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A kind of preparation method of nanophase transfer catalyst hydrogel for synthesizing 2-methyl-4-heptafluoroisopropylaniline

A technology of heptafluoroisopropylaniline and phase transfer catalyst, applied in organic compound/hydride/coordination complex catalyst, chemical instrument and method, preparation of amino compound from amine, etc., can solve the problem of phase transfer catalyst tetrabutyl Ammonium hydrogen sulfate is used in large quantities, cannot be reused, and has high production costs. It achieves the effects of low production costs, reduced impact, and easy recovery.

Active Publication Date: 2022-04-08
南京科力硕生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the phase transfer catalyst tetrabutylammonium hydrogen sulfate used in the reaction process is used in a large amount and cannot be reused, so that the production cost is too high

Method used

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  • A kind of preparation method of nanophase transfer catalyst hydrogel for synthesizing 2-methyl-4-heptafluoroisopropylaniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The preparation method of embodiment 1 2-methyl-4-heptafluoroisopropylaniline

[0036] (1) Weigh 100g of multi-walled carbon nanotubes and 10g of Tween-80 into 1L of water, ultrasonically disperse for 30min, the ultrasonic power is 1000W, then add 10g of cyclodextrin, stir and mix at room temperature for 1h, centrifuge and wash 3 times, the centrifugation speed 8000rpm, the centrifugation time is 5min, and the nano phase transfer catalyst is obtained after natural air drying.

[0037] (2) Weigh 100g of polyvinyl alcohol and add it to 1L of water, heat and stir to 95°C, after it is completely dissolved, cool down to 40°C, then add 50g of nano phase transfer catalyst, stir and mix at room temperature for 2h, then freeze at -20°C for 24h, After thawing at room temperature, the nano phase transfer catalyst hydrogel was obtained.

[0038] (3) Add 200g of nano phase transfer catalyst hydrogel, 155g of 2-methylaniline, 95g of sodium bisulfite, 200g of sodium dithionite, 155g ...

Embodiment 2

[0039] Example 2 The preparation method of 2-methyl-4-heptafluoroisopropylaniline

[0040] (1) Weigh 100g of multi-walled carbon nanotubes and 10g of Span-80 into 1L of water, ultrasonically disperse for 30min, and the ultrasonic power is 1000W, then add 10g of PEG-400, stir and mix at room temperature for 2h, centrifuge and wash 3 times, the centrifugation speed 8000rpm, centrifugation time is 10min, freeze-dried to obtain nano phase transfer catalyst.

[0041] (2) Weigh 100g of gelatin and add it to 1L of water, heat and stir to 80°C, after it is completely dissolved, cool down to 40°C, then add 50g of nano-phase transfer catalyst, stir and mix at room temperature for 2h, then freeze at -20°C for 24h, and thaw at room temperature Finally, the nano phase transfer catalyst hydrogel is obtained.

[0042](3) Add 200g of nano phase transfer catalyst hydrogel, 155g of 2-methylaniline, 95g of sodium bisulfite, 200g of sodium dithionite, 155g of sodium bicarbonate, and 720g of ice ...

Embodiment 3

[0043] Example 3 The preparation method of 2-methyl-4-heptafluoroisopropylaniline

[0044] (1) Weigh 2000g of multi-walled carbon nanotubes and 200g of Tween-80 into 20L of water, ultrasonically disperse for 30min, the ultrasonic power is 2000W, then add 200g of cyclodextrin, stir and mix at room temperature for 1h, centrifuge and wash 3 times, the centrifugation speed 8000rpm, the centrifugation time is 5min, and the nano phase transfer catalyst is obtained after natural air drying.

[0045] (2) Weigh 2000g of polyvinyl alcohol and add it to 20L of water, heat and stir to 95°C, after it is completely dissolved, cool down to 40°C, then add 1000g of nano phase transfer catalyst, stir and mix at room temperature for 2h, then freeze at -20°C for 24h, After thawing at room temperature, the nano phase transfer catalyst hydrogel was obtained.

[0046] (3) Add 4000g of nano phase transfer catalyst hydrogel, 3100g of 2-methylaniline, 1900g of sodium bisulfite, 4000g of sodium dithion...

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Abstract

The invention belongs to the field of synthesis of fine chemical intermediates, and discloses a preparation method of a nano phase transfer catalyst hydrogel for synthesizing 2-methyl-4-heptafluoroisopropylaniline. Specifically, the method includes the following steps: (1) Ultrasonic mixing of multi-walled carbon nanotubes and surfactants, adding phase transfer catalyst, stirring and mixing, and centrifugal drying to obtain nano phase transfer catalyst; (2) Encapsulation of nano phase with hydrogel Transfer catalyst; (3) Under the action of nanophase transfer catalyst hydrogel and initiator, 2-methylaniline and heptafluoro-2-bromopropane react to synthesize 2-methyl-4-heptafluoroisopropylaniline. Compared with the prior art, the nano phase transfer catalyst hydrogel used in the present invention can be reused, reduces the use cost of the phase transfer catalyst, and improves the production efficiency of 2-methyl-4-heptafluoroisopropylaniline .

Description

technical field [0001] The invention belongs to the field of synthesis of fine chemical intermediates, in particular to a method for preparing a nano phase transfer catalyst hydrogel for synthesizing 2-methyl-4-heptafluoroisopropylaniline. Background technique [0002] 2-Methyl-4-heptafluoroisopropylaniline, as a class of perfluoroalkylaniline derivatives, can be widely used as raw materials or intermediates of pesticides, medicines, coatings, rubber, surfactants, etc. In the field of pesticides, 2-methyl-4-heptafluoroisopropylaniline is the key intermediate of flubendiamide. The industrial production of 2-methyl-4-heptafluoroisopropylaniline needs to meet the goals of high efficiency, safety, low cost, and low pollution, so that the process can create higher economic and social benefits. [0003] Phase transfer catalysis is a kind of organic synthesis method used in heterogeneous reactions. Phase transfer catalysts can speed up the reaction rate, lower the reaction tempera...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06C07C209/68C07C211/52
CPCB01J31/069B01J31/068B01J31/065C07C209/68B01J2231/4205B01J35/23C07C211/52
Inventor 许晖曹逊
Owner 南京科力硕生物科技有限公司