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Preparation method and application of carbonyl cobalt catalyst

A technology of cobalt carbonyl catalyst and application method, which is applied in the direction of carbon monoxide or formate reaction preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems such as the preparation method of cobalt carbonyl catalyst that are not clearly stated, and achieve selectivity And the effect of high yield, good activity and selectivity, and low cost

Active Publication Date: 2016-01-13
山东玉皇盛世化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In summary, the method for preparing 3-hydroxypropionate methyl ester using cobalt carbonyl catalysts for ethylene oxide has been reported, but the preparation method of cobalt carbonyl catalysts has not been clearly stated.

Method used

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  • Preparation method and application of carbonyl cobalt catalyst
  • Preparation method and application of carbonyl cobalt catalyst

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Embodiment 1

[0030] Dissolve 0.7472g of cobalt acetate in 60mL of methanol, then add 1.5671g of hydrosulfite and 0.5304g of cobalt powder to prepare a solution, add the solution to the autoclave, and seal the autoclave; 2 Replace the air in the autoclave with gas for 3 times, then replace the gas in the autoclave with CO gas for 3 times, fill the autoclave with CO gas to make the CO gas pressure in the autoclave 2MPa; heat the autoclave to make it Raise the temperature to 50°C, and react for 3 hours at a stirring speed of 200r / min; after the reaction is completed, cool down and centrifuge to obtain an alcoholic solution of cobalt carbonyl catalyst; take 20.8g of the solution and place it in a high-pressure reactor , add 0.8559g3-hydroxypyridine, 6.6075g ethylene oxide, 7.21g methanol, seal the autoclave, first use N 2 The air in the autoclave was replaced with gas for 3 times, and the gas in the autoclave was replaced with CO for 3 times. CO gas was filled into the high-pressure reactor to...

Embodiment 2

[0032] Dissolve 0.7472g of cobalt acetate in 60mL of methanol, then add 2.0894g of hydrosulfite and 0.3536g of cobalt powder to make a solution, add the solution to the autoclave, and seal the autoclave; first replace the autoclave with argon Air 4 times, then replace the gas in the autoclave with CO gas 4 times, fill the autoclave with CO gas, make the pressure of CO gas in the autoclave 3MPa; heat the autoclave to 60°C, and stir At a speed of 200r / min, react for 4 hours; after the reaction is completed, cool down and centrifuge to obtain an alcohol solution of cobalt carbonyl catalyst; take 20.8g of the solution, place it in a high-pressure reactor, and add 0.8559g of 3-hydroxypyridine , 6.6075g ethylene oxide, 7.21g methanol, seal the autoclave, first replace the air in the autoclave with argon 4 times, then replace the gas in the autoclave 4 times with CO, and fill the autoclave with CO gas to make the CO gas The pressure is 7.5MPa, the temperature of the reaction kettle i...

Embodiment 3

[0034] Dissolve 0.7472g of cobalt acetate in 60mL of methanol, then add 1.5671g of hydrosulfite and 0.5304g of cobalt powder to prepare a solution, add the solution to the autoclave, and seal the autoclave; 2 Replace the air in the autoclave with CO gas for 5 times, then replace the gas in the autoclave with CO gas for 5 times, and fill the autoclave with CO gas to make the CO gas pressure in the autoclave 4MPa; heat the autoclave to make it Raise the temperature to 60°C, and react for 5 hours at a stirring speed of 200r / min; after the reaction is completed, cool down and centrifuge to obtain an alcohol solution of cobalt carbonyl catalyst; take 20.8g of the solution and place it in a high-pressure reactor , add 0.8559g3-hydroxypyridine, 6.6075g ethylene oxide, 7.21g methanol, seal the autoclave, first use N 2 Replace the air in the autoclave with gas 6 times, then replace the gas in the autoclave with CO 6 times, fill the high-pressure reactor with CO gas to make the CO gas p...

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Abstract

The invention relates to a preparation method and application of a carbonyl cobalt catalyst through which 3-methyl lactate is prepared in an ethylene oxide methyl esterification mode. The preparation method of the carbonyl cobalt catalyst is characterized in that cobalt powder is used as a reducing agent, soluble cobalt salt and cobalt powder and an auxiliary reducing agent are placed into a high-pressure reaction kettle according to a mole ratio to be sealed, gas in the reaction kettle is replaced with inert gas, and stirring, cooling and centrifugal separation are carried out to obtain the carbonyl cobalt catalyst. The preparation method of the carbonyl cobalt catalyst is low in cost and has the better activity and selectivity compared with other preparation methods of the carbonyl cobalt catalyst, and no other carbonyl compound is produced in the preparation method; however, if manganese powder, zinc powder, iron powder, nickel powder and the like are adopted, corresponding carbonyl compound by-products are produced, impurities are introduced, and then the catalytic effect of the catalyst is affected. The selectivity and yield of the carbonyl cobalt catalyst through which the 3-methyl lactate is prepared in the ethylene oxide methyl esterification mode are high.

Description

technical field [0001] The invention relates to a preparation method and application of a cobalt carbonyl catalyst used for preparing 3-hydroxypropionate methyl ester by ethylene oxide methyl esterification. Background technique [0002] 1,3-Propanediol (1,3-PDO) is an important organic fine chemical. It can be used as a raw material for the production of antifreeze, plasticizer, preservative and emulsifier, and is also widely used in food, cosmetic and pharmaceutical industries. At present, the most important use of 1,3-PDO is as a monomer raw material for the synthesis of a new polyester fiber material - polytrimethylene terephthalate (PTT). Because the 1,3-PDO molecule has a suitable carbon chain length and symmetrical molecular configuration, PTT not only has the excellent characteristics of polyethylene terephthalate, but also has good resilience, anti-ultraviolet and anti-aging properties. pollution performance. The excellent performance of PTT makes it one of the h...

Claims

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Application Information

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IPC IPC(8): B01J23/75B01J27/20C07C69/675C07C67/37
Inventor 刘长城黄国宝冯靓婧冯汝明候红霞王玉强陈双喜王瑛王胜伟
Owner 山东玉皇盛世化工股份有限公司
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