Polyacid based metal organic framework crystal material, preparation method and application thereof in catalytic synthesis of p-benzoquinone compounds

A technology of organic frameworks and crystal materials, applied in the field of catalytic chemistry, to achieve the effects of novel structure, excellent catalytic activity, and excellent catalytic performance

Active Publication Date: 2019-10-22
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there has been no literature report on the selective synthesis of corresponding quinone compounds using POMOF crystal materials for the oxidation of alkylphenols or other substrates with

Method used

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  • Polyacid based metal organic framework crystal material, preparation method and application thereof in catalytic synthesis of p-benzoquinone compounds
  • Polyacid based metal organic framework crystal material, preparation method and application thereof in catalytic synthesis of p-benzoquinone compounds
  • Polyacid based metal organic framework crystal material, preparation method and application thereof in catalytic synthesis of p-benzoquinone compounds

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Polyacid-based metal-organic framework crystal material H[Cu II (ttb)(H 2 O) 3 ] 2 [Cu II (ttb)Cl] 2 [PW 12 o 40 ]·4H 2 The preparation method of O, concrete steps are as follows:

[0041] 1) Synthesize precursor K by conventional methods 4 [PW 11 V V o 40 ]·xH 2 O (Domaille, P.J., Inorg. Synth., John Wiley & Sons.: 1990; Vol.27, 96-104);

[0042] 2)K 4 [PW 11 V V o 40 ]·xH 2 O (0.3g, ~0.1mmol) was dissolved in 10mL water, then CuCl 2 2H 2 O (0.0682g, 0.40mmol) and Httb (0.0491g, 0.23mmol), continued to stir for 0.5h, adjusted the pH to 2.0-2.8 with dilute hydrochloric acid, and continued to stir for 0.5h, then transferred to a polytetrafluoroethylene reactor. After heating at 180°C for about 6 days in an oven, slowly cool to room temperature to obtain a green bulk crystalline material with a yield of about 52% (based on K 4 [PW 11 V V o 40 ]·xH 2 O).

[0043] The 0.0682g CuCl 2 2H 2 O can be prepared from 0.0767g CuCl 2 2H 2 O or 0.0998~0....

Embodiment 2

[0045] Polyacid-based metal-organic framework crystalline materials [ClCu 6 I (trz) 4 ][ClCu 5 I (trz) 4 ] 2 [Cu II (H 2 O)][PW 12 o 40 ] The preparation method, concrete steps are as follows:

[0046] 1) Synthesize precursor K by conventional methods 4 [PW 11 V V o 40 ]·xH 2 O (Domaille, P.J., Inorg. Synth., John Wiley & Sons.: 1990; Vol.27, 96-104);

[0047] 2)K 4 [PW 11 V V o 40 ]·xH 2 O (0.35g, ~0.12mmol) was dissolved in 10mL water, then Cu(OAc) was added 2 ·H 2 O (0.1497g, 0.75mmol) and trz (0.0794g, 1.15mmol), continue to stir for 0.5h, adjust the pH to 1.4-1.6 with dilute hydrochloric acid, after continuing to stir for 0.5h, transfer to a polytetrafluoroethylene reactor After heating at 180° C. for about 5 days, slowly cool to room temperature to obtain a brown-black bulk crystalline material with a yield of about 61% (based on K4 [PW 11 V V o 40 ]·xH 2 O).

[0048] The 0.1497g Cu(OAc) 2 ·H 2 O can be obtained from 0.1398g Cu(OAc) 2 ·H 2 ...

Embodiment 3

[0050] Polyacid-based metal-organic framework crystalline materials [ClCu 6 I (trz) 4 ][ClCu 5 I (trz) 4 ] 2 [Cu II (H 2 O)][PW 12 o 40 ] The preparation method, concrete steps are as follows:

[0051] 1) Synthesis of precursor H by conventional methods 3 PW 12 o 42 ·xH 2 O (John, C.B.J., Inorg. Synth., John Wiley & Sons.: 1939; Vol.1, 132-133);

[0052] 2)H 3 PW 12 o 42 ·xH 2 O (0.32g, ~0.12mmol) was dissolved in 10mL water, then Cu(OAc) was added 2 ·H 2 O (0.1497g, 0.75mmol) and trz (0.0794g, 1.15mmol), continue to stir for 0.5h, adjust the pH to 1.4-1.6 with dilute hydrochloric acid, after continuing to stir for 0.5h, transfer to a polytetrafluoroethylene reactor After heating at 180°C for about 5 days, slowly cool to room temperature to obtain a brown-black bulk crystalline material with a yield of about 31% (based on K 4 [PW 12 o 40 ]·xH 2 O).

[0053] The 0.1497g Cu(OAc) 2 ·H 2 O can be obtained from 0.1398g Cu(OAc) 2 ·H 2 O or 0.1194~0.1279g...

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Abstract

Belonging to the technical field of catalytic chemistry, the invention in particular relates to a polyacid based metal organic framework crystal material, a preparation method and application thereofin catalytic synthesis of p-benzoquinone compounds. The material can be used as a heterogeneous catalyst, and has excellent catalytic performance in the reaction of catalyzing oxidation of alkylphenol, alkoxybenzene and 2-methylnaphthalene to synthesize corresponding p-benzoquinone, especially in the reaction of catalyzing the oxidation of 2, 3, 6-trimethylphenol to synthesize 2, 3, 5-trimethylbenzoquinone, the substrate almost can be completely converted in 10-20min, the yield of benzoquinone is as high as 96%-99%, and the conversion frequency is also as high as 300-600h<-1>. In addition, the catalyst can be reused without change of the structure and catalytic activity. The material has the characteristics of simple preparation process and high product purity, and has potential application prospects in the catalysis field.

Description

technical field [0001] The invention belongs to the technical field of catalytic chemistry, and in particular relates to a preparation method of a class of polyacid-based metal-organic framework crystal materials and a method for efficiently synthesizing p-benzoquinone compounds by catalyzing the oxidation of alkylphenols, alkoxybenzenes and 2-methylnaphthalene application. Background technique [0002] p-Benzoquinones are important intermediates for the synthesis of drugs, health products and fine chemicals, and play important roles in many biological systems. Selective oxidation of synthetic raw materials with low oxidation states (such as phenols, aromatics, etc.) is the main way to prepare p-benzoquinones. Traditional oxidation methods usually use stoichiometric metal oxidants (CrO 3 , MnO 2 , V 2 o 5 ) and strong acid solutions, but always with the generation of large amounts of hazardous waste and by-products of over-oxidation. Use the environmentally friendly O ...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J31/22C07C46/06C07C50/04C07C50/28C07C50/12
CPCB01J31/1691B01J2231/763B01J2531/0241B01J2531/16C07C46/06C08G83/008C07C2602/28C07C50/04C07C50/28C07C50/12
Inventor 安海艳常深圳
Owner DALIAN UNIV OF TECH
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