Method for preparing 2, 2-bis (3-nitro-4-hydroxyphenyl) hexafluoropropane by microchannel reactor

A microchannel reactor, hydroxyphenyl technology, applied in chemical instruments and methods, chemical/physical/physical chemical reactors, preparation of nitro compounds, etc. Exacerbating problems such as rapid reaction, avoiding intermediate separation steps, and reducing by-products

Pending Publication Date: 2021-07-13
海南夸克科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, because bisphenol AF contains active phenolic hydroxyl groups, nitration reaction is very easy to occur. At the same time, due to the exothermic addition of nitric acid, the temperature of the reactant rises sharply, which will cause the phenomenon of intensified side reactions.
[0006] So far, there has been no report on the preparation of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane by nitration reaction in a microchannel reactor

Method used

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  • Method for preparing 2, 2-bis (3-nitro-4-hydroxyphenyl) hexafluoropropane by microchannel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Refer to figure 1 Determine the connection method, the heat transfer medium of the heat exchanger is heat transfer oil. The diameter of the microchannel reactor is 0.5mm.

[0031] (2) 150g of bisphenol AF and 600g of dichloromethane were mixed and stirred to form a bisphenol AF solution; 86g of nitric acid (concentration 65%) and 172g of sulfuric acid (concentration 98%) were prepared into a mixed acid solution. After the two systems were preheated at 0°C, they were pumped into the microchannel reactor through the metering pump at the flow rate of 25g / min and 8.6g / min respectively. At this time, the molar ratio of bisphenol AF to mixed acid was 1:2, and the reaction temperature was controlled The temperature is 45°C, the residence time is 30s, and the temperature of the reaction product is lowered through the cooling coil to obtain a discharge liquid containing 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane.

[0032] (3) Add 1 L of 5% sodium bicarbonate solutio...

Embodiment 2

[0035] (1) Refer to figure 1 Determine the connection method, the heat transfer medium of the heat exchanger is heat transfer oil. The diameter of the microchannel reactor is 3mm.

[0036] (2) 150g of bisphenol AF and 750g of dichloroethane were mixed and stirred to form a bisphenol AF solution; 108g of nitric acid (concentration 65%) and 324g of sulfuric acid (concentration 95%) were prepared into a mixed acid solution. After the two systems were preheated at 10°C, they were pumped into the microchannel reactor at the flow rate of 15g / min and 7.2g / min respectively through the metering pump. At this time, the molar ratio of bisphenol AF to nitric acid was 1:2.5, and the reaction temperature was controlled The temperature is 30°C, and the residence time is 60s. The temperature of the reaction product is lowered through the cooling coil to obtain a discharge liquid containing 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane.

[0037] (3) Add 1 L of 5% sodium bicarbonate solut...

Embodiment 3

[0039] (1) Refer to figure 1 Determine the connection method, the heat transfer medium of the heat exchanger is heat transfer oil. The diameter of the microchannel reactor is 5mm.

[0040] (2) 150g of bisphenol AF and 900g of chloroform were mixed and stirred to form a bisphenol AF solution; 120g of nitric acid (concentration 70%) and 480g of sulfuric acid (concentration 90%) were prepared into a mixed acid solution. After the two systems were preheated at 20°C, they were pumped into the microchannel reactor at the flow rate of 11.7g / min and 6.7g / min respectively through the metering pump. At this time, the molar ratio of bisphenol AF to nitric acid was 1:3, and the reaction was controlled The temperature was 15° C., and the residence time was 90 s. The temperature of the reaction product was lowered through a cooling coil to obtain a discharge liquid containing 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane.

[0041](3) Add 1 L of 5% sodium bicarbonate solution to the di...

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Abstract

The invention discloses a method for preparing 2, 2-bis (3-nitro-4-hydroxyphenyl) hexafluoropropane by a microchannel reactor. The method comprises the following steps: (1) fully mixing and preheating bisphenol AF and an organic solvent to obtain a bisphenol AF solution, and respectively introducing the bisphenol AF solution and a preheated nitrating agent as two strands of materials into a continuous flow microchannel reactor through a metering pump; (2) controlling the flow rate of the material through a metering pump, enabling the bisphenol AF solution and the nitrating agent to respectively enter a micro-channel reactor module for mixed reaction, and enabling a product to flow out from an outlet of the reactor; and (3) carrying out post-treatment on the material obtained from the outlet of the microchannel reactor to obtain a pure product of 2, 2-bis (3-nitro-4-hydroxyphenyl) hexafluoropropane. The method provided by the invention can realize continuous production, has mild reaction conditions, high reaction efficiency and high yield, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for preparing 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane with a microchannel reactor. Background technique [0002] 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane is a very important chemical raw material and is also used for the synthesis of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane It can be used as a monomer for the preparation of polymer materials, and is widely used in the fields of aviation, aerospace, electronics, automobiles, electronic communications, and precision machinery automation. [0003] At present, most of the industrial preparation of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane uses concentrated nitric acid, nitric acid mixed acid, metal nitrate and other nitrating agents to complete the nitration reaction, but the actual production will The production of a large amount of acidic wastewater does not conform to the production c...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/26B01J19/00
CPCC07C201/08B01J19/0093C07C205/26
Inventor 韩津蓝艳
Owner 海南夸克科技有限公司
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