Preparation method of beta-zeolite

A beta zeolite and a technology for preparation steps, applied in the field of preparation of zeolite molecular sieves, can solve the problems of reducing synthesis cost, complex treatment method, short crystallization time and the like, and achieve the effect of reducing synthesis cost

Inactive Publication Date: 2014-10-01
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As early as 1989, the patent USP4847055 of Mobil Corporation of the United States reported a method for synthesizing zeolite beta with tetraethylammonium bromide as a template, but a special silicon source was involved in this method, and its silicon source The processing method is relatively complicated, which complicates the synthesis process while reducing the synthesis cost
Subsequently, the patent USP5164169 of Mobil Company in 1992 reported a kind of synthetic route with tetraethylammonium hydroxide and tetraethylammonium bromide mixture as template agent again, but introduced chelating agent in this synthetic system, makes synthetic system complication
Chinese patents CN1198404A, CN1249270A and CN1249271A have reported the method for synthesizing zeolite beta with tetraethylammonium halide or / and tetraethylammonium hydroxide as template, in this method part or all replaces quaternary ammonium base with halide, reduces The synthesis cost of β zeolite is excluded, but F is introduced in this series of patents - ions, due to F - The presence of ions makes this method difficult to achieve industrial scale production
Chinese patent CN1377827A has also reported a kind of beta zeolite synthesis route that uses tetraethylammonium bromide as template agent, template agent consumption is few, crystallization time is short and does not need chelating agent in this method, but the synthesis of this method Beta zeolite silicon aluminum ratio (SiO 2 / Al 2 o 3 ) only concentrated in 10~55

Method used

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  • Preparation method of beta-zeolite

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Experimental program
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Effect test

Embodiment 1

[0023] Take 6.75g deionized water, add 1.10g tetraethylammonium bromide (effective content 95%), 0.42g sodium hydroxide (effective content 96%), 0.36g sodium aluminate (Al 2 o 3 Content 45%), stir until the mixed solution is clear, add 3.00g coarse-porous silica gel (SiO 2 content 96%), stirred for 2 hours, aged at 80°C for 12 hours, placed the resulting initial reaction mixture on a multi-layer sieve plate in the reactor, and added 1.00 g of deionized water and 0.50 g of triethylamine at the bottom of the reactor, Crystallize at 140° C. for 24 hours, filter, wash and dry the resulting sample to obtain a zeolite beta sample.

Embodiment 2

[0025] Take 6.75g deionized water, add 1.50g tetraethylammonium bromide (effective content 95%), 0.48g sodium hydroxide (effective content 96%), 0.18g sodium aluminate (Al 2 o 3 Content 45%), stir until the mixed solution is clear, add 3.00g coarse-porous silica gel (SiO 2 content 96%), stirred for 2 hours, aged at 80°C for 12 hours, placed the resulting initial reaction mixture on a multi-layer sieve plate in the reactor, and added 0.85g deionized water and 0.55g triethylamine to the bottom of the reactor, Crystallize at 140° C. for 24 hours, filter, wash and dry the resulting sample to obtain a zeolite beta sample.

Embodiment 3

[0027] Take 9.25g deionized water, add 1.60g tetraethylammonium bromide (effective content 95%), 0.45g sodium hydroxide (effective content 96%), 0.16g sodium aluminate (Al 2 o 3 Content 45%), stir until the mixed solution is clear, add 3.00g of white carbon black (SiO 2 content 98%), stirred for 2 hours, aged at 80°C for 12 hours, placed the resulting initial reaction mixture on a multi-layer sieve plate in the reactor, and added 0.80 g of deionized water and 0.50 g of triethylamine to the bottom of the reactor, Crystallize at 140° C. for 24 hours, filter, wash and dry the resulting sample to obtain a zeolite beta sample.

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Abstract

The invention relates to a preparation method of beta-zeolite. The preparation method comprises the following steps: adding tetraethyl ammonium halide, an aluminum source, and a silicon source into a sodium hydroxide solution, carrying out low-temperature aging for 2 to 16 hours at a temperature of 40 to 100 DEG C, placing the reaction mixture on a multi-layer screening plate in a reactor, adding water and an auxiliary template agent namely low-carbon organic amine into the reactor bottom, heating, carrying out crystallization for 24 to 60 hours at a temperature of 130 to 160 DEG C, filtering, washing, and drying so as to obtain the beta-zeolite. The mole ratios of the materials in the synthesis system are as follows: SiO2/Al2O3=30-300, TEA+/SiO2=0.05-0.30, Na2O/SiO2=0.15-0.80, and H2O/SiO2=7-15. The mole ratios of the materials in the reactor bottom are as follows: H2O/SiO2=0.5-2.0, and R/SiO2=0.08-0.18. The preparation method has the advantages of low synthesis cost and high synthesis efficiency.

Description

technical field [0001] The invention relates to a preparation method of zeolite molecular sieve, specifically, a preparation method of beta zeolite. Background technique [0002] Beta zeolite is a large-porous high-silica zeolite with a three-dimensional twelve-membered ring channel structure. Studies have shown that β zeolite exhibits good catalytic performance in petroleum refining and petrochemical processes such as hydrocracking, isomerization, alkylation, olefin hydration, cracking and dewaxing, and its application prospects are broad. Structurally speaking, the large pore size and unique topological structure of zeolite β ensure good diffusion properties of reactant and product molecules in its crystal structure and good accessibility to active sites; compositionally, β Zeolite's relatively high and adjustable silicon-aluminum ratio in a wide range ensures its good thermal and hydrothermal stability, resulting in the adjustable acidity of zeolite beta, which enables i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 窦涛戴宝琴巩雁军张志华吴志杰孙发民张军亮谢彬秦丽红李海岩吕倩安东俊孙生波王甫村马守涛张庆武王燕李淑杰于秀娟
Owner PETROCHINA CO LTD
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