A kind of mcm-41 ordered mesoporous material and preparation method thereof

A MCM-41, mesoporous material technology, applied in chemical instruments and methods, molecular sieve compounds, inorganic chemistry, etc., can solve the cumbersome preparation process of mesoporous materials, restrict the development and application of mesoporous materials, energy-consuming mesoporous materials specific surface area and other problems, to achieve the effect of improving comprehensive utilization rate, concentrated pore size distribution, and good pore performance.

Active Publication Date: 2022-08-09
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Up to now, there have been research reports on the preparation of MCM-41 ordered mesoporous materials using iron tailings as raw materials by traditional low-temperature hydrothermal process, such as the MCM-41 mesoporous materials prepared by researchers from Northeastern University using iron tailings. The specific surface area is about 527m 2 / g(Honghao Yu, Xiangxin Xue, Dawei Huang.Synthesis of mesoporous silica materials(MCM-41) from iron oretailings.Materials Research Bulletin.44(2009),2112–2115.); MCM-41 mesoporous material was prepared as the raw material, the silicon source extraction rate was about 65% during the preparation process, and the specific surface area of ​​the prepared MCM-41 was only 882m 2 / g(Guang Yang, Yanxi Deng, Hao Ding, Zhixiang Lin, YuankaiShao, Yan Wang. A facile approach to synthesize MCM-41 mesoporous materials from mironore tailing: Influence of the synthesis conditions on structural properties. Applied Clay Science. 111(2015). 61 ; There are two main problems in the research on the preparation of mesoporous materials by obtaining silicon sources from iron tailings. The specific surface area of ​​porous materials is low, which seriously restricts the development and application of mesoporous materials prepared from iron tailings

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  • A kind of mcm-41 ordered mesoporous material and preparation method thereof
  • A kind of mcm-41 ordered mesoporous material and preparation method thereof
  • A kind of mcm-41 ordered mesoporous material and preparation method thereof

Examples

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Embodiment 1

[0036] (1) Using iron tailings as raw materials, the chemical composition analysis of iron tailings is shown in Table 1, and the phase composition is shown in the appendix figure 1As shown, 8 mol / L hydrochloric acid solution is the leaching agent. According to the ratio of solid-liquid ratio of 1:1.5 (g / mL), iron tailings and hydrochloric acid aqueous solution are mixed, and the turbid liquid is obtained after magnetic stirring at 150 ° C for 3 hours. , after cooling it to room temperature, carry out suction filtration, wash the solid product obtained by suction filtration with deionized water to neutrality (same pH as deionized water), and dry at a temperature of 60 ° C to obtain acid-insoluble slag, acid-insoluble slag The chemical composition analysis is shown in Table 1.

[0037] (2) using the acid-insoluble residue obtained in step (1) as a raw material, the mass ratio of the acid-insoluble residue and sodium hydroxide is 1:2.2 (g / g), and the solid matter (acid-insoluble ...

Embodiment 2

[0044] (1) Using iron tailings as raw materials, 4 mol / L sulfuric acid solution as leaching agent, taking iron tailings and hydrochloric acid aqueous solution according to the ratio of solid-liquid ratio of 1:3 (g / mL) and mixing, at a temperature of 100 ° C After magnetic stirring for 6 hours, a turbid liquid was obtained, which was cooled to room temperature and then subjected to suction filtration. The solid product obtained by suction filtration was washed with deionized water until neutral (the same pH as deionized water), and dried at a temperature of 60 ° C to obtain Acid insoluble residue.

[0045] (2) using the acid-insoluble residue obtained in step (1) as a raw material, the mass ratio of the acid-insoluble residue and sodium hydroxide is 1:2.2 (g / g), and the solid matter (acid-insoluble residue and sodium hydroxide) and deionized The solid-to-liquid ratio of water is 1:2 (g / mL), mix acid-insoluble residue, sodium hydroxide and deionized water, heat it with water at ...

Embodiment 3

[0049] (1) Using iron tailings as raw materials, 2 mol / L hydrochloric acid solution as leaching agent, taking iron tailings and hydrochloric acid aqueous solution according to the ratio of solid-liquid ratio of 1:6 (g / mL) and mixing, at a temperature of 120 ° C After magnetic stirring for 5 hours, a turbid liquid was obtained, which was cooled to room temperature and then subjected to suction filtration. The solid product obtained by suction filtration was washed with deionized water until neutral (same pH as deionized water), and dried at a temperature of 60 ° C to obtain Acid insoluble residue.

[0050] (2) using the acid-insoluble residue obtained in step (1) as a raw material, the mass ratio of the acid-insoluble residue and sodium hydroxide is 1:2.2 (g / g), and the solid matter (acid-insoluble residue and sodium hydroxide) and deionized The solid-to-liquid ratio of water is 1:2 (g / mL), mix acid-insoluble residue, sodium hydroxide and deionized water, heat it with water at ...

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Abstract

The invention provides an MCM-41 ordered mesoporous material and a preparation method thereof. The preparation method comprises using iron tailings as a raw material, leaching with an inorganic strong acid solution, performing solid-liquid separation, washing and drying after heating and stirring to obtain acid-insoluble slag; mix acid-insoluble slag and alkali metal hydroxide in a mass ratio of 1:1.4-2.4, add deionized water, carry out hydrothermal reaction, and then separate solid-liquid to obtain silicon source; combine silicon source with surfactant , deionized water and ethanol are mixed, the pH value of the mixed solution is adjusted, the gel reaction is carried out by stirring at room temperature, and then washed, dried and ground to obtain the precursor; the precursor is calcined at 540 ~ 850 ° C for 5 ~ 9h, the MCM-41 ordered mesoporous material was obtained. The method has the advantages of simple operation, high silicon source extraction rate, and improved comprehensive utilization rate of iron tailings; the obtained mesoporous material has regular and orderly pore structure, adjustable pore size and high specific surface area.

Description

technical field [0001] The invention relates to the technical field of functional materials, in particular to an MCM-41 ordered mesoporous material and a preparation method thereof. Background technique [0002] Ordered mesoporous material is a new type of nanostructured material that emerged rapidly in the 1990s. It has been highly valued by the international physics, chemistry and materials academic circles since its birth, and has rapidly developed into one of the interdisciplinary research hotspots. The synthesis of mesoporous materials began as early as 1971, but it was not until 1992 that Mobil reported the synthesis of M41S series of mesoporous materials. MCM-41 mesoporous material is a kind of M41S series, the pores are arranged in hexagonal order, the size is uniform, the pore size can be continuously adjusted in the range of 2-10nm, the specific surface area is large, and it has excellent ion exchange, catalysis and adsorption performance. It has a wide range of u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/00C01B39/00
CPCC01B37/00C01B39/00C01P2006/12C01P2006/14Y02E60/10
Inventor 杨华明路畅傅梁杰张毅欧阳静刘赛男陈洪运唐爱东
Owner CENT SOUTH UNIV
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