Defective metal-organic framework desulfurization adsorbent and preparation method and application thereof

Abstract

The invention relates to a defective metal-organic framework desulfurization adsorbent and a preparation method and application thereof. The preparation method comprises the following steps: dissolving trimesic acid and 5-hydroxyisophthalic acid in a solvent, and carrying out ultrasonic treatment to obtain a mixed solution I; uniformly mixing the mixed solution I with copper nitrate trihydrate to obtain a mixed solution II; and then carrying out microwave-assisted synthesis on the mixed solution II to obtain the defective metal-organic framework desulfurization adsorbent. Hydroxyisophthalic acid is introduced in the synthesis process to modify synthesized HKUST-1, microwave-assisted synthesis is adopted to rapidly prepare the defective-metal organic framework, the defective metal organic framework can be rapidly synthesized through the method, meanwhile, the defective metal organic framework has the high crystallinity and the micro-medium hierarchical pore structure, the whole preparation process saves energy consumption and is environmentally friendly, high adsorption sulfur capacity is kept in fixed bed adsorption, and the preparation method is suitable for high-efficiency removal of sulfides in oil products.

Description

technical field

[0001] The invention relates to the field of adsorption purification, in particular to a defect metal-organic framework desulfurization adsorbent and its preparation method and application. Background technique

[0002] Globally, natural gas and oil still dominate the world's energy. Although the world's energy is transitioning to clean energy, oil continues to play an irreplaceable role. The sulfur content of sulfide in crude oil is between 0.05-6wt%, and the main components of sulfide are mercaptan, sulfide and thiophene sulfide (thiophene, benzothiophene, dibenzothiophene), etc., the above-mentioned sulfide-containing During the transportation and use of fuel, it will corrode pipelines, increase equipment maintenance costs, and corrode engines. Also, when sulfur-containing fuels are burned, they emit SO into the atmosphere X , forming acid rain, polluting the environment and endangering human health. In recent years, with the continuous enhancement of p...

Examples

Embodiment 1

[0032] Trimellitic acid and 5-hydroxyisophthalic acid were mixed and dissolved in 15 mL ethanol solution at a ratio of 1:9, and ultrasonicated at room temperature for 15 min. Dissolve 2g of copper nitrate trihydrate in 15mL of deionized water, mix the two solutions evenly and place them in a polytetrafluoroethylene lining, place them in a microwave hydrothermal synthesizer, set the heating program to 5°C min -1 The heating rate is heated from 25°C to 100°C and kept for 15 minutes, then at 2°C min -1 The heating rate is heated to 120°C for 30min, and the power is 700W. After the reaction is completed, cool to room temperature, filter and wash with absolute ethanol and DMF solution several times, dry, extrude and grind to obtain defective metal-organic framework desulfurization adsorption agent.

[0033] On the fixed bed adsorption desulfurization device, use the adsorbent of this embodiment to evaluate the desulfurization of oil products. Use n-octane to configure simulated g...

Embodiment 2

[0035] Trimellitic acid and 5-hydroxyisophthalic acid were mixed and dissolved in 15 mL ethanol solution at a ratio of 1:4, and ultrasonicated at room temperature for 15 min. Dissolve 2g of copper nitrate trihydrate in 15mL of deionized water, mix the two solutions evenly and place them in a polytetrafluoroethylene lining, place them in a microwave hydrothermal synthesizer, set the heating program to 5°C min -1 The heating rate is heated from 25°C to 100°C and kept for 15 minutes, then at 2°C min -1 The heating rate is heated to 120°C for 30min, and the power is 700W. After the reaction is completed, cool to room temperature, filter and wash with absolute ethanol and DMF solution several times, dry, extrude and grind to obtain defective metal-organic framework desulfurization adsorption agent.

[0036]On the fixed bed adsorption desulfurization device, use the adsorbent of this embodiment to evaluate the desulfurization of oil products. Use n-octane to configure simulated ga...

Embodiment 3

[0038] Trimellitic acid and 5-hydroxyisophthalic acid were mixed and dissolved in 15 mL ethanol solution at a ratio of 3:7, and ultrasonicated for 15 min at room temperature. Dissolve 2g of copper nitrate trihydrate in 15mL of deionized water, mix the two solutions evenly and place them in a polytetrafluoroethylene lining, place them in a microwave hydrothermal synthesizer, set the heating program to 5°C min -1 The heating rate is heated from 25°C to 100°C and kept for 15 minutes, then at 2°C min -1 The heating rate is heated to 120°C for 30min, and the power is 700W. After the reaction is completed, cool to room temperature, filter and wash with absolute ethanol and DMF solution several times, dry, extrude and grind to obtain defective metal-organic framework desulfurization adsorption agent.

[0039] On the fixed bed adsorption desulfurization device, use the adsorbent of this embodiment to evaluate the desulfurization of oil products. Use n-octane to configure simulated g...

technical field

[0001] The invention relates to the field of adsorption purification, in particular to a defect metal-organic framework desulfurization adsorbent and its preparation method and application. Background technique

[0002] Globally, natural gas and oil still dominate the world's energy. Although the world's energy is transitioning to clean energy, oil continues to play an irreplaceable role. The sulfur content of sulfide in crude oil is between 0.05-6wt%, and the main components of sulfide are mercaptan, sulfide and thiophene sulfide (thiophene, benzothiophene, dibenzothiophene), etc., the above-mentioned sulfide-containing During the transportation and use of fuel, it will corrode pipelines, increase equipment maintenance costs, and corrode engines. Also, when sulfur-containing fuels are burned, they emit SO into the atmosphere X , forming acid rain, polluting the environment and endangering human health. In recent years, with the continuous enhancement of p...

Examples

Embodiment 1

[0032] Trimellitic acid and 5-hydroxyisophthalic acid were mixed and dissolved in 15 mL ethanol solution at a ratio of 1:9, and ultrasonicated at room temperature for 15 min. Dissolve 2g of copper nitrate trihydrate in 15mL of deionized water, mix the two solutions evenly and place them in a polytetrafluoroethylene lining, place them in a microwave hydrothermal synthesizer, set the heating program to 5°C min -1 The heating rate is heated from 25°C to 100°C and kept for 15 minutes, then at 2°C min -1 The heating rate is heated to 120°C for 30min, and the power is 700W. After the reaction is completed, cool to room temperature, filter and wash with absolute ethanol and DMF solution several times, dry, extrude and grind to obtain defective metal-organic framework desulfurization adsorption agent.

[0033] On the fixed bed adsorption desulfurization device, use the adsorbent of this embodiment to evaluate the desulfurization of oil products. Use n-octane to configure simulated g...

Embodiment 2

[0035] Trimellitic acid and 5-hydroxyisophthalic acid were mixed and dissolved in 15 mL ethanol solution at a ratio of 1:4, and ultrasonicated at room temperature for 15 min. Dissolve 2g of copper nitrate trihydrate in 15mL of deionized water, mix the two solutions evenly and place them in a polytetrafluoroethylene lining, place them in a microwave hydrothermal synthesizer, set the heating program to 5°C min -1 The heating rate is heated from 25°C to 100°C and kept for 15 minutes, then at 2°C min -1 The heating rate is heated to 120°C for 30min, and the power is 700W. After the reaction is completed, cool to room temperature, filter and wash with absolute ethanol and DMF solution several times, dry, extrude and grind to obtain defective metal-organic framework desulfurization adsorption agent.

[0036]On the fixed bed adsorption desulfurization device, use the adsorbent of this embodiment to evaluate the desulfurization of oil products. Use n-octane to configure simulated ga...

Embodiment 3

[0038] Trimellitic acid and 5-hydroxyisophthalic acid were mixed and dissolved in 15 mL ethanol solution at a ratio of 3:7, and ultrasonicated for 15 min at room temperature. Dissolve 2g of copper nitrate trihydrate in 15mL of deionized water, mix the two solutions evenly and place them in a polytetrafluoroethylene lining, place them in a microwave hydrothermal synthesizer, set the heating program to 5°C min -1 The heating rate is heated from 25°C to 100°C and kept for 15 minutes, then at 2°C min -1 The heating rate is heated to 120°C for 30min, and the power is 700W. After the reaction is completed, cool to room temperature, filter and wash with absolute ethanol and DMF solution several times, dry, extrude and grind to obtain defective metal-organic framework desulfurization adsorption agent.

[0039] On the fixed bed adsorption desulfurization device, use the adsorbent of this embodiment to evaluate the desulfurization of oil products. Use n-octane to configure simulated g...

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