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Synthetic method of nano aluminum-rich beta-zeolite

A beta zeolite and aluminum-rich technology, which is applied in the synthesis field of aluminum-rich beta zeolite, can solve the problems of long crystallization time, low yield and crystallinity, and achieve less lattice defects, low water content and good thermal stability. Effect

Active Publication Date: 2011-05-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method uses ethyl silicate and metal aluminum powder as raw materials, and tetraethylammonium hydroxide is used as a template, the gel silica-alumina ratio is at least 12, and the prepared beta zeolite has a silica-alumina ratio of at least 14.4, but the method’s The crystallization time is as long as 62 days, and the yield and crystallinity are very low

Method used

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  • Synthetic method of nano aluminum-rich beta-zeolite
  • Synthetic method of nano aluminum-rich beta-zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Mix 3.0g pseudo-boehmite (31.8% by weight on ignition) with 20.0g water to make a slurry and disperse evenly, then add HCl dropwise to carry out acidification to form a sol, wherein HCl:Al 2 o 3 =0.25 (molar ratio), add 80~120 order 6.8g fine-pore chromatographic silica gels (burning minus 10.0% by weight) wherein, and ultrasonic dispersion is uniformly mixed, wherein: SiO 2 / Al 2 o 3 The molar ratio is 5; after drying at 120°C, it is crushed into 40-200 mesh silica-alumina colloidal particles.

[0038] (2) Add template agent TEAF to the silica-alumina colloid particles obtained in step (1) to mix and crystallize, and the silica-alumina colloid particles (using SiO 2 meter), template agent tetraethylammonium fluoride TEAF and water according to SiO 2 :TEAF:Water=1:0.05:2.0 molar ratio, mix evenly, then place in a rotary oven, dynamically crystallize at 80°C for 48 hours, then dynamically crystallize at 140°C for 48 hours, then take out Sample 2 was obtained by ...

Embodiment 2

[0041] (1) Mix 3.1g of alumina trihydrate and 63g of water to make a slurry and disperse evenly, acidify with acetic acid to form a sol, in which acetic acid and Al 2 o 3 The mol ratio is 0.35, then add 80~120 orders 10.3g of white carbon black particles (fire reduction 6.8% by weight) wherein, and ultrasonic dispersion is uniformly mixed, wherein: SiO 2 / Al 2 o 3 The molar ratio is 8; then, after drying at 120°C, it is crushed into 40-200 mesh silica-alumina colloidal particles.

[0042] (2) Add templating agent, TEAOH, HF, and water to the silica-alumina colloid particles obtained in step (1) and mix and crystallize evenly, wherein the molar ratio of each raw material is as follows: TEA + / SiO 2 =0.08, F - / TEA + = 1.5, H 2 O / SiO 2 =4.5, then placed in a rotary oven, dynamically crystallized under the condition of 100°C for 24 hours, then dynamically crystallized under the condition of 170°C for 48 hours, then took out suction filtration, washed, dried, and roasted t...

Embodiment 3

[0045] (1) According to ethyl silicate (as SiO 2 Total): ammonium fluoride: water = 1.0:0.015:4.0 molar ratio, add ammonium fluoride and ethyl silicate successively into water and mix thoroughly, at pH 6-8, temperature 25-40°C , aged for 24 hours to obtain silica gel, dried the obtained silica gel at 120°C for 48 hours, and ground into silica gel particles of 40-200 mesh.

[0046] Mix 6.1g of aluminum hydroxide with 45.1g of water, beating and dispersing evenly, acidify with formic acid to form aluminum sol, wherein formic acid and Al 2 o 3 The molar ratio is 0.55. 13.9g of silica gel particles (13.8% by weight) were added into the aluminum sol and ultrasonically dispersed and uniformly mixed, wherein: SiO 2 / Al 2 o 3 The molar ratio is 10; then, after drying at a temperature of 120°C, it is crushed into 40-200 mesh silica-alumina colloidal particles.

[0047] (2) the silica-alumina colloid particles obtained in step (1) are mixed with TEABr, NH 4 F, mixed with water, t...

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Abstract

A method for synthesizing nano aluminum-rich beta-zeolite comprises the steps as follows: (1) an alumino silica gel which is formed by mixing an aluminum source and acid is evenly mixed with aluminum source particles, dried and crushed into alumino silica gel particles, wherein, the mol ratio of the aluminum source to the silicon source is 0.05-0.2; and (2) a template agent is added to the alumino silica gel particles obtained in the step (1) and evenly mixed to produce a reaction mixture which is crystallized at the temperature of 80-190 DEG C for 1-6 days, therefore a product is obtained through recovery. The mol ratios of the feeding ingredients of the reaction mixture are as follows: the mol ratio of the template agent to the silicon source equals 0.1-1.0, and that of water to the silicon source equals 2-12. The template agent is a mixture of a tetraethylammonium compound and a fluoride, or tetraethylammonium fluoride dihydrate. The method provided by the invention is characterized by high yield of a single kettle and low moisture of the synthesis system. The beta-zeolite synthesized by the method provided by the invention has high relative crystallinity, few lattice defects and good thermal stability, and the ratio between the silicon and aluminum of the synthesized beta-zeolite is 5-20, which is up to the nano crystal grain dimension.

Description

technical field [0001] The invention relates to a synthesis method of beta zeolite, in particular to a synthesis method of aluminum-rich beta zeolite with nanoscale grains. Background technique [0002] Beta zeolite was first synthesized by the classic hydrothermal crystallization method in 1967 by Mobil Corporation of the United States. The zeolite has a unique three-dimensional (or two-dimensional) pore structure, has high catalytic activity for hydrocracking and hydroisomerization, and can be used for hydrocracking and hydroisomerization after modification or loading of certain metal components. Petroleum refining and petrochemical processes such as hydrofining, hydrodewaxing, and diesel decondensation. [0003] At present, beta zeolite is industrially used to catalyze alkylation reactions, for example: catalyze the reaction of benzene and ethylene to produce ethylbenzene, and catalyze the reaction of benzene and propylene to produce cumene. The silicon-alumina ratio of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 王志光宋家庆宋守强曾光乐何鸣元
Owner CHINA PETROLEUM & CHEM CORP
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