
C, slurry prepared by a steps is mixed into spinneret with the superfine bacteria cellulose fiber obtained to b step, it is uniform obtains surface
Wrap the superfine bacteria cellulose fiber of slurry；
D, the surface that step c obtains uniformly is wrapped to the superfine bacteria cellulose fiber of slurry with the heating speed of 50~80 DEG C/min
Rate is warming up to 1200~1800 DEG C, and heat preservation fires 3~8h and carries out porcelain, and the superfine bacteria cellulose of inner core is through pyrolysis carbonization and stone
Mo Hua forms the loose ceramic fibre of inner core；
E, the loose ceramic fibre of the inner core that Step d is prepared immerses in manganese salt solution, and lithium hydroxide is then added, and heats
To 70 DEG C, lithia solution and manganese salt solution precipitation reaction generation colloid, dry, roasting in the loose inner core of ceramic fibre
It burns, obtains the complex Li-Mn-oxide of threadiness；
F, the complex Li-Mn-oxide for the threadiness that step e is prepared carries out pickling, lithium ion is removed, in ceramic fibre
Core forms lithium gap, obtains the fiber adsorbing substance that lithium is carried for salt lake bittern.
2. a kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern according to claim 1, which is characterized in that
Described in a steps grinding use nano-level grinder, the grinder be vertical lapping machine, valve body grinder, horizontal mill or
The grain size of one kind in disk grinder, the mixing nanometer powder after grinding is 50~200nm.
3. a kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern according to claim 1, which is characterized in that
Superfine bacteria cellulose fiber described in b step is prepared by following methods：
I, the bacteria cellulose original film being prepared using acetobacter xylinum, it is wet after NaOH solution is handled to obtain bacteria cellulose
Film；
II, cellulose wet-coating that step I is prepared punctured through licker-in surface needle thorn high speed, isolated and combing effect, made
Bacterial cellulose wet-coating becomes superfine bacteria cellulose fiber.
4. a kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern according to claim 3, which is characterized in that
The licker-in includes central shaft, and roller is cased on central shaft, and the outer wall of roller is pierced equipped with needle-shaped teasing needle, and diameter of cylinder is
300~600mm, needle pierce 0.5~3cm of length, a diameter of 0.01~2mm in needle thorn stick portion, a diameter of 10~80um in needle puncture tip portion,
Needle puncture tip minister's degree is 1~10mm, 20~800/cm of needling density2。
5. a kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern according to claim 3, which is characterized in that
The moisture content of the bacteria cellulose fibre is 150~10000%, 50~300nm of fibre diameter, fibre length 500nm~
100000nm。
6. a kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern according to claim 1, which is characterized in that
The temperature of the spinneret is 120~200 DEG C, and spin rate is 2~9m/s, spinneret a diameter of 1 × 10-5~3 × 10-5m。
7. a kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern according to claim 1, which is characterized in that
Manganese salt solution described in step e is at least one of manganese sulfate solution, manganese chloride or manganese nitrate, the wherein concentration of manganese containing solution
For 0.1mol/L~0.2mol/ L.
8. a kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern according to claim 1, which is characterized in that
Calcination temperature 100~300 described in step e DEG C, roasting time are 3~5h.
9. a kind of preparation method for the fiber adsorbing substance carrying lithium for salt lake bittern according to claim 1, which is characterized in that
The pickling use mass concentration for 1~10% H2SO4Solution, liquid-solid ratio are 2.5~3, pickling under the conditions of 50~90 DEG C
15~60min.
10. a kind of fibre carrying lithium for salt lake bittern being prepared according to preparation method described in claim 1~9 any one
Tie up adsorbent.
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| CN109821499A (en) * | 2019-03-13 | 2019-05-31 | 成都理工大学 | The whisker net of lithium carbonate knits material and preparation method thereof in a kind of enrichment salt lake bittern |
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| CN115212844A (en) * | 2022-08-09 | 2022-10-21 | 杭州电子科技大学 | Composite adsorbent for extracting lithium from salt lake brine and preparation method thereof |
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