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Method for preparing high-silicon CHA type SSZ-13 molecular sieve

A molecular sieve and high-silicon technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, inorganic chemistry, etc., to achieve the effects of high solid phase yield, increased solid phase yield, and shortened crystallization time

Active Publication Date: 2018-03-06
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the CHA-type SSZ-13 zeolite molecular sieve silicon-alumina (Si / Al) synthesized by this method in a conventional inorganic alkali system is relatively low, usually between 2.5 and 16.

Method used

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  • Method for preparing high-silicon CHA type SSZ-13 molecular sieve
  • Method for preparing high-silicon CHA type SSZ-13 molecular sieve
  • Method for preparing high-silicon CHA type SSZ-13 molecular sieve

Examples

Experimental program
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Effect test

preparation example Construction

[0030] Preparation of starting material LTL type L zeolite:

[0031] Under the condition of stirring at room temperature, 40 g of deionized water, 1.48 g of sodium hydroxide (NaOH, 96 wt%) and 3.164 g of KOH were stirred in a beaker until dissolved, and then 1.088 g of NaAlO 2 (Al 2 o 3 , 41.3wt%; Na 2 O, 35%), slowly add 8.696g of white carbon black (SiO 2 , 92wt%), stirred vigorously for 2h. The resulting reaction gel was transferred to a stainless steel reaction vessel with a Teflon liner. Static aging at room temperature for 24 hours, constant temperature crystallization at 170°C for 12 hours, quenching to room temperature, washing the product, filtering, and drying to obtain NaK type L zeolite molecular sieve powder, which was used as the starting material of Example 1; NaK type L Zeolite and 1mol / L NH 4 The Cl aqueous solution was mixed with a solid-to-liquid ratio of 1g: 20mL and added to the conical flask, heated in a water bath at 80°C and stirred for 2 hours, t...

Embodiment 1

[0041] NaK type L zeolite was converted into SSZ-13 molecular sieve as the starting zeolite. Proceed as follows:

[0042] Under stirring conditions at room temperature, 20.925g of N,N,N-trimethyladamantane ammonium hydroxide solution (TMADaOH, 25wt%), 21.431g of deionized water and 0.345g of sodium hydroxide (NaOH, 96wt%), Mix and stir in a beaker until clear, then slowly add 4.575 g of silica (SiO 2 , 92wt%), after stirring vigorously for 2h, add 0.95g of NaK type L zeolite (SiO in L zeolite 2 is 15% of the total mass of the silicon source), after stirring for 1 h, finally add 0.105 g of roasted SSZ-13 seed crystals accounting for 2% of the total mass of the silicon source, stir vigorously at room temperature for 1 h, and transfer the above mixture to a polytetrafluoroethylene Lined stainless steel reactor. Crystallize at 155°C for 72h, take it out, and quench it to room temperature, wash it with deionized water until neutral, dry it at 100°C, and roast it in air at 550°C ...

Embodiment 2

[0044] NH 4 Type L zeolite was used as the starting zeolite to synthesize SSZ-13 molecular sieve. Proceed as follows:

[0045] Under stirring conditions at room temperature, 13.95 g of N,N,N-trimethyladamantane ammonium hydroxide solution (TMADaOH, 25 wt%), 19.237 g of deionized water and 0.345 g of sodium hydroxide (NaOH, 96 wt%) were mixed in Mix and stir in a beaker until clear, then slowly add 5.005g of white carbon black (SiO 2 , 92wt%), after stirring vigorously for 2h, add NH 4 Type L zeolite 0.445g (SiO in L zeolite 2 is 7% of the total mass of the silicon source), stirred for 1 h, and finally added 0.0525 g of roasted SSZ-13 seed crystals accounting for 1% of the total mass of the silicon source, continued to stir at room temperature for 1 h, and transferred the above mixture to a polytetrafluoroethylene-lined stainless steel reactor. Crystallize at 155°C for 60h, take it out, and then quench it to room temperature, wash it with deionized water until neutral, dry...

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Abstract

The invention discloses a method for synthesizing a high-silicon CHA type SSZ-13 molecular sieve by utilizing topologic reconstruction of a seed crystal and LTL type L zeolite. The method comprises the following steps: weighing water, an alkali source, a template agent, an additional solid silicon source, L zeolite and a seed crystal to carry out a crystallization reaction, completely reacting toobtain a crystallization reaction product, cooling and washing to be neutral, and drying to obtain crude molecular sieve powder; and calcining the crude molecular sieve powder in air at the temperature of 550 DEG C for a certain time, thereby obtaining the final product SSZ-13 molecular sieve. According to the method disclosed by the invention, the high-silicon CHA type SSZ-13 molecular sieve is synthesized by adopting direct topologic reconstruction of the LTL type L zeolite at a low silica-alumina ratio, and the initial L zeolite does not need to be subjected to dealuminzation pretreatment.By regulating the addition amount of the L zeolite, the silica-alumina ratio of the product SSZ-13 molecular sieve can be regulated in a wide range, the solid phase yield is increased, the productioncost can be reduced, and industrialized production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of catalysts (molecular sieves), and specifically relates to a method for synthesizing high-silicon CHA-type SSZ-13 molecular sieves by using crystal seeds and LTL-type L zeolite topology reconstruction. Background technique [0002] Molecular sieves have been widely used due to their regular and orderly structure, adjustable skeleton composition, high specific surface area and adsorption capacity, cation exchangeability, good shape selectivity of pores, high thermal stability and chemical stability, etc. It is widely used in the field of catalytic industry. A new type of molecular sieve SSZ-13 with CHA crystal structure was synthesized by American chemist Zones SI by hydrothermal method. SSZ-13 molecular sieve has an ellipsoidal cage with an eight-membered ring structure and a three-dimensional intersecting pore structure. Its specific surface area is large, and there are many exchangeable cations and surf...

Claims

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Application Information

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IPC IPC(8): C01B39/48
CPCC01B39/48C01P2002/72C01P2004/03C01P2004/38C01P2004/61C01P2004/62
Inventor 李玉平张翊刘瑞边慧敏李晓峰窦涛
Owner TAIYUAN UNIV OF TECH
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