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Frame compound catalyst material containing mixed valence Cu and preparation method thereof

A technology of framework compounds and mixed valence states, applied in the direction of organic compound/hydride/coordination complex catalysts, copper organic compounds, physical/chemical process catalysts, etc., can solve the problem of high corrosion in the liquid phase method and low activity in the gas phase method , hindering development and other issues, to achieve the effect of good crystallinity, easy recycling, and increased reactivity

Inactive Publication Date: 2015-05-13
LUOYANG NORMAL UNIV
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  • Claims
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Problems solved by technology

Foreign scholar Dan studied the catalytic performance of activated carbon-supported PdCl2, CuClx catalytic system in gas-phase carbonylation of diethyl carbonate to DEC V. The ethanol conversion rate was about 10%, and the DEC selectivity was about 80%, and made an in-depth elaboration on the catalyst structure characterization and reaction mechanism; Ma Xinbin et al. studied the Cup and CuY catalysts, the ethanol conversion rate was 4.5%, the DEC selectivity was about 70%, and the by-products and reaction mechanism were also studied. However, the copper catalyst in the comprehensive alcohol oxidative carbonylation reaction has the disadvantages of low activity in the gas phase method, high corrosion and poor stability in the liquid phase method, and has hindered the industrialization of the oxidative carbonylation process due to its high corrosion. Study on Homogeneous Catalytic System

Method used

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  • Frame compound catalyst material containing mixed valence Cu and preparation method thereof
  • Frame compound catalyst material containing mixed valence Cu and preparation method thereof
  • Frame compound catalyst material containing mixed valence Cu and preparation method thereof

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preparation example Construction

[0023] The preparation method of the framework compound catalyst material containing mixed valence Cu, the specific steps are as follows:

[0024] Step 1. Take the organic ligand 4-(5-sulfonyl) 8-hydroxyquinolyl-phthalic acid, and dissolve it in the mixed solution of water and organic solvent to obtain solution A, which is set aside; the organic solvent is DMF, methanol ethanol or DMSO, and the volume ratio of water to organic solvent is 0.5: 1~4:1;

[0025] Step 2, get divalent divalent copper source and 4,4'-bipyridine, described divalent copper source is Cu(OAc) 2 h 2 O, CuSO 4 · 5H 2 O or copper nitrate dihydrate is added to the solution A obtained in step 1, wherein the added divalent copper source, 4,4'-bipyridyl and organic ligand 4-(5-sulfonyl) 8-hydroxyquinoline The mol ratio of base-phthalic acid is 3:3:2, obtains solution B after stirring evenly, for subsequent use;

[0026] Step 3. Stir the solution B in step 2 with a magnetic stirrer at room temperature and...

Embodiment 1

[0030]A preparation method of a framework compound catalyst material containing mixed valence Cu, the specific steps are as follows:

[0031] Step 1, take the organic ligand 4-(5-sulfonyl) 8-hydroxyquinolyl-phthalic acid, dissolve it in the mixed solution of water and organic solvent, the organic solvent is methanol, and the volume of water and organic solvent Ratio is 0.5: 1.2, obtains solution A, for subsequent use;

[0032] The 4-(5-sulfonyl) 8-hydroxyquinolyl-phthalic acid has the following structural formula:

[0033]

[0034] Step 2, take divalent copper source Cu(OAc) 2 h 2 O and 4,4'-bipyridine were added to the solution A obtained in step 1, wherein the added divalent copper source, 4,4'-bipyridine and organic ligand 4-(5-sulfonyl)8- The mol ratio of hydroxyquinolinyl-phthalic acid is 3:3:2, obtains solution B after stirring, for subsequent use;

[0035] Step 3. Stir the solution B in step 2 with a magnetic stirrer at normal temperature and pressure for 20 min...

Embodiment 2

[0043] A preparation method of a framework compound catalyst material containing mixed valence Cu, the specific steps are as follows:

[0044] Step 1, take the organic ligand 4-(5-sulfonyl) 8-hydroxyquinolyl-phthalic acid, dissolve it in the mixed solution of water and organic solvent, the organic solvent is ethanol, and the volume of water and organic solvent Ratio is 4:1, obtains solution A, for subsequent use;

[0045] Step 2: Take divalent copper source CuSO 4 · 5H 2 O and 4,4'-bipyridine were added to the solution A obtained in step 1, wherein the added divalent copper source, 4,4'-bipyridine and organic ligand 4-(5-sulfonyl)8- The mol ratio of hydroxyquinolinyl-phthalic acid is 3:3:2, obtains solution B after stirring, for subsequent use;

[0046] Step 3. Stir the solution B in step 2 with a magnetic stirrer at normal temperature and pressure for 30 minutes, then adjust the pH value to 6 to obtain the precursor solution C, and set aside;

[0047] Step 4. Transfer th...

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Abstract

The invention discloses a frame compound catalyst material containing mixed valence Cu, the chemical formula is {[Cu3(H2O)6(SQPA)2(bipy)]2bipy](b).( / b)4H2O}n, wherein n is greater than 1. The preparation method of the catalyst material is as follows: step one, dissolving an organic ligand in a mixed solution of water and organic solvent to obtain a solution A; step two, adding copper source and 4,4'-dipyridyl into the solution A, uniformly stirring to obtain a solution B; step three, stirring the solution B by using a magnetic stirrer at normal temperature and pressure, and the regulating pH value to obtain a precursor solution C; step four, transferring the precursor solution C into a reaction kettle to react, cooling after reaction, collecting the crystal, washing and drying to obtain a blue crystal metal organic frame compound catalyst material. The catalyst material has good heat stability and catalysis and can be recycled.

Description

technical field [0001] The invention belongs to the field of transition metal catalyst materials, and mainly relates to a framework compound catalyst material containing mixed valence Cu and a preparation method thereof. Background technique [0002] In recent years, with the deterioration of the human living environment, research on green chemistry and chemical engineering has gradually emerged. In the chemical industry, the development of clean, environmentally friendly chemicals and synthetic processes has become particularly important. The development of benzoxazole derivatives industry originated from its extremely low ecotoxicity and bioaccumulation, good antiviral and antibacterial properties, etc., and is known as an environmentally friendly chemical. Its molecular structure contains benzene rings, alkoxy It is mainly used as carbonylation reagents, oil additives, surfactants and lithium battery electrolyte additives, etc., with good reactivity and a wide range of u...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07F1/08
Inventor 冯勋徐晨马录芳张甜王利亚郎雪明
Owner LUOYANG NORMAL UNIV
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