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Preparation method for germanium-free IWR zeolite molecular sieve

A zeolite molecular sieve and heteroatom technology, applied in molecular sieve catalysts, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc., can solve the problems of high cost of template agents, large amount of use, poor structural stability of IWR zeolite molecular sieves, etc. The effect of low cost, saving synthesis cost and easy promotion

Active Publication Date: 2018-12-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a synthetic method for IWR zeolites by using cheap The germanium-free IWR zeolite molecular sieve can be synthesized from a commercially available organic template agent, and the resulting IWR zeolite molecular sieve has good structural stability.

Method used

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  • Preparation method for germanium-free IWR zeolite molecular sieve
  • Preparation method for germanium-free IWR zeolite molecular sieve
  • Preparation method for germanium-free IWR zeolite molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0029] Dissolve 0.25g boric acid in 2.693g 45wt% choline hydroxide aqueous solution, add 3g Ludox (HS-40, 40%) and stir evenly, finally add 1g 37% NH 4 F aqueous solution. The vessel was stirred open overnight to evaporate some of the water until the reaction mixture reached the final molar composition.

[0030] The above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 170°C for crystallization for 168 hours. After the reaction, the solid was filtered, washed with distilled water, and dried at 100° C. to obtain a solid powder. The raw powder solid is placed in a muffle furnace and roasted at a temperature of 550° C. for 5 hours to obtain the final product. After calcination, the sample shows a stable IWR structure, and the XRD pattern is as follows figure 1 As shown, the SEM photos are as figure 2 shown.

[0031] The stability of the IWR zeolite molecular sieve was analyzed according to the following method: so...

Embodiment 2

[0033] Dissolve 0.6g boric acid in 2.693g 45wt% choline hydroxide aqueous solution, add 3g Ludox (HS-40, 40%) and stir evenly, finally add 1g 37% NH 4 F aqueous solution. The vessel was stirred open overnight to evaporate some of the water until the reaction mixture reached the final molar composition.

[0034] The above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 170°C for crystallization for 120 hours. The solid obtained after the reaction is filtered, washed, dried and calcined is IWR molecular sieve.

Embodiment 3

[0036] Dissolve 0.9g boric acid in 2.693g 45wt% choline hydroxide aqueous solution, add 4.16g tetraethyl orthosilicate (TEOS) and add 1.2g 37% NH 4 F aqueous solution. The vessel was left open and stirred overnight to evaporate the ethanol and some of the water until the reaction mixture reached the final molar composition.

[0037]The above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 160°C for crystallization for 192 hours. The solid obtained after the reaction is filtered, washed, dried and calcined is IWR molecular sieve.

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Abstract

The invention relates to a preparation method for a germanium-free IWR zeolite molecular sieve. The problems in the prior art that template agents and Ge elements used to synthetize an IWR zeolite molecular sieve are expensive and obtained IWR zeolite molecular sieve structures are poor in stability can be solved. The preparation method uses choline hydroxide which is cheap and can be obtained from markets as an organic template agent; a mixture can be formed according to the mole of choline hydroxide / SiO2 = 0.1-1.5, SiO2 / B2O3 = 0.5-100, oxide of a heteroatomic metal W / SiO2 = 0-0.2, F<-> / SiO2= 0.1-1.5, H2O / SiO2 = 1-50; and hydrothermal crystallization can be performed on the mixture so that the porous crystallized IWR zeolite molecular sieves can be obtained. The obtained IWR zeolite molecular sieves is stable in structure through synthesis; and the preparation method is wide in synthesis range, simple in operation and convenient for popularization.

Description

technical field [0001] The invention relates to a preparation method of a zeolite molecular sieve, more specifically a preparation method of a germanium-free IWR zeolite molecular sieve. technical background [0002] Zeolite molecular sieves are crystalline porous silicate materials that are widely used as adsorbents, ion exchangers, and industrial catalysts. At present, there are 231 molecular sieve topologies approved by the International Molecular Sieve Association. [0003] Molecular sieves with multidimensional pore structures have diffusion advantages in catalytic reactions, and when the pores in each direction have different pore sizes, molecular sieves can exhibit unique shape-selective catalytic capabilities. From the perspective of petrochemical industry, molecular sieves with 12-membered ring × 10-membered ring channel structure have excellent catalytic performance in aromatic alkylation reactions. [0004] IWR zeolite molecular sieves and CIT, SSZ-26, SSZ-33 an...

Claims

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Application Information

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IPC IPC(8): C01B39/12C01B39/04C01B39/06B01J29/70
CPCB01J29/70C01B39/04C01B39/06C01B39/12C01P2002/72C01P2004/03
Inventor 付文华杨为民袁志庆滕加伟陶伟川
Owner CHINA PETROLEUM & CHEM CORP
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