Green preparation method of high silica-alumina ratio hydrogenous molecular sieve

A hydrogen-type molecular sieve, high silicon-aluminum ratio technology, applied in molecular sieve compounds, molecular sieve characteristic silicates, chemical instruments and methods, etc., can solve the problems of failure of recycling routes, consumption of crystal seeds, enrichment of inorganic salts such as sodium bromide and other issues to achieve the effect of reducing production process steps, saving water and energy consumption, and saving production time

Inactive Publication Date: 2019-03-19
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthesis of zeolite molecular sieves mainly includes water source, alkali source, template agent, silicon source and aluminum source. Among them, the alkali source generally adopts inorganic alkali such as sodium hydroxide, and most of the silicon and aluminum sources use low-cost raw materials with high sodium ions. Synthetic products It is a sodium zeolite, but the molecular sieve catalyst, as an active component of an acid-catalyzed mechanism, needs to undergo an ion exchange step, which is time-consuming, energy-consuming, and water-consuming; the patent (CN 103626200A) proposes a one-step synthesis of hydrogen-type EUO by a sodium-free method The method of zeolite has few ion exchange steps, the method is simple, and has the disadvantages of reducing energy consumption, saving time, and less waste water.
Most of the molecular sieve templates are relatively cheap bromine or chlorine-containing quaternary ammonium salts. If the mother liquor of the system is recycled, it will inevitably lead to the enrichment of inorganic salts such as sodium bromide, which will destroy the charge balance of the molecular sieve synthesis system and ma

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  • Green preparation method of high silica-alumina ratio hydrogenous molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Get 5.8g of deionized water, 10g of 1.02mol / L hexamethyldiammonium hydroxide solution, 6.0g of ammonium-type silica sol, wherein SiO 2 The mass ratio is 30%wt, 0.0136g pseudo-boehmite (Al 2 o 3The mass ratio is 75%wt) and mixed, stirred at room temperature for 1h, installed in a stainless steel reactor, and crystallized at 180°C for 48h. After the crystallization is completed, cool, filter, wash until neutral, and dry to record as A0. The sample is calcined at 400°C for 6 hours to obtain a hydrogen-type EU-1 molecular sieve. Among them, the molecular sieve mother liquor is collected during the suction filtration process, and its hydroxide, silica, and alumina components are analyzed; deionized water, hexamethyldiammonium hydroxide, ammonium-type silica sol, and pseudoboehmite are added in the first cycle. Continue to crystallize after the gel ratio is consistent with the initial feeding. The crystallization temperature time and treatment method are the same as A0, and...

Embodiment 2

[0027] Take 8.0g of deionized water, 10g of hexamethyldiammonium hydroxide solution (0.3mol / L), 6.429g of ethyl orthosilicate (SiO 2 The mass ratio is 28wt%wt), 0.0408g pseudo-boehmite (Al 2 o 3 The mass ratio is 75%wt), mixed at room temperature for 1 hour, installed in a stainless steel reactor, and crystallized at 200°C for 24 hours. After the crystallization is completed, cool, filter with suction, wash until neutral, and dry to record as B0. The sample is calcined at 600°C for 3 hours to obtain a hydrogen-type EU-1 molecular sieve. Among them, the molecular sieve mother liquor is collected during the suction filtration process, and its hydroxide component, silica component, and alumina component are analyzed; deionized water, hexamethyldiammonium hydroxide, ethyl orthosilicate, and pseudoboehmite are added in the first cycle. After the proportion of the stone and the initial feeding gel was consistent, the crystallization continued. The crystallization temperature, time...

Embodiment 3

[0029] Take 0.4g of deionized water, 5.0g of hexamethonium hydroxide solution (3.0mol / L), 1.818g of silica gel (SiO 2 The mass ratio is 99%wt), 0.0272g pseudo-boehmite (Al 2 o 3 The mass ratio is 75%wt), mixed at room temperature for 1 hour, installed in a stainless steel reactor, and crystallized at 200°C for 24 hours. After the crystallization is completed, cool, filter, wash until neutral, and dry to record as C0. The sample is calcined at 600°C for 3 hours to obtain a hydrogen-type EU-1 molecular sieve. Among them, the molecular sieve mother liquor is collected during the suction filtration process, and its hydroxide component, silica component, and alumina component are analyzed; deionized water, hexamethylbisammonium hydroxide, silica gel, pseudoboehmite and initial feeding are added in the first cycle. After the gel ratio is consistent, continue to crystallize. The crystallization temperature, time and processing method are the same as C0, and sample C1 is obtained. A...

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Abstract

The invention relates to the technical field of molecular sieve preparation, and discloses a green preparation method of a high silica-alumina ratio hydrogenous molecular sieve, comprising the following steps: mixing and crystallizing a silicon source with Na2O less than 100ppm, an aluminum source, water and hexamethonium hydroxide, then cooling, and performing suction filtration to obtain an EU-1molecular sieve semi-finished product and molecular sieve crystallization mother liquor, and drying and roasting the EU-1 molecular sieve semi-finished product to obtain the hydrogenous EU-1 molecular sieve. According to the invention, in a sodium-free system, a hydrogenous zeolite molecular sieve is obtained by high temperature roasting at 400-600 DEG C, production process steps are reduced, water consumption and energy consumption are saved, and production time is saved; compared with a sodium-containing ion synthesis system, in the system, low-positive-charge-density quaternary ammonium cation is easier to match with a high silica-alumina molecular sieve framework with low negative charge, and a molecular sieve with high silica-alumina ratio phase region SiO2/Al2O3 being equal to 100-500 and sodium oxide content being lower than 500ppm is synthesized.

Description

technical field [0001] The invention relates to the technical field of molecular sieve preparation, in particular to a green preparation method of a high silicon-aluminum ratio hydrogen type molecular sieve. Background technique [0002] Zeolite molecular sieve is a kind of aluminosilicate crystal, which is widely used in adsorption, catalysis and ion exchange due to its unique pore structure, suitable acid distribution, good thermal and hydrothermal stability, and ultra-high specific surface area. field. In recent years, with the increasingly severe environmental pressure, how to make green and efficient production has become the first task of all walks of life. Among them, the chemical industry, as the main polluting industry of wastewater, waste gas and waste, has become a concern of the government and relevant researchers. [0003] There are many synthesis methods of zeolite molecular sieves: mainly hydrothermal synthesis, steam phase inversion, solvent-free synthesis,...

Claims

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Application Information

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IPC IPC(8): C01B39/04C01B37/00
CPCC01B37/005C01B39/04C01P2006/12C01P2006/14
Inventor 李晓峰张燕挺刘春滋窦涛
Owner TAIYUAN UNIV OF TECH
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