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OMS-2 type composite material with mixed crystal phase as well as preparation method and application of OMS-2 type composite material

A technology of OMS-2 and composite materials, applied in the field of nanomaterials and catalytic materials, can solve the problems of insufficient surface chemistry, singleness, and limited catalytic activity of materials, achieve excellent catalytic oxidation activity, simple operation method, and good repeatability Effect

Active Publication Date: 2019-07-23
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although, in recent years, many literatures and patents have reported the controllable preparation of OMS-2 materials, but the OMS-2 materials prepared by these methods only have a single manganese crystal phase, which limits the OMS to a certain extent. -2 The types of adsorption, activation, and dissociation active sites on the surface of the material, and the chemical degree of the surface of the material is not rich enough, which limits the improvement of the catalytic activity of the OMS-2 material in the field of heterogeneous catalytic oxidation
However, using a simple one-step reflux method, through the use of specific additives, OMS-2 type materials containing mixed crystalline phases, especially those containing Mn 2 o 3 ·H 2 The OMS-2 type composite material with O / OMS-2 two-phase crystalline phase has not been reported yet

Method used

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  • OMS-2 type composite material with mixed crystal phase as well as preparation method and application of OMS-2 type composite material
  • OMS-2 type composite material with mixed crystal phase as well as preparation method and application of OMS-2 type composite material
  • OMS-2 type composite material with mixed crystal phase as well as preparation method and application of OMS-2 type composite material

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preparation example Construction

[0024] One aspect of the embodiments of the present invention provides a method for preparing an OMS-2 type composite material with a mixed crystalline phase, which includes:

[0025] Reacting the uniformly mixed reaction system containing potassium permanganate, divalent manganese salt, additives and nitric acid at 25-100°C for 5-24 hours to obtain an OMS-2 type composite material with mixed crystalline phases;

[0026] Wherein, the additive includes any one or a combination of two or more of tungstic acid, sodium phosphotungstate, sodium tungstate, sodium metatungstate, sodium phosphate, potassium phosphate, potassium dihydrogen phosphate and disodium hydrogen phosphate.

[0027] In some typical embodiments, the preparation method specifically includes: uniformly mixing an aqueous potassium permanganate solution with an aqueous solution containing divalent manganese salts, additives and nitric acid at 25-50°C to form the uniform mixing reaction system.

[0028] In some embo...

Embodiment 1

[0045] (1) At room temperature, dissolve 0.5mol manganese sulfate, 0.3mmol tungstic acid and 20mL nitric acid in 400mL distilled water, add 1L distilled aqueous solution containing 0.3mol potassium permanganate dropwise into the above mixed solution, stir and mix evenly, and then Stir and react at 80°C for 20 hours, filter, wash with distilled water, and dry at 120°C for 5 hours to obtain an OMS-2 composite material. Material phase identification: the XRD spectrum of the OMS-2 type composite material obtained in this embodiment is as follows figure 1 shown.

[0046] (2) Catalytic application

[0047] The selective oxidation of p-chlorobenzyl alcohol to p-chlorobenzaldehyde was used to consider the catalytic oxidation activity of the OMS-2 type composite material prepared in this example. Add 2mmol of p-chlorobenzyl alcohol, 50mg of OMS-2 type composite material as a catalyst, 3mL of dimethyl carbonate in the reaction bottle, stir and react at 90°C for 18 hours in an oxygen a...

Embodiment 2

[0049] (1) At room temperature, dissolve 0.6mol manganese nitrate, 3mmol sodium tungstate and 30mL nitric acid in 300mL distilled water, add 1L distilled aqueous solution containing 0.4mol potassium permanganate dropwise into the above mixed solution, stir and mix evenly, and then Stir and react at 100°C for 24 hours, filter, wash with distilled water, and dry at 100°C for 12 hours to obtain an OMS-2 composite material. The XRD spectrum pattern of the OMS-2 type composite material that present embodiment obtains is as figure 2 shown.

[0050] (2) Catalytic application

[0051] The selective oxidation of benzyl alcohol to benzaldehyde was used to evaluate the catalytic oxidation activity of the OMS-2 type composite material prepared in this example. Add 0.02mol benzyl alcohol, 0.6g OMS-2 type composite material as catalyst, 50mL dimethyl carbonate in the reaction flask, stir and react at 90°C for 20 hours in an oxygen atmosphere, filter and remove the solid catalyst after th...

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Abstract

The invention discloses an OMS-2 type composite material with a mixed crystal phase as well as a preparation method and application of the OMS-2 type composite material. The preparation method comprises the following steps: enabling a uniformly mixed reaction system, which contains potassium permanganate, a divalent manganese salt, an additive and nitric acid, to react for 5-24h at 25-100 DEG C toobtain the OMS-2 type composite material with the mixed crystal phase; wherein the additive comprises any one kind or more than two kinds of combinations of tungstic acid, sodium phosphotungstate, sodium tungstate, sodium metatungstate, sodium phosphate, potassium phosphate, monopotassium phosphate and disodium hydrogen phosphate. The operation method of the OMS-2 type composite material is simple, high in yield and good in repeatability, the obtained OMS-2 type composite material has a two-phase crystal phase of Mn2O3.H2O / OMS-2 as well as substantially improved specific surface area and oxidative activity, and the OMS-2 type composite material has excellent catalytic oxidation activity in the selective catalytic oxidation application of organic compounds such as benzyl alcohol compounds,amine compounds, saturated nitrogen heterocycles, thiols and thioethers.

Description

technical field [0001] The invention relates to an OMS-2 catalytic material, in particular to an OMS-2 composite catalytic material with a mixed crystal phase, belonging to the field of nanometer materials and catalytic materials. Background technique [0002] Manganese oxides have various oxidation states, such as MnO, MnO 2 , Mn 2 o 3 and Mn 3 o 4 etc., where MnO 2 It has various crystal forms and bulk phase structures such as α, β, γ, δ, etc., making it one of the inorganic mineral materials with great application potential. Manganese dioxide octahedral molecular sieve OMS-2 as a synthetic one-dimensional tunnel structure α-MnO 2 Nanomaterials, consisting of 2x2 coedged MnO 6 Composed of structural units, the pore size is 0.46nm. OMS-2 has mild surface acidity and alkalinity, rich pore structure and lattice oxygen, good structural stability and ion exchange, so it exhibits excellent electrical conductivity, adsorption, ion exchange and catalytic properties. In pa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/34B01J37/10B01J35/10C07D217/02C07D209/08C07C315/02C07C317/22C07C319/14C07C321/30C07C209/68C07C211/28C07C45/38C07C47/54C07C47/55
CPCB01J23/34B01J37/10C07D217/02C07D209/08C07C315/02C07C319/14C07C209/68C07C45/38B01J35/615C07C317/22C07C321/30C07C211/28C07C47/54C07C47/55
Inventor 孟旭赵培庆陈革新苟明霞毕秀茹
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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