CN107243318A - A kind of preparation method of titanium-type lithium ion sieve adsorbant - Google Patents
A kind of preparation method of titanium-type lithium ion sieve adsorbant Download PDFInfo
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- CN107243318A CN107243318A CN201710330635.1A CN201710330635A CN107243318A CN 107243318 A CN107243318 A CN 107243318A CN 201710330635 A CN201710330635 A CN 201710330635A CN 107243318 A CN107243318 A CN 107243318A
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- 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
- B01J20/02—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
Abstract
The present invention relates to a kind of preparation method of titanium-type lithium ion sieve adsorbant, it is comprised the following steps that：The acylate of titanium dioxide and lithium is mixed to form solid-phase mixture, dispersant ground and mixed is added, then dries, then temperature-programmed calcination obtains lithium ion sieve presoma Li2TiO3, finally by Li2TiO3Presoma is modified using inorganic acid and obtains ion sieve H2TiO3.This method technique is simple, and obtained titanium-type lithium ion sieve adsorbant epigranular, particle agglomeration is few, the characteristics of obtained lithium ion sieve has adsorbance height, the fast rate of adsorption, high adsorptive selectivity and good absorption stability.
Description
Technical field
The present invention relates to a kind of preparation method of adsorbent, more particularly to a kind of preparation method of titanium-type lithium ion sieve adsorbant.
Background technology
Lithium is a kind of important strategic resource.The compound consumption of lithium and lithium increases year by year, and only just to consume lithium total for field of batteries
The 39% of amount.Demand for lithium is far longer than its supply.Most lithium resource is all with the shape of liquid ion in the world
Formula is stored in seawater, bittern and underground water etc., therefore is the trend of present lithium resource exploitation to the exploitation of liquid lithium resource.
Ion exchange adsorption is a kind of method that lithium is carried from liquid lithium resource well, and common adsorbent is divided into organic suction
Attached dose (such as ion exchange resin) and inorganic adsorbent (such as lithium ion sieve).Common lithium ion sieve has aluminum salt adsorbent, manganese type
Lithium ion sieve and titanium-type lithium ion sieve.The adsorbance of aluminum salt adsorbent is relatively low, and manganese type lithium ion sieve is higher to the adsorbance of lithium, but
It is the problem of there is manganese molten damage.Not only adsorbance is high for titanium-type lithium ion sieve, while titanium is molten to damage low, is conducive to liquid to propose the industry of lithium
Change development.
The synthetic method of common titanium-type lithium ion sieve has sol-gal process, hydrothermal synthesis method and solid phase method.Sol-gal process is closed
Into temperature is low, synthesis absorbent particles are uniform, but synthesis technique is complicated, is unfavorable for industrialized production, hydrothermal synthesis method conjunction
It is simpler into technique, but the time of synthesis is longer, synthetic reaction needs to carry out at elevated pressures.The letter of Solid phase synthesis technique
It is single, but sintering temperature is higher, there is particle agglomeration after roasting, it is uneven the problem of.The present invention uses solid phase-Melting Synthesis
Titanium-type lithium ion sieve, synthesis technique is simple, and sintering temperature is low, and the absorbent particles of acquisition are evenly distributed, particle crystal formation is complete.Inhale
Attached dose of adsorbance is high, adsorptive selectivity is good, absorption stability is good.
The content of the invention
It is an object of the invention to provide a kind of preparation method for preparing titanium-type lithium ion sieve adsorbant, this method technique is simple, system
The titanium-type lithium ion sieve adsorbant epigranular obtained, particle agglomeration is few, and obtained lithium ion sieve has adsorbance height, absorption speed
The characteristics of rate is fast, adsorptive selectivity is high, absorption stability is good.
The technical scheme is that：A kind of preparation method of titanium-type lithium ion sieve adsorbant, it is comprised the following steps that：By dioxy
The acylate for changing titanium and lithium is mixed to form solid-phase mixture, and wherein the mass fraction of titanium dioxide is 25%~40%, then is added
Enter dispersant ground and mixed, then dried in air atmosphere at 25 DEG C~50 DEG C, then 500 are warming up in air atmosphere Program
DEG C~900 DEG C, 2~8h of roasting obtains lithium ion sieve presoma Li2TiO3, by Li2TiO3Presoma is modified using inorganic acid and obtained
Ion sieve H2TiO3。
It is preferred that the organic acid hydrochlorate of described lithium is lithium acetate or propionic acid lithium.It is preferred that the particle diameter of described titanium dioxide be 30nm~
100nm。
It is preferred that described dispersant is at least one of ethanol or water；The addition quality of dispersant is solid phase mixing amount of substance
1%~10%.It is preferred that described drying time is 1~5h.
It is preferred that the program of described heating is：With 3 °/min~10 °/min heating rate from room temperature to 65 DEG C~200 DEG C
It is incubated 1~3h；500 DEG C~900 DEG C 2~8h of insulation are warming up to identical heating rate again.
It is preferred that described inorganic acid is one kind in hydrochloric acid, nitric acid or sulfuric acid or two kinds；The concentration of inorganic acid is 0.05mol/L
~0.2mol/L.It is preferred that the time that inorganic acid is modified is 6h~12h.
The preparation-obtained H of the present invention2TiO3When lithium ion sieve is used to adsorb lithium ion in simulation bittern, its lithium adsorbance reaches
30mg/g~50mg/g.And have good stability.
Using inorganic acid pickling desorption after titanium-type lithium ion sieve adsorbant absorption lithium ion, the adsorbent after desorption, which is repeated, to be made
With.
Wherein, described lithium-containing solution can be bittern or seawater, or simulate the lithium-containing solution prepared.Described liquid lithium money
In source, lithium ion content is 40mg/L~800mg/L.The solid-to-liquid ratio of described titanium-type lithium ion sieve adsorbant and liquid lithium solution
For 0.5g/L~4g/L.Adsorption temp of the described titanium-type lithium ion sieve adsorbant in liquid lithium solution is 20 DEG C~50 DEG C.
Adsorption time of the described titanium-type lithium ion sieve adsorbant in liquid lithium solution is 0.5h~24h, by H2TiO3Lithium ion sieve is used
In the solution for adsorbing different lithium contents, its lithium adsorbance can reach 30mg/g~50mg/g, and have good stability, to other metals
Ion is substantially not present adsorption phenomena.
Agents useful for same and raw material of the present invention are commercially available.
Beneficial effect：
1st, present invention process is simple, the characteristics of relatively low using the acylate fusing point of lithium so that the acylate and titanium dioxide of lithium
Titanium spontaneously forms uniform solid-liquid mixing system in low temperature, to reach the well-mixed effect of raw material, without by additional
Physical method (such as high-energy ball milling) mixed, simplify preparation technology.
2nd, the characteristics of present invention can decompose the substantial amounts of carbon dioxide of generation and vapor in high temperature using the acylate of lithium, point
The a large amount of gases of generation of solution can hinder the generation of particle agglomeration, so that the problem of avoiding particle agglomeration caused by high-temperature roasting, has
Effect ground suppresses the reunion of titanium-type lithium ion sieve adsorbant particle, the titanium-type lithium ion sieve adsorbant even particle distribution of acquisition.
3rd, the present invention can use low-temperature bake synthetic adsorbent, and sintering temperature can as little as 500 DEG C, and traditional solid phase method prepares titanium
Sintering temperature needed for type lithium ion sieve presoma is higher, thus this method roasting energy consumption is low.
4th, molten damage of the titanium of the titanium-type lithium ion sieve adsorbant prepared by the present invention is less than 0.02%, therefore improves lithium ion sieve suction
Attached dose of cycle life.
5th, prepared by the present invention the titanium-type lithium ion sieve adsorbant rate of adsorption is fast, adsorption capacity big, the cyclical stability of absorption
Height, is adsorbed at 30 DEG C, and the adsorbance of adsorbent remains to maintain 39mg/g after circulation 5 times.
Brief description of the drawings
Fig. 1 is the scattered titanium dioxide of embodiment 1 and lithium acetate mixture, grinding, dry after the obtained TG-DTA of sample.
Fig. 2 is titanium-type lithium ion sieve adsorbant presoma Li made from embodiment 12TiO3XRD.
Fig. 3 is titanium-type lithium ion sieve adsorbant presoma Li made from embodiment 12TiO3SEM figure.
Fig. 4 is titanium-type lithium ion sieve adsorbant H made from embodiment 12TiO3XRD.
Fig. 5 is the XRD picture of 5 absorption of titanium-type lithium ion sieve adsorbant made from embodiment 2.
Fig. 6 changes for 5 circulation absorption amounts of titanium-type lithium ion sieve adsorbant made from embodiment 2.
Embodiment
Below by embodiment, the present invention will be further described, and its purpose, which is only that, is better understood from present disclosure, but
Therefore do not limit the present invention among described scope of embodiments.
SEM INSTRUMENT MODELs：S-4800,Hitachi,Japan；ICP INSTRUMENT MODELs：Optima DV7000,PerkinElme,
USA；XRD INSTRUMENT MODELs：Rigaku SmartLab Series X-ray powder diffractometers, scanning range：10-70 °, step-length 0.02,
Sweep speed：20 °/min, scanning voltage 40kV, electric current 40mA.
Embodiment 1
1st, 7.5617g lithium acetates are mixed into (mass ratio 60 with 5.0411g particle diameters for 30nm titanium dioxide:40), using water as
Dispersant, dispersant addition is 1%, and 0.5h is ground in mortar, and 1h is then dried at 50 DEG C, is dried to obtain after grinding
The TG-DTA of sample is shown in Fig. 1.65 DEG C are warming up to from room temperature with 3 °/min heating rate in air atmosphere, 3h is stopped, with phase
Same heating rate is warming up to 750 DEG C, and roasting 5h obtains titanium-type lithium ion sieve presoma Li2TiO3.Titanium-type lithium ion sieve presoma
Li2TiO3X ray diffracting spectrum and SEM spectrum see Fig. 2 and Fig. 3.By Fig. 2 it can be found that prepared titanium-type lithium ion sieve
Presoma meets Li2TiO3Base peak collection of illustrative plates.It is more equal that Fig. 3 indicates prepared titanium-type lithium ion sieve presoma particle diameter
One, particle diameter is about 100nm.
2nd, 3g titanium-type lithium ion sieve presomas Li is weighed2TiO3, under the conditions of 60 DEG C, carry out pickling with 0.2mol/ hydrochloric acid and change
Property, stir after 6h and filter under magnetic stirring, filter residue is cleaned with deionized water, titanium-type lithium is obtained after then drying 5h at 60 DEG C
Ion sieve adsorbant H2TiO3, its X ray diffracting spectrum is shown in Fig. 4.Fig. 4 shows modified through peracid, the diffraction of titanium-type lithium ion sieve
Peak is offset to the right, and this explanation lithium ion and hydrogen ion have carried out ion exchange.
3rd, 0.5g titanium-type lithium ion sieve is weighed, lithium concentration is put into and is simulated for 300mg/L in bittern, the constant temperature magnetic at 30 DEG C
Power stirring and adsorbing 24h, the adsorbance of titanium-type lithium ion sieve is 50mg/g.
Embodiment 2
12.3232g lithium acetates mix to (mass ratio is 65 with the titanium dioxide that 6.6356g particle diameters are 30nm:35), made with ethanol
For dispersant, the addition of dispersant is 5%, and 2h is ground in grinding, and 5h is then dried at 25 DEG C, in air atmosphere from
Room temperature is warming up to 85 DEG C with 5 °/min heating rate, stops 1h, continues to be warming up to 750 DEG C with identical heating rate, is calcined 2h
Obtain titanium-type lithium ion sieve presoma Li2TiO3。
2nd, 3g titanium-type lithium ion sieve presomas Li is weighed2TiO3, under the conditions of 60 DEG C, carry out pickling with 0.05mol/ hydrochloric acid and change
Property, stir after 6h and filter under magnetic stirring, filter residue is cleaned with deionized water, titanium-type lithium is obtained after then drying 5h at 60 DEG C
Ion sieve adsorbant H2TiO3。
3rd, weighing 0.5g titanium-type lithium ion sieve is used for simulation bittern absorption 30 DEG C at constant temperature of the lithium concentration for 70mg/L
Magnetic agitation adsorbs 24h, and its adsorbance is 39.2mg/g.
4th, the sample after lithium will be adsorbed, at 60 DEG C, carries out pickling desorption with concentration 0.1mol/L hydrochloric acid, desorption time is
10h.Then the titanium-type lithium adsorbent regenerated in 60 DEG C of dry 5h.Cyclic process repeats according to 3 and 4, circulation absorption
Ion sieve XRD afterwards is as shown in Figure 5.Fig. 5 is indicated after multiple regenerative adsorption, titanium-type lithium ion sieve XRD diffraction maximum collection of illustrative plates
Do not change, illustrate that prepared titanium-type lithium ion sieve structure is very stable.The internal circulating load of titanium-type lithium ion sieve such as Fig. 6 institutes
Show, the adsorbance of adsorbent can be stablized in 39mg/g, illustrate that adsorbent has good sorption cycle stability.
5th, 0.5g titanium-type lithium ion sieve is weighed, for sodium ion, magnesium ion, potassium ion, calcium ion, each ion concentration of lithium ion
100mg/L simulation bittern absorption is respectively may be about, temperature constant magnetic stirring adsorbs 24h at 30 DEG C, calculates titanium-type lithium ion sieve
To the adsorbance of each metal ion.
The adsorptive selectivity of the titanium-type lithium ion sieve of table 1
As shown in Table 1, adsorbent is 38.28mg/g to lithium ion adsorbance, is only 0.096mg/g to magnesium ion adsorbance, right
Absorption is not present in other metal ions, and selectivity is good.Embodiment 3
10.4226g lithium lactates mix to (mass ratio is 75 with the titanium dioxide that 3.4742g particle diameters are 100nm:25), with ethanol
As dispersant, the addition of dispersant is 10%, and 2h is ground in grinding, 1h is then dried at 50 DEG C, in air atmosphere
In be warming up to 85 DEG C from room temperature with 5 °/min heating rate, stop 1h, continuation is warming up to 500 with 5 °/min heating rate
DEG C, roasting 8h obtains titanium-type lithium ion sieve presoma Li2TiO3。
The preparation of titanium-type lithium ion sieve, absorption, pickling desorption and embodiment 1 are identical, and its adsorbance is 30.5mg/g.
Embodiment 4
8.5369g lithium lactates mix to (mass ratio is 70 with the titanium dioxide that 3.6586g particle diameters are 100nm:30), using water as
Dispersant, the addition of dispersant is 6%, and 1h is ground in grinding, 3h is then dried at 40 DEG C, from room in air atmosphere
Temperature is warming up to 200 DEG C with 10 °/min heating rate, stops 2h, continues to be warming up to 900 DEG C, roasting with identical heating rate
3h obtains titanium-type lithium ion sieve presoma Li2TiO3。
The preparation of titanium-type lithium ion sieve, absorption, pickling desorption and embodiment 1 are identical, and its adsorbance is 27.9mg/g.
Claims (9)
1. a kind of preparation method of titanium-type lithium ion sieve adsorbant, it is comprised the following steps that：By titanium dioxide and the organic acid of lithium
Salt is mixed to form solid-phase mixture, and the wherein mass fraction of titanium dioxide is 25%~40%, adds dispersant ground and mixed,
Then dried at 25 DEG C~50 DEG C, then temperature programming is to 500 DEG C~900 DEG C, 2~8h of roasting obtains lithium ion sieve presoma
Li2TiO3, by Li2TiO3Presoma is modified using inorganic acid and obtains ion sieve H2TiO3。
2. preparation method according to claim 1, it is characterised in that the organic acid hydrochlorate of described lithium is lithium acetate or third
Sour lithium.
3. preparation method according to claim 1, it is characterised in that the particle diameter of described titanium dioxide be 30nm~
100nm。
4. preparation method according to claim 1, it is characterised in that described dispersant is at least one in ethanol or water
Kind；The addition quality of dispersant is the 1%~10% of solid phase mixing amount of substance.
5. preparation method according to claim 1, it is characterised in that described drying time is 1~5h.
6. preparation method according to claim 1, it is characterised in that the program of described heating is：With 3 °/min~10 °/
Min heating rate is warming up to 65 DEG C~200 DEG C 1~3h of insulation；500 DEG C~900 DEG C 2~8h of insulation are warming up to again.
7. preparation method according to claim 1, it is characterised in that described inorganic acid is in hydrochloric acid, nitric acid or sulfuric acid
It is a kind of or two kinds；The concentration of inorganic acid is 0.05mol/L~0.2mol/L.
8. preparation method according to claim 1, it is characterised in that the time that described inorganic acid is modified is 6h~12h.
9. preparation method according to claim 1, it is characterised in that preparation-obtained H2TiO3Lithium ion sieve is used to adsorb
When simulating lithium ion in bittern, its lithium adsorbance reaches 30mg/g~50mg/g.
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Cited By (8)
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| CN108745276A (en) * | 2018-04-18 | 2018-11-06 | 南京工业大学 | A kind of preparation method of mixed-forming lithium ion adsorbent |
| CN108940181A (en) * | 2018-06-12 | 2018-12-07 | 南京工业大学 | A kind of titanium-type lithium ion sieve adsorbant and application |
| CN110106356A (en) * | 2019-05-24 | 2019-08-09 | 江苏特丰新材料科技有限公司 | A kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine |
| CN111029478A (en) * | 2019-12-13 | 2020-04-17 | 昆山国显光电有限公司 | OLED light-emitting device and preparation method thereof |
| CN111185139A (en) * | 2020-01-13 | 2020-05-22 | 西藏自治区地质矿产勘查开发局中心实验室 | Preparation method of hydrophilic spherical composite lithium ion sieve adsorbent |
| CN111558350A (en) * | 2020-06-16 | 2020-08-21 | 东北林业大学 | Preparation method of HTO/cellulose aerogel microspheres for extracting lithium from seawater |
| CN112473616A (en) * | 2020-11-04 | 2021-03-12 | 中国科学院青海盐湖研究所 | Porous C-MnOx/Sn-Al-H2TiO3Ion sieve, preparation method and application thereof |
| CN112844298A (en) * | 2019-11-28 | 2021-05-28 | 天津大学 | Lithium ion sieve adsorbent and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108745276A (en) * | 2018-04-18 | 2018-11-06 | 南京工业大学 | A kind of preparation method of mixed-forming lithium ion adsorbent |
| CN108940181A (en) * | 2018-06-12 | 2018-12-07 | 南京工业大学 | A kind of titanium-type lithium ion sieve adsorbant and application |
| CN110106356A (en) * | 2019-05-24 | 2019-08-09 | 江苏特丰新材料科技有限公司 | A kind of method of powder-type titanium system's ion-exchanger separation Lithium from Salt Lake Brine |
| CN112844298A (en) * | 2019-11-28 | 2021-05-28 | 天津大学 | Lithium ion sieve adsorbent and preparation method and application thereof |
| CN111029478A (en) * | 2019-12-13 | 2020-04-17 | 昆山国显光电有限公司 | OLED light-emitting device and preparation method thereof |
| CN111185139A (en) * | 2020-01-13 | 2020-05-22 | 西藏自治区地质矿产勘查开发局中心实验室 | Preparation method of hydrophilic spherical composite lithium ion sieve adsorbent |
| CN111558350A (en) * | 2020-06-16 | 2020-08-21 | 东北林业大学 | Preparation method of HTO/cellulose aerogel microspheres for extracting lithium from seawater |
| CN112473616A (en) * | 2020-11-04 | 2021-03-12 | 中国科学院青海盐湖研究所 | Porous C-MnOx/Sn-Al-H2TiO3Ion sieve, preparation method and application thereof |
| CN112473616B (en) * | 2020-11-04 | 2022-05-31 | 中国科学院青海盐湖研究所 | Porous C-MnOx/Sn-Al-H2TiO3Ion sieve, preparation method and application thereof |
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Application publication date: 20171013 |