Method for preparing SSZ-39 molecular sieve by taking fluorine-modified Y-type molecular sieve as raw material

A SSZ-39, molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, hydrocarbon production from oxygen-containing organic compounds, etc., can solve the problems affecting the quality of SSZ-39 molecular sieve, inappropriate control indicators, and complex preparation processes, etc. Achieve good hydrothermal stability, high crystallinity, and improve the effect of pore structure

A SSZ-39, molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, hydrocarbon production from oxygen-containing organic compounds, etc., can solve the problems affecting the quality of SSZ-39 molecular sieve, inappropriate control indicators, and complex preparation processes, etc. Achieve good hydrothermal stability, high crystallinity, and improve the effect of pore structure

CN110950354AActive Publication Date: 2020-04-03CHINA CATALYST HLDG CO LTD
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  • Method for preparing SSZ-39 molecular sieve by taking fluorine-modified Y-type molecular sieve as raw material
  • Method for preparing SSZ-39 molecular sieve by taking fluorine-modified Y-type molecular sieve as raw material
  • Method for preparing SSZ-39 molecular sieve by taking fluorine-modified Y-type molecular sieve as raw material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Weigh 2247.6g of deionized water, 359.7g of 30wt% sodium hydroxide aqueous solution and 1385.2g of 31.5wt% N,N-dimethyl-3,5-dimethylpiperidinium hydroxide aqueous solution, After stirring and mixing for 0.5 hours at 35°C, add 1004.7g of fluorine-modified Y-type molecular sieve F-USY-3 (SiO 2 / Al 2 o 3 Molar ratio=22.60), continue stirring and mixing at 25~35° C. for 0.5 hour.

[0045] SiO in the final sol 2 :Al 2 o 3 :Na 2 O:ROH:H 2 O molar ratio 22.60:1.00:2.10:4.20:300.00

[0046] The above sol was transferred to a steel autoclave lined with polytetrafluoroethylene, and crystallized at a stirring speed of 50 rpm and a temperature of 135° C. for 7 days.

[0047] After the crystallization reaction is completed, the obtained crystallized product is recovered by filtration, washed with deionized water until the pH is 7-8, and finally dried at 90-120°C. According to powder X-ray powder diffraction (XRD) analysis, the obtained crystallized sample is AEI type zeolit...

Embodiment 2

[0050] Weigh 3579.5g of deionized water, 377.3g of 30wt% sodium hydroxide aqueous solution and 697.8g of 30.2wt% N,N-diethyl-2,6-dimethylpiperidinium hydroxide aqueous solution, After stirring and mixing for 0.5 hours at 35°C, add 346.0g of fluorine-modified Y-type molecular sieve F-USY-4 (SiO 2 / Al 2 o 3 Molar ratio=30.51), continue stirring and mixing at 25~35° C. for 6 hours.

[0051] SiO in the final sol 2 :Al 2 o 3 :Na 2 O:ROH:H 2 O molar ratio 30.51:1.00:8.20:6.50:1400.00

[0052] The above sol was transferred to a steel autoclave lined with polytetrafluoroethylene, and crystallized at a stirring speed of 300 rpm and a temperature of 135° C. for 7 days.

[0053] After the crystallization reaction is completed, the obtained crystallized product is recovered by filtration, washed with deionized water until the pH is 7-8, and finally dried at 90-120°C. According to XRD test, the obtained crystallized sample is AEI type zeolite; figure 1 Scanning electron micrograp...

Embodiment 3

[0056] Weigh 2824.9g of deionized water, 361.3g of 30wt% sodium hydroxide aqueous solution, 287.2g of 31.5wt% N,N-dimethyl-3,5-dimethylpiperidinium hydroxide aqueous solution, 30.2wt% 352.4g of N,N-diethyl-2,6-dimethylpiperidinium hydroxide aqueous solution and 1111.2g of 29.5wt% silica sol were stirred and mixed at 25-35°C for 6 hours, and then 63.0g of Fluorine-modified Y-type molecular sieve F-HY(SiO 2 / Al 2 o 3 Molar ratio=5.19), continue stirring and mixing at 25~35° C. for 6 hours.

[0057] SiO in the final sol 2 :Al 2 o 3 :Na 2 O:ROH:H 2 O molar ratio 46.00:1.00:10.20:8.50:1800.00, where N,N-dimethyl-3,5-dimethylpiperidinium hydroxide and N,N-diethyl-2,6-di The molar ratio of methylpiperidinium hydroxide is 1:1.

[0058] The above sol was transferred to a steel autoclave lined with polytetrafluoroethylene, and crystallized at a stirring speed of 300 rpm and a temperature of 145° C. for 4 days.

[0059]After the crystallization reaction is completed, the obtain...

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Abstract

The invention discloses a method for preparing an SSZ-39 molecular sieve by taking a fluorine-modified Y-type molecular sieve as a raw material. The method comprises the following steps: dipping a Y-type molecular sieve in a fluorine-containing aqueous solution, and drying and roasting the Y-type molecular sieve to obtain a fluorine-doped Y-type molecular sieve; mixing and stirring deionized water, an alkali source, a template agent and a silicon source well in proportion, and adding the fluorine-doped Y-type molecular sieve to prepare sol; and transferring the sol into a crystallization kettle, filtering, washing and drying the crystallization product after complete crystallization, carrying out ion exchange, and carrying out roasting to obtain a hydrogen type SSZ-39 molecular sieve. According to the invention, the Y-type molecular sieve raw material is modified by a fluorine doping method, so that the SSZ-39 molecular sieve can be prepared by complete crystal transformation in a short time under the condition of relatively low silica-alumina ratio, and the raw material and production costs can be obviously reduced. The SSZ-39 molecular sieve prepared by the method has the characteristics of short crystallization time, high crystallinity, controllable grain size, good grain dispersity and the like, and can be applied to the fields of methanol-to-olefin reaction, carriers of selective catalytic reduction catalysts and the like.

Description

technical field [0001] The invention relates to a method for preparing SSZ-39 molecular sieve by using fluorine-modified Y-type molecular sieve as a raw material, in particular to using fluorine-modified Y-type molecular sieve as all aluminum source and part or all silicon source, and preparing silicon A method for preparing SSZ-39 molecular sieves after crystallization reaction of aluminum sol. The invention also relates to the application of the SSZ-39 molecular sieve as a methanol-to-olefin (MTO) catalyst and a selective catalytic reduction (SCR) catalyst carrier. Background technique [0002] Zones et al. synthesized SSZ-39 aluminosilicate molecular sieve for the first time in 1999. The molar ratio of silicon dioxide and aluminum oxide (silicon-aluminum ratio) is between 10 and 100. The skeleton topology of the molecular sieve is AEI. The basic structural units of double six-membered rings (D6R) are linked by some four-membered rings to form a three-dimensional channel ...

Claims

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Application Information

Patent Timeline
03 Apr 2020
Publication
CN110950354A
IPC
C01B39/24; B01J29/70; C07C1/20; C07C11/02
CPC
B01J29/70; C01B39/24; C01P2002/72; C01P2004/03; C07C1/20; C07C11/02
Inventors
王于; 于浩淼