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Beta molecular sieve synthesizing method

A molecular sieve and seed crystal technology, applied in the direction of crystalline aluminosilicate zeolite, can solve the problems of difficult industrialized production, uneven stirring, etc., and achieve the effects of reducing production costs, simple and easy operation, and reducing crystallization reaction time.

Active Publication Date: 2015-07-22
SHANGHAI NOVEL CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has problems such as uneven stirring during the operation of the large kettle, which is difficult for industrialized production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Treat Beta molecular sieve seed crystals with ammonium fluoride: prepare 20ml of 10wt% ammonium fluoride solution, add 5g Beta molecular sieve seed crystals, heat and stir in a water bath at 70°C for 4 hours to obtain suspension A.

[0040] (2) Take 12g TEAOH solution (industrial grade, TEAOH≥25wt%) and 1.5g NaAlO 2 Solid (chemically pure, Al 2 o 3 , 49wt%) stirring the preparation solution, adding 50g silica sol (industrial grade, SiO 2 ≥30wt%), mixed uniformly to form silica-alumina gel, wherein the molar ratio of each material is: SiO 2 / Al 2 o 3 = 35, TEA + / SiO 2 =0.08,H 2 O / SiO 2 =10. Add 3 g of the well-stirred suspension A to the silica-alumina gel, suspension A / silicon-alumina gel=4.7wt%. After continuing to stir for 30 minutes, put it into a stainless steel reaction kettle, seal it at 150°C and crystallize for 18 hours to obtain a milky white suspension B.

[0041] (3) Suspension B was filtered and washed, dried at 110°C for 6 hours, and calcine...

Embodiment 2

[0044] Repeat Example 1, change the concentration of Beta molecular sieve seed crystal seed pretreatment liquid ammonium fluoride in step (1), change to 5wt%, 14wt%, 18wt% respectively, other conditions are constant; The product crystalline phase that obtains is Beta Molecular sieves have relative crystallinity of 72.1%, 82.4%, and 80.5%, respectively.

Embodiment 3

[0046] Repeat Example 1, change the temperature and time of Beta molecular sieve seed crystal seed pretreatment liquid ammonium fluoride in step (1), respectively change to 60 ℃, 5 hours; 80 ℃, 3 hours; 90 ℃, 1 hour, other conditions The crystal phases of the obtained products are all Beta molecular sieves, and their relative crystallinities are 79.5%, 81.8%, and 84.2%, respectively.

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Abstract

The invention relates to a Beta molecular sieve synthesizing method. The Beta molecular sieve synthesizing method comprises the following steps: (1) firstly pretreating a Beta molecular sieve seed crystal by using pretreatment liquid so as to obtain turbid liquid A; (2) preparing uniform gel by using a silicon source, an aluminium source, a template agent and water, adding the turbid liquid A, uniformly mixing, transferring into a stainless steel reaction kettle, and carrying out hydro-thermal treatment under an airtight condition so as to obtain turbid liquid B; (3) separating out white solid matters in the turbid liquid B, drying and roasting to obtain a Beta molecular sieve. The Beta molecular sieve synthesizing method is characterized in that the Beta molecular sieve is pretreated and is used as the seed crystal, so that a relatively good structural guiding role can be achieved, meanwhile, an active material in the pretreatment liquid can serve as a mineralizing agent and can promote the crystal growth, and the Beta molecular sieve with wide silica-alumina ratio range and good degree of crystallinity is obtained.

Description

technical field [0001] The invention relates to a method for synthesizing crystalline aluminosilicate molecular sieves, in particular to a method for synthesizing Beta molecular sieves through seed crystal modification. Background technique [0002] Beta molecular sieves were synthesized for the first time in 1967 by Mobil Corporation of the United States using the classic hydrothermal crystallization method (USP3,308,069). The molecular sieve has a three-dimensional twelve-membered ring channel structure. Due to its unique topology and good thermal and hydrothermal stability, it can be used in alkylation, hydrocracking, hydroisomerization, hydrofinishing, hydrocarbon cracking, etc. It shows excellent catalytic performance and is an important catalytic material. [0003] The high cost of synthesis restricts the application of Beta molecular sieves in industry. For many years, the low-cost synthesis of Beta molecular sieves with a controllable silicon-aluminum ratio has bee...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 兰春锋夏建超夏娟文怀有谈赟
Owner SHANGHAI NOVEL CHEM TECH
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