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A kind of L-type molecular sieve containing germanium and preparation method thereof

A molecular sieve, L-type technology, applied in the field of germanium-containing molecular sieve and its preparation and application, can solve the problems of alkane aromatization performance that have not been reported related to

Active Publication Date: 2021-06-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] CN104271242A discloses catalysts prepared from a variety of germanium-containing materials, and the germanium content of the catalyst is 0.1wt% to 10wt%, but the influence of L-type molecular sieves containing a small amount of germanium on the alkane aromatization performance of the PtKL catalyst system has not been reported so far

Method used

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  • A kind of L-type molecular sieve containing germanium and preparation method thereof
  • A kind of L-type molecular sieve containing germanium and preparation method thereof
  • A kind of L-type molecular sieve containing germanium and preparation method thereof

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preparation example Construction

[0020] The preparation method of the L-type molecular sieve provided by the invention comprises:

[0021] Mix the inorganic base, germanium source, aluminum source, silicon source and water to obtain a reaction gel; wherein, the molar composition of the reaction gel is: (6-20) SiO 2 :Al 2 o 3 : (0.01-0.12)GeO 2 :(1-6)M:(80-300)H 2 O;

[0022] The obtained reaction gel is subjected to hydrothermal crystallization, and the solid product obtained after crystallization is washed and dried.

[0023] Preferably, the molar composition of the reaction gel is: (10-15) SiO 2 :Al 2 o 3 : (0.04-0.10)GeO 2 :(2-6)M:(140-300)H 2 O.

[0024] In the method of the present invention, H 2 The molar ratio of O to M is preferably not more than 75.

[0025] In the method of the present invention, the temperature of the hydrothermal crystallization can be 100-200°C, preferably 150-180°C, the time is 10-200 hours, preferably 24-72 hours, and the drying temperature can be 80-120°C , the ti...

example 1

[0039] Example 1 Preparation of the directing agent used in the present invention.

[0040] Example 1

[0041] Preparation of directing agent

[0042] According to the molar composition of the feeding mixture, it is 8K 2 O·Al 2 o 3 14SiO2 2 ·320H 2 For the formula of O, 6g of hydrated alumina (the content of alumina is 70% by mass, the same below) was added to 132g of the solution containing 36.89g of KOH, heated and dissolved to obtain a mixed solution. With stirring, the mixed solution was added to 138 g of silica sol (containing 25% by mass SiO) preheated to 50° C. 2 , the pH value is 9, the same below), stirred for 0.5 hours to form a reaction gel, and aged the reaction gel at 34°C for 72 hours to obtain a translucent sol, which was used as a directing agent.

example 2

[0048] The germanium-containing L-type molecular sieve of the present invention is prepared.

[0049] Add 5.01g of hydrated alumina to 43.50g containing 9.97gKOH and 0.19gGeO 2 In the solution, heated and dissolved to obtain a mixed solution, the mixed solution was added to 81.52g of silica sol under stirring, and 8.08g of the directing agent prepared in Example 1 was added, and stirred for 0.5 hours to form a reaction gel, and its molar composition was: 10SiO 2 ·Al 2 o 3 0.05GeO 2 2.75K 2 O·160H 2 O, Al in the directing agent 2 o 3 Al in the reaction gel 2 o 3 The molar ratio is 3.0%.

[0050] Transfer the above reaction gel into the reaction kettle and crystallize at 170°C for 72 hours, then rapidly cool to 40°C, the product is centrifuged and washed until the pH value of the liquid phase is 10-11, and the obtained solid is dried at 120°C for 10 hours to obtain Germanium-containing L-type molecular sieve raw powder GL-1, its X-ray powder diffraction analysis spectr...

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Abstract

The invention relates to a germanium-containing L-type molecular sieve and a preparation method thereof. The chemical composition of the molecular sieve is: (0.8‑1.3)M·(0.001‑0.007)GeO 2 ·Al 2 o 3 ·(4-7)SiO2 2 , where M is K 2 O or K 2 O and Na 2 A combination of O. The L-type molecular sieve provided by the invention is used for preparing an aromatization catalyst, and has good aromatization conversion rate, target aromatic hydrocarbon yield and stability.

Description

technical field [0001] The invention relates to a germanium-containing molecular sieve and its preparation and application, in particular to a germanium-containing L-type molecular sieve and its preparation and application. Background technique [0002] L-type molecular sieve (International Molecular Sieve Association code: LTL) is a synthetic molecular sieve developed by Union Carbide Company in 1965, and no equivalent has been found in nature so far. L-type molecular sieve is a kind of basic macroporous molecular sieve. Its crystal is cylindrical and has a one-dimensional channel structure parallel to the axis of the cylinder. Then rotate according to the sixfold axis to produce a twelve-membered ring channel with a pore diameter of 0.71nm and a dynamic diameter of 0.81nm. The typical chemical composition molecular formula of L-type molecular sieve is as follows: [0003] (0.9~1.3)M 2 / n O: Al 2 o 3 :xSiO 2 :yH 2 O, [0004] In the formula, M is a metal ion, and the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/32B01J29/60B01J29/62C07C5/41C07C15/04
CPCB01J29/60B01J29/62B01J2229/18B01J2229/183C01B39/32C01P2002/72C01P2002/82C01P2004/03C07C5/417C07C2529/62C07C15/04Y02P20/52
Inventor 杨尚王嘉欣丁璟臧高山张玉红于宁王涛
Owner CHINA PETROLEUM & CHEM CORP
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