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Method for preparing molecular sieve from lithium slag

A molecular sieve and lithium slag technology, applied in the field of solid waste comprehensive utilization technology and molecular sieve material preparation, can solve the problems of long pretreatment time, unfavorable production efficiency, inconvenient operation, etc., achieve short reaction time, increase economic added value, save resource effect

Active Publication Date: 2021-10-26
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the use of industrial waste residues to prepare molecular sieves requires high-temperature activation in the early stage, which has the disadvantages of high energy consumption and inconvenient operation. At the same time, the pretreatment time is long, which is not conducive to improving production efficiency.

Method used

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  • Method for preparing molecular sieve from lithium slag
  • Method for preparing molecular sieve from lithium slag
  • Method for preparing molecular sieve from lithium slag

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A kind of method utilizing lithium slag to prepare molecular sieve, comprises the steps:

[0032] (1) 10 grams of lithium slag (the weight percent content of each component is: SiO2:70.32%, Al2O3:25.10%, Fe2O3 content is 0, others: 4.58%, the main crystal phase is leaching spodumene) into In 80mL of 3.5mol / L sodium hydroxide solution, the solid-to-liquid ratio is 1:8 (g / mL), after mixing evenly, a mixture is obtained;

[0033] (2) Ultrasonicate the mixed material by using a plug-in ultrasonic reactor, ultrasonicate for 60 minutes at 45°C, ultrasonic frequency 100KHz, ultrasonic output power 900W, and obtain the material after ultrasonic;

[0034] (3) put the material after ultrasonication into a hydrothermal reaction kettle for hydrothermal crystallization, the crystallization temperature is 95°C, and the crystallization time is 11h to obtain a crystallized product;

[0035] (4) Filter the crystallized product, wash the product with water until pH = 9, and finally dry ...

Embodiment 2

[0038] A kind of method utilizing lithium slag to prepare molecular sieve, comprises the steps:

[0039] (1) 10 grams of lithium slag (the weight percent content of each component is: SiO2: 67.69%, Al2O3: 28.75%, Fe2O3: 0.47%, others: 3.09%, the main crystal phase is leaching spodumene) is added to 90mL In the 4mol / L sodium hydroxide solution, solid-liquid ratio is 1:9 (g / mL), after mixing uniformly, obtain compound;

[0040](2) Ultrasonicate the mixture by using a plug-in ultrasonic reactor, ultrasonicate for 60 minutes at 70°C, ultrasonic frequency 130KHz, ultrasonic output power 1800W, and obtain the ultrasonicated material;

[0041] (3) put the ultrasonicated material into a hydrothermal reaction kettle for hydrothermal crystallization, the crystallization temperature is 100°C, and the crystallization time is 8h to obtain a crystallized product;

[0042] (4) Filter the crystallized product, wash the product with water to pH = 10, and finally dry at 150° C. for 0.5 h to ob...

Embodiment 3

[0044] A kind of method utilizing lithium slag to prepare molecular sieve, comprises the steps:

[0045] (1) 10 grams of lithium slag (the weight percent content of each component is: SiO2: 64.32%, Al2O3: 30.65%, Fe2O3: 0.99%, others: 4.04%, the main crystal phase is leaching spodumene) is added to 80mL In the 3.25mol / L sodium hydroxide solution, the solid-to-liquid ratio is 1:8 (g / mL), after mixing uniformly, the mixture is obtained;

[0046] (2) Ultrasonicate the mixture by using a plug-in ultrasonic reactor, ultrasonicate for 90min at 40°C, ultrasonic frequency 90KHz, ultrasonic output power 1000W, and obtain the ultrasonicated material;

[0047] (3) put the material after ultrasonication into a hydrothermal reaction kettle for hydrothermal crystallization, the crystallization temperature is 90°C, and the crystallization time is 12h, to obtain a crystallized product;

[0048] (4) Filter the crystallized product, wash the product with water to pH = 8, and finally dry at 120...

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Abstract

The invention discloses a method for preparing a molecular sieve from lithium slag, and belongs to the technical field of molecular sieve materials. The method comprises the steps that firstly, the lithium slag is added into an alkaline compound aqueous solution of sodium, the mixture is mixed to be uniform and then placed in an ultrasonic reactor, ultrasonic treatment is conducted for 0.1-180 min at the temperature of 20-95 DEG C, the ultrasonic frequency is 10-130 KHz, the output power is 0.1-1800 W, hydrothermal crystallization is conducted on the material obtained after ultrasonic treatment, a product is filtered and washed with water till the pH is 8-10, and finally drying is conducted to obtain the molecular sieve. Compared with the prior art, the method has the advantages that the molecular sieve is prepared from the lithium slag, waste is turned into wealth, the raw material cost is low, high-temperature activation treatment is not needed, the reaction conditions are mild, the NaX, NaA, NaP, NaX / NaA eutectic, NaX / NaP eutectic, NaA / NaP eutectic or NaX / NaA / NaP eutectic molecular sieve can be obtained by changing the synthesis conditions, and the method has a good application prospect.

Description

technical field [0001] The invention relates to a method for preparing molecular sieves by using lithium slag, and belongs to the technical field of solid waste comprehensive utilization technology and preparation of molecular sieve materials Background technique [0002] Lithium slag is a solid waste produced during the production of lithium carbonate by the spodumene sulfuric acid method, and its main components are oxides such as silicon and aluminum. At present, in China, spodumene is used as raw material to produce one ton of lithium carbonate products by sulfuric acid method, which will produce nearly ten tons of lithium slag. Every year, a huge amount of lithium slag is usually disposed of by landfill or open-air stacking, which not only takes up space, but also With the wind and rain, it pollutes the environment and urgently needs to be treated and developed. How to effectively utilize waste lithium slag, turn waste into treasure, and create economic and social bene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02C01B39/22C01B39/14
CPCC01B39/02C01B39/22C01B39/14C01B39/023C01P2002/72
Inventor 张林朱沈杰王海燕崔群黄邵祖
Owner NANJING UNIV OF TECH