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Production process of deuterated acetonitrile

A deuterated acetonitrile and production process technology, applied in the field of deuterated acetonitrile production process, can solve the problems of low deuterated degree of deuterated acetonitrile, high catalyst consumption, etc., achieve the effects of reducing consumption, increasing contact area, and saving production costs

Pending Publication Date: 2022-05-06
山东汉峰新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The deuterated acetonitrile synthesis process mainly adopts the exchange method, and under the action of the basic metal salt catalyst, the hydrogen-deuterium exchange reaction occurs between acetonitrile and heavy water. high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The present embodiment provides a kind of supported catalyst, is made by the following steps:

[0021] Nano Al 2 o 3 Placed in a constant temperature drying oven, pretreated at 120°C for 3 hours in an air atmosphere to obtain dry nano-Al 2 o 3 , then add 15g of potassium carbonate to 200mL of deionized water, stir magnetically for 4h at room temperature to obtain potassium carbonate solution, then add 60g of dry nano-Al 2 o 3 , stirred for 4 hours, left to stand for 24 hours for aging treatment, then placed in an oven at 120°C for 4 hours, and finally placed in a box-type resistance furnace for calcination at 200°C for 4 hours to obtain a supported catalyst.

Embodiment 2

[0023] The present embodiment provides a kind of supported catalyst, is made by the following steps:

[0024] Nano Al 2 o 3 Placed in a constant temperature drying oven, pretreated at 120°C for 4 hours in an air atmosphere to obtain dry nano-Al 2 o 3 , then add 18g of potassium carbonate to 200mL of deionized water, stir magnetically for 4h at room temperature to obtain potassium carbonate solution, then add 60g of dry nano-Al 2 o 3 , stirred for 5 hours, left to stand for 24 hours for aging treatment, then placed in an oven at 120°C for 4 hours, and finally placed in a box-type resistance furnace for calcination at 200°C for 4 hours to obtain a supported catalyst.

Embodiment 3

[0026] The present embodiment provides a kind of supported catalyst, is made by the following steps:

[0027] Nano Al 2 o 3 Placed in a constant temperature drying oven, pretreated at 120°C for 5 hours in an air atmosphere to obtain dry nano-Al 2 o 3 , then add 20g of potassium carbonate to 200mL of deionized water, stir magnetically for 4h at room temperature to obtain potassium carbonate solution, then add 60g of dry nano-Al 2 o 3 , stirred for 6 hours, left to stand for 24 hours for aging treatment, then placed in an oven at 120°C for 4 hours, and finally placed in a box-type resistance furnace for calcination at 200°C for 4 hours to obtain a supported catalyst.

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PUM

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Abstract

The invention relates to a production process of deuterated acetonitrile, which belongs to the technical field of fine chemical engineering, and comprises the following steps: step 1, adding acetonitrile, heavy water and a supported catalyst into a reaction bottle, heating to 60 DEG C, stirring to react for 5 hours, distilling the reaction product at 95 DEG C, and collecting the distillation product to obtain a deuterated acetonitrile-water azeotrope; 2, sodium sulfate is added into the deuterated acetonitrile-water azeotrope, liquid separation is conducted after stirring, an upper-layer substance is collected, and a deuterated acetonitrile finished product is obtained.According to the method, the organic phase acetonitrile in the deuterated acetonitrile-water azeotrope is separated out by adopting the two-phase property phenomenon of a concentrated alkali method, deuterated acetonitrile with the purity and the deuterated degree is obtained, and the purity of the deuterated acetonitrile is greatly improved. A supported catalyst is adopted to replace a conventional alkali metal catalyst, the contact area between the catalyst and reaction raw materials is increased, the consumption of a potassium carbonate catalyst is reduced, and the production cost is saved.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a production process of deuterated acetonitrile. Background technique [0002] Deuterated acetonitrile is an organic solvent that can be used as an aprotic solvent in organic reactions. Deuterated acetonitrile is also an organic solvent used in NMR chromatography. Mainly used as nuclear magnetic resonance reagents, pharmaceuticals and synthesis, photoelectric material modification, laboratory special reagents, chemicals, scientific research, testing, etc. [0003] The deuterated acetonitrile synthesis process mainly adopts the exchange method, under the action of the basic metal salt catalyst, the hydrogen-deuterium exchange reaction occurs between acetonitrile and heavy water, but the deuterated acetonitrile obtained by the existing production process has a low degree of deuteration and a relatively high catalyst consumption. high. Contents of the inventio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/03C07C253/34C07C253/00C07B59/00
CPCC07C253/00C07C253/34C07B59/001C07B2200/05C07C255/03Y02P20/584
Inventor 林崇熙张坤王化建殷浩战垒刘锦辉
Owner 山东汉峰新材料科技有限公司