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A class of multi-acid-based metal-organic framework crystal materials, its preparation method and its application in the catalytic synthesis of p-benzoquinone compounds

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

Active Publication Date: 2021-04-20
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 low oxidation states. Therefore, a novel polyacid-based metal organic framework crystal material was developed for high Active and highly selective synthesis of p-benzoquinones is very necessary

Method used

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  • A class of multi-acid-based metal-organic framework crystal materials, its preparation method and its application in the catalytic synthesis of p-benzoquinone compounds
  • A class of multi-acid-based metal-organic framework crystal materials, its preparation method and its application in the catalytic synthesis of p-benzoquinone compounds
  • A class of multi-acid-based metal-organic framework crystal materials, its preparation method and its application in the catalytic synthesis of p-benzoquinone compounds

Examples

Experimental program
Comparison scheme
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

The invention belongs to the technical field of catalytic chemistry, and specifically relates to a class of polyacid-based metal-organic framework crystal materials, a preparation method and its catalytic synthesis of benzene-kun compounds. The material can be used as a heterogeneous catalyst to catalyze alkylphenols, It has excellent catalytic performance in the oxidation synthesis of alkoxybenzene and 2‑methylnaphthalene, especially in the synthesis of 2,3,5‑trimethylphenol by oxidation of 2,3,6‑trimethylphenol In the reaction of Benzine, almost complete conversion of the substrate can be achieved within 10-20min, the yield of Benzine is as high as 96%-99%, and its conversion frequency is as high as 300-600h ‑1 ; In addition, the catalyst can be reused, and the structure and catalytic activity do not change; the preparation process of the material is simple, the product is high in purity, and has potential application prospects in the field of catalysis.

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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Patent Type & Authority Patents(China)
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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