Composite material containing double-pore structure Y-type zeolite, and preparation method thereof

A composite material and pore structure technology, which is applied in the directions of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the problems of low feed utilization rate, large recovery and processing capacity of mother liquor, and low crystallinity of synthetic products. achieve the effect of avoiding secondary reactions

Active Publication Date: 2010-06-23
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The ratio of the directing agent used in claim 4 of this patent is different from that of conventional directing agents, and the ratio of sodium to aluminum and silicon to aluminum used in claim 5 is relatively high, which will lead to low utilization rate of feeding and large recovery of mother liquor , low crystallinity of the actual synthesized product, etc.

Method used

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  • Composite material containing double-pore structure Y-type zeolite, and preparation method thereof
  • Composite material containing double-pore structure Y-type zeolite, and preparation method thereof
  • Composite material containing double-pore structure Y-type zeolite, and preparation method thereof

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preparation example Construction

[0027] The present invention also provides the preparation method of above-mentioned composite material, comprises the following steps:

[0028] (1) Kaolin is roasted and dehydrated at 500-890° C., and pulverized to obtain metakaolin powder with a particle size of less than 2 μm and no less than 50% of it;

[0029] (2) Add silicon source, 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 mixture of O, wherein the weight ratio of directing agent and metakaolin is 0.1-1.0;

[0030] (3) The reaction raw material mixture is crystallized at 50-98° C. with programmed temperature increase in stages and variable speed, filtering, washing and drying to obtain a Y-type zeolite composite material product with a double-pore structure.

[0031] In the preparation method provided by the present invention, the kaolin mentioned in the step (1) includes halloysite, kaolin, h...

Embodiment 1

[0046] The preparation of directing agent: get 250 grams of sodium silicate solutions (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 26° C. for 24 hours to obtain a directing agent. The composition of the directing agent is 16Na 2 O:Al 2 o 3 : 15 SiO 2 : 320H 2 O (the same below).

[0047] Kaolin with an average particle size of 4 μm (Suzhou, Yangshan brand, China Kaolin Company, crystal content is 80% by weight) was roasted at 800 ° C for 4 hours to obtain metakaolin powder, which was pulverized to make a powder with a particle size of less than 2.0 μm. Less than 50% metakaolin powder.

[0048] Get 500 grams of pulverized metakaolin powder, add 2500 grams of sodium silicate solution (containing 20.05% by weight of SiO 2 , 6.41 wt% Na 2 (2), 200 grams of directing agent, 80 grams ...

Embodiment 2

[0055] Get the metakaolin powder after the crushing of 500 gram embodiment 1, add 2500 gram sodium silicate solution (containing the SiO of 20.05% by weight) under stirring 2 , 6.41 wt% Na 2 (0), 200 grams of directing agent, 120 grams of concentration is 30% by weight of sodium hydroxide solution, 1000 grams of deionized water. Raise the temperature to 75°C and stir for 2 hours at a stirring speed of 1000 rpm, and keep the temperature at 75°C for 8 hours; raise the temperature to 90°C with stirring, and crystallize at a constant temperature for 28 hours at a stirring speed of 200 rpm. After the crystallization was completed, the crystallization tank was cooled, filtered, and washed with water until the pH value of the washing solution was less than 10. Drying at 120° C. for 2 hours gave composite material Y-2.

[0056] Y-2 has figure 2 , 3 The characteristics of X-ray diffraction are determined, wherein the NaY content is 80.4% by weight, the unit cell constant is 2.472nm...

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Abstract

The invention discloses a composite material containing double-pore structure Y-type zeolite, which is characterized in that the composite material contains NaY zeolite and the balance of amorphous matrix; based on the weight of the composite material, the NaY zeolite accounts for 40 to 85 percent; the secondary structure of the composite material is a similar sphere; the similar sphere is formed by staggering and stacking Y-type zeolite generated by crystallization andmetakaolin amorphous intermediates generated during crystal transformation, and has gaps and holes; the sphere also has nest channels inside; the particle size is 3,000 to 25,000 nm; the surface area measured by a BET method is 280 to 800 M<2> / g; the total pore volume is 0.35 to 0.45 ml / g; the pore volume of 1.7 to 300 nm middle / big holes is 0.05 to 0.150 ml / g and accounts for 20 to 35 percent of the total pore volume.

Description

technical field [0001] The present invention is a Y-type zeolite composite material with double-pore structure synthesized in situ by kaolin and its preparation method. Specifically, it is a Y-type zeolite-containing large particle prepared by in-situ crystallization of kaolin raw powder. Composite material with particles having a double-porous structure and a preparation method thereof. Background technique [0002] Since USP 3119659 announced the use of kaolin as raw material to synthesize zeolite in 1964, research in this area has been continuously carried out. Early work was mainly devoted to the synthesis of pure-phase zeolite, such as USP3574538 discloses a method for synthesizing Y-type zeolite with kaolin, kaolin is roasted into amorphous metakaolin, and a certain amount of sodium silicate and sodium hydroxide are added , making the molar ratio of silica / alumina close to that of the zeolite to be synthesized, then adding 0.1-10% by weight of a directing agent, and c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/24
Inventor 周继红闵恩泽舒兴田宗保宁罗一斌
Owner CHINA PETROLEUM & CHEM CORP
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