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Method and device for synthesizing six-membered cyclic compound by continuous method

A cyclic compound and continuous method technology, applied in chemical instruments and methods, organic cyclization, organic chemistry, etc., can solve the problems of low reaction conversion rate, low safety performance, high energy consumption, etc., to improve product quality and yield , reaction conversion rate and safety performance improvement, energy consumption reduction effect

Inactive Publication Date: 2008-08-13
武汉新景化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0020] The object of the present invention is to provide a method and device for continuous synthesis of six-membered cyclic compounds, which solve the problems of low reaction conversion, low safety performance and high energy consumption in the existing methods, and improve product quality and Yield, to ensure the follow-up product quality

Method used

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  • Method and device for synthesizing six-membered cyclic compound by continuous method
  • Method and device for synthesizing six-membered cyclic compound by continuous method
  • Method and device for synthesizing six-membered cyclic compound by continuous method

Examples

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Effect test

Embodiment 1

[0029] Acrolein and vinyl methyl ether are mixed according to the molar ratio of 1:1.1, and then pumped into the mixing tank by a high-pressure metering pump at a pressure of 4 MPa, and then enter the first-stage tubular reactor. The temperature is controlled at 130°C, and the circulation ratio is circulation: output =10:1, the discharge part enters the 2-stage reactor, the temperature is controlled at 160°C, the circulation ratio is controlled at 5:1, the discharge part is controlled to enter the 3-stage reactor, and the temperature is controlled at 180°C. The material at the outlet of the third-stage reactor is separated from the raw materials acrolein and butadiene to obtain 2-methoxy-3,4-2H-dihydropyran with a content of 95%, a one-way conversion rate of 90%, and a yield of 92%.

Embodiment 2

[0031] Acrolein and vinyl ethyl ether are mixed according to the molar ratio of 1:1.1, then pumped into the mixing tank by a high-pressure metering pump at a pressure of 5 MPa, and then enter the first-stage tubular reactor. The temperature is controlled at 140° C., and the circulation ratio is circulation: discharge = 15:1, the discharge part enters the second-stage reactor, the temperature is controlled at 160°C, the circulation ratio is controlled at 5:1, the discharge part is controlled to enter the third-stage reactor, the temperature is controlled at 200°C, and the material at the outlet of the third-stage reactor passes through The raw materials of acrolein and butadiene are separated to obtain 2-ethoxy-3,4-2H-dihydropyran with a content of 92%, a single-pass conversion rate of 88%, and a yield of 91%.

Embodiment 3

[0033] Acrolein and butadiene are mixed according to the molar ratio of 1:1.1, then pumped into the mixing tank by a high-pressure metering pump at a pressure of 3 MPa, and then enter the first-stage tubular reactor. The temperature is controlled at 80-100°C, and the circulation ratio is: circulation: out Material=50:1, the discharge part enters the 2nd section reactor, the temperature is controlled at 100-200 °C, the circulation ratio is controlled at 20:1, the discharge part enters the 3rd section reactor, the temperature is controlled at 200 °C, and the circulation ratio is controlled as 10:1, the material at the outlet of the third-stage reactor is separated from the raw materials acrolein and butadiene to obtain 1,2,5,6-tetrahydrobenzaldehyde with a content of 93%, a single-pass conversion rate of 91%, and a yield of 94%.

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Abstract

The invention relates to a compound production method, particularly to a synthesis method and apparatus of hexahydric cyclocompounds by using a continuation method. Dienophile and diene mixtures are added in a multi-segment tubular reactor according to a mol ratio of 1-2:1 to perfrom reaction, the reaction temperature of a first segment is controlled in 50-200 DEG C, the cycle ratio is circulation:discharge=15:1, the discharged portion enters into a second segment of reactor, the temperature is controlled in 100-300 DEG C to perform reaction, the cycle ratio is 5:1, the discharged portion enters into a third segment of reactor, the temperature is controlled in 150-350 DEG C to perform reaction, the discharged material of the end reactor is separated, cooled and then materials are educed to be rectified so as to obtain products, the non-reacted materials is cycled to continue reaction. The invention improves the reaction conversion rate and safty performance, largely reduces energy consumption, enhaces product quality and yield, ensures subsequent product quality.

Description

technical field [0001] The invention relates to a production method of a compound, in particular to a method for continuously synthesizing a six-membered cyclic compound and a device thereof. Background technique [0002] Compounds containing a reactive double or triple bond (dienophiles) undergo 1,4-addition to conjugated dienes (dienes) to form six-membered cyclic compounds: [0003] [0004] This reaction is named Diels-Alder reaction, which is very easy to carry out and has a fast reaction speed, and has a wide range of applications. It is a very important method for synthesizing cyclic compounds. The Diels-Alder reaction is an unsaturated compound containing a double bond or a triple bond (with carbonyl or carboxyl electron-withdrawing groups on its flanks - a dienophile) and a chain or cyclic compound containing a conjugated double bond system (a diene ) from a "1,4-" addition cyclization reaction to generate a six-membered carbocyclic hydrogenated aromatic compoun...

Claims

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Application Information

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IPC IPC(8): C07B37/12C07D309/30C07C47/42
Inventor 王明星阎璟琪焦格明江柏生
Owner 武汉新景化工有限责任公司
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