Preparation method of porous spinning composite material and lithium extraction application thereof

A composite material and spinning technology, applied in the field of porous spinning composite materials and lithium ion adsorption materials, can solve the problems of unfavorable large-scale industrial operation, low lithium concentration, poor cycle stability, etc., and achieve easy continuous industrial operation and preparation. Simple process flow and the effect of solving poor fluidity

Active Publication Date: 2021-04-09
TIANJIN UNIV OF SCI & TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005]1. Patent CN101898113A discloses a polyvinyl chloride as binder, manganese lithium ion sieve (LMO: LiMn2O 4, Li1.6Mn1.6O4, Li4Mn 5O12) as the core material of the spherical lithium-ion composite adsorbent, although the problem of poor fluidity has been improved, the adsorption rate of the coated lithium-ion sieve decreased significantly
[0006]2. Patent CN106902781B discloses a mesoporous hollow silicon sphere loaded with HMO, which has a large specific surface area and adsorption rate, but the lithium ion sieve directly Exposed to the surface of the hollow silica spheres in contact with the solution, so the cycle stability is poor
[0007] 3. Patent CN102211012A discloses a polyvinylidene fluoride as a binder, N,N-dimethylacetamide as a solvent, Li1.6 Mn1.6O4 The lithium-ion sieve mixed matrix membrane with the core material is used for lithium extraction from seawater. However, the loading of the core material per unit mass is small and the adsorption balance The time is long (12 hours), and the efficiency of lithium extraction is low
[0008] 4. Patent CN109225121A discloses a polyacrylonitrile as binder, H1.6Mn1.6 The hollow fiber membrane with O4 as the core material, although the lithium extraction efficiency has been further improved, but the manganese dissolution loss is serious due to the disproportionation reaction during hydrochloric acid elution, the cycle stability is poor, and the corresponding Membrane modules are easy to be polluted, and the maintenance cost of membrane equipment is expensive, which is not conducive to large-scale industrial operation
[0009]Due to the low salinity of lithium mineralization in geothermal water, generally only 1-10g / L, and low lithium concentration (5-30mg / L), its green and efficient extraction Difficult; on the other hand, for the surface brine of salt lakes with low salinity, due to the dissolution loss of manganese-based lithium ion sieves, it is easy to cause pollution and has poor cycle stability. The adsorption materials mentioned in the above patents are not suitable for geothermal water and Lithium extraction from surface brine of low salinity salt lake

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  • Preparation method of porous spinning composite material and lithium extraction application thereof
  • Preparation method of porous spinning composite material and lithium extraction application thereof
  • Preparation method of porous spinning composite material and lithium extraction application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Example 1: Polysulfone-H 2 TiO 3 Preparation of porous spinning composites and its geothermal extraction of lithium

[0045] Weigh 10 g of polysulfone particles into a beaker, add 90 g of N-methylpyrrolidone into the beaker, and heat and stir with a constant temperature water bath magnetic stirrer until the polysulfone particles are completely dissolved.

[0046] Weigh 10g H 2 TiO 3 Add the powder and 8g of water-soluble porogen PEG-400 into the above polysulfone mixed solution, mix well and stir evenly, and make the H-type lithium ion sieve powder H 2 TiO 3 Uniformly dispersed in polysulfone mixed solution.

[0047] Polysulfone / H 2 TiO 3 Add the composite spinning stock solution to the raw material tank of the wet spinning equipment, adjust the number of spinneret holes to 40, the diameter of the spinneret holes to be 0.07mm, the spinneret speed to be 13m / min, and the drafting and winding speed to be 16m / min , sprayed into the coagulation bath through the spinn...

Embodiment 2

[0051] Example 2: Polyacrylonitrile-H 4 Ti 5 o 12 Preparation of Spinning Composite Materials and Its Geothermal Extraction of Lithium

[0052] Weigh 10 g of polyacrylonitrile powder into a beaker, add 90 g of dimethylformamide into the beaker, and heat and stir with a constant temperature water bath magnetic stirrer until the polyacrylonitrile powder is completely dissolved.

[0053] Weigh 5g H 4 Ti 5 o 12 The powder is added into the above polyacrylonitrile mixed solution, fully mixed and stirred evenly, so that the lithium ion sieve powder is uniformly dispersed in the polyacrylonitrile mixed solution.

[0054] PAN / H 4 Ti 5 o 12 Add the composite spinning stock solution to the raw material tank of the wet spinning equipment, adjust the number of spinneret holes to 50, the diameter of the spinneret holes to be 0.05mm, the spinneret speed to be 10m / min, and the drafting and winding speed to be 110m / min , through the spinneret into the coagulation bath, through phase ...

Embodiment 3

[0056] Embodiment 3: polyacrylonitrile-Li 2 TiO 3 Preparation of Spinning Composite Materials and Its Geothermal Extraction of Lithium

[0057] Weigh 10.5 g of polyacrylonitrile powder into a beaker, add 90 g of dimethylformamide into the beaker, heat and stir with a constant temperature water bath magnetic stirrer until the polyacrylonitrile powder is completely dissolved.

[0058] Weigh 10g Li 2 TiO 3 The powder is added into the above polyacrylonitrile mixed solution, fully mixed and stirred evenly, so that the lithium ion sieve powder is uniformly dispersed in the polyacrylonitrile mixed solution.

[0059] Polyacrylonitrile / Li 2 TiO 3 Add the composite spinning stock solution to the raw material tank of the wet spinning equipment, adjust the number of spinneret holes to 40, the diameter of the spinneret holes to be 0.07mm, the spinneret speed to be 10m / min, and the drafting and winding speed to be 10m / min , spun into the coagulation bath through the spinneret, formed...

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Abstract

The invention discloses a method for preparing a porous spinning composite material and lithium extraction application of the porous spinning composite material, and the method comprises the following steps: (1) mixing, heating and stirring a high-molecular polymer and an organic solvent to fully dissolve the high-molecular polymer, and standing for defoaming; (2) adding lithium ion sieve powder and a water-soluble pore-foaming agent into the mixed solution, and fully stirring and uniformly mixing; (3) spraying the mixed solution into a coagulating bath by using wet spinning equipment, and carrying out phase inversion molding; and (4) drawing, washing, drying and curing to obtain the porous spinning composite adsorbing material. The obtained porous spinning composite adsorbing material is applied to extraction of lithium in liquid lithium ore. The method effectively solves the problems of poor fluidity and cycle stability of the powder material, and greatly enhances the adsorption rate and adsorption capacity compared with granular or rod-like adsorption materials, thereby having favorable application prospects in the development and utilization of lithium resources in salt lake brine, underground brine, geothermal water and the like.

Description

technical field [0001] The invention belongs to the field of material chemical industry, and relates to lithium ion adsorption materials, in particular to a method for porous spinning composite materials. Background technique [0002] Lithium, as the lightest metal, is widely used in aerospace, lithium-ion batteries, nuclear industry, ceramics, electronic devices and other fields, and is known as the "strategic energy metal" in the 21st century. With the continuous development of modern high-tech, people's demand for lithium is increasing day by day. The sources of lithium are mainly divided into two categories: one is solid lithium ore resources such as lepidolite, spodumene, and petalite, and the other is mainly salt lake brine, concentrated seawater, geothermal water, underground brine, etc. liquid lithium ore resources. However, with the increasing depletion of solid lithium ore resources and the high energy consumption during extraction, people have gradually turned t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30C22B26/12C22B3/24
CPCB01J20/262B01J20/28023C22B26/12C22B3/24Y02P10/20B01J20/3007B01J20/3064B01J20/04
Inventor 邓天龙赵凯宇余晓平李明礼多吉郭亚飞
Owner TIANJIN UNIV OF SCI & TECH
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