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A kind of preparation method of organic-inorganic hybrid material supporting ruthenium catalyst for synthesizing 1-aminopropanol

A hybrid material, ruthenium catalyst technology, applied in the preparation of organic compounds, the preparation of aminohydroxy compounds, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of low yield, high cost, large catalyst consumption, etc. problem, to achieve the effect of high activity, low cost and high yield

Inactive Publication Date: 2015-08-05
淮北新兴实业有限责任公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the existing problems of large catalyst consumption, high cost and low yield when synthesizing L-aminopropanol by catalytic hydrogenation, and to provide an organic-inorganic hybrid material for synthesizing L-aminopropanol The preparation method of supported ruthenium catalyst, in order to reduce the cost of synthesizing L-amino propanol and improve its productive rate

Method used

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  • A kind of preparation method of organic-inorganic hybrid material supporting ruthenium catalyst for synthesizing 1-aminopropanol
  • A kind of preparation method of organic-inorganic hybrid material supporting ruthenium catalyst for synthesizing 1-aminopropanol

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Embodiment 1

[0016] The present embodiment prepares catalyst sample 1 as follows:

[0017] a. Pretreat the silica gel to obtain spare silica gel

[0018] Add 10g of 100-200 mesh silica gel H, 120mL of 98% concentrated sulfuric acid and 15mL of 69% concentrated nitric acid into flask A, and stir in an oil bath at 140°C for 24 hours. Wash the silica gel H several times until the washing liquid is neutral, filter it with suction, take the solid intermediate A, wash the solid intermediate A with ethanol, and then put the filter cake in a vacuum drying oven at 140°C after suction filtration. Conditioned drying for 6 hours to obtain spare silica gel;

[0019] b. Grafting modified ethylenediamine structural units on the surface of spare silica gel

[0020] Add 60 mL of absolute anhydrous toluene and 1.4 g of N-(3-triethoxysilylpropyl) ethylenediamine to flask B, stir at room temperature for 30 min, then add 4 g of the spare silica gel obtained in step a, and stir until The spare silica gel is ...

Embodiment 2

[0024] This embodiment prepares catalyst sample 2 in the same manner as in Example 1, and changes the quality of N-(3-triethoxysilylpropyl) ethylenediamine into 1.8g in step b, and the obtained in step b The spare silica gel modified with ethylenediamine structural units on the surface has a mass percentage of nitrogen of 2.62% as measured by elemental analysis.

Embodiment 3

[0026] The present embodiment prepares catalyst sample 3 as follows:

[0027] a. Pretreat the silica gel to obtain spare silica gel

[0028] Add 10g of 100-200 mesh silica gel H, 120mL of 98% concentrated sulfuric acid and 15mL of 69% concentrated nitric acid into flask A, and stir in an oil bath at 100°C for 24 hours. Wash the silica gel H several times until the washing liquid is neutral, and filter with suction to obtain the solid intermediate A, wash the solid intermediate A with ethanol, and then place the filter cake in a vacuum drying oven at 140°C after suction filtration. Dry for 7 hours to obtain spare silica gel;

[0029] b. Grafting modified ethylenediamine structural units on the surface of spare silica gel

[0030] Add 80 mL of absolute anhydrous toluene and 1.4 g of N-(3-triethoxysilylpropyl) ethylenediamine to flask B, stir at room temperature for 30 min, then add 4 g of the spare silica gel obtained in step a, and stir until The spare silica gel is uniforml...

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Abstract

The invention discloses a preparation method of an organic-inorganic hybrid material ruthenium-loaded catalyst for synthesizing L-alaninol. The preparation method is characterized by comprising the following steps: pre-treating silica gel to obtain backup silica gel; grafting and modifying an ethidene diamine structural unit on the surface of the backup silica gel; and then loading ruthenium. According to the preparation method, an organic-inorganic hybrid material is used as a carrier, so that the prepared ruthenium-loaded catalyst is high in activity, and the hydrogenation of aminopropionic acid can be realized in a neutral aqueous phase under a relatively low temperature to realize the preparation of L-alaninol; in addition, the preparation method is low in cost, high in yield and simple in process.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and relates to a preparation method of a catalyst used for synthesizing L-aminopropanol. Background technique [0002] L-Aminopropanol is a key intermediate in the synthesis of the third-generation quinolone broad-spectrum antibacterial drug levofloxacin, and it is also widely used as a chiral source and chiral modifier in asymmetric synthesis. In recent years, in the antibacterial drug market, the annual sales amount of levofloxacin has firmly occupied the first place. At present, the method of industrial production of L-aminopropanol is to first esterify aminopropionate, and then use metal Borohydride is used as a reducing agent, and the reducing agent is used in a large amount, expensive, and the residue pollutes the environment. [0003] In the selective catalytic hydrogenation reaction, the performance of the catalyst is the main factor affecting the reaction. Patent: CN1016488...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02C07C213/02C07C215/08C07C279/12C07C277/08
Inventor 王磊吴金城李品华王永秋杨光厚张培红
Owner 淮北新兴实业有限责任公司
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