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A kind of method that utilizes micro-reaction device to prepare antioxidant 6ppd

A technology of micro-reaction device and anti-aging agent, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of low yield and long reaction time, and achieve large specific surface area, good product quality, The effect of high operational flexibility

Active Publication Date: 2018-08-31
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is to provide a method for preparing anti-aging agent 6PPD using a micro-reaction device, so as to solve the problems of low yield and long reaction time in the prior art

Method used

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  • A kind of method that utilizes micro-reaction device to prepare antioxidant 6ppd
  • A kind of method that utilizes micro-reaction device to prepare antioxidant 6ppd
  • A kind of method that utilizes micro-reaction device to prepare antioxidant 6ppd

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Effect test

Embodiment 1

[0030] In the microchannel reaction device, the diameter of the connecting pipe is 1 mm, the length of the liquid inlet pipe is 15 cm, the length of the connecting pipe between the microreactor and the outlet is 20 cm, and the specification of the back pressure valve is 8 bar.

[0031] Take 5g of p-aminodiphenylamine, add 200mL of methanol, and weigh 6.8g of methyl isobutyl ketone into the solution, stir at room temperature for 5min, mix evenly, transfer to the Erlenmeyer flask and pass into the microreactor. Pre-introduce hydrogen, exhaust the air in the gas-liquid reactor, block the gas outlet, adjust the hydrogen pressure reducing valve, the pressure is 10bar, and the gas flow rate is controlled by the gas flow meter to 0.05L / min. The liquid flow rate was controlled to be 0.3 mL / min, and the temperature was controlled to be 100°C. The liquid outlet is connected to the solid-liquid reactor filled with catalyst, and the temperature of the reactor is controlled at 100°C. The e...

Embodiment 2

[0033] In the microchannel reaction device, the inner diameter of the connecting pipe is 1 mm, the length of the liquid inlet pipe is 15 cm, the length of the connecting pipe between the microreactor and the outlet is 20 cm, and the specification of the back pressure valve is 8 bar.

[0034] Take 5g of p-aminodiphenylamine, add 200mL of methanol, and weigh 6.8g of methyl isobutyl ketone into the solution, stir at room temperature for 5min, mix evenly, transfer to the Erlenmeyer flask and pass into the microreactor. Pre-introduce hydrogen, exhaust the air in the gas-liquid reactor, block the gas outlet, adjust the hydrogen pressure reducing valve, the pressure is 10bar, and the gas flow rate is controlled by the gas flow meter to 0.1L / min. The liquid flow rate was controlled to be 1.0 mL / min, and the temperature was controlled to be 80°C. The liquid outlet is connected to the solid-liquid reactor filled with catalyst, and the temperature of the reactor is controlled at 80°C. Th...

Embodiment 3

[0036] In the microchannel reaction device, the diameter of the connecting pipe is 1 mm, the length of the liquid inlet pipe is 15 cm, the length of the connecting pipe between the microreactor and the outlet is 20 cm, and the specification of the back pressure valve is 8 bar.

[0037] Take 5g of p-aminodiphenylamine, add 200mL of methanol, and weigh 6.8g of methyl isobutyl ketone into the solution, stir at room temperature for 5min, mix evenly, transfer to the Erlenmeyer flask and pass into the microreactor. Pre-introduce hydrogen, exhaust the air in the gas-liquid reactor, block the gas outlet, adjust the hydrogen pressure reducing valve, the pressure is 10bar, and the gas flow rate is controlled by the gas flow meter to 0.05L / min. The liquid flow rate was controlled to be 1 mL / min, and the temperature was controlled to be 100°C. The liquid outlet is connected to the solid-liquid reactor filled with catalyst, and the temperature of the reactor is controlled at 100°C. The eff...

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Abstract

The invention discloses a method for preparation of an anti-aging agent 6PPD by using a micro-reactor; a homogeneous solution of p-aminodiphenyl amine and methyl isobutyl ketone and hydrogen gas are subjected to a reaction in a gas-liquid reactor, then are introduced into a solid-liquid reactor and are subjected to a reaction, and the obtained reaction liquid repeats the above operations. Compared with the prior art, the gas-liquid reactor and the solid-liquid reactor are connected in series, the gas-solid-liquid three-phase reaction is performed in a micro-channel, and eventually, the conversion rate of raw materials is improved and the reaction time is shortened. The micro-reactor has the advantages of large specific surface area and strong heat transfer and mass transfer abilities, and enables the reactions to be carried out efficiently; and the reaction temperature, time and material ratio and other conditions can be precisely controlled through the micro-channel reactor, by-products are reduced, and the security is improved.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for preparing anti-aging agent 6PPD by using a micro-reaction device. Background technique [0002] Antiaging agent 6PPD (Chinese name: (N-(1,3-dimethylbutyl)-N'-phenyl-p-phenylenediamine), CAS No.: 793-24-8) is an amine antiaging agent with medium performance One of the excellent general-purpose anti-aging agents, it has a good protective effect on thermal oxygen, cracking and flex fatigue aging, and has a passivation effect on variable-valence metals. Suitable for natural rubber, butadiene rubber, styrene-butadiene rubber, nitrile rubber and neoprene. Widely used in rubber products under dynamic and static stress and periodic deformation, it is the best choice for tire tread, sidewall, inner tube and conveyor belt protection system. Rubber anti-aging agent 6PPD is the development direction of rubber anti-aging agent in the future. With the development of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/52C07C211/55
CPCC07C209/52C07C249/02C07C211/55C07C251/08
Inventor 郭凯陈斌李昕黄思宇张锴朱晨杰欧阳平凯
Owner NANJING TECH UNIV
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