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Method for synthesizing 2-amino-4-chloro-5-nitrophenol in micro-channel reactor

A microchannel reactor, nitrophenol technology, applied in chemical instruments and methods, preparation of aminohydroxy compounds, chemical/physical/physical-chemical reactors, etc., can solve production safety and environmental pollution, high cost and low production efficiency and other problems, to achieve the effect of reducing production and by-products, reducing the possibility of safety accidents, and reducing production risks

Inactive Publication Date: 2020-04-03
沈阳感光化工研究院有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 2-Amino-4-chloro-5-nitrophenol is an important intermediate in the synthesis of photosensitive materials, dyes, medicines and pesticides. It has a wide range of uses and is a promising intermediate. -5 Nitrophenol has never had an ideal industrial production method
These two methods are backward in technology, long in process, low in yield and heavy in pollution.
A document in the Photosensitive Society discloses a method for obtaining 3,4-dinitropyrazole by nitration reaction in a conventional reactor, which may cause production safety and environmental pollution, and is not conducive to continuous production
Moreover, due to the relationship between the size of the equipment, the traditional batch reactor often has the problem of low mass and heat transfer efficiency of the reactor, which is easy to cause uneven temperature and concentration, resulting in low yield, low production efficiency, and poor quality stability of intermittent operation products. , especially when dealing with "dangerous processes" such as nitrification and hydrogenation reduction, the safety hazards of the kettle reaction process are great, and due to factors such as reaction atom economy and process practicability, the alternatives to these "dangerous processes" are often costly and the route is longer

Method used

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  • Method for synthesizing 2-amino-4-chloro-5-nitrophenol in micro-channel reactor
  • Method for synthesizing 2-amino-4-chloro-5-nitrophenol in micro-channel reactor
  • Method for synthesizing 2-amino-4-chloro-5-nitrophenol in micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-5

[0018] Example 1-5: Synthesis of 5-chloro-2-methyl-6-nitro-benzoxazole of the present invention: under ice-water bath, 11g of concentrated sulfuric acid and 7g of 65% fume were mixed at a molar ratio of 1.1:1 Slowly mix nitric acid to obtain nitric-sulfur mixed acid, under ice-water bath, dissolve 16.7g (0.1mol) 5-chloro-2-methylbenzoxazole in 98% sulfuric acid at a molar ratio of 1:1, and mix nitric-sulfur mixed acid and the sulfuric acid solution of 5-chloro-2-methylbenzoxazole are pumped into the microchannel reactor respectively, and the flow rate of the sulfuric acid solution of 5-chloro-2-methylbenzoxazole is controlled to be 0.5mL / min in this example, The flow rate of nitric acid mixed acid is 0.3mL / min, the retention time is 10min, and the reaction temperature is 10°C.

[0019] Control the molar ratio of nitric acid to 5-chloro-2-methylbenzoxazole to be 1-1.2:1. After the two liquids are mixed and contacted in the microchannel reactor at 10°C for a moment and react, th...

Embodiment 6-10

[0023] Embodiment 6-10: The difference between this example and Example 1 is: the synthesis of 5-chloro-2-methyl-6-nitro-benzoxazole in this example: under ice-water bath, the molar ratio is 1 -1.8:1 Slowly mix concentrated sulfuric acid and 65% fuming nitric acid to obtain nitric-sulfur mixed acid, under ice-water bath, mix 16.7g (0.1mol) 5-chloro-2-methylbenzoxan with a molar ratio of 1:1 Azole was dissolved in 98% sulfuric acid, and the sulfuric acid solutions of nitric acid and 5-chloro-2-methylbenzoxazole were pumped into the microchannel reactor respectively. In this case, 5-chloro-2-methylbenzoxazole was controlled. The flow rate of the sulfuric acid solution of oxazole was 0.4 L / min, the flow rate of nitric acid mixed acid was 0.5 mL / min, the retention time was 8 min, and the reaction temperature was 10°C.

[0024] Control the molar ratio of nitric acid to 5-chloro-2-methylbenzoxazole to be 1:1. After the two liquids are mixed and contacted instantly in the microchanne...

Embodiment 1

[0027] Embodiment 11-15: The difference between this example and Example 1 is: the synthesis of 5-chloro-2-methyl-6-nitro-benzoxazole in this example: under ice-water bath, the molar ratio is 1.2 :1 24g vitriol oil and 14g 65% fuming nitric acid are slowly mixed to obtain nitric acid mixed acid, under ice-water bath, 33.4g (0.2mol) 5-chloro-2-methylbenzene will be mixed in molar ratio 1:1-1.5 oxazole is dissolved in 98% sulfuric acid, and the sulfuric acid solution of nitric acid and 5-chloro-2-methylbenzoxazole is pumped into the microchannel reactor respectively. In this example, 5-chloro-2-methyl The flow rate of the sulfuric acid solution of benzoxazole is 0.5mL / min, the flow rate of nitric acid mixed acid is 0.4mL / min, the retention time is 5min, and the reaction temperature is 5°C.

[0028] Control the molar ratio of nitric acid to 5-chloro-2-methylbenzoxazole to be 1:1. After the two liquids are mixed and contacted in a microchannel reactor at 5°C for a moment and react...

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Abstract

The invention discloses a method for synthesizing 2-amino-4-chloro-5-nitrophenol. The 2-amino-4-chloro-5-nitrophenol is prepared from 5-chloro-2-methylbenzoxazole through a series reaction using a micro-channel reactor and a batch reactor. The 2-amino-4-chloro-5-nitrophenol is synthesized by utilizing the micro-channel reactor, so that the adverse consequences that the process is difficult to control, dangers are caused by local overheating easily, side reactions are generated easily and the like in a conventional tank reactor are avoided, the intrinsic safety of the method is improved, and the method has the advantages of high production efficiency, high economical property, easiness in industrialization, and realization of continuous production. The micro-channel reactor has the characteristics of low price, convenience in transportation and cleaning, high heat and mass transfer efficiency, and easiness in industrial amplification. The synthesis method has the advantages of simple, cheap and accessible starting materials, simple technique, effectiveness in lowering of the production cost, and suitableness for industrial production.

Description

technical field [0001] The invention belongs to the technical field of synthesizing photosensitive materials and pharmaceutical intermediates, in particular to a method for synthesizing 2-amino-4-chloro-5-nitrophenol in a microchannel reactor. Background technique [0002] 2-Amino-4-chloro-5-nitrophenol is an important intermediate in the synthesis of photosensitive materials, dyes, medicines and pesticides. It has a wide range of uses and is a promising intermediate. There is no ideal industrial production method for -5 nitrophenol. At present, there are two main production methods for this intermediate, one is to synthesize 2-amino-4-chloro-5-nitrophenol through phosgene and 2-amino-4-chlorophenol; the other is traditional still-type closed-loop , nitrification, hydrolysis three-step method or two-step method. These two methods are backward in technology, long in process, low in yield and heavy in pollution. A document in the Photosensitive Society discloses a method fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/00C07C215/76B01J19/00
CPCC07C213/00C07D263/56B01J19/0093
Inventor 李响翟治宇刘勇
Owner 沈阳感光化工研究院有限公司
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