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A kind of cobalt-phosphine catalyst and its preparation method and application

A technology of catalyst and cobalt source, which is applied in the field of cobalt-phosphine catalyst and its preparation, can solve the problems of high price, easy oxidation by air, and decreased yield of target catalyst, and achieve cost reduction, simplified composition, and avoiding the introduction of cocatalysts Effect

Active Publication Date: 2021-06-15
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to data, cobalt-phosphine catalysts currently use Co 2 (CO) 8 [Organometallics,1984,3,174-177] obtained by ligand exchange reaction with phosphine ligands, the disadvantage is that the raw material Co 2 (CO) 8 Expensive and easily oxidized by air, resulting in a decrease in the yield of the target catalyst

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  • A kind of cobalt-phosphine catalyst and its preparation method and application
  • A kind of cobalt-phosphine catalyst and its preparation method and application

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preparation example Construction

[0021] An aspect of the embodiments of the present invention provides a method for preparing a cobalt-phosphine catalyst, which includes:

[0022] In a reducing atmosphere, the first homogeneously mixed reaction system including cobalt source, phosphine ligand and solvent is reacted at 70-140° C. for 1-6 hours, and the cobalt-phosphine catalyst is obtained through post-treatment.

[0023] In some embodiments, the preparation method includes: adding a cobalt source, a phosphine ligand and a solvent into a reaction vessel and mixing them uniformly to form the first uniformly mixed reaction system, and introducing a reducing gas into the reaction vessel , keeping the pressure in the reaction vessel at 2-8MPa, then reacting at 70-140° C. for 1-6 hours, and then post-processing to prepare the cobalt-phosphine catalyst.

[0024] Further, the cobalt source includes cobalt isooctanoate and / or cobalt naphthenate, but is not limited thereto.

[0025] Further, the cobalt source is deriv...

Embodiment 1

[0056] The preparation method of the cobalt-phosphine catalyst of the present embodiment is as follows:

[0057] Add 40g toluene, 60g cobalt isooctanoate (10% cobalt content) and 18.9g tributylphosphine respectively in the stainless steel autoclave of 300mL, with 1MPa H 2 / CO(1:1) is replaced 4 times, filled with H 2 / CO (1:1) 2MPa, add CO to the total pressure of 3MPa, slowly raise the temperature to 120°C and keep it for 2h, during the reaction, 3MPa of CO has been fed to keep the reaction at a constant pressure. After the reaction, the temperature was lowered, and the slurry was filtered after pressure relief, and washed with toluene until the filtrate was clear. The filter cake was transferred to a vacuum drying oven at 40° C. for 20 h, and the yield of the cobalt-phosphine catalyst (1) was calculated to be about 65.1% after weighing.

[0058] figure 1 It is the infrared spectrum of the catalyst (1) obtained in this embodiment, wherein, a is the infrared spectrum of the...

Embodiment 2

[0060] The preparation method of this example is basically the same as that of Example 1, except that the toluene in Example 1 is changed to 40 g of petroleum ether, CO is added to a total pressure of 5 MPa, and the temperature is slowly raised to 100° C. and maintained for 1.5 hours. The yield of cobalt-phosphine catalyst (1) obtained in this example is about 73.7%.

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Abstract

The invention discloses a cobalt-phosphine catalyst as well as its preparation method and application. The preparation method of the cobalt-phosphine catalyst comprises: reacting the first homogeneously mixed reaction system containing a cobalt source, a phosphine ligand and a solvent at 70-140°C for 1-6 hours in a reducing atmosphere, and then post-processing to prepare Cobalt-phosphine catalyst. The present invention also provides a method for synthesizing β-hydroxycarboxylic acid esters, which includes: in a CO atmosphere, making the second homogeneously mixed reaction system comprising epoxy compounds, methanol, and cobalt-phosphine catalysts at a pressure of 2-2 React for 5-60 hours under the condition of 8MPa and temperature of 30-110°C to prepare β-hydroxy carboxylate. The preparation method of the cobalt-phosphine catalyst of the present invention is simple, the cost is low, and the yield is high. At the same time, the obtained catalyst can efficiently convert epoxy compounds into β-hydroxycarboxylates, and the catalyst has good stability and is convenient for storage, transportation and use. and recycling.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to a cobalt-phosphine catalyst and a preparation method thereof, and the application of the catalyst in a method for synthesizing beta-hydroxy carboxylate with epoxy compounds as raw materials. Background technique [0002] β-Hydroxycarboxylate compounds with bifunctional groups have a wide range of applications in the fields of organic chemistry and polymer chemistry. For example: optically active β-hydroxycarboxylates are used to synthesize many medicines, agricultural chemicals, and natural products; they can also be used as monomers of polymer polyβ-hydroxycarboxylates, which have good biocompatibility , degradable, non-irritating and non-immunogenic, widely used in medical materials, packaging materials, biodegradable films, drug sustained and controlled release materials, orthopedics and medical surgical sutures and other fields. At present, β-hydroxy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/24B01J37/08C07C67/37C07C69/675
CPCB01J31/24B01J37/08B01J2231/49B01J2531/845C07C67/37C07C69/675
Inventor 郧栋曾波杨冰筱刘祺任夏春谷
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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