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Rapid hydrothermal-synthesized H-LTA-type molecular sieve and preparation method and application thereof

A hydrothermal synthesis and molecular sieve technology, which is applied in the direction of molecular sieve catalysts, molecular sieves and base exchange compounds, chemical instruments and methods, etc., can solve the problems of complex operation procedures, low primary ion exchange rate, and easily etched zeolite channel structure, etc., to achieve The raw materials are cheap and easy to obtain, the ability to resist etching and skeleton collapse is improved, and the effect of avoiding strong water absorption and low water resistance

Active Publication Date: 2019-03-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the ion exchange method, Na-LTA type is usually used for water washing or pickling in a salt solution containing target ions. The operation process is complicated, and it is easy to etch the zeolite pore structure, and the primary ion exchange rate is low.

Method used

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  • Rapid hydrothermal-synthesized H-LTA-type molecular sieve and preparation method and application thereof
  • Rapid hydrothermal-synthesized H-LTA-type molecular sieve and preparation method and application thereof
  • Rapid hydrothermal-synthesized H-LTA-type molecular sieve and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Feeding molar ratio H 2 O-SiO 2 -Al 2 O 3 -(TMA) 2 O=272:12.4:1:4.9

[0050] 1.60g Al(OH) 3 The powder (purity: 99.9%, 3500 mesh) was dissolved in 5.00 g of high-purity water, 35.50 g of tetramethylammonium hydroxide solution (the mass content of TMAOH was 25 wt%) was added to the obtained solution, and the mixture was stirred uniformly to obtain a suspension. Under stirring and normal temperature conditions (25℃, RH=40%), 24.80g SiO was gradually added dropwise to the aluminum source 2 Sol (SiO 2 The mass content is 30wt%), the initial gel is obtained after 2 hours of stirring, which is aged for 2 hours at room temperature, and then transferred to a hydrothermal kettle for rotation and crystallization. The crystallization time was 3 days and the crystallization temperature was 101°C to obtain the initial product. The product was washed 3 to 4 times by centrifugation and ultrasound, the pH of the supernatant 2 O-XO 2 -Y 2 O 3 =1:7.5:1.

[0051] XRD test results such as figu...

Embodiment 2

[0053] Feeding molar ratio H 2 O-SiO 2 -Al 2 O 3 -(TMA) 2 O=214:10.2:1:3.5

[0054] 1.60g Al(OH) 3 The powder (purity: 99.9%, 3500 mesh) was dissolved in 5.00 g of high-purity water, and 25.50 g of tetramethylammonium hydroxide solution (the mass content of TMAOH was 25 wt%) was added to the obtained solution, and the mixture was stirred uniformly to obtain a suspension. Under stirring and normal temperature conditions (25°C, RH=40%), gradually add 20.50g of SiO to the configured aluminum source and template agent mixture. 2 Sol (SiO 2 The mass content is 30wt%), the initial gel is obtained after 2.5 hours of stirring, which is aged at room temperature for 4 hours, and then transferred to a hydrothermal kettle to rotate and crystallize. The crystallization time was 3 days and the crystallization temperature was 101°C to obtain the initial product. The product was washed 3 to 4 times by centrifugation and ultrasound, the pH of the supernatant 2 O-XO 2 -Y 2 O 3 =1:4.9:1.

[0055] XR...

Embodiment 3

[0057] Feeding molar ratio H 2 O-SiO 2 -Al 2 O 3 -(TMA) 2 O=226:9.2:1:4.1

[0058] 1.60g Al(OH) 3 The powder (purity: 99.9%, 3500 mesh) is dissolved in 5.00 g of high-purity water, 30.50 g of tetramethylammonium hydroxide solution (the TMAOH mass content is 25 wt%) is added to the obtained solution, and the mixture is stirred uniformly to obtain a suspension. Under stirring and normal temperature conditions (25℃, RH=40%), gradually add 18.45g SiO 2 Sol (SiO 2 The mass content is 30% by weight), the initial gel is obtained after stirring for 1 h, which is aged for 2 h at room temperature, and then transferred to a hydrothermal kettle for rotation and crystallization. The crystallization time was 2 days and the crystallization temperature was 100°C to obtain the initial product. The product was washed 3 to 4 times by centrifugation and ultrasound, the pH of the supernatant 2 O-XO 2 -Y 2 O 3 =1:3.0:1.

[0059] After testing, the SAR of the obtained H-LTA molecular sieve is 3.0, and t...

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Abstract

The invention provides a rapid hydrothermal-synthesized H-LTA-type molecular sieve and a preparation method and application thereof. The molecular sieve has a chemical composition of mH2O:nXO2:Y2O3 ata molar ratio, wherein X is a tetravalent element, Y is a trivalent element, 0>m>2.4, and n = 3.0-7.5. The molecular sieve is an LTA-type molecular sieve with high crystallinity, an SAR of 3.0-7.5, aBET specific surface area of 825-913 m<2> / g and a nanometer size of 280-400 nm. The preparation method of the H-LTA-type molecular sieve comprises the steps: adding an organic guiding agent tetramethylammonium hydroxide (TMAOH) to a trivalent element source or a tetravalent element source so as to prepare a divergent turbid liquid or sol, adding a tetravalent element source or a trivalent elementsource dropwise and gradually, performing even stirring, performing aging at room temperature, performing static or stirring crystallization at 90-120 DEG C for 1-3 days, and performing four steps including centrifugation, washing, drying and calcination. The method has simple preparation and a short synthesis cycle, the product has high crystallinity and a large specific surface area, and targetions can be exchanged in one step in ion exchange or impregnation application, so that the exchange step is simplified.

Description

Technical field [0001] The invention belongs to the field of inorganic chemistry, and specifically relates to a rapid hydrothermal synthesis of H-LTA molecular sieve and a preparation method and application thereof. Background technique [0002] Zeolite molecular sieves have regular pore structure, ion exchange capacity, catalysis and adsorption and separation capabilities, and have been widely used as ion exchange materials, industrial catalysts and industrial adsorbents. [0003] The main structure of zeolite molecular sieve is TO 4 The tetrahedron (T mainly includes Si, Al and other elements) is connected to form an octahedral structural unit through the double eight-membered ring. Earlier, there was a patent report on the microporous eight-membered ring LTA molecular sieve, which has great advantages in the adsorption and separation process. The big advantage has received widespread attention. Patent US.3375205 and US.3314752 reported that LTA type molecular sieve is a kind of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48B01J20/18B01J29/70
CPCB01J20/186C01B39/48B01J29/70C01P2004/62C01P2006/12C01P2002/72C01P2004/03
Inventor 王树东顾一鸣孙天军赵生生柯权力郭亚
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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