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Composite a-type molecular sieve raw powder containing wave-absorbing material and full zeolite molecular sieve, their preparation method and application

A technology of zeolite molecular sieve and wave-absorbing materials, which is applied in the field of molecular sieves, can solve the problems of destroying the molecular sieve skeleton, reducing the content of lithium ions, and failing to produce finished products, so as to improve the efficiency of adsorption treatment, improve the adsorption performance, and improve the passing performance.

Active Publication Date: 2021-05-25
CATLION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent application CN200810050070.2 (2008) discloses the preparation method of Li-LSX molecular sieve, which is to obtain K + -LSX, and then exchanged multiple times with ammonium ion aqueous solution to obtain NH 4 -LSX, finally Li-LSX is obtained by Lithium exchange, and NH needs to be recovered during Lithium exchange 3 Facilitates Li exchange; this method employs NH 4 + The transitional exchange method improves the utilization rate of Li, and the treatment process is relatively complicated, and due to the poor hydrothermal stability of the low-silicon-alumina molecular sieve framework itself, there is a possibility of destroying the molecular sieve framework in the frequent hydrothermal ion exchange process, resulting in the final The finished product cannot be used for lithium-ion non-aqueous electrolyte to remove impurities
Another reason why the Li-LSX prepared in this application cannot be used for the removal of impurities in lithium-ion non-aqueous electrolytes is that it involves the preparation of molecular sieve raw powder, but in actual use, molecular sieve raw powder often needs to go through a ball making process Only small balls can be used normally; in the ball making process, it is inevitable to add binders and other additives, so even if the Li exchange degree is high in the early stage, after the ball making process, the content of lithium ions will inevitably decrease accordingly, and at the same time When the lithium-ion non-aqueous electrolyte deeply absorbs a small amount of water, the ion exchange in the binder and other materials will also cause secondary pollution of other ions, especially sodium ion pollution is fatal to the lithium-ion non-aqueous electrolyte
[0005] In addition to the above problems, in the process of removing impurities from a large number of lithium-ion non-aqueous electrolytes, there are also problems of how to efficiently desorb and regenerate molecular sieves that have adsorbed impurities, and the problem of controlling the manufacturing cost of adsorbents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] This embodiment relates to a preparation method of all-zeolite lithium-type molecular sieve containing wave-absorbing material, including steps S1-S5.

[0037] S1, in-situ synthesis of composite A-type molecular sieve raw powder with wave-absorbing function:

[0038] According to the molar ratio of materials 3Na 2 O:2SiO 2 :Al 2 o 3 :128H 2 0, take sodium silicate and sodium aluminate, be made into solution respectively, then add sodium hydroxide to two solutions respectively, then two solutions are mixed evenly;

[0039] Weigh 1 kg of silicon carbide powder and add it to the alkaline silica-alumina sol reaction solution (feeding according to the theoretical output of 9 kg of A-type molecular sieve), put it into a microwave reactor, and react at 100W for 10 minutes to obtain a composite 4A molecular sieve raw powder containing silicon carbide wave-absorbing materials.

[0040] S2, ball making:

[0041] Weigh 8kg (dry basis) of composite 4A molecular sieve raw powd...

Embodiment 2

[0059] This embodiment relates to a preparation method of all-zeolite lithium-type molecular sieve, including steps S1-S4.

[0060] S1, ball making:

[0061] Weigh 8kg (dry basis) commercial 4A molecular sieve (chemical formula is 3Na 2 O:2SiO 2 :Al 2 o 3 :128H 2 O) Original powder, kaolin 2kg, placed in a Φ500mm mixer, mixed for 30 minutes;

[0062] Weigh 5kg of the mixture, put it into the EIRICH automatic molding machine, inject the mixed solution for molding, and the diameter of the molding particles is 1.2-1.8mm;

[0063] The shaped particles are placed in a vacuum muffle furnace, and fired at 350-550° C. for 2-3 hours to obtain spherical particle materials.

[0064] Take the spherical granular material and put it in a drying dish to cool to room temperature, take a sample to measure the static water adsorption, and the static water adsorption reaches 20.0wt%.

[0065] S2, turn crystal:

[0066] According to the ratio of the weight ratio of the obtained crystalliz...

Embodiment 3

[0079] This embodiment relates to a preparation method of all-zeolite calcium-type molecular sieve containing wave-absorbing material, including steps S1-S5.

[0080] S1, in-situ synthesis of composite A-type molecular sieve raw powder with wave-absorbing function:

[0081]According to the material molar ratio 12M 2 O:60SiO 2 :Al 2 o 3 :400H 2 O, take sodium silicate and mix with water to form a solution, and add aluminum isopropoxide and sodium hydroxide to form a solution after weighing tetramethylammonium hydroxide solution; mix the two solutions evenly, and the four The molar ratio of methyl ammonium hydroxide (TMA) to sodium ions is 1.675;

[0082] Weigh 0.5kg of silicon carbide powder and add it into the reaction solution of alkaline silica-alumina sol (feeding according to the theoretical output of 9.5kg of A-type molecular sieve), put it into a microwave reactor, react at 100W for 60min, and obtain a composite 4A molecular sieve raw material containing silicon car...

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Abstract

The invention relates to a composite A-type molecular sieve raw powder containing a wave-absorbing material and a full zeolite molecular sieve, their preparation method and application, and belong to the technical field of molecular sieves. The original powder of composite A-type molecular sieve containing wave-absorbing material includes micro-nano size wave-absorbing material, and A-type molecular sieve obtained by in-situ growth with wave-absorbing material as seed crystal; The wave-absorbing material-containing compound A-type molecular sieve raw powder is made into a wave-absorbing material-containing all-zeolite molecular sieve. The all-zeolite molecular sieve containing wave-absorbing material prepared by the invention can deeply absorb specific molecules, and can be rapidly regenerated through microwave heating.

Description

technical field [0001] The invention relates to a technology in the field of molecular sieves, in particular to a composite A-type molecular sieve raw powder containing a wave-absorbing material and a full zeolite molecular sieve, their preparation method and application. Background technique [0002] Lithium-ion batteries are mainly composed of positive electrodes, negative electrodes, and electrolytes. Lithium ions must be intercalated between the positive and negative electrodes through the electrolyte to charge and discharge; during the first charge and discharge process of lithium-ion batteries, there will also be A reaction occurs between the liquid and the electrode material to form a solid electrolyte interface film (SEI), which has an important impact on the performance of lithium-ion batteries. However, the electrolyte will inevitably be mixed with trace impurities such as water, acid and alcohol during the production process. Even in commercial electrolytes with e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/18B01J20/30B01J20/34B01D15/00
CPCB01J20/186B01J20/3441B01D15/00Y02P70/50
Inventor 龚强
Owner CATLION CO LTD
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