Method for preparing manganese oxide ionic sieve precursor LixMn3-xO4 by using one-step method

A precursor and ion sieve technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of no process simplification, good adsorption effect, complicated treatment process, low degree of industrialization, etc., and achieve low cost and simple operation , the effect of less by-products

Active Publication Date: 2018-09-21
西安金藏膜环保科技有限公司
View PDF8 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw material used in this document is the trivalent manganese raw material Mn 2 o 3 , instead of manganese salt, the reaction process not only has high temperature and high energy consumption, but also has a complicated preparation process and a low degree of industrialization;
[0005] Also, "CN103121724A prepares lithium ion sieve MnO 2 0.5H 2 O and its precursor Li 1.6 mn 1.6 o 4 method", using inorganic manganese salts and lithium salts as raw materials, one-step hydrothermal synthesis of intermediates and then low-temperature roasting to obtain the required precursor Li 1.6 mn 1.6 o 4 ; Then carry out acid treatment to the precursor, extract the Li in it, become H-type ion sieve, and then get the ion sieve adsorbent MnO which has sieving effect to lithium ion through washing, filtering and drying 2 0.5H 2 O; obtained by hydrothermal synthesis first, and then roasted, the preparation process is complicated and the preparation time is long
[0006] In addition, "CN106311190A preparation method of porous manganese lithium ion sieve adsorbent" uses manganese salt and lithium salt as raw materials, uses chitosan solution as dispersant, undergoes hydrothermal reaction, and roasts at low temperature to obtain lithium ion sieve precursor Li 4 mn 5 o 12 ; Then the precursor is acid-treated, the Li therein is extracted, washed with acid leaching, filtered and dried to obtain lithium ion sieve H 4 mn 5 o 12 In this patent, it takes multi-step treatment to obtain the precursor, hydrothermal and roasting, the treatment process is complicated, and the reaction time is long. The prepared adsorbent takes more than 10 hours to reach the adsorption equilibrium, and the adsorption time is long
[0007] It can be seen that the preparation methods in the prior art do not really realize the simplification of the process and the good adsorption effect. The present invention is based on the simple preparation process (one-step method) and the good preparation method of the obtained adsorbent.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing manganese oxide ionic sieve precursor LixMn3-xO4 by using one-step method
  • Method for preparing manganese oxide ionic sieve precursor LixMn3-xO4 by using one-step method
  • Method for preparing manganese oxide ionic sieve precursor LixMn3-xO4 by using one-step method

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0034]The preparation process of the present invention is as follows: mix manganese salt, liquid-phase inorganic / organic oxidizing agent and lithium-containing inorganic powder, put the mixture in a mechanically sealed high-speed grinding device for mechanical grinding for 1-4 hours, and make it generate a one-step solid phase reaction to obtain a mixture; wherein, the manganese salt powder raw materials include but not limited to various industrial grade, analytical pure or battery grade manganese chloride, manganese nitrate and other salt raw materials, and the particle size of the manganese salt powder is below 500 μm; lithium-containing inorganic The powder is one or more of lithium hydroxide and lithium carbonate. The particle size of the lithium-containing inorganic powder is less than 500 μm; the ratio of the amount of lithium to the amount of manganese is 1 to 0.5:1; liquid-phase oxidants include but are not limited to hydrogen peroxide, peracetic acid or peroxybenzoic ...

Embodiment 1

[0039] Accurately weigh 200g of manganese nitrate tetrahydrate and 42g of lithium hydroxide monohydrate and mix them thoroughly, add 300mL of 30% hydrogen peroxide, place it in an eccentric vibrating mill, set the speed at 1500r / min, repeat the grinding cycle for 4h, solidification occurs After the phase reaction, dry and evaporate the obtained slurry at 70°C to remove organic by-products and water to obtain the lithium manganese oxide intermediate, and react the lithium manganese oxide intermediate at 550°C for 6h in an aerobic environment , you can get manganese oxide lithium ion sieve precursor Li 1.6 mn 1.6 o 4 . Precursor Li 1.6 mn 1.6 o 4 Delithium treatment in 0.5M hydrochloric acid, take 1g for Li + In the aqueous phase solution with a concentration of 220mg / L, it was adsorbed at pH=8 for 6h, and the adsorption amount of lithium was measured to be 23.8mg / g. The saturated lithium ion sieve was placed in 0.5M hydrochloric acid solution for analysis, and the analys...

Embodiment 2

[0043] Accurately weigh 200g of manganese nitrate tetrahydrate, 300mL of 30% hydrogen peroxide, 100mL of peroxybenzoic acid and 42g of lithium hydroxide monohydrate and fully mix them in the eccentric vibrating mill. After the phase reaction, the obtained slurry was dried and evaporated at 70°C to remove organic by-products and water to obtain a lithium manganese oxide intermediate, and the lithium manganese oxide intermediate was reacted at 500°C for 6h in an aerobic environment , you can get manganese oxide lithium ion sieve precursor LiMn with a particle size distribution range of 50-1000nm 2 o 4 . The precursor LiMn 2 o 4 Delithium treatment in 0.5M hydrochloric acid, take 1g for Li + In an aqueous phase solution with a concentration of 220 mg / L, it was adsorbed at pH=8 for 4 hours, and the adsorption amount of lithium was measured to be 21.3 mg / g. The saturated lithium ion sieve was placed in 0.5M hydrochloric acid solution for analysis, and the analysis rate reached...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
Particle sizeaaaaaaaaaa
Login to view more

Abstract

The invention discloses a method for preparing a manganese oxide ionic sieve precursor LixMn3-xO4 by using a one-step method. The method comprises the following steps: mixing a manganese salt, an oxidant and lithium-containing inorganic powder, preparing slurry through a one-step liquid-solid reaction in a sealed environment, directly drying the slurry, and further carrying out roasting annealingtreatment, thereby obtaining manganese oxide ionic sieve precursor LixMn3-xO4. The manganese oxide ionic sieve precursor LixMn3-xO4 is subjected to lithium removal modification in an acid solution, that is, lithium can be selectively adsorbed from lithium-containing solutions such as brine water and seawater. The preparation disclosed by the invention is simple in operation process, low in sintering temperature, free of wastewater or waste material generation, rich in raw material source, low in price, low in energy consumption and is an energy-saving and environment-friendly green and economic lithium ionic sieve production method.

Description

technical field [0001] The invention belongs to the field of energy-saving production of inorganic compounds, in particular to one-step preparation of manganese ion sieve precursor Li x mn 3-x o 4 Methods. Background technique [0002] Li x mn 3-x o 4 It is a general term for manganese oxide ion sieve precursors. The most studied lithium manganese oxide ion sieve precursors are LiMn 2 o 4 , Li 1.33 mn 1.67 o 4 (Li 4 mn 5 o 12 ) and Li 1.6 mn 1.6 o 4 (LiMnO 2 ). Usually, the methods for preparing the above precursors include soft chemical methods, sol-gel methods, hydrothermal methods, etc. The existing synthesis methods generally use MnOOH as a manganese source to synthesize LiMnO 2 , and the synthesis of MnOOH itself is relatively complicated, requiring high operating conditions, and MnOOH is unstable in the air, which is not conducive to industrial production; in the preparation process of the hydrothermal method, other additives such as oxidants need to ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): B01J20/04B01J20/30
CPCB01J20/04
Inventor 王磊孟晓荣吴浩黄丹曦陈立成李陈陈铖霍姗姗
Owner 西安金藏膜环保科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products