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Supramolecular structures unsymmetrical oxide catalyst and its preparing method

An oxidation catalyst and molecular structure technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of immobilization of asymmetric catalysts and surface active centers The problems of construction and characterization, insufficient research on heterogeneous catalysts, and constraints on the research and development of synthetic chiral sulfoxides have achieved the effect of improving selectivity

Inactive Publication Date: 2010-01-27
BEIJING UNIV OF CHEM TECH
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  • Description
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Problems solved by technology

[0007] At present, most of the asymmetric oxidation of sulfides uses homogeneous catalysts, and the research on heterogeneous catalysts is not deep enough, and there are few studies on the immobilization of asymmetric catalysts, the construction of surface active centers, and characterization, which restricts the synthesis. Further Development of Chiral Sulfoxide Research

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Step A: take by weighing 0.06mol Mg(NO 3 ) 2 ·6H 2 O and 0.03mol Al(NO 3 ) 3 9H 2 O was dissolved in 122mL deionized water to prepare a mixed salt solution, and another 0.144mol NaOH and 0.03mol NaOH 2 CO 3 Dissolve in 122mL of deionized water, quickly nucleate the alkali solution and mixed salt solution in a rotating liquid film reactor at room temperature, crystallize the resulting slurry in a high-pressure bomb at 130°C for 24 hours, and wash the product by centrifugation to neutrality; take out a small amount After the sample was dried at 80°C for 12 hours, it was characterized to obtain Mg 3 Al-CO 3 LDHs, its Mg 2+ / Al 3+ =3.

[0024] Step B: 1.20g L-tartaric acid (C 4 h 6 o 6 , 0.008mol) solid powder and 0.4mL tetraisopropyl titanate (0.0013mol) were added into a three-necked flask filled with 50mL of n-butanol, stirred and heated to reflux temperature, and kept for reaction for 1h. The mixed solution system became cloudy and then gradually became c...

Embodiment 2

[0028] Step A: take by weighing 0.09mol Mg(NO 3 ) 2 ·6H 2 O and 0.03mol Al(NO 3 ) 3 9H 2 O was dissolved in 122mL deionized water to prepare a mixed salt solution, and another 0.192mol NaOH and 0.03mol NaOH 2 CO 3 Dissolve in 122mL of deionized water, quickly nucleate the alkali solution and mixed salt solution in a rotating liquid film reactor at room temperature, crystallize the resulting slurry in a high-pressure bomb at 130°C for 24 hours, and wash the product by centrifugation to neutrality; take out a small amount After the sample was dried at 80°C for 12 hours, it was characterized to obtain Mg 3 Al-CO 3 LDHs, its Mg 2+ / Al 3+ =3.

[0029] Step B: 1.20g L-tartaric acid (C 4 h 6 o 6 , 0.008mol) solid powder and 0.4mL tetraisopropyl titanate (0.0013mol) were added into a three-necked flask filled with 50mL of n-butanol, stirred and heated to reflux temperature, and kept for reaction for 1h. The mixed solution system became cloudy and then gradually became c...

Embodiment 3

[0033] Step A: take by weighing 0.12mol Mg(NO 3 ) 2 ·6H 2 O and 0.03mol Al(NO 3 ) 3 9H 2 O was dissolved in 122mL deionized water to prepare a mixed salt solution, and another 0.24mol NaOH and 0.03mol NaOH 2 CO 3 Dissolve in 122mL of deionized water, quickly nucleate the alkali solution and mixed salt solution in a rotating liquid film reactor at room temperature, crystallize the resulting slurry in a high-pressure bomb at 130°C for 24 hours, and wash the product by centrifugation to neutrality; take out a small amount After the sample was dried at 80°C for 12 hours, it was characterized to obtain Mg 3 Al-CO 3 LDHs, its Mg 2+ / Al 3+ =3.

[0034] Step B: 1.20g L-tartaric acid (C 4 h 6 o 6 , 0.008mol) solid powder and 0.4mL tetraisopropyl titanate (0.0013mol) were added into a three-necked flask filled with 50mL of n-butanol, stirred and heated to reflux temperature, and kept for reaction for 1h. The mixed solution system became cloudy and then gradually became cl...

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Abstract

A super-molecular structure asymmetric oxidation catalyst and the preparation method thereof, belong to the technique field for synthesizing the super-molecular catalyst. The general formula of the chemical composition is as follows: ((A<2->)a(tartrate<2->)b(CO3<2->)cTidOe) (M<2+>1-XM<3+>x(OH)2) MH2O. The method comprises the following steps: preparing the volknerite precursor with interlaminar anion as CO3<2-> and the molar ratio between the bivalence kations and the tervalence kations of the laminated board M<2+> / M<3+> equals to 2 to 4; refluxing-heating the L-tartaric acid and titanic acid ester respectively according to the molar ratio of 1:1 to 12:1, and preparing out the titanium tartrate complex and n-butyl alcohol solution with different mixture ratio to the tartaric acid; stirring and reacting the prepared solution to the volknerite precursor with CO3<2-> as the interlaminar anion at the refluxing temperature, sufficiently washing and centrifugation the product with the water of the absolute ethyl alcohol, then vacuum drying and the intercalary volkerite supramolecular structure asymmetrical oxidation catalyst of the titanium tartrate complex is obtained. The advantage is that the selectivity of the reaction product is increased.

Description

technical field [0001] The invention belongs to the technical field of supramolecular catalyst synthesis, and in particular provides a supramolecular structure asymmetric oxidation catalyst and a preparation method thereof. Background technique [0002] With the development of medicinal chemistry and biochemistry in recent years, the demand for optically active organic compounds is increasing internationally. On the one hand, this is because many new and highly effective drugs are optically active organic compounds with chiral centers, and on the other hand, because studies on the pharmacological activity of such drugs have proved that only one configuration of the optical isomer has pharmacological activity. , the other optical isomer may not only have no pharmacological activity, but may even be toxic and have side effects on the human body. The first way to obtain pure optically active isomers is to remove the other enantiomer through the resolution of enantiomers, but t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J31/26
CPCB01J31/2239B01J2231/70B01J31/1691B01J2531/46
Inventor 何静师慧敏
Owner BEIJING UNIV OF CHEM TECH
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