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Method and system for continuously preparing tetrabutylurea by utilizing phosgene

A technology of tetrabutylurea and phosgene, applied in the preparation of urea derivatives, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of long reaction residence time, low space-time yield, low phosgene yield and the like

Pending Publication Date: 2022-05-13
QINGDAO UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Wherein patent document CN102702029A and CN108203400A have provided the process that adopts single phosgene to utilize batch reactor to prepare tetrabutylurea, have lower space-time yield; CN1668582A has provided a kind of method for continuously preparing tetrasubstituted urea, but Adopting the traditional two-stage series tank operation, due to the low water solubility of the raw material phosgene, the phosgene yield is low and the reaction residence time is long

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  • Method and system for continuously preparing tetrabutylurea by utilizing phosgene
  • Method and system for continuously preparing tetrabutylurea by utilizing phosgene

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[0019] The technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Apparently, the described embodiments are only some of the embodiments of this application, not all of them. Based on the embodiments in this application, all other embodiments obtained by those skilled in the art without making creative efforts belong to the scope of protection of this application.

[0020] In the description of this application, it should be noted that unless otherwise specified and limited, the terms "installation", "connection", and "connection" should be understood in a broad sense, for example, it can be a fixed connection or a detachable connection. Connected, or integrally connected; it can be mechanically connected, or electrically connected, or can communicate with each other; it can be directly connected, or indirectly connected through an intermedi...

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Abstract

The invention discloses a method and a system for continuously preparing tetrabutylurea by utilizing phosgene. The method comprises the following steps: dissolving phosgene in an organic solvent, feeding the obtained solution and an alkaline aqueous solution of dibutylamine into a first-stage photochemical reactor with high-strength mixing performance, carrying out an adiabatic first-stage reaction in the first-stage reactor, and feeding a reactant into a second-stage photochemical reaction kettle with long retention time to complete the residual reaction. After the reaction is finished, the reaction liquid is sent to an oil and water phase separator for separation, the water phase is subjected to wastewater treatment, the organic phase is sequentially subjected to distillation to recover the solvent for recycling, unreacted dibutylamine and an intermediate product dibutyl methylamine acyl chloride are evaporated and sent back to the secondary photochemical reactor to improve the reaction yield, and finally the product tetrabutyl urea is evaporated under high vacuum. And tower kettle residues are used as solid wastes. According to the method disclosed by the invention, continuous preparation of the tetrabutylurea is realized under the condition of not adding a catalyst, and unreacted dibutylamine and an intermediate product dibutyl methylamine acyl chloride can be repeatedly utilized, so that the utilization rate of raw materials is improved.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a method and system for continuously preparing tetrabutylurea by utilizing phosgene. Background technique [0002] Tetrabutylurea (molecular formula: C 17 h 36 N 2 O) is an intermediate in organic synthesis. It is a transparent or slightly yellowish liquid at room temperature. It is mainly used to replace trioctyl phosphate as a hydroanthraquinone solvent in the new process of producing hydrogen peroxide by anthraquinone method. [0003] The preparation method of tetrabutyl urea can be divided into phosgene method and non-phosgene method, and non-phosgene method is superior to the shortcomings such as more by-products, low yield and high cost, and is currently not competitive in industrial devices; phosgene The method also includes solid phosgene method, diphosgene method and single phosgene method. In the preparation process of the triphosgene and diphosgene me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C273/18C07C275/06B01D3/10B01J19/00
CPCC07C273/1809C07C273/189B01J19/00B01D3/10B01J2219/0004B01J2219/00033C07C275/06
Inventor 毕荣山蒋晓杨海兴刘彤慧闫科嘉侯梓桐陈海凤
Owner QINGDAO UNIV OF SCI & TECH