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Alkali-free metal system synthesis method of ZSM-5 molecular sieve containing phosphorus in crystal

A technology of ZSM-5 and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of high price and achieve the effect of reducing synthesis cost

Active Publication Date: 2017-01-04
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Nichiappan lingappan et al. (Bull.Chem.Soc.Jpn, 1996,69,1125-1128) used quaternary phosphorus salts as templates, and roasted them after synthesis to obtain phosphorus-containing ZSM-5 molecular sieves, wherein the phosphorus content was between 0.4 and 0.6wt% range, but the quaternary phosphorus salt is usually prepared by the reaction of trisubstituted phosphorus and hydrohalic acid, and the price is high
CN101468808A discloses a method for directly preparing phosphorus-containing ZSM-5 molecular sieves from a mixed system of silicon source, aluminum source, organic amine template agent, and acidic phosphorus source, and explores the use of phosphorus-containing molecular sieves in the cracking of linear alkane tetradecane reaction behavior, but the preparation method described in the patent still uses a large amount of organic amine templates, and introduces basic metal

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  • Alkali-free metal system synthesis method of ZSM-5 molecular sieve containing phosphorus in crystal
  • Alkali-free metal system synthesis method of ZSM-5 molecular sieve containing phosphorus in crystal
  • Alkali-free metal system synthesis method of ZSM-5 molecular sieve containing phosphorus in crystal

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preparation example Construction

[0024] The synthetic method of the phosphorus-containing ZSM-5 molecular sieve provided by the invention comprises the following steps:

[0025] (1) Tetramethylammonium hydroxide is mixed with the aluminum source, and the Al in the tetramethylammonium hydroxide and the aluminum source in the mixture 2 o 3 The molar ratio is 0.2 to 40:1, and the mixture is treated in a closed reactor at 50 to 300°C for 0.1 to 5 hours to obtain an intermediate product, which is an alkali metal-free aluminum source;

[0026] (2) Mix the intermediate product obtained in step (1) with organophosphorus template, silicon source, and deionized water, and the molar ratio in the mixture is: SiO 2 :Al 2 o 3 =40~1000, organophosphorus template: SiO 2 =0.01~10,H 2 O: SiO 2 =2~20, the organophosphorus template is selected from tetrabutylphosphine bromide, triphenylethylphosphorus bromide, triphenylbutylphosphorus bromide, triphenylbenzylphosphorus bromide, hexamethyl One or more of diphenylphosphoric...

Embodiment 1

[0051] Take by weighing 0.65g pseudo-boehmite (Changling Catalyst Factory, Al 2 o 3 content is 70%), it is mixed with 16.0g tetramethylammonium hydroxide aqueous solution (Shanghai Yongsheng Reagent Factory, analytically pure, TMAOH content 10%), mixture molar ratio TMAOH / Al 2 o 3 =3.6, place it in a crystallization kettle containing a polytetrafluoroethylene liner, react with 150°C for 2 hours and cool to room temperature, after that, mix it with 20g silica gel (Qingdao Ocean Chemical Co., Ltd., SiO 2 content 99.1%), 10.2g tetrabutylphosphine hydroxide (Sinopharm Chemical Reagent Co., Ltd., analytically pure, TBPOH content 40%) and 15.1g water mix homogeneously, the mixture molar ratio SiO 2 / Al 2 o 3 =60, TBPOH / SiO 2 =0.05,H 2 O / SiO 2 =7.0. The mixture was hydrothermally crystallized at 150°C for 48 hours in a high-pressure reactor, dried at 110°C for 20 hours after centrifugal filtration, and calcined at 550°C for 3 hours to obtain molecular sieve sample ZP-1.

[0...

Embodiment 2

[0057] Take by weighing 0.37g pseudo-boehmite (Changling Catalyst Factory, Al 2 o3 content is 70%), it is mixed with 22.0g tetramethylammonium hydroxide aqueous solution (Shanghai Yongsheng Reagent Factory, analytically pure, TMAOH content 10%), mixture molar ratio TMAOH / Al 2 o 3 =8.0, place it in a crystallization kettle containing a polytetrafluoroethylene lining, react with 140°C for 2 hours and then cool to room temperature. After that, mix it with 20g silica gel (Qingdao Ocean Chemical Co., Ltd., SiO 2 content 99.1%), 10.0g tetrabutylphosphine hydroxide (Sinopharm Chemical Reagent Co., Ltd., analytically pure, TBPOH content 40%) and 15.6g water mix homogeneously, the mixture molar ratio SiO 2 / Al 2 o 3 =100, TBPOH / SiO 2 =0.05,H 2 O / SiO 2 =7.0. The mixture was hydrothermally crystallized at 150°C for 48h in an autoclave. The phosphorus-containing ZSM-5 molecular sieve synthesized after crystallization was centrifugally filtered, dried at 110°C for 20 hours, and cal...

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Abstract

The invention relates to an alkali-free metal system synthesis method of a ZSM-5 molecular sieve containing phosphorus in the crystal. The alkali-free metal system synthesis method comprises: mixing tetramethylammonium hydroxide and an aluminum source, treating the mixture in a closed reaction kettle to obtain an intermediate product, uniformly mixing the intermediate product, an organic phosphor template agent, a silicon source and deionized water, and carrying out hydrothermal crystallization. According to the present invention, the low-cost silicon source, the low-cost aluminum source and the low-cost organic template agent are used, the preparation steps are simple, the operation is easy, and the high crystallinity ZSM-5 molecular sieve containing the phosphorus in the crystal and having two different sizes of the grains is obtained.

Description

technical field [0001] The present invention relates to a method for synthesizing phosphorus-containing ZSM-5 molecular sieves, more specifically to a method for synthesizing intracrystalline phosphorus-containing ZSM-5 molecular sieves with two different grain sizes in an alkali-free metal system method. Background technique [0002] ZSM-5 molecular sieve is a medium-pore molecular sieve with high silicon three-dimensional straight channel with MFI structure. It has a unique pore structure, good shape-selective catalysis and isomerization performance, high thermal stability, high specific surface The range of silicon-aluminum ratio, unique surface acidity and low carbon formation are widely used as catalysts and catalyst supports, and are successfully used in alkylation, isomerization, disproportionation, catalytic cracking, methanol to gasoline, methanol Olefins and other production processes. [0003] The synthesis system of ZSM-5 molecular sieves usually uses inorganic...

Claims

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Application Information

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IPC IPC(8): C01B39/40
Inventor 张欣王萍王殿中罗一斌欧阳颖徐广通舒兴田
Owner CHINA PETROLEUM & CHEM CORP