Method for synthesis of beta-zeolite

A synthesis method, the technology of zeolite beta, which is applied in the field of synthesis of zeolite beta, can solve the problems such as difficulty in obtaining nano-silicon-alumina ratio of zeolite beta, and achieve good selectivity and cracking activity, high acid strength, and high hydrothermal stability.

Active Publication Date: 2011-08-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The existing method for preparing nano-beta zeolite is difficult to obtain nano-beta zeolite with a silicon-aluminum ratio of not less than 300

Method used

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  • Method for synthesis of beta-zeolite
  • Method for synthesis of beta-zeolite

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) Aluminum trihydrate (containing Al 2 o 3 56.5% by weight, produced by Shandong Aluminum Works) mixed with water, hydrochloric acid (analytically pure, concentration 37% by weight), acidified to form a sol, HCl:Al 2 o 3 =0.25 (molar ratio); then add 80-120 mesh coarse-porous silica gel (produced by Qingdao Ocean Chemical Factory), and then use ultrasonic waves to fully mix the silica gel and acidified peptized pseudo-boehmite at room temperature to obtain a silica-alumina gel. where nH in the above mixture 2 O / (nSiO 2 +nAl 2 o 3 )=10.0 (molar ratio), the consumption of silica gel and aluminum oxide trihydrate makes the SiO of the obtained silica-alumina gel 2 / Al 2 o 3 The molar ratio is 350;

[0034] (2) drying the silica-alumina gel obtained in step (1) at a temperature of 120° C. for 48 hours, and grinding it into 40-200 mesh silica-alumina gel particles;

[0035] (3) the silica-alumina colloid particle (with SiO2) gained in step (2) 2 meter), template ...

Embodiment 2

[0037] (1) Pseudoboehmite (containing Al 2 o 3 68.21% by weight, produced by Shandong Aluminum Works) mixed with water, acidified with acetic acid (Beijing Chemical Reagent Company, analytically pure), to form a sol, acetic acid and Al 2 o 3 The molar ratio of the silica gel to pseudo-boehmite is 0.35; then add 80-120 mesh fine-pore silica gel (produced by Qingdao Ocean Chemical Factory), the molar ratio of silica gel to pseudo-boehmite (based on SiO 2 / Al 2 o 3 ) is 650, and then use ultrasonic dispersion to fully mix silica gel and acidified peptized pseudo-boehmite at room temperature to obtain silica-alumina gel, wherein nH in the above mixture 2 O / (nSiO 2 +nAl 2 o 3 )=12.0 (molar ratio);

[0038] (2) drying the silica-alumina gel obtained in step (1) at a temperature of 120° C. for 48 hours, and grinding it into 40-200 mesh silica-alumina gel particles;

[0039] (3) the silica-alumina colloidal particle of step (2) gained is used as the raw material of synthesizi...

Embodiment 3

[0041] (1) aluminum hydroxide (containing Al 2 o 3 56.8% by weight, produced by Shandong Aluminum Works) as aluminum source, mix with water, acidify with formic acid (Beijing Chemical Reagent Company, analytically pure, concentration 40.0% by weight), form sol, formic acid: Al 2 o 3 =0.55; Add 120~200 meshes of mesoporous silica gel (produced by Qingdao Ocean Chemical Factory) afterwards, the mol ratio of silica gel and aluminum hydroxide is SiO 2 / Al 2 o 3 It is calculated as 1050, and then dispersed by ultrasonic wave, so that the silica gel and the acidified peptized pseudo-boehmite are fully mixed at room temperature to obtain a silica-alumina gel, wherein the nH in the above mixture 2 O / (nSiO 2 +nAl 2 o 3 )=16.0 (molar ratio).

[0042] (2) Dry the silica-alumina gel obtained in step (1) at 80°C for 24 hours, then dry at 120°C for 24 hours, and then grind it into 40-200 mesh silica-alumina gel particles;

[0043] (3) the silica-alumina colloid particle of step (2)...

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Abstract

The present invention relates to a synthetic method of beta zeolite comprising the steps as follows: an aluminium sources selected from one or a plurality of pseudoboehmite, hydrated alumina, aluminum hydroxide, aluminium chloride hydrate and SB aluminium hydroxide is acidified by acid and mixed with silica gel, the silica gel is fully mixed with the aluminum source by ultrasonic waves, dried, ground, and mixed with a tetraethylammonium ion template agent, fluoride and water, and crystallized at the temperature of 100-190 DEG C for 1-4 days. The mol ratio of TEA<+> and SiO2 in the mixture is 0.05-0.5, the mol ratio of the TEA<+> and F<-> is 1-2, and the mol ratio of H2O and the SiO2 is 2-10. The method can be used for synthesizing nano beta zeolite with the ratio of silicon to aluminium being not less than 300.

Description

technical field [0001] The invention relates to a synthesis method of zeolite beta. Background technique [0002] Beta zeolite is a high-silica zeolite with crossed twelve-membered ring channel system. Its silicon-aluminum ratio can be adjusted from tens to all-silicon. It has good thermal stability, hydrothermal stability, acidity and good Hydrophobic, after its modification, it is not easy to coke and have a long service life when used to catalyze hydrocarbon reactions. , Alkylation and transalkylation reactions have excellent catalytic performance. [0003] In 1967, the Mobil Company of the United States first synthesized zeolite beta by the classic hydrothermal crystallization method (Wadlinger R.L, Kerr G.T, Rosinski E.J., USP3,308,069). The synthetic method announced by US3308069 comprises: will contain Na 2 O, Al 2 o 3 , TEAOH, SiO 2 The mixture with water is made into a slurry, and the crystallization reaction is carried out in an autoclave at 75-200°C for 3-60...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 王志光宋家庆何鸣元
Owner CHINA PETROLEUM & CHEM CORP
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