A kind of hybrid material and preparation method thereof
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A technology of hybrid materials and applications, applied in the field of multi-component metal-organic hybrid materials and their preparation
Active Publication Date: 2021-07-09
FUSHUN RES INST OF PETROLEUM & PETROCHEMICALS SINOPEC CORP +1
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[0004] At present, domestic diesel adsorption desulfurization has just started, and it is still in the laboratory research stage
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Embodiment 1
[0025]According to the mass fraction of copper nitrate, nickel nitrate, zinc nitrate and aluminum nitrate in the solution is 13.7wt%, 4.1wt%, 3.7wt%, 3.2wt%, weigh the raw materials and add ternary solvent (water 3 wt%-ethanol 25 wt%) %-N,N-dimethylformamide 72wt%), after stirring at 50°C to dissolve it completely, adjust the pH value of the solution to 6; then, add the ternary complexing agent (2,5-dihydroxy - 9.0wt% terephthalic acid - 11.1wt% terephthalic acid - 79.9wt% trimesic acid) into the solution, stir rapidly to make it evenly mixed, then transfer the solution to a stainless steel lined with polytetrafluoroethylene In the reaction kettle, it was crystallized at 100°C for 16h. After the crystallization, the product was washed with acetone for 5 times, and suction-filtered, and the filter cake was molded and placed in an oven at 190° C. for 24 hours to dry. Prepare A1# sample, XRD spectrogram ( figure 1 ) at 2θ=6.5°, 9.3°, 11.4°, 13.2°, 14.5°, 16.5°, 17.5°, 19.1°, 20...
Embodiment 2
[0027] The preparation method is the same as in Example 1, except that the ternary solvent is water 1 wt%-ethanol 30 wt%-N,N-dimethylformamide 69wt%; the crystallization temperature is 120°C, and the crystallization time is 18h. The drying temperature is 160°C, and the drying time is 20h. Make A2# sample, the relative intensity I / I of XRD spectrogram, each diffraction peak 0 respectively listed in figure 1 and Table 1.
Embodiment 3
[0029] The preparation method is the same as in Example 1, except that the ternary solvent is water 5wt%-ethanol 10wt%-N,N-dimethylformamide 85wt%; the crystallization temperature is 140°C, the crystallization time is 12h, and the drying temperature is The temperature is 180°C, and the drying time is 16h. Make A3# sample, the relative intensity I / I of XRD spectrogram, each diffraction peak 0 respectively listed in figure 1 and Table 1.
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Abstract
The invention discloses a hybrid material and a preparation method thereof. The hybrid material is composed of Cu, Ni, Zn, Al multiple metals and a complexing agent, and the mass percentage of the Cu element in the hybrid material is calculated as CuO. 5%-40%, the mass percentage of the Ni element in the hybrid material is 1%-30% in terms of NiO, and the mass percentage of the Zn element in the hybrid material is 1%-30% in terms of ZnO, The Al element is Al 2 o 3 The mass percentage calculated in the hybrid material is 1%-30%, and the complex complexing agent is composed of 2,5-dihydroxy-terephthalic acid, terephthalic acid and 1,3,5-benzenetricarboxylic acid , the molar ratio of 2,5‑dihydroxy‑terephthalic acid, terephthalic acid and 1,3,5‑benzenetricarboxylic acid is (0.05‑0.15): (0.1‑0.5):1. The hybrid material uses a specific ternary solvent system and complex complexing agent to introduce Zn, Ni and Al into the Cu-containing hybrid material through isomorphic substitution, and retains the basic crystal structure of the Cu-containing hybrid material.
Description
technical field [0001] The invention relates to a hybrid material and a preparation method thereof, in particular to a multi-element metal-organic hybrid material and a preparation method thereof. Background technique [0002] In the 21st century, in view of the hazards of sulfur compounds after burning thiophene sulfides in diesel oil, and the society's high attention to the atmospheric environment and human health, countries around the world have formulated strict fuel emission standards and new regulations, and have taken measures to improve fuel quality. Taking European and American diesel as an example, developed countries such as Europe and the United States have imposed strict restrictions on the sulfur content in diesel, from 350ppm in Euro III in 2000 to 50ppm in Euro IV in 2005, and then to 2008. The latest Euro V standard sulfur content is less than 10ppm sulfur-free diesel. The U.S. Environmental Protection Agency (EPA) issued low-sulfur diesel regulations, req...
Claims
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