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Synthesis method of ultralow-sodium high-silicon nano ZSM-5 molecular sieve

A technology of ZSM-5 and synthesis method, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of unfavorable industrial production and high cost of silica-alumina glue, and achieve the reduction of synthesis cost, silicon The effect of high aluminum ratio, reduction of production cost and discharge of ammonia nitrogen sewage

Active Publication Date: 2015-03-04
CHINA NAT OFFSHORE OIL CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method uses solid silica-alumina gel as raw material, and the single-pot yield is high, but the cost of silica-alumina gel is relatively high, which is not conducive to large-scale industrial production

Method used

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  • Synthesis method of ultralow-sodium high-silicon nano ZSM-5 molecular sieve
  • Synthesis method of ultralow-sodium high-silicon nano ZSM-5 molecular sieve
  • Synthesis method of ultralow-sodium high-silicon nano ZSM-5 molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0025] Weigh 18g of NaOH solid and dissolve it in 1160g of deionized water, slowly add 520g of acidic silica sol under mechanical stirring, and continue stirring to form a sol. Add 25.8g of template agent TEAC, stir evenly, slowly add 7.8g of aluminum sulfate under stirring, mechanically stir continuously during the adding process, so that the reactant is latex-like. After aging at room temperature for 8 hours, the latex-like reactant was added to a dynamic stirring reactor for programmed temperature hydrothermal crystallization. The heating rate of the reactor was 2°C / min. The crystallization temperature is 180°C and the crystallization time is 48h. The resulting product is filtered and washed until the filtrate is neutral, and after drying and roasting, 175g of ZSM-5 type zeolite molecular sieve is obtained. Through XRF analysis, SiO 2 / Al 2 o 3 =133.69, Na 2 The O content is 0.0485%, and the average crystal grain diameter is 50nm.

Embodiment 2

[0027] Weigh 22g of NaOH solid and dissolve it in 1160g of deionized water, slowly add 520g of acidic silica sol under mechanical stirring, and continue stirring to form a sol. Add 25.8g of template agent TEAC, stir evenly, slowly add 11.4g of aluminum sulfate under stirring, mechanically stir continuously during the addition process, so that the reactant is latex-like. After aging at room temperature for 8 hours, the latex-like reactant was added to a dynamic stirring reactor for programmed temperature hydrothermal crystallization. The heating rate of the reactor was 2°C / min. The crystallization temperature is 180°C and the crystallization time is 48h. The resulting product is filtered and washed until the filtrate is neutral, dried and roasted to obtain 170 g of ZSM-5 type zeolite molecular sieve, which is analyzed by XRF, and SiO 2 / Al 2 o 3 =98.86,Na 2 The O content is 0.0694%, and the average crystal grain diameter is 55nm.

Embodiment 3

[0029] Weigh 24g of NaOH solid and dissolve it in 1160g of deionized water, slowly add 520g of acidic silica sol under mechanical stirring, and continue stirring to form a sol. Add 25.8g of template agent TEAC, stir evenly, slowly add 11.4g of aluminum sulfate under stirring, mechanically stir continuously during the addition process, so that the reactant is latex-like. After aging at room temperature for 8 hours, the latex-like reactant was added to a dynamic stirring reactor for programmed temperature hydrothermal crystallization. The heating rate of the reactor was 2°C / min. The crystallization temperature is 180°C and the crystallization time is 48h. The resulting product is filtered and washed until the filtrate is neutral, and after drying and roasting, 175g of ZSM-5 type zeolite molecular sieve is obtained. Through XRF analysis, SiO 2 / Al 2 o 3 =101.27,Na 2 The O content is 0.114%, and the average crystal grain diameter is 53nm.

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Abstract

The invention relates to a synthesis method of an ultralow-sodium high-silicon nano ZSM-5 molecular sieve, which is characterized by comprising the following steps: 1) dissolving NaOH in water, slowly adding a silicon source selected from silica sol, wherein the Na2O:SiO2:H2O mole ratio is (0.08-0.2):1:(20-26), and the dropwise addition speed of the silica sol is controlled at about 50g / minute; 2) after the silica sol in the step 1) is uniformly dispersed in the alkali, respectively dissolving a template agent and an aluminum source in a small amount of water, adding into the sol in the step 1) while slowly stirring, and aging at room temperature for 8 hours, wherein the silica-alumina ratio is 80-240, and the mole ratio of the template agent to the silicon oxide is 0.05-0.1; 3) transferring the sol in the step 2) into a reaction kettle for hydrothermal crystallization, heating at the rate of 2 DEG C / minute, pre-crystallizing at 110-130 DEG C for 3 hours, heating to the crystallization temperature of 180+ / -10 DEG C, crystallizing for 40-80 hours, and mechanically stirring; and carrying out conventional filtration, washing, drying and roasting to obtain the product.

Description

technical field [0001] The invention relates to the technical field of molecular sieve synthesis, in particular to a method for synthesizing ultra-low-sodium and high-silicon nano ZSM-5 molecular sieves. Background technique [0002] ZSM-5 zeolite is a kind of aluminosilicate with unique three-dimensional intersecting channels and ten-membered ring pore structure. Because of its good hydrothermal stability, skeleton thermal stability and strong acidity, it is an ideal material for catalysis. So far, ZSM-5 zeolite has been widely used in the alkylation of aromatic hydrocarbons, catalytic cracking, and aromatization of light hydrocarbons. Important industrial processes such as methanol to gasoline. Since the first synthesis of ZSM-5 zeolite by Mobil Corporation of the United States in 1972, researchers have been continuously optimizing the synthesis conditions to obtain catalysts with corresponding catalytic performance. Among them, the ratio of silicon to aluminum in the fr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40B82Y30/00
CPCC01B39/40C01P2002/72C01P2004/03C01P2004/64
Inventor 于海斌裴仁彦汪洋臧甲忠王银斌郭春垒张耀日霍志萍张雪梅彭晓伟
Owner CHINA NAT OFFSHORE OIL CORP
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