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Continuous pyrolysis fluorination process and equipment of arylamine hydrogen fluoride diazonium salt

A process and technology of pyrolysis liquid, which is applied in the field of continuous pyrolysis fluorination process and equipment of arylamine hydrogen fluoride diazonium salt, which can solve the problem that the complete pyrolysis conversion of diazonium salt cannot be guaranteed, and there is no successful precedent for industrialization, and the The problem of uneven time distribution can reduce energy consumption and labor costs, eliminate security risks, and shorten the response cycle.

Pending Publication Date: 2021-07-23
大连鼎燕医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the uneven distribution of reaction residence time in this process, the complete conversion of diazonium salt pyrolysis cannot be guaranteed, and the equipment configuration is relatively complicated. So far, no successful industrialization precedent has been seen.

Method used

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  • Continuous pyrolysis fluorination process and equipment of arylamine hydrogen fluoride diazonium salt
  • Continuous pyrolysis fluorination process and equipment of arylamine hydrogen fluoride diazonium salt
  • Continuous pyrolysis fluorination process and equipment of arylamine hydrogen fluoride diazonium salt

Examples

Experimental program
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Effect test

example 1

[0065] use as figure 1 The falling film pyrolysis reactor with structure and configuration has three stages in total. The solution of aniline hydrogen fluoride diazonium salt prepared by conventional methods is continuously added to the upper part of the falling film pyrolysis reactor, and the temperatures of the first, second, and third stage reactors are controlled as follows: 20°C, 30°C, 40°C, control the temperature of the receiving tank at 45-50°C, and continue to keep warm in the receiving tank for 2 hours after the feeding is completed, and the reaction is regarded as the end of the reaction when no nitrogen is generated. After separation and purification by conventional methods, fluorobenzene with a content of 99.9% was obtained, and the yield was 91.8%.

example 2

[0067] use as figure 1 There are 5 stages of falling film pyrolysis reactors in structure and configuration. The solution of aniline hydrogen fluoride diazonium salt prepared by conventional methods is continuously added to the upper part of the falling film pyrolysis reactor to control the first, second, third, fourth and fifth reactors. The temperatures in the receiving tank were 20°C, 25°C, 30°C, 35°C, and 40°C respectively, and the temperature in the receiving tank was controlled at 45-50°C. End of reaction. After separation and purification by conventional methods, fluorobenzene with a content of 99.9% was obtained, and the yield was 92.2%.

example 3

[0069] use as figure 1 The structure and configuration of the falling film pyrolysis reactor has 5 stages in total. The solution of p-toluidine hydrogen fluoride diazonium salt prepared by conventional methods is continuously added to the upper part of the falling film pyrolysis reactor to control the first, second, third, fourth, and fifth stages The temperature of the reactor is 20°C, 25°C, 30°C, 35°C, and 40°C, and the temperature in the receiving tank is controlled at 45-50°C. After the feeding is completed, the reaction is continued for 2 hours in the receiving tank, so that no nitrogen gas is seen. Generation is considered complete for the reaction. After separation and purification by conventional methods, p-fluorotoluene with a content of 99.9% was obtained, and the yield was 93.5%.

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Abstract

The invention discloses a continuous pyrolysis fluorination process and equipment for arylamine hydrogen fluoride diazonium salt. The equipment mainly comprises a falling film pyrolysis reaction device, the reaction device comprises multiple stages of falling film pyrolysis reactors which are sequentially connected in series from top to bottom, and any stage of falling film pyrolysis reactor is formed by processing a corrosion-resistant cylinder material. Any stage of falling film pyrolysis reactor comprises a plurality of material pore channels and a plurality of cold and hot medium pore channels; the plurality of material pore channels are longitudinally arranged in the reactor in parallel, and the plurality of cold and hot medium pore channels are transversely arranged in the reactor in parallel; different reaction temperatures are controlled by each stage of reactor, a cascade temperature control system with temperature programmed from top to bottom is formed, continuous and safe production of the pyrolytic fluorination reaction of the arylamine hydrogen fluoride diazonium salt is realized through the combination of the process and the equipment, and meanwhile, the yield of the product is improved.

Description

technical field [0001] The invention belongs to the technical field of chemical preparation, and in particular relates to a continuous pyrolysis fluorination process and equipment of arylamine hydrogen fluoride diazonium salt. Background technique [0002] The synthesis process of arylamine hydrogen fluoride diazonium salt to prepare fluorinated aromatics by thermal decomposition reaction is as follows: [0003] [0004] In the formula, the position of the substituent R is not limited, the number of the substituent R is zero to more, and the substituent R includes but not limited to an alkyl group or a halogen. [0005] According to existing literature reports, the above process may be realized through the following three processes. [0006] Process 1: Since the above reaction is an exothermic reaction, in order to ensure that the heat transfer rate is greater than the exothermic rate, the existing industrial preparation process can only control the reaction rate by slow...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J6/00B01J19/24C07C25/13C07C17/093
CPCB01J6/008B01J19/247B01J19/245C07C17/093C07C25/13
Inventor 王洋陈荣业蔡鲁伯吕永智董志军李龙
Owner 大连鼎燕医药化工有限公司
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