Preparation method for Cu(I)-Y molecular sieve adsorption desulphurizing agent

A technology of adsorption desulfurization and molecular sieve, which is applied in the field of Cu-Y molecular sieve preparation, can solve the problems of long exchange time and achieve the effects of simple process, high copper content and strong adsorption and desulfurization ability

Inactive Publication Date: 2009-02-18
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation method of normal temperature LPIE method is simple, but to obtain a higher degree of ion exc

Method used

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  • Preparation method for Cu(I)-Y molecular sieve adsorption desulphurizing agent
  • Preparation method for Cu(I)-Y molecular sieve adsorption desulphurizing agent
  • Preparation method for Cu(I)-Y molecular sieve adsorption desulphurizing agent

Examples

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preparation example Construction

[0014] When using the NaY molecular sieve synthesized in situ on the magnetic substrate to synthesize the Cu(I)-Y molecular sieve adsorbent, a preferred preparation method comprises the following steps:

[0015] A Synthesis of Magnetic NaY Molecular Sieves

[0016] First, prepare the directing agent: mix water glass and high alkali sodium metaaluminate solution, stir evenly, and age at room temperature to 100° C. for 12 to 36 hours, preferably at 40 to 50° C. and for 24 to 30 hours. Then, the directing agent, the water glass and the low-alkali sodium metaaluminate solution are mixed, and the aluminum sulfate solution and the deionized water are sequentially added under stirring to obtain a synthetic gel. Then, add fine particles of the magnetic matrix (preferably 100-500 mesh) into the synthetic gel, stir evenly, and then crystallize at 80-120°C for 20-60h, preferably at a crystallization temperature of 95-105°C. The time is 48-56 hours. The crystallization process is prefer...

Embodiment 1～6

[0026] This example illustrates the preparation of the Cu(I)-Y molecular sieve adsorbent of the present invention.

[0027] NaY molecular sieve (Si / Al molar ratio is 2.31, produced by Catalyst Factory of Changling Branch of Sinopec Corporation) and Cu(NO 3 ) 2 (Analytical grade, Beijing Yili Fine Chemicals Co., Ltd.) solution (concentration: 0.5mol / L) was mixed at a solid-liquid ratio of 0.05:1, and ion exchange was carried out at 100°C, 135°C or 150°C, and the exchange time was 3h, 6h or 12h, then wash with deionized water until neutral, dry in air at 100°C for 18h, and then dry in 500°C N 2 Roasting in medium for 3h, and continue in N 2 Cool to room temperature in the atmosphere and store in airtight. The exchange equipment used is a pressure-resistant closed exchange tank, and the stirring equipment is a self-made rotary oven with controllable temperature and rotation speed, and the rotation speed is 30 rpm.

[0028] The operating conditions and physical and chemical pr...

Embodiment 7～12

[0034] This example illustrates the gasoline adsorption desulfurization performance of the Cu(I)-Y molecular sieve adsorbent prepared in the present invention. The sulfur content in the oil was determined by gas chromatography-atomic emission spectrometry (GC-AED).

[0035] The Cu(I)-Y molecular sieve adsorbent prepared in Examples 1-6 is adopted to investigate the effect of model gasoline (n-octane, total sulfur content is 1012 μg·mL) by batch method. -1 , the composition of sulfur-containing compounds is shown in Table 2), and the desulfurization performance was adsorption and desulfurization for 1.0 h at room temperature, normal pressure, and the operating conditions of an agent-oil weight ratio of 1:50. By measuring the sulfur content of gasoline before and after desulfurization, the desulfurization rate of the adsorbent was calculated, and the results are shown in Table 3.

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Abstract

A preparation method for a Cu(I)-Y molecular sieve absorption desulfurizer comprises the following steps of: mixing a Y type molecular sieve with Cu2+ aqueous solution, carrying out ion exchange under a hydrothermal condition of between 100 and 200 DEG C for 3-18 hours, and then carrying out washing, filtering, drying and calcination in the inert atmosphere or the vacuum. The method can shorten ion exchange time, improve ion exchange rate, and improve the absorption desulfurization capability of the absorbent.

Description

technical field [0001] The present invention relates to a kind of preparation method of Cu(I)-Y molecular sieve, specifically, the present invention relates to a kind of preparation method of Cu(I)-Y molecular sieve adsorption desulfurization agent. Background technique [0002] In 2001, according to 13X, Y, ZSM-5 and other molecular sieves with d 10 the s 0 The mechanism that metal cations in the d-block of the outer electron structure can form π-complex bonds with sulfur atoms in sulfur-containing compounds, R.T.Yang et al. first modified Cu(I)-Y, Ag(I)-Y and other metals Molecular sieves are used in gasoline adsorption desulfurization process (R.T.Yang, A.Takahashi, F.H.Yang.Ind.Eng.Chem.Res., 2001, 40, 6236). In 2004, U.S. Patent US 2004 / 0,040,891 Al, US 2004 / 0,200,758 Al disclosed an adsorbent for removing sulfur in hydrocarbon fuels and a preparation method thereof, wherein Cu(I)- Y molecular sieve adsorbent has good adsorption and desulfurization performance. [0...

Claims

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Application Information

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IPC IPC(8): B01J20/18C10G25/05
Inventor 慕旭宏谷涛
Owner CHINA PETROLEUM & CHEM CORP
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