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Metal-modified 13X molecular sieve desulphurization adsorbent and its preparation method and use

A technology of metal modification and molecular sieve, applied in separation methods, non-metallic elements, chemical instruments and methods, etc., can solve the problems of harsh operating conditions, insufficient desulfurization depth, high operating costs, etc., achieve high activity at room temperature, reduce equipment investment, Effect of reducing production cost

Inactive Publication Date: 2016-02-03
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] In summary, the current patents or literature on desulfurization adsorbents still have the following deficiencies: 1. It is still necessary to find a simpler preparation method for the adsorbent, which will help to improve the dispersion of components; 2. The desulfurization process consumes a lot of energy, the operating conditions are relatively harsh, and the operating costs are high. The adsorption process and conditions still need to be further simplified, preferably at normal temperature and pressure; 3. The adsorption capacity of the adsorbent needs to be further improved; 4. Desulfurization The depth is not enough, it is difficult to remove sulfur from 50-200ppm to below 10ppm

Method used

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  • Metal-modified 13X molecular sieve desulphurization adsorbent and its preparation method and use

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Effect test

Embodiment 1

[0036] The preparation method of metal-modified 13X molecular sieve desulfurization adsorbent adopts the following steps:

[0037] (1) preparation concentration is that the cerium nitrate solution of 0.1mol / L is standby as active component ion exchange salt solution;

[0038] (2) Take 13X molecular sieve, add step (1) to obtain cerium nitrate solution, the mass ratio of 13X molecular sieve and cerium nitrate solution is 1:10, carry out ion exchange reaction, the reaction temperature of ion exchange is 20 ℃, ion exchange time is 48h , followed by filtration, washing, and drying at 100° C. for 12 h;

[0039] (3) Place the product obtained in step (2) in a tube furnace, and activate it by roasting under a nitrogen atmosphere. The roasting temperature rise rate is 2°C / min, the roasting temperature is 300°C, and the roasting time is 5h. After cooling in the furnace, That is, a metal ion-exchanged molecular sieve desulfurization adsorbent is obtained.

[0040] The prepared metal-m...

Embodiment 2

[0043] The preparation method of metal-modified 13X molecular sieve desulfurization adsorbent adopts the following steps:

[0044] (1) preparation concentration is that the cerium nitrate solution of 0.025mol / L is standby as active component ion exchange salt solution;

[0045] (2) Get 13X molecular sieve, add step (1) to obtain cerium nitrate solution, the mass ratio of 13X molecular sieve and cerium nitrate solution is 1:50, carry out ion exchange reaction, the reaction temperature of ion exchange is 90 ℃, ion exchange time is 2h , followed by filtration, washing, and drying at 120° C. for 6 h;

[0046] (3) Place the product obtained in step (2) in a tube furnace, and activate it by roasting under a nitrogen atmosphere. The heating rate of the roasting is 1°C / min, the roasting temperature is 700°C, and the roasting time is 1h. After cooling in the furnace, That is, a metal ion-exchanged molecular sieve desulfurization adsorbent is obtained.

[0047] The prepared metal-modi...

Embodiment 3

[0049] The preparation method of metal-modified 13X molecular sieve desulfurization adsorbent adopts the following steps:

[0050] (1) preparation concentration is that the cobalt nitrate solution of 0.2mol / L is standby as active component ion exchange salt solution;

[0051] (2) Take 13X molecular sieve, add step (1) to obtain cobalt nitrate solution, the mass ratio of 13X molecular sieve and cobalt nitrate solution is 1:30, carry out ion exchange reaction, the reaction temperature of ion exchange is 80 ℃, ion exchange time is 24h , followed by filtration, washing, and drying at 100° C. for 10 h;

[0052] (3) Place the product obtained in step (2) in a tube furnace and activate it by roasting under a nitrogen atmosphere. The roasting temperature rise rate is 5°C / min, the roasting temperature is 400°C, and the roasting time is 8h. After cooling in the furnace, That is, a metal ion-exchanged molecular sieve desulfurization adsorbent is obtained.

[0053] The prepared metal-mo...

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Abstract

The invention relates to a metal-modified 13X molecular sieve desulphurization adsorbent and its preparation method and use. The preparation method comprises preparing a metal salt solution as an active ingredient ion exchange salt solution for next use, taking a 13X molecular sieve, adding the 13X molecular sieve into the ion exchange salt solution for ion exchange reaction, carrying out filtration, washing the filter residues, carrying out drying, putting the dried filter residues into a tube furnace, carrying out roasting activation, and carrying out furnace cooling to obtain the molecular sieve desulphurization adsorbent subjected to metal ion exchange. The molecular sieve desulphurization adsorbent can be used for ultra-deep removal of sulfocompounds such as thiophene and its derivatives in gasoline and diesel oil. The metal-modified 13X molecular sieve desulphurization adsorbent has a large specific surface area and a rich micropore structure, can effectively remove a trace amount of sulfocompounds in gasoline, has the advantages of low cost, simple preparation processes, high removal depth and regeneration convenience, can be used for deep removal of sulfocompounds in fuel oil products and preparation of ultral-low sulphur clean fuel oil, reduces oil product combustion sulfide discharge-caused environmental pollution and improves environment quality.

Description

technical field [0001] The invention belongs to the field of environmental protection adsorption materials and energy chemical materials, and in particular relates to a metal-modified 13X molecular sieve desulfurization adsorbent and its preparation method and application, which is suitable for the removal of sulfur-containing compounds in the field of petrochemical industry, or the preparation of sulfur-free gasoline. Background technique [0002] With the rapid development of the automobile industry and the transportation industry, the consumption of gasoline and diesel has shown a rapid growth trend. The sulfur oxides produced by the combustion of fuel oil are one of the main pollutants in the atmosphere, which will cause major environmental pollution problems such as acid rain and photochemical smog, which has caused people to pay more and more attention to environmental protection. In view of this, governments around the world are increasingly restricting the sulfur con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/16B01J20/30B01J20/34C10G25/00
Inventor 叶丽萍张亚光张磊杨丙星罗勇李建龙
Owner SHANGHAI RES INST OF CHEM IND
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