Hydrophobic catalyst with two-dimensional open hydrophobic space and preparation method thereof

A catalyst and open technology, applied in organic chemical methods, preparation of organic compounds, preparation of carbon-based compounds, etc., can solve rare problems and achieve uniform dispersion and high-efficiency catalytic oxidation reactions

Inactive Publication Date: 2013-01-02
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the phospholipid-like bilayer structure has received more and more

Method used

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  • Hydrophobic catalyst with two-dimensional open hydrophobic space and preparation method thereof
  • Hydrophobic catalyst with two-dimensional open hydrophobic space and preparation method thereof
  • Hydrophobic catalyst with two-dimensional open hydrophobic space and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0023] Example 1

[0024] Step A: Add Zn(NO 3 ) 2 ·6H 2 O 0.007mol (about 2.0824g), Al(NO 3 ) 3 ·9H 2 O0.0035mol (about 1.31295g), urea 0.0245mol (about 1.4715g), prepared urea concentration of 0.035mol / L, Zn 2+ Concentration 0.01mol / L, Al 3+ A solution with a concentration of 0.005mol / L. Set a 105°C magnetic stirring in an oil bath and reflux for 27h. 4 times of deionized water, 3 times of anhydrous ethanol for suction filtration, and vacuum drying at room temperature for 12 hours to obtain Zn-Al-CO 3 LDHs.

[0025] Step B: Go to CO at 600mL 2 Add Zn-Al-CO to deionized water 3 LDHs 0.6000g, NaNO 3 76.4910g, HNO 3 200μL, prepared hydrotalcite 1.000g / L, NaNO 3 Concentration 1.5mol / L, HNO 3 A mixed solution with a concentration of 0.005mol / L. In a nitrogen atmosphere, the reaction was carried out at room temperature for 48 hours. Centrifuge and wash several times. Vacuum and dry at room temperature for 12 hours to obtain Zn-Al-NO 3 LDHs.

[0026] Step C: Remove CO at 200mL 2 Add Zn...

Example Embodiment

[0029] Example 2

[0030] Step A: Take a method similar to Step A in Example 1 to obtain Zn-Al-CO 3 LDHs.

[0031] Step B: Obtain Zn-Al-NO according to the method similar to step B in Example 1 3 LDHs precursor.

[0032] Step C: Remove CO at 200mL 2 Add Zn-Al-NO to deionized water 3 LDHs 0.5g, sodium dodecylbenzene sulfonate 0.07mol / L (about 4.8787g). Set 70°C magnetic stirring in an oil bath and react for 48h. Centrifugation, washing several times, and vacuum drying at room temperature for 24 hours to obtain Zn-Al-DBS LDHs.

[0033] Step D: Add 0.1 g of Zn-Al-DBS LDHs to 200 mL of n-butanol, and reflux at 120°C for 36 hours. Add 0.02g of Mn(TPP)OAc, stir and mix for 12h, evaporate the solvent, centrifuge at 5000rpm, and wash with ethanol and dichloromethane. Vacuum drying, room temperature for 12h, the product [Zn 0.66 Al 0.34 (OH) 2 ][(DBS 2- ) 0.17 (Mn(TPP)OAc) 0.0143 ]·0.21H 2 O.

[0034] Add 1 mg of the synthesized catalyst to an anhydrous oxygen-free reaction tube containing 1...

Example Embodiment

[0035] Example 3

[0036] Step A: Take a method similar to Step A in Example 1 to obtain Zn-Al-CO 3 LDHs.

[0037] Step B: Obtain Zn-Al-NO according to the method similar to step B in Example 1 3 LDHs precursor.

[0038] Step C: Remove CO at 200mL 2 Add Zn-Al-NO to deionized water 3 LDHs 0.5g, sodium dodecyl sulfonate (SAS) 0.05mol / L (about 2.7238g). Set 70°C magnetic stirring in an oil bath and react for 48h. Centrifugation, washing several times, and vacuum drying at room temperature for 24 hours to obtain Zn-Al-AS LDHs.

[0039] Step D: Add 0.1 g of Zn-Al-AS LDHs to 200 mL of n-butanol, and reflux at 120°C for 36 hours. Add 0.02g tetraphenylporphine iron chloride Fe(TPP)Cl, stir and mix for 12h, evaporate the solvent, centrifuge at 5000rpm, and wash with ethanol and dichloromethane. Vacuum drying, room temperature for 12h, the product [Zn 0.62 Al 0.38 (OH) 2 ][(AS 2- ) 0.19 (Fe(TPP)Cl) 0.0107 ]·0.32H 2 O).

[0040] Add 1 mg of the synthesized catalyst to an anhydrous oxygen-free ...

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Abstract

The invention provides a hydrophobic catalyst with two-dimensional open hydrophobic space, which belongs to the technical field of catalysts. The catalyst is an oxidation catalyst with a supramolecular phospholipid-like bi-molecule layer intercalated structure, a metal complex B is inserted into the layers of amphiphilic anionic dydrotalcite [M<2+>1-xM<3+>x(OH)2]<x+> (A<n->)x/n.mH2O, wherein A is an amphiphilic anion. A preparation method for the catalyst comprises the following steps: preparing a hydrotalcite precursor with NO3<-> ions as interlayer anions; then introducing the amphiphilic anion into the hydrotalcite precursor with the NO3<-> ions as the interlayer anions by using an ion exchange method so as to obtain amphiphilic anion intercalated hydrotalcite; and then swelling the hydrotalcite with hydrophobic space by using n-butanol, adding the metal complex, carrying out mixing under stirring, evaporating a solvent for recombination and carrying out washing and drying. The hydrophobic catalyst provided by the invention has significantly improved activity compared with a corresponding homogeneous metal complex catalyst.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular provides a catalyst which simulates the bimolecular layer structure of phospholipids in living organisms and has a two-dimensional open hydrophobic space and a preparation method thereof. Background technique [0002] Selective oxidation is the core technology for converting most compounds into high-yield oxygenates. Among the common metal catalysts for catalytic selective oxidation, since Ru has a valence state of 0 to +8 and forms a variety of oxidation states through different oxidation mechanisms, it can efficiently catalyze a variety of oxidation reactions such as alkane oxidation, olefin compound ring Oxidation and oxidative cracking, oxidation of ether and alcohol compounds and oxidation of amine and amide compounds. However, as a rare precious metal, Ru's limited output and high price limit the large-scale commercial application of Ru, so the substitution of precious ...

Claims

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Application Information

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IPC IPC(8): B01J31/26B01J35/02C07B33/00C07D301/08C07D303/04C07D303/14C07C45/38C07C47/54C07C49/86
Inventor 何静刘玉清
Owner BEIJING UNIV OF CHEM TECH
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