Method for synthesizing Y type molecular sieve

A synthesis method and molecular sieve technology, which are applied in the directions of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the problems of high molecular sieve cost, high production cost, pipeline blockage, etc., and achieve good thermal stability and Hydrothermal stability, superior catalyst coking, and reduced secondary cracking effects

Active Publication Date: 2013-12-25
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

However, the quaternary ammonium base used in this method is commercially available chemicals, therefore, the cost of preparing molecular sieves by this method is relatively high, and it is difficult to realize industrial production
[0004] At present, many synthetic methods of small-grain NaY molecular sieves have been reported, and they can be summed up mainly as follows: the method introduced by USP3755538 is to add B, V, P in the guide agent , Mo, Ge and other metal elements, the crystal grain size of the synthetic NaY molecular sieve is 200-600nm, but the skeleton silicon aluminum of the product synthesized by this method is relatively low; in EP0435625A2, a Y-type molecular sieve smaller than 100nm was synthesized by the method of improving the system alkalinity, But the silicon-aluminum ratio of the molecular sieve synthesized by this method is also relatively low; the method introduced by CN10033593C is to add sodium silicate solution in the conventional directing agent with light transmittance75% improvement Directing agent solution, the crystal grain size of the synthesized NaY molecular sieve is 100-300nm, but this method is easy to cause pipeline blockage; USP3516786 adopts adding dispersion medium, such as methanol, ethanol, acetone, dimethyl sulfone, N, N-dimethyl Formamide, tetrahydrofuran, etc., the molecular sieves synthesized have a grain size of 10-100nm, but the production cost of this method is high, and it pollutes the environment

Method used

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  • Method for synthesizing Y type molecular sieve
  • Method for synthesizing Y type molecular sieve

Examples

Experimental program
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Embodiment 1

[0025] The preparation method of sodium metaaluminate solution: dissolve sodium hydroxide into deionized water, then add gibbsite evenly, react at 140°C for 5 hours, wait for the solution to cool to room temperature, and use it after filtration. Sodium metaaluminate solutions with different caustic ratios can be prepared according to experimental needs.

[0026] 1) Preparation of crystallization directing agent: 51.57g high alkalinity sodium metaaluminate solution (ρ=1330g / L, equivalent Al 2 o 3 Concentration is 40.2g / L, caustic ratio is 11.6) joins 89.75g water glass (SiO 2 The mass fraction is 19.68%, the modulus is 2.91), after stirring evenly, stir and age at room temperature for 24h, then add 10.91g of low alkalinity sodium metaaluminate solution (ρ=1400g / L, equivalent Al 2 o 3 The concentration is 192g / L, the caustic ratio is 2.5) and 4.54gH 2 O, after stirring evenly, transfer the mixture to a reaction kettle lined with polytetrafluoroethylene and rotate and age at ...

Embodiment 2

[0031] 1) The proportioning, raw materials and preparation method of the crystallization directing agent are the same as in Example 1;

[0032] 2) the proportioning, raw materials and preparation method of silica-alumina gel are the same as in Example 1;

[0033] 3) Add the prepared silica-alumina gel into a stainless steel reaction kettle lined with polytetrafluoroethylene, seal it and rotate it at 80°C at 30r / min for 10h, then at 90°C at 30r / min for 20h , rapidly cooling the reaction kettle, the crystallized product was centrifuged and washed until the pH value of the filtrate was less than 9, and the filtered solid product was dried at 110°C.

[0034] Physical and chemical characterization of the product: determine the relative crystallinity, average particle size and SiO of the product 2 / Al 2 o 3 Listed in Table 1. It can be seen from the XRD spectrum that the synthetic product is NaY molecular sieve.

Embodiment 3

[0036] 1) The proportioning, raw materials and preparation method of the crystallization directing agent are the same as in Example 1;

[0037] 2) According to the molar ratio is 3.3Na 2 O:Al 2 o 3 : 9.8SiO2 2 : 200H 2 O prepares silica-alumina gel, and all the other are identical with embodiment 1;

[0038] 3) Add the prepared silica-alumina gel into a stainless steel reaction kettle lined with polytetrafluoroethylene, seal it, and conduct static crystallization at 80°C for 10 hours, then statically crystallize at 100°C for 22 hours, cool the reaction kettle quickly, and crystallize The product was centrifuged and washed until the pH value of the filtrate was less than 9, and the solid product obtained by filtration was dried at 110°C.

[0039] Physical and chemical characterization of the product: determine the relative crystallinity, average particle size and SiO of the product 2 / Al 2 o 3 Listed in Table 1. It can be seen from the XRD spectrum that the synthesized...

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Abstract

The invention discloses a method for synthesizing a Y type molecular sieve, and belongs to the technical field of preparation of catalysts. The method comprises the following steps of: mixing sodium metaaluminate and a silicon source in a reaction kettle, and performing rotary ageing to obtain a directing agent; adding the sodium metaaluminate and the directing agent into the silicon source in sequence, stirring, adding acidic aluminum salt, and continuously stirring to obtain silicon-aluminum gel; and crystallizing the silicon-aluminum gel in two steps, centrifuging, and drying to obtain the NaY type molecular sieve. The silicon-aluminum ratio of the synthesized NaY type molecular sieve is more than 5.0, and the average particle size of the sieve is not more than 100nm. The NaY type molecular sieve synthesized by the method is high in specific surface area, has higher performance in the aspects of converting macromolecules, reducing the secondary cracking of a product and the coking of a catalyst, and the like compared with the conventional Y type molecular sieve, is high in thermal stability and hydrothermal stability, is prepared from low-cost industrial raw materials, is environment-friendly, and has an industrial application prospect, and a framework of the sieve is high in silicon-aluminum ratio.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, in particular to a method for synthesizing a Y-type molecular sieve. Background technique [0002] Y-type molecular sieves are widely used as catalysts or catalyst carriers in the petrochemical industry, especially in the field of catalytic cracking. With the heavy and inferior quality of catalytic cracking raw materials, the requirements for catalysts are becoming more and more stringent. The conventional Y-type molecular sieve has a small pore size, and it is difficult for heavy oil macromolecules to enter the pores. At the same time, it also limits the rapid diffusion of molecules, which is unfavorable for reducing secondary cracking and coking rate. Nano Y-type molecular sieve has a large proportion of surface atoms, a large number of catalytic active centers, and a high intracrystalline diffusion rate. It is superior to conventional Y-type molecular sieves in terms of convertin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/24
Inventor 张晓丽宋家庆徐向宇姚小强
Owner BEIJING UNIV OF CHEM TECH
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