Macroporous hybrid material and preparation method thereof

A hybrid material and pore volume technology, applied in chemical instruments and methods, inorganic chemistry, refined hydrocarbon oil, etc., to achieve high desulfurization rate, improve diffusion, and improve adsorption capacity.

Active Publication Date: 2019-05-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, domestic diesel adsorption desulfurization ha

Method used

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  • Macroporous hybrid material and preparation method thereof
  • Macroporous hybrid material and preparation method thereof
  • Macroporous hybrid material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 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; secondly, add 0.23wt% cetyl trimethyl bromide Ammonium was used as a template, and 0.11wt% of 3-mercaptopropyltrimethoxysilane was added as a mercapto modifier, and mixed evenly; then, a ternary complexing agent (2,5-dihydroxy-terephthalic acid 9.0 wt%-terephthalic acid 11.1wt%-trimellitic acid 79.9wt%) was added to the solution, stirred rapidly to make it evenly mixed, and then the solution was transferred to a stainless steel reaction kettle lined with polytetrafluoroethylene, at 100 Crystallization at ℃ for 16h. After the crystallization, the product was washed with acetone for 5 times, and suction-filtered, and the fil...

Embodiment 2

[0033] 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 template is sodium dodecylbenzenesulfonate, The dosage is 0.42%; the thiol modifier is mercaptoacetic acid, the dosage is 0.21%; the crystallization temperature is 120°C, the crystallization time is 18h, the drying temperature is 160°C, and the drying time is 20h. Prepared A2# sample with a pore volume of 0.817 cm 3 / g, XRD spectrum, the relative intensity I / I of each diffraction peak 0 , and the average pore size distribution are listed in figure 1 , Table 1 and image 3 middle.

Embodiment 3

[0035] 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 template agent is dodecylamine, and the dosage is 0.89%; The active agent is methyl thioglycolate, the dosage is 0.45%; the crystallization temperature is 140°C, the crystallization time is 12h, the drying temperature is 180°C, and the drying time is 16h. Prepare A3# sample, the pore volume is 0.810cm 3 / g, XRD spectrum, the relative intensity I / I of each diffraction peak 0 , and the average pore size distribution are listed in figure 1 , Table 1 and image 3 middle.

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Abstract

The invention discloses a hybrid material. The pore volume of the hybrid material is 0.3-1.2 cm<3>/g, and the hybrid material consists of Cu, Ni, Zn and Al multielement metals and a composite complexing agent; the mass percentage of the Cu element in the hybrid material, calculated as CuO, is 5-40%, the mass percentage of the Ni element in the hybrid material, calculated as NiO, is 1-30%, the masspercentage of the Zn element in the hybrid material, calculated as ZnO, is 1-30%, the mass percentage of the Al element in the hybrid material, calculated as Al2O3, is 1-30%, the balance is the composite complexing agent, and the composite complexing agent comprises 2,5-dihydroxy-terephthalic acid, terephthalic acid and 1,3,5-benzene tricarboxylic acid. A preparation method of the hybrid materialcomprises the following step: introducing Zn, Ni and Al into a Cu-containing hybrid material by means of isomorphous substitution. The hybrid material has excellent desulfurization performance, and the desulfurization rate reaches 99% or above.

Description

technical field [0001] The invention relates to a macroporous hybrid material and a preparation method thereof, in particular to a multi-element metal macroporous 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...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30B01J20/28C10G25/00
Inventor 张信伟李杰王海洋尹泽群刘全杰
Owner CHINA PETROLEUM & CHEM CORP
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