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Process for preparing compound catalytic material of nanometer molecular sieve/silicon aluminum oxides

A technology of composite catalytic materials and nano-molecular sieves, which is applied in the direction of molecular sieve catalysts, physical/chemical process catalysts, and nano-structure manufacturing. It can solve the problems of nano-molecular sieve structure damage, large nano-molecular sieve particles, and long preparation time. Effects of improving catalytic performance and simplifying operation

Inactive Publication Date: 2009-10-28
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the preparation time is longer
[0008] The methods for synthesizing nano-molecular sieves in the above-mentioned documents or patents are either complicated in process and take a long time, or the particles of the synthesized nano-molecular sieves are large and exceed the nanometer range; in the preparation of the catalytic material containing nano-molecular sieves described in CN02100379.3, due to the inclusion of acidic In the process of silica sol or acid aluminum sol, the structure of nano molecular sieve will be destroyed to a certain extent

Method used

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  • Process for preparing compound catalytic material of nanometer molecular sieve/silicon aluminum oxides

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Preparation method of nanometer Y-type molecular sieve / amorphous silicon-aluminum composite material.

[0027] Nano Y-type molecular sieves were prepared by directing agent method.

[0028] Directing agent preparation: use water glass as the silicon source and sodium metaaluminate as the aluminum source. Mix 150ml of water glass (modulus 3.0) with 200ml of water to obtain solution A; add 9.5g of sodium metaaluminate and 40g of sodium hydroxide to 200ml of water until completely dissolved to obtain solution B; Stir at ~20°C for 1 hour to prepare the molar ratio: 9Na 2 O:Al 2 o 3 : 8SiO 2 : 100H 2 A directing agent for O, aged for 6-48 hours for later use.

[0029] Preparation of nano Y-type molecular sieve: Dissolve 32g of sodium metaaluminate and 5g of sodium hydroxide in 400ml of water to obtain solution C; mix 300ml of water glass with 300ml, then add 50ml of Tween-20 to obtain solution D. Pour solution D into solution C to obtain sol E, and stir E a...

Embodiment 2

[0033] The preparation of the directing agent is the same as in Example 1.

[0034] The preparation of the nanometer Y-type molecular sieve is the same as in Example 1, except that the power of the microwave treatment is 600 W and the treatment time is 15 minutes to obtain the nanometer Y-type molecular sieve.

[0035] Transfer the Y-type molecular sieve containing mother liquor obtained above to a 500ml plastic beaker, add 144g sodium metaaluminate, and at 50°C, adjust the pH value of the system to 8.0 with hydrochloric acid to form a gel, then filter, wash, Dry at 120° C. for 12 hours, and calcined at 500° C. for 4 hours to obtain a Y / ASA composite catalytic material, wherein the content of Y molecular sieve is 30 wt %. According to the XRD test, the SiO of Y molecular sieve 2 / Al 2 o 3 The ratio is 4.85, the unit cell constant a 0 It is 2.4735, the relative crystallinity is 36.8%, and the silicon-aluminum molar ratio of silicon-aluminum oxide is 1.1:1.

[0036] After A...

Embodiment 3

[0038] The preparation of the directing agent is the same as in Example 1.

[0039] The preparation of the nanometer Y-type molecular sieve is the same as in Example 1, except that the power of microwave treatment is 400W and the treatment time is 25 minutes to obtain the nanometer Y-type molecular sieve.

[0040] Transfer the Y-type molecular sieve containing mother liquor obtained above to a 500ml plastic beaker, add 72g of sodium metaaluminate, and at 50°C, adjust the pH of the system to 8.5 with sulfuric acid to form a gel. Then filter, wash, Dry at 120° C. for 12 hours, and calcined at 500° C. for 4 hours to obtain a Y / ASA composite catalytic material, wherein the content of Y molecular sieve is 15 wt%. According to the XRD test, the SiO of Y molecular sieve 2 / Al 2 o 3 The ratio is 4.85, the unit cell constant a 0 It is 2.4735, the relative crystallinity is 28.2%, and the silicon-aluminum molar ratio of silicon-aluminum oxide is 2.1:1.

[0041] After Ar ion etching ...

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Abstract

The invention provides a method for preparing a nano-molecular sieve / silicon-aluminum oxide composite catalytic material, which is characterized in that the method comprises: firstly using a guiding agent method to synthesize a nano-molecular sieve, and the precipitation step in the synthesis is treated by microwave and / or ultrasonic waves , then add the aqueous solution of the mixture of water glass and aluminum source to the slurry containing nano-molecular sieve, add acid to adjust the pH to 7-9.5 to form a gel; then dry and roast the gel to obtain the composite catalytic material, wherein the aluminum source Selected from sodium metaaluminate or aluminum sulfate, this method keeps the particle size of the product molecular sieve below 100nm and the nano molecular sieve in it is not easy to aggregate, without going through the acidic sol process to avoid the molecular sieve being damaged by acid. The composite material is suitable for the catalysis of heavy oil macromolecules Cracking and hydrocracking reactions.

Description

technical field [0001] The invention provides a preparation method of a composite catalytic material containing nanometer molecular sieve, in particular, it relates to a preparation method of nanometer molecular sieve / silicon aluminum oxide composite catalytic material. Background technique [0002] Nano-molecular sieves refer to molecular sieves with particle sizes ranging from 1 to 100 nm. The ratio of the number of atoms on the surface to the total number of atoms in the bulk increases sharply as the particle size decreases, making nano-molecular sieves a new material with unique catalytic properties. . The characteristics of nano-molecular sieves are as follows: 1) It has a larger outer surface area, which exposes more active centers, effectively eliminates the diffusion effect, and fully exerts the catalyst efficiency; 2) Has more pores exposed to the outside , It is not easy to be blocked by reaction deposits, which is beneficial to prolong the reaction operation peri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/06B82B3/00
Inventor 刘百军汪梅卢义鹏
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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