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Nano-grade Y type zeolite synthesized from kaolin and its preparation metod

A kaolin, nano-scale technology, applied in the field of nano-scale Y-type zeolite and its preparation, can solve the problems of agglomeration, difficulty in filtration, poor hydrothermal stability, etc., and achieve the effects of good dispersion, energy saving, and dosage reduction

Inactive Publication Date: 2004-10-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the smaller the zeolite crystal grains, the worse its hydrothermal stability. In addition, the smaller the crystal grains, the greater the surface energy, and the easier it is to aggregate into agglomerates, making filtration more difficult.
Therefore, the insufficiency of the gel method to synthesize small particles NaY has become the biggest obstacle to its industrial application.

Method used

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  • Nano-grade Y type zeolite synthesized from kaolin and its preparation metod
  • Nano-grade Y type zeolite synthesized from kaolin and its preparation metod
  • Nano-grade Y type zeolite synthesized from kaolin and its preparation metod

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Experimental program
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preparation example Construction

[0024] The preparation method of zeolite provided by the invention comprises the following steps:

[0025] (1) Convert kaolin to metakaolin by roasting and dehydrating at 500-690°C, pulverize it, and then make it into a powder with a particle size of less than 230 microns,

[0026] (2) Add sodium silicate, directing agent, sodium hydroxide solution and water to metakaolin powder to make a ratio of (1-2.5) Na 2 O:Al 2 o 3 :(4~9)SiO 2 :(40~100)H 2 The reaction raw material of O, wherein the weight ratio of directing agent and metakaolin is 0.1~1.0,

[0027] (3) crystallize the reaction raw material obtained in step (2) under stirring at 88-98° C., then filter and dry.

[0028] In the method, raw kaolin powder is roasted at a relatively low temperature to obtain metakaolin, and the kaolin used is selected from hard kaolin, soft kaolin or coal gangue, and its average particle size is less than 4 microns, so it is raw soil without molding treatment. The calcination temperatur...

example 1

[0043] The nanoscale Y-type zeolite of the present invention is prepared.

[0044] (1) Preparation of directing agent: get 250 grams of sodium silicate solution (containing 20.05% by weight of SiO 2 , 6.41 wt% Na 2 (0), slowly add 120 grams of sodium metaaluminate solution (containing 3.15% by weight of Al) under rapid stirring at 30°C 2 o 3 , 21.1 wt% Na 2 O), stirred for 1 hour, and aged at 20°C for 48 hours to obtain a directing agent. The composition of the directing agent is 16Na 2 O:Al 2 o 3 : 15SiO 2 : 320H 2 O.

[0045] (2) Preparation of zeolite

[0046] Kaolin with an average particle size of 4 μm (Suzhou, Yangshan brand, China Kaolin Company, crystal content is 80% by weight), roasted at 660 ° C for 3 hours to obtain metakaolin powder, pulverized to make metakaolin powder with a particle size of less than 230 μm .

[0047] Get 500 grams of pulverized metakaolin powder, add 2000 grams of sodium silicate solution (containing 20.05% by weight of SiO 2 , 6....

example 2

[0049] Zeolite Y-2 was prepared according to the method of Example 1, except that the raw material kaolin was roasted at 680° C. for 4 hours, and the stirring speed was 600 rpm when the reaction raw material was crystallized. X-ray diffraction measurement of NaY content in Y-2 is 52.4% by weight, its physical and chemical properties are shown in Table 1, and the X-ray diffraction spectrum is shown in figure 1 , field emission scanning electron microscope (SEM) photos of different magnifications are shown in Figure 2-5 .

[0050] From figure 1 As can be seen from the X-diffraction spectrum of the present invention, the zeolite of the present invention has a characteristic peak of NaY, and the content of NaY can be deduced from the height of the characteristic peak.

[0051] 5000x magnification SEM from Y-2 figure 2 As can be clearly seen in , the zeolites of the present invention consist of nested spheres with a diameter of less than 3000 nm. SEM with 20000x magnification...

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Abstract

A nano-class Y zeolite prepared from raw kaolinite powder through crystallizing has 30-85 wt.% for NaY content. Its primary particles can be rod-shaped, flaky or block crystal. Its secondary particle is the nest-type sphere. It can be made into HY, REY, or REHY and used as the catalyst for catalytic cracking.

Description

technical field [0001] The invention relates to a Y-type zeolite synthesized by kaolin crystallization and a preparation method thereof, specifically, a nano-scale Y-type zeolite prepared by in-situ crystallization of kaolin raw powder and a preparation method thereof. Background technique [0002] Since USP3,119,659 announced the use of kaolin as raw material to synthesize zeolite in 1964, research in this area has been continuously carried out. Early work is mainly devoted to the synthesis of pure zeolite, as US3,574,538 discloses a method for synthesizing Y-type zeolite with kaolin, kaolin is roasted into amorphous metakaolin, and a certain amount of sodium silicate and hydroxide are added Sodium to make the molar ratio of silica / alumina close to that of the zeolite to be synthesized, then add 0.1 to 10% by weight of a directing agent, crystallize at 60 to 110°C to obtain zeolite Y with high purity, and its silica / alumina The molar ratio of alumina is 4.5-5.95. [0003]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/08C10G11/02
CPCB01J29/084C10G11/02C01B39/24B01J29/08
Inventor 周继红闵恩泽杨海鹰宗保宁
Owner CHINA PETROLEUM & CHEM CORP
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