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Preparation method of high silicon aluminium ratio small crystal NaY molecular sieve

A technology with high silicon-aluminum ratio and small crystal grains, which is applied in the direction of crystalline aluminosilicate zeolite and octahedral crystalline aluminosilicate zeolite, etc., can solve the problems of difficult removal of cesium ions and low utilization rate of silicon, and achieve good structural stability Good performance and catalytic activity, cheap raw materials, easy to obtain the effect of simple and easy process

Active Publication Date: 2006-06-14
PETROCHINA CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the cesium ions in the product of this method are not easy to remove, and multiple exchanges and roasting are required [as described in USP4714601], and the seed crystal must be prepared by a specific method
In addition, the silicon-aluminum ratio of raw materials is required to be as high as 65-135 when feeding, but the utilization rate of silicon is low, and a large amount of high-concentration silicon waste liquid is discharged

Method used

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  • Preparation method of high silicon aluminium ratio small crystal NaY molecular sieve
  • Preparation method of high silicon aluminium ratio small crystal NaY molecular sieve
  • Preparation method of high silicon aluminium ratio small crystal NaY molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0053] Get 10.53g of sodium hydroxide solid (produced by Beijing Chemical Plant, with a purity of 99%) and dissolve it in 30.95g of water. After cooling to room temperature, add 2.22g of sodium metaaluminate (produced by Tianjin Jinke Fine Chemical Research Institute, Al 2 o 3 Content is 45wt%, Na 2 O content is 41wt%) to make high alkali sodium metaaluminate solution. Then add 36.73g water glass (produced by Beijing Red Star Soda Soda Factory, SiO 2 The content is 28.83wt%, Na 2 The O content is 8.84wt%), mixed evenly, and aged at 40° C. for 4 hours to prepare the directing agent.

[0054] Put 14.21g of water in a beaker, control the temperature of the liquid in the beaker to 60°C, and add 12.79g of 50wt% Al at the same time under rapid stirring 2 (SO 4 ) 3 (Nanzhao Huaxin Chemical Co., Ltd. produces, and purity is 99%) solution and 31.91g water glass. After stirring evenly, add 1.90g of the above-mentioned directing agent, the pH value of the gel is 12.5, after stirri...

Embodiment 2

[0061] The source of each raw material and the preparation of the directing agent are the same as in Example 1.

[0062] Keep the beaker containing 13.47g of water at a constant temperature of 50°C, and add 12.66g of 50wt% Al at the same time under rapid stirring 2 (SO 4 ) 3 Solution and 31.55g of water glass were stirred evenly, and then 4.40g of the above-mentioned directing agent was added, and the pH value of the gel was 12.8. The material in the beaker was kept at 50°C throughout the above process. After stirring evenly, put it into a stainless steel reaction kettle, shake and crystallize at 60°C for 4 hours, then raise the temperature to 100°C for static crystallization for 36 hours, then filter, wash, and dry to obtain NaY molecular sieve products.

[0063] According to XRD, the silicon-aluminum ratio of NaY molecular sieve products is 6.2, the relative crystallinity is 98%, the average grain size is 488 nanometers, and the BET specific surface area is 750m 2 / g.

Embodiment 3

[0065] Each raw material source is with embodiment 1.

[0066] Except that the preparation of the directing agent is prepared by stirring and aging at 15° C. for 24 hours, the others are the same as in Example 2. According to XRD, the silicon-aluminum ratio of NaY molecular sieve products is 6.3, the relative crystallinity is 90%, the average grain size is 510 nanometers, and the BET specific surface area is 740m 2 / g.

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Abstract

The present invention provides a high silica-alumina ratio small grain size NaY molecular sieve and its preparation method. It is made up by adopting non-template agent direct synthesis process, and its preparation method includes the following steps: firstly, stirring and ageing for 0.5-48 hr at 15-60deg.C to obtain crystallization guide agent, then making said guide agent, water silicon source and aluminum silicon into reaction mixture, then crystallizing said mixture at twice, first step is dynamic crystallization, temperature is controlled at 20-80deg.C and crystallization time is 0.5-24 hr, second step is static crystallization, temperature is controlled at 90-140deg.C and the crystallization time is 5-100 hr, finally, filtering, washing and drying so as to obtain the invented product whose relative crystallinity is greater than 80%.

Description

technical field [0001] The present invention relates to a method for preparing NaY molecular sieve with high silicon-aluminum ratio and small crystal grain, to be precise, it relates to a method for directly synthesizing NaY molecular sieve with high silicon-aluminum ratio and small crystal grain without adding any template agent or additive in the reaction mixture . Background technique [0002] Y-type molecular sieves are widely used in catalytic cracking, hydrocracking, isomerization and other oil refining processes as catalyst active components or catalyst supports. Y-type molecular sieves synthesized by conventional methods generally have a grain size of about 1000 nm. The Y-type molecular sieve with a small grain size has a larger external area and a higher intracrystalline diffusion rate, which is better than the conventional grain size in terms of improving the ability to convert macromolecules, reducing secondary cracking of products, and reducing coking of catalys...

Claims

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Application Information

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IPC IPC(8): C01B39/02C01B39/24
Inventor 申宝剑高雄厚曾鹏晖王宝杰王玉超刘宏海庞新梅秦松郭金涛郭巧霞郑俊鹤龚朝兵张莉何金龙段长艳赵连鸿
Owner PETROCHINA CO LTD
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