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Coordinated molybdenum-oxygen heterocyclic catalyst, and preparation method and application thereof

A technology of catalyst and oxygen heterocycle, applied in the field of coordination molybdenum oxygen heterocycle catalyst and its preparation, can solve the problem of low selectivity of propylene oxide

Active Publication Date: 2021-09-14
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The primary purpose of the present invention is to overcome the problem of low selectivity of propylene oxide in the above-mentioned prior art, and provide a coordination molybdenum-oxygen heterocyclic catalyst, which has higher propylene oxide selectivity when the catalyst is used for the preparation of propylene oxide, At the same time, it can efficiently utilize tert-butyl hydroperoxide

Method used

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  • Coordinated molybdenum-oxygen heterocyclic catalyst, and preparation method and application thereof
  • Coordinated molybdenum-oxygen heterocyclic catalyst, and preparation method and application thereof
  • Coordinated molybdenum-oxygen heterocyclic catalyst, and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] One coordinating oxetane molybdenum catalyst, the following chemical structure:

[0032] Where L 1 for

[0033] The method for preparing a coordination oxetane molybdenum catalyst, comprising the steps of:

[0034] . S1 3.5g of molybdenum trioxide was added to the round bottom flask, was slowly added under stirring to 10ml 30% hydrogen peroxide solution, stirred at reflux for 10h at 50 deg.] C to form a clear solution A; ethyl acetate formulation taken 2mol a solution B;

[0035] S2. Under stirring, solution A to solution B obtained was filtered solution C, the reaction solution was refluxed for 3h C continues placed in the refrigerator at 8 ℃ refrigerator 5d 50 ℃, until crystals precipitated crystals were filtered, washed drying, to give ligand oxetanyl molybdenum catalyst MoOO · EAC.

Embodiment 2

[0037] One coordinating oxetane molybdenum catalyst, the following chemical structure:

[0038] Where L 1 for

[0039] The method for preparing a coordination oxetane molybdenum catalyst, comprising the steps of:

[0040] . S1 5g of molybdenum trioxide was added to the round bottom flask, was slowly added under stirring to 20ml 30% hydrogen peroxide solution, stirred at reflux for 15h at 40 ℃ A to form a clear solution; take 3mol N, N- two dimethylformamide formulated as a solution B;

[0041] S2. Under stirring, solution A to solution B obtained was filtered solution C, the reaction solution was refluxed for 5h C continues placed in the refrigerator at 2 ℃ refrigerated 6d 40 ℃, until crystals precipitated crystals were filtered, washed drying, to give ligand oxetanyl molybdenum catalyst MoOO · DMF.

Embodiment 3

[0043] One coordinating oxetane molybdenum catalyst, the following chemical structure:

[0044] Where L 1 for

[0045] The method for preparing a coordination oxetane molybdenum catalyst, comprising the steps of:

[0046] . S1 6g molybdenum trioxide was added to the round bottom flask, was slowly added under stirring to 12ml 30% hydrogen peroxide solution, stirred at reflux for 10h at 45 ℃ A to form a clear solution; take 2mol 4- dimethylaminopyridine pyridine formulated as a solution B;

[0047] S2. Under stirring, solution A to solution B obtained was filtered solution C, the reaction solution was continued to reflux for 4h C was placed in a refrigerator at 5 ℃ refrigerated 2d 45 ℃, until crystals precipitated crystals were filtered, washed drying, to give ligand oxetanyl molybdenum catalyst MoOO · DMAP.

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Abstract

The invention discloses a coordinated molybdenum-oxygen heterocyclic catalyst, and a preparation method and application thereof. The chemical structural formula of the catalyst is shown in the specification, and L in the formula is selected from one of formulas also shown in the specification. The preparation method comprises the following steps: S1, adding molybdenum trioxide into hydrogen peroxide, refluxing and stirring to obtain a solution A, and adding a micromolecular N / O ligand into methylbenzene to obtain a solution B; wherein the micromolecular N / O ligand is selected from one of ethyl acetate, N, N-dimethylformamide or 4-dimethylaminopyridine; and S2, filtering the solution A into the solution B to obtain a solution C, carrying out reflux reaction on the solution C for 1-5 hours, and refrigerating at 2-8 DEG C to obtain a crystal, namely the coordinated molybdenum-oxygen heterocyclic catalyst. The coordinated molybdenum-oxygen heterocyclic catalyst has high epoxypropane selectivity and tert-butyl hydroperoxide utilization rate when being used for preparing epoxypropane from propylene, and can be used for efficiently preparing epoxypropane from propylene.

Description

Technical field [0001] The present invention relates to the technical field of preparing materials, and more particularly, to a coordinate oxygen heterocycle catalyst and preparation method and application of molybdenum. Background technique [0002] Propylene oxide (PO) is an important intermediate in the production of polyether, polyurethane, dimethyl carbonate, nonionic surfactants, emulsifiers, demulsifiers and other chemical products, the annual output of nearly 10 million tons, has broad application prospects. PO industrially prepared mainly chlorohydrin method, a direct oxidation method and the co-oxidation method. Chlorohydrin due to severe corrosion and contamination problems are out technique. Direct oxidation of hydrogen peroxide and oxygen gas into oxidation method, a hydrogen peroxide method is less stable, security is not high; oxygen rules in the basic research stage. Co-oxidation method (ethylbenzene, cumene and isobutane, etc.) to activate the preparation of C-H ...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07D303/04C07D301/08
CPCB01J31/2213C07D301/08C07D303/04B01J2531/64Y02P20/52
Inventor 纪红兵熊超薛灿周贤太何耀荣徐德靖
Owner SUN YAT SEN UNIV
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