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L-type molecular sieve containing germanium and preparation method thereof

A molecular sieve, L-type technology, applied to germanium-containing molecular sieves and the fields of preparation and application, can solve problems such as no relevant reports on the aromatization performance of alkanes, and achieve the effect of good aromatization activity

Active Publication Date: 2019-12-10
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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  • L-type molecular sieve containing germanium and preparation method thereof
  • L-type molecular sieve containing germanium and preparation method thereof
  • 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 an L-type molecular sieve containing germanium and a preparation method thereof. The molecular sieve has the chemical composition of (0.8-1.3)M.(0.001-0.007)GeO2.Al2O3.(4-7)SiO2, wherein M is K2O or a combination of K2O and Na2O. The L-Type molecular sieve provided by the invention is used for preparing an aromatization catalyst, and has good aromatization conversion rate,target aromatics 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 Applications(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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