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Resol-assisted synthetic large aperture ordered mesopore metallic oxide material and preparation method of material

A phenolic resin prepolymerization, large pore size technology, applied in chemical instruments and methods, tin oxide, tungsten oxide/tungsten hydroxide, etc., can solve problems such as narrow pore size distribution

Inactive Publication Date: 2015-12-09
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(B.Z.Tian, ​​X.Y.Liu, B.Tu, C.Z.Yu, J.Fan, L.M.Wang, S.H.Xie, G.D.Stucky, D.Y.Zhao, Nat.Mater.2003, 2, 159-163; B.Z.Tian, ​​X.Y.Liu, B.Tu, C.Z.Yu, J.Fan, L.M.Wang, S.H.Xie, G.D.Stucky, D.Y.Zhao, Nat.Mater.2003, 2, 159-163; W.Dong, Y.Sun, C.W.Lee, W.Hua, X.Lu, Y. Shi, S. Zhang, J. Chen and D. Zhao, J. Am. Chem. Soc. 2007, 129, 13894-13904; T. Yu, Y. Deng, L. Wang, R. Liu, L. Zhang, B. TuandD.Zhao,Adv.Mater.2007,19,2301-2306.K.Niesz,P.D.Yang,G.A.Somorjai,Chem.Commun.2005,1986-1987.Q.Yuan,A.-X.Yin,C.Luo , L.-D.Sun, Y.-W.Zhang, W.-T.Duan, H.-C.Liu, C.-H.Yan, J.Am.Chem.Soc.2008, 130, 3465- 3472.) Due to the limitation of the chain length of the hydrophilic segment and the hydrophobic segment of the surfactant, the pore diameter and wall thickness of the synthesized mesoporous metal oxide material are generally not more than 8nm, and when the high temperature roasting removes the template agent or affects the resulting mesoporous During the high-temperature crystallization process of porous materials, the framework loses effective support due to the removal of the template agent, and the high-temperature calcination causes the material framework to shrink and reorganize, which will eventually lead to the collapse of the entire mesoporous framework.

Method used

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  • Resol-assisted synthetic large aperture ordered mesopore metallic oxide material and preparation method of material
  • Resol-assisted synthetic large aperture ordered mesopore metallic oxide material and preparation method of material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Synthesis of mesoporous tungsten oxide material with high specific surface area

[0023] 0.10g PEO-b-PS (M n =18500gmol -1 ) into 5.0g THF solution, stirred to obtain a uniform solution (2.0wt%), added 0.3g concentrated hydrochloric acid (37wt%) and 0.5g resol THF solution (20wt%) and stirred evenly, then added 0.3gWCl 6 , stirred for 2h, the solution gradually changed from orange to ink blue.

[0024] The solution was transferred to a petri dish and volatilized at room temperature for 60 minutes to turn dark blue. The petri dish was transferred to an oven at 70°C to further volatilize the solvent and cured for 48 hours to obtain a blue transparent composite film. The composite film was scraped off from the Petri dish to obtain a blue powder.

[0025] Put the newly prepared sample in a tube furnace, and bake it at 350°C for 3h under a nitrogen atmosphere, with a heating rate of 1.0°C / min, to obtain gray-black WO 3 / C Composite. Then, the obtained sample ...

Embodiment 2

[0026] Example 2: Synthesis of mesoporous tin oxide material with high specific surface area

[0027] 0.10g PEO-b-PMMA (M n =24700gmol -1 ) was dissolved in 5.0g of THF solution, 0.4g of resol in THF solution (10wt%) was added, and after stirring for 30min, a uniform solution (2.0wt%) was obtained. 0.6g of SnCl 4 Dissolve in 0.9g of acetylacetone (AcAc) solution, stir for 30min, then mix the two solutions, add 0.6g of concentrated hydrochloric acid (37wt%), stir for 30min, and obtain a light red transparent solution.

[0028] The solution was transferred to a petri dish, and after 10 minutes of volatilization at room temperature, the petri dish was transferred to a 40°C oven to further volatilize the solvent for 24 hours, and then the temperature of the oven was raised to 100°C to cure for 24 hours to obtain a light yellow transparent composite film. The film was scraped off the Petri dish to give a pale yellow powder.

[0029] Put the as-made sample in a tube furnace and ...

Embodiment 3

[0030] Example 3: Synthesis of mesoporous niobium oxide material with high specific surface area

[0031] 0.24gNbCl 5 Dissolve in 2.16gTHF, and then add a few drops of nitric acid to promote its dissolution. Next, add 0.6gresol THF solution (mass fraction is 30%) and 5.0gPEO-b-PS (M n =32500gmol -1 ) THF solution (mass fraction is 2%, 0.1gPEO-b-PS dissolved in 4.9gTHF). After mixing evenly, 0.25 g of nitric acid and 5 g of THF were added, and magnetically stirred for one hour to obtain an orange solution.

[0032] The solution was transferred to a Petri dish, and after volatilization at room temperature for 2 hours, the Petri dish was transferred to an oven at 50°C for further volatilization of the solvent for 12 hours, and then the temperature of the oven was raised to 150°C for curing for 48 hours to obtain an orange transparent composite film. The membrane was scraped from the Petri dish and ground to an orange powder.

[0033] The freshly prepared samples were placed ...

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Abstract

The invention belongs to the technical field of nano porous materials, in particular to a resol-assisted synthetic large aperture ordered mesopore metallic oxide material and a preparation method of the material. According to the material and the preparation method thereof, an amphiphilic block copolymer (PEO-b-PS and PEO-b-PMMA) with large molecular weight hydrophobic segments is taken as a template agent, the principle of assisted self-assembly of resol is utilized, and in a solvent evaporation process, the resol fixes a metal precursor to a hydrophilic end of the template agent, the self-assembly is induced through solvent evaporation, so as to enable the template agent and a mesoporous material precursor to react to form microphase separation, and obtain an ordered mesostructure; after using large molecular weight hydrophobic block to form a large hydrophobic area, and removing the template agent, the large aperture ordered mesopore metallic oxide material is obtained. The synthetic mesoporous material has a super large aperture, the shape of the pore channel of the material is spherical, the mesoporous of the material is orderly arranged, and the material has a bimodal mesoporous structure and a super high specific surface area; the method is simple, the raw material is easy to obtain and the material is suitable for enlarged production.

Description

Technical field [0001] The present invention is a technology field of nano -porous materials, which involves a large -pore -diameter -oriented medium metal oxide material and their preparation methods. Background technique [0002] In recent years, metal oxide materials and composite materials have been widely used in the aspects of optical electron transmission, optical guidance, sensing, photocatalytic dyeing solar cells, battery packs, and water purification.Essence(A.hagfeldt, j.tang, y.y.wu, e.w.mcfarland, g.d.stucky, chem.commun.2004,1670-1671; T.kawahara, y.konishi, h.tada, n.tohge, j.nishii, s.18,2579-2582; M.zukalova, A.ZUKAL, L.kavan, M.K.NAZEERUDDIN, P.Liska, M.Gratzel, Nanolett.2005, 5,1789-1792. As we all know, the nature of metal oxide materials and composite materialsTo a large extent, they depend on their surface properties and high ratio.) Especially the crystallization level of metal oxide materials has an important impact on its application. Because the orderly...

Claims

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Application Information

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IPC IPC(8): C01G41/02C01G19/02C01G33/00B82Y40/00
Inventor 邓勇辉任元李宇慧纪广慧
Owner FUDAN UNIV
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