Preparation method of atom self-doped porous material

A porous material and self-doping technology, which is applied in the field of catalysis and new energy material preparation, can solve the problems of precursor pore system shrinkage, weaken pore wall, destroy original pore system, etc., achieve high specific surface utilization and eliminate mass transfer Cliff, to achieve the effect of coupled mass transfer

Inactive Publication Date: 2021-01-26
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] There are many dead and closed pores in the materials obtained by the above technology, which cannot be effectively used by guest molecules, reducing the mass transfer efficiency of the entire pore system, and it is difficult to meet the current application requirements of coupled mass transfer and engineering enhancement.
How to open up these low-utilization channels, improve their connectivity with the pore system, and optimize the entire pore system still faces many challenges in this technology
[0005] The above-mentioned technologies generally require the introduction of potassium hydroxide, sodium hydroxide, etc. as activators to be directly activated at high temperature. It is difficult to get through the dead and closed cells, and there is no effective support in the pore system. The pore walls are still dead after being greatly shrunk by heat. and closed pores, the precursor's own pore system shrinks or even fails; at the same time, the activator etches the precursor to create new channels. This process essentially weakens the pore wall and aggravates the shrinkage of its own pore system. reduced yield
Although the specific surface area can reach 3000 m 2 / g, but the connectivity of the pores is poor and the utilization rate is still low. Judging from the actual application effect, the relevant application performance does not increase proportionally with the increase of the specific surface area, and some performances even do not increase but decrease.

Method used

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  • Preparation method of atom self-doped porous material
  • Preparation method of atom self-doped porous material
  • Preparation method of atom self-doped porous material

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: In this embodiment, seaweed is selected as the precursor, ethanol aqueous solution is the polar solvent, water is the freeze-swell liquid, and sodium citrate is the filler. The specific steps are as follows:

[0032] First put 5 grams of seaweed into 60 ml of ethanol aqueous solution, seal it in a hydrothermal reactor, heat it at 110°C for 12 hours, then take it out and soak it in water, pack it in a ziplock bag, and freeze it in liquid nitrogen for 2 hours , remove and dry.

[0033] Then soak in saturated sodium citrate aqueous solution for 24 hours, and then dry at 60°C for 8 hours. Put the obtained laver into a corundum boat and put it into a tube furnace. Raise the temperature to 850°C, keep it for 1 hour, and then cool down to room temperature to take out the sample;

[0034] First wash with distilled water 3 times, then soak in distilled water for 24 hours; take out and dry at 110° C. for 6 hours to obtain a porous material.

[0035] From attached f...

Embodiment 2

[0040] Embodiment 2: In the present embodiment, a kind of method for preparing the porous material of self-doping atom, select polymer material ion-exchange resin as precursor, distilled water is polar solvent, water is freeze expansion liquid, calcium bicarbonate is Filling, the specific steps are as follows:

[0041] First put 10 grams of ion exchange resin into 60 ml of distilled water, seal it in a hydrothermal reactor, heat it at 120°C for 12 hours, then wash and soak it with distilled water, pack it in a ziplock bag, and freeze it in dry ice for 5 hours; remove and dry.

[0042] Then soak in saturated calcium bicarbonate aqueous solution for 2 hours at 0°C, then dry at 90°C for 1 hour to convert it into calcium carbonate, soak in calcium bicarbonate aqueous solution for 2 hours and dry again, put the filled ion exchange resin into corundum Put the boat into a tube furnace, use argon flow as the inert atmosphere, raise the temperature from room temperature to 800 °C at 2...

Embodiment 3

[0045] Embodiment 3: In this embodiment, a mixture of laver and phenolic resin polymer is selected as the precursor, water is used as the polar solvent, saline is used as the freeze expansion liquid, and sodium hydroxide and hydrochloric acid are used as fillers. Specific steps are as follows:

[0046] First put 10 grams of seaweed and 5 grams of phenolic resin polymer into 120 ml of distilled water at the same time, seal it in a hydrothermal reaction kettle and heat it at 120°C for 10 hours, then wash and soak it with distilled water, and pack it in a ziplock bag. Place it in minus 50°C ethylene glycol aqueous solution and freeze it for 4 hours, take it out and dry it.

[0047] Then soak in saturated sodium hydroxide aqueous solution at 20°C for 2 hours, then dry at 50°C for 8 hours, then put it into the reaction kettle and fumigate it with concentrated hydrochloric acid to convert it into sodium chloride, and then put the obtained precursor into the corundum boat, Put it in...

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Abstract

The invention belongs to the technical field of catalysis and new energy material preparation, and provides a preparation method of an atom self-doped porous material in order to solve the problems that dead holes and closed holes in a porous material prepared through a traditional method are not communicated smoothly, the active sites and the surface utilization rate are low, and rapid diffusionand transmission, rapid reaction and timely separation of guest molecules are inconvenient. The method comprises: soaking a precursor with a freezing expansion liquid, sealing, packaging, and freezing, wherein the volume of the precursor expands to crack the hole wall; drying to remove water, soaking with a filler solution, and drying to obtain a filled precursor; and carrying out heating treatment in an inert atmosphere, washing to remove the filler, and drying to obtain the atom self-doped porous material. According to the invention, heteroatoms contained in the porous material are retainedto realize autonomous doping, so that the porous material with spongy pore systems, high active site yield and high surface utilization rate is obtained; and the raw materials are wide, the process issimple, the green and environment-friendly effects are realized, the cost is low, the yield is high, the obtained material is mainly composed of micropores and mesopores, and the coupling mass transfer and reaction of guest molecules are convenient.

Description

technical field [0001] The invention belongs to the technical field of preparation of catalysis and new energy materials, and in particular relates to a preparation method of a self-doped atom porous material. Background technique [0002] Porous materials have large specific surface area and pore volume, adjustable pore size and surface functional groups. Among them, carbon materials have broad application prospects in the fields of catalysis, gas adsorption, lithium-ion batteries, and electrochemical energy storage. Hard templates and soft templates are mainly used. The template method is the method of carbonizing the organic precursor and removing the template. In recent years, carbon materials have also been prepared by pyrolysis of different biomass. [0003] Available technologies include: (1) Porous materials synthesized with resins as precursors. Related patent applications include melamine resin (2018102621620), phenolic resin (2013107478109, 2019101092889), ion exc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05C01B32/312C01B32/354B01J21/18B01J35/10
CPCC01B32/05C01B32/312C01B32/354B01J21/18B01J35/10
Inventor 薛春峰李晓红郝亚楠刘刚郝晓刚
Owner TAIYUAN UNIV OF TECH
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