Preparation for KCo(CO)4, and application of KCo(CO4) in catalyzing carbonyl-methyl esterification reaction of ethylene oxide

A technology for oxirane carbonyl methyl esterification reaction, applied in physical/chemical process catalysts, carbon monoxide or formate reaction preparation, organic compound/hydride/coordination complex catalysts, etc. Removal, difficult separation, complex operation and other problems, to achieve the effect of low cost, short reaction time and high activity

Inactive Publication Date: 2016-01-27
南京大学扬州化学化工研究院
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  • Abstract
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  • Application Information

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Problems solved by technology

Na 2 S 2 o 3 / Fe-Mn catalyst reacts carbon monoxide with cobalt salt at normal temperature and pressure to synthesize sodium cobalt tetracarbonyl. This method is difficult to separate after the reaction, and other metal ions in the product are difficult to remove, and the operation is complicated.
There is also sodium borohydride reduction method to prepare sodium tetracarbonyl cobalt, adding sodium borohydride to generate a large amount of gas, the reaction is rapid and difficult to control

Method used

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  • Preparation for KCo(CO)4, and application of KCo(CO4) in catalyzing carbonyl-methyl esterification reaction of ethylene oxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1.0g anhydrous CoCl 2 , 1.4gKBH 4 , 0.2gKOH was placed in a reaction kettle containing 20mL tetrahydrofuran (THF), carbon monoxide (CO) was replaced 3 times, P co =2MPa, react at room temperature for 2h. After the reaction, filter to obtain KCo(CO) 4 of THF solution. Will get KCo(CO) 4 THF solution, 3.4g ethylene oxide, 20mL methanol, added to the reactor, filled with carbon monoxide (CO) and replaced 3 times, P co =2MPa, reacted at 75°C for 5h. After the reaction, it was directly filtered, and the filtrate was analyzed by GC to obtain the conversion rate of ethylene oxide and the selectivity of 3-HPE.

Embodiment 2

[0016] 1.0g anhydrous CoCl 2 , 1.4gKBH 4 , 0.2gKOH was placed in a reaction kettle containing 20mL tetrahydrofuran (THF), carbon monoxide (CO) was replaced 3 times, P co =2MPa, reacted under ice bath for 2h. After the reaction, filter to obtain KCo(CO) 4 of THF solution. Will get KCo(CO) 4 THF solution, 3.4g ethylene oxide, 20mL methanol, added to the reactor, filled with carbon monoxide (CO) and replaced 3 times, P co =2MPa, reacted at 75°C for 5h. After the reaction, it was directly filtered, and the filtrate was analyzed by GC to obtain the conversion rate of ethylene oxide and the selectivity of 3-HPE.

Embodiment 3

[0018] 1.0g anhydrous CoCl 2 , 1.4gKBH 4 , 0.2gKOH was placed in a reaction kettle containing 20mL of methanol, carbon monoxide (CO) was replaced 3 times, P co =2MPa, reacted under ice bath for 2h. After the reaction, filter to obtain KCo(CO) 4 methanol solution. Will get KCo(CO) 4 methanol solution, 3.4g ethylene oxide, 20mL methanol, added to the reactor, filled with carbon monoxide (CO) and replaced 3 times, P co =2MPa, reacted at 75°C for 5h. After the reaction, it was directly filtered, and the filtrate was analyzed by GC to obtain the conversion rate of ethylene oxide and the selectivity of 3-HPE.

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Abstract

The invention provides a novel method for efficiently preparing a KCo(CO)4 catalyst and applying the KCo(CO)4 catalyst in catalyzing a carbonyl-methyl esterification reaction of ethylene oxide to prepare methyl 3-hydroxypropionate with a low cost. The method is mild in reaction condition and short in reaction time in a process for preparing KCo(CO)4. The obtained KCo(CO)4 can be used for efficiently catalyzing the carbonyl methyl esterification reaction of ethylene oxide. The whole process is short in reaction time and low in cost.

Description

1. Technical field: [0001] The present invention relates to the use of KBH 4 Reduced CoCl 2 Preparation of KCo(CO) 4 It is also used to catalyze the oxirane carbonyl methyl esterification reaction to prepare 3-hydroxy propionate methyl ester. 2. Background technology: [0002] 1,3-Propanediol (1,3-PDO) is mainly used in the production of new polyester poly(trimethylene terephthalate) (PTT), and can also be used in the synthesis of various drugs, plasticizers, detergents, emulsifiers and other fine Raw material for chemical products. The PTT synthesized by 1,3-PDO and terephthalate (ester) not only has the chemical stability of polyethylene terephthalate (PET), but also has the good resilience and anti-pollution of nylon 6 and nylon 66 It is a new type of polyester fiber with a very wide application prospect. This makes 1,3-PDO have a very large market demand. Currently, 1,3-PDO is prepared by three main processes: acrolein hydration and hydrogenation, ethylene oxide ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/02B01J31/20C07C67/36C07C69/675
Inventor 范以宁刘玉炳赵兵张忠良陆海孟周军许波连
Owner 南京大学扬州化学化工研究院
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