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Method for preparing methylcyclopentanol by oxidation of methylcyclopentane waste oil

A technology for methyl cyclopentanol and methyl cyclopentane, which is applied in the field of preparing methyl cyclopentanol by ozone oxidation, can solve problems such as only in the theoretical calculation stage, and achieve the effects of less pollution, simple equipment and safe system

Inactive Publication Date: 2016-03-30
HENAN UNIV OF URBAN CONSTR
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the utilization of methylcyclopentane waste oil, the literature has reported that azeotropic distillation with methanol is used to separate cyclohexane and methylcyclopentane components, and to obtain methylcyclopentane with a purity of more than 99%. Pentane, but it is still only in the stage of theoretical calculation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Take 600ml waste oil (methylcyclopentane accounts for about 50%, cyclohexane accounts for 45%, other C 5-6 Alkanes account for about 5%) and activated 300g molecular sieves, put them into a normal-pressure reactor, heat to 95°C and keep for about 1 hour to remove linear C 4-6 alkanes.

[0029] (2) Get the nickel catalyst (15g), 80ml of adsorption-treated waste oil, and 100ml of n-butyric acid, mix them and pour them into a 250ml three-necked bottle. A condensation reflux tube is installed on the three-necked bottle, and the temperature of the condensate is -20°C. Introduce 3% ozone into the there-necked flask with an ozone generator, and react for 5 hours at a gas flow rate of 3 L / min. The methylcyclopentanol content in the product was about 15.3%.

[0030] (3) After the step (2) is oxidized, the system uses a funnel to separate the nickel catalyst and the reaction solution; the nickel catalyst can be reused.

[0031] (4) Add saturated sodium hydroxide solution ...

Embodiment 2

[0034] (1) Take 600ml waste oil (methylcyclopentane accounts for about 50%, cyclohexane accounts for 45%, other C 5-6 Alkanes account for about 5%) and activated 300g molecular sieves, put them into a normal-pressure reactor, heat to 95°C and keep for about 1 hour to remove linear C 4-6 alkanes.

[0035] (2) Take the nickel catalyst (15g), 80ml of adsorption-treated waste oil, and 100ml of isobutyric acid, mix them and pour them into a 250ml three-necked bottle. A condensation reflux tube is installed on the three-necked bottle, and the temperature of the condensate is -20°C. Introduce 3% ozone into the there-necked flask with an ozone generator, and react for 5 hours at a gas flow rate of 3 L / min. The methylcyclopentanol content in the product was about 17.6%.

[0036] (3) After the step (2) is oxidized, the system uses a funnel to separate the nickel catalyst and the reaction solution; the nickel catalyst can be reused.

[0037] (4) Add sodium hydroxide solution to the r...

Embodiment 3

[0040] (1) Take 600ml waste oil (methylcyclopentane accounts for about 50%, cyclohexane accounts for 45%, other C 5-6 Alkanes account for about 5%) and activated 300g molecular sieves, put them into a normal-pressure reactor, heat to 90°C and keep for about 1 hour to remove linear C 4-6 alkanes.

[0041] (2) Take the nickel catalyst (15g), 80ml of waste oil treated by adsorption, and 100ml of propionic acid, mix them and pour them into a 250ml three-necked bottle. A condensation reflux tube is installed on the three-necked bottle, and the temperature of the condensate is -20°C. Introduce 3% ozone into the there-necked flask with an ozone generator, and react for 5 hours at a gas flow rate of 3 L / min. The methylcyclopentanol content in the product was about 15.5%.

[0042] (3) After the step (2) is oxidized, the system uses a funnel to separate the nickel catalyst and the reaction solution; the nickel catalyst can be reused.

[0043] (4) Add sodium hydroxide solution to the...

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PUM

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Abstract

The invention discloses a method for preparation of methylcyclopentanol from nylon chemical methylcyclopentane waste oil. The method includes: mixing a raw material liquid with a liquid acid in proportion, in the presence of a nickel catalyst, using 3-30% ozone produced by an ozone generator to oxidize the mixture, using a funnel to separate the nickel catalyst from the oxidized system, adding a saturated sodium hydroxide solution to the reaction solution till neutral, conducting extraction, then distilling an extraction agent out of an organic phase so as to obtain a mixed system of methylcyclopentanol, methylcyclopentanone and cyclohexanone, and finally using a 10-40% sodium hydrogen sulfite solution to wash the crude product 1-3 times, thus obtaining methylcyclopentanol with purity of more than 97%. The method provided in the invention has the advantages of simple reaction condition, convenient catalyst recovery, rapid reaction speed, safe reaction, and simple operation, and the product methylcyclopentanol is an important pharmaceutical intermediate. According to the invention, the nylon chemical methylcyclopentane waste oil obtains resource utilization, enterprise waste oil emission is reduced, and new products can be added for enterprises, thus achieving the purpose of income generating.

Description

technical field [0001] The invention belongs to the field of fine chemical synthesis technology and industrial waste resource reuse, and in particular relates to a method for preparing methylcyclopentanol by using methylcyclopentane waste oil as a raw material and using an ozone oxidation method under the condition of a nickel catalyst. Background technique [0002] Methylcyclopentane is a by-product in the process of hydration of cyclohexene to generate cyclohexanol in the cyclohexanol plant of Nylon Chemical Company. The components in the waste oil are methylcyclopentane accounting for about 50%, cyclohexane accounting for 45%, Other C 5-6 Alkanes account for about 5%. In recent years, with the expansion of nylon chemical production scale, the discharge of waste oil in the production process is increasing year by year. Reasonable design of routes, comprehensive utilization of waste oil, and development of new chemical products can not only reduce the industry's discharge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C35/06C07C29/48
Inventor 赵海鹏刘伟李霞王红专杨晓林冰于新功张秀欣娄恒灿
Owner HENAN UNIV OF URBAN CONSTR