Method for synthesizing 1, 8-diazabicyclo undec-7-ene by adopting loop reactor

A loop reactor, diazabicyclo technology, applied in chemical instruments and methods, chemical/physical/physical-chemical stationary reactors, chemical industry, etc. Development, poor heat and mass transfer effects, etc., to achieve the effect of increased catalyst life and usage times, high energy utilization, and small energy loss

Inactive Publication Date: 2021-03-16
山东中科新材料研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional stirred reactors have problems such as limited rotation speed of stirring paddles, large energy loss, poor contact between gas and liquid phases, poor heat and mass transfer effects, and poor sealing, which restrict the further development of this type of reactor.

Method used

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  • Method for synthesizing 1, 8-diazabicyclo undec-7-ene by adopting loop reactor
  • Method for synthesizing 1, 8-diazabicyclo undec-7-ene by adopting loop reactor
  • Method for synthesizing 1, 8-diazabicyclo undec-7-ene by adopting loop reactor

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Embodiment 1

[0031] A kind of 1, the synthetic method of 8-diazabicycloundec-7-ene of the present invention, comprises the following steps:

[0032] Step 1: Add 3000kg caprolactam, 1800kg xylene, and 15kgKOH to the addition reaction kettle (3), stir and raise the temperature to 60°C and start adding 1560kg of acrylonitrile dropwise, and control the temperature of the dropwise addition at 70~80°C. After the dropwise addition, keep warm for 6 hours and end reaction;

[0033] Step 2: For the first time, feed the material into the loop reactor I6 with the feed pump I4 at 1400kg / hr, and turn on the circulation pump I8; at the same time, add 12.1kg of carbon-containing single-supported nickel alloy catalyst from the catalyst preparation kettle I7, and turn on the NH3 Buffer tank 2 outlet valve, Venturi ejector I5 inlet suction 66kgNH 3 / hr, start heating up, open H 2 Outlet valve of buffer tank 1, pressurize to 2.5Mpa, control temperature at 80°C, pass through cross-flow filter 10 after the rea...

Embodiment 2

[0036] Step 1: Add 3000kg of caprolactam, 1200kg of cumene, and 24kg of NaOH to the addition reaction kettle 3, stir and raise the temperature to 60°C and start adding 1680kg of acrylonitrile dropwise, and control the temperature of 60~70°C during the dropwise addition. After the dropwise addition, keep warm for 6 hours to end the reaction ;

[0037] Step 2: For the first time, the material is input into the loop reactor I6 with the feed pump I4 at 1280kg / hr, the circulation pump I8 is turned on, and the carbon-containing single-supported nickel alloy catalyst 12kg / hr is added from the catalyst preparation kettle I7 at the same time, and the NH 3 Buffer tank 2 outlet valve, Venturi injector I 5 inlet suction 60.3kgNH 3 / hr, start heating up, open H 2 Buffer tank 1 outlet valve, boost the pressure to 2Mpa, and control the temperature at 85°C. After the reaction is qualified, it is extracted at 85.3kg / hr through the cross-flow filter 10. Control the circulation amount and the...

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Abstract

According to A method for synthesizing the 1, 8-diazabicyclo undecene-7-ene by adopting the loop reactor, cyano hydrogenation is carried out by adopting a loop reactor technology, so that the mass andheat transfer efficiency is higher, the reaction pressure and temperature are reduced, the generation of secondary amine and tertiary amine is reduced by matching with a carbon-containing supported nickel alloy catalyst, and the yield is increased; cyclization dehydration is carried out by adopting a loop reactor technology, so that continuous reaction is realized; the same solvent is adopted inthe three-step reaction, so that the production efficiency is improved, and the solvent loss and energy consumption are reduced; and the total yield reaches 82% or above.

Description

Technical field: [0001] The invention belongs to the technical field of synthetic chemical engineering, and in particular relates to a method for synthesizing 1,8-diazabicycloundec-7-ene by using a loop reactor. Background technique: [0002] 1,8-Diazabicycloundec-7-ene (hereinafter referred to as DBU) is a super basic organic amine, which is widely used in the medical, pharmaceutical, electronic material and construction industries. Since DBU was jointly developed and researched by Japan's Sanyo Chemical Industry Co., Ltd. and the U.S. Abbott Laboratory in 1966, industrial products have been sold on the market in the early 1970s. The route adopted is to use caprolactam-acrylonitrile as the raw material, the first step is addition reaction, using toluene as the solvent, using inorganic base (KOH or NaOH) as the catalyst, reacting caprolactam and acrylonitrile, the product CEC is distilled to recover the solvent and enter the next step ; In the second step of hydrogenation r...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07D487/04B01J19/18B01J19/00B01J8/00
CPCC07D487/04B01J19/00B01J19/18B01J19/0006B01J8/00Y02P20/10
Inventor倪平李沈巍
Owner山东中科新材料研究院有限公司