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Cu/mesoporous organic silicon oxide nanotube desulfurization adsorbent and preparation method thereof

An organic silicon oxide and nanotube technology, applied in chemical instruments and methods, inorganic chemistry, alkali metal oxides/hydroxides, etc., can solve the problem of poor dispersion of metal active components, low mass transfer and diffusion efficiency, high price, etc. problem, to achieve the effect of enhancing mass transfer and diffusion performance, good application prospects, and low cost

Active Publication Date: 2020-10-02
泰州九润环保科技有限公司
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Problems solved by technology

[0005] Aiming at the above-mentioned technical problems, the present invention firstly develops a Cu / mesoporous organosilica nanotube desulfurization adsorbent, which overcomes the low efficiency of mass transfer and diffusion of traditional desulfurization adsorbents, poor dispersion of metal active components, easy shedding, Expensive technical flaws with good application prospects

Method used

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  • Cu/mesoporous organic silicon oxide nanotube desulfurization adsorbent and preparation method thereof
  • Cu/mesoporous organic silicon oxide nanotube desulfurization adsorbent and preparation method thereof
  • Cu/mesoporous organic silicon oxide nanotube desulfurization adsorbent and preparation method thereof

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Experimental program
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Embodiment 1

[0022] Dissolve P123 in an HCl solution with a concentration of 1M, stir to fully dissolve it to obtain a solution (1); dissolve the silicon source represented by formula (I) in ethanol, stir and dissolve it sufficiently to obtain a silicon source with a concentration of 1M solution; the silicon source solution is added dropwise to the solution (1), and a copper nitrate solution with a concentration of 0.05M is added, so that the molar ratio of the silicon source, soft template agent, and metallic copper in the solution system is 3:0.8:1, Continue to stir for 8 hours; transfer the obtained mixture into a stainless steel reaction kettle with polytetrafluoroethylene, react at 100°C for 24 hours, naturally cool to room temperature after the reaction, filter, and use ethanol to remove the soft template agent in the filtered product The reflux extraction obtained the Cu / mesoporous organosilica nanotube desulfurization adsorbent of this embodiment, wherein Cu accounted for 6.4 wt% of...

Embodiment 2

[0024] Dissolve P123 in an HCl solution with a concentration of 1.5M, stir to fully dissolve it to obtain a solution (1); dissolve the silicon source represented by formula (I) in ethanol, stir and dissolve it sufficiently to obtain a solution with a concentration of 1.2M Silicon source solution; the silicon source solution is added dropwise to the solution (1), adding a concentration of 0.05M copper nitrate solution, so that the molar ratio of silicon source, soft template agent, and metallic copper in the solution system is 3:0.8: 0.5, continue to stir for 8 hours; transfer the resulting mixture into a stainless steel reactor with polytetrafluoroethylene, react at 110°C for 20 hours, naturally cool to room temperature after the reaction, filter, and use ethanol to filter the soft template in the filtered product reflux extraction to obtain the Cu / mesoporous organosilica nanotube desulfurization adsorbent of this embodiment, wherein Cu accounts for 4.2 wt% of the mass of the a...

Embodiment 3

[0026] Use thiophene, benzothiophene, dibenzothiophene, 4-methyl-dibenzothiophene, and n-hexane to prepare simulated oil, and the initial sulfur concentration is 100-300μg / g. Add the Cu / mesoporous organosilica nanotube desulfurization adsorbent prepared above to the prepared simulated oil, add 1g of adsorbent per 100ml of simulated oil, place it in a shaker at 40°C for 5h, and make the adsorption reached adsorption equilibrium. The sulfur concentration in the simulated oil after adsorption equilibrium was measured by a microcoulomb sulfur analyzer, and the equilibrium adsorption sulfur capacity of the adsorbent was calculated, which is listed in Table 1. As a comparison, Cu-SBA-15 (Cu content 6wt%) prepared by the impregnation method and Cu-BTC prepared by the ordinary hydrothermal method were also subjected to the sulfur adsorption of the above simulated oil, and the results are also listed in Table 1.

[0027] As can be seen from Table 1, the Cu / mesoporous organosilica nano...

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Abstract

The invention relates to a Cu / mesoporous organic silicon oxide nanotube desulfurization adsorbent and a preparation method thereof, and belongs to the technical field of oil refining and adsorption separation. The Cu / mesoporous organic silicon oxide nanotube desulfurization adsorbent is obtained by carrying out hydrolytic polycondensation on an organic silicon source containing a bipyridine groupunder the guidance of P123 and loading metal copper on the surface and the inner wall of a nanotube in an in-situ coordination loading manner. The adsorben overcomes the technical defects of low masstransfer diffusion efficiency, poor metal dispersibility, easy shedding and high price of traditional adsorbents, and has the advantages of simple preparation process and low cost. During adsorption desulfurization, the equilibrium adsorption capacity of the adsorbent to thiophene sulfides is obviously higher than that of Cu-SBA-15 and is 24% higher than that of Cu-BTC, and the adsorbent has a good application prospect in the field of deep adsorption desulfurization.

Description

technical field [0001] The invention relates to a Cu / mesoporous organic silicon oxide nanotube desulfurization adsorbent and a preparation method thereof, belonging to the technical field of oil refining and adsorption separation. Background technique [0002] The non-sulfurization of fuel oil such as gasoline and diesel oil is the development trend of the world today, and the removal of sulfur compounds in fuel oil is a major problem in the world today. Traditional hydrodesulfurization can effectively remove most of the simple organic sulfur compounds in gasoline, diesel and other fuel oils, such as ethanethiol, sulfide, disulfide, etc.; but for some complex sulfur compounds, such as Thiophene, benzothiophene, dibenzothiophene and its derivatives, such as 4-methyldibenzothiophene (4-MDBT), 4,6-dimethyldibenzothiophene (4,6-DMDBT) in octane It is difficult to effectively remove the alkane without loss, so that the purpose of deep desulfurization cannot be achieved. [0003...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C10G25/00
CPCB01J20/223B01J20/28007B01J20/3057C10G25/003C10G2300/202
Inventor 朱轶宁仲超徐卿
Owner 泰州九润环保科技有限公司
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