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Preparation method of heptafluoroisobutyronitrile

A technology of heptafluoroisobutyronitrile and heptafluoroisobutyramide, which is applied to the purification/separation of carboxylic acid nitriles, organic chemistry, etc., can solve the problems of easy deactivation of catalysts, low reaction yield, harmful environment, etc., and achieve improved product quality. Selectivity, simple preparation process, no effects of three wastes

Pending Publication Date: 2022-03-01
ZHEJIANG RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The patent CN109320436A of Beijing Yuji Company discloses a method for preparing perfluoronitrile by dehydration of heptafluoroisobutyramide catalyzed by metal oxides. The product has a purity of 99.5% and a yield of 99.2%. However, cobalt with a high price is used in this method , niobium and other catalysts, and the catalyst is easily deactivated, the composition is complex and difficult to recycle, and these heavy metal compounds are harmful to the environment
[0010] When adopting the dehydration of heptafluoroisobutyramide to prepare heptafluoroisobutyronitrile, most of the dehydrating agents / catalysts disclosed in the prior art are dehydrating agents such as trifluoroacetic anhydride or trifluoroacetic anhydride / triethylamine / N,N-di Mixed dehydration system such as methyl formamide system or metal oxidant such as cobalt oxide, or the reaction yield is low, or the catalyst is easily deactivated and the cost is high

Method used

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  • Preparation method of heptafluoroisobutyronitrile
  • Preparation method of heptafluoroisobutyronitrile
  • Preparation method of heptafluoroisobutyronitrile

Examples

Experimental program
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Embodiment 1

[0032] 3A molecular sieves were calcined at 300°C for 4 hours under the protection of nitrogen, and 100g of 3A molecular sieves were loaded into a tubular reactor, and heptafluoroisobutyramide (213g, 1mol) was heated in a preheater, preheated to 160°C, and put into a tubular reactor. In the reactor, the reaction temperature is 200°C, the residence time is 30s, the reaction pressure is 0.05MPa, and the material flow rate is 0.2m / s. Heptafluoroisobutyronitrile was collected and tested: the purity of heptafluoroisobutyronitrile was 99.0%, and the yield was 93.2%.

Embodiment 2

[0034] The 5A molecular sieve was roasted at 300°C for 4 hours under the protection of nitrogen, and 100g of 5A molecular sieve was loaded into the tubular reactor. Heptafluoroisobutyramide (213g, 1mol) was heated in the preheater, preheated to 160°C, and entered into the tubular reaction device, the reaction temperature is 200°C, the residence time is 30s, the reaction pressure is 0.05MPa, and the material flow rate is 0.2m / s. Heptafluoroisobutyronitrile was collected and tested: the purity of heptafluoroisobutyronitrile was 98.7%, and the yield was 90.1%.

Embodiment 3

[0036] The β molecular sieve was roasted at 300°C for 4 hours under the protection of nitrogen, and 100g of the β molecular sieve was loaded into the tubular reactor, and heptafluoroisobutyramide (213g, 1mol) was sent to the preheater for heating, preheated to 160°C, and entered into the tubular reaction device, the reaction temperature is 200°C, the residence time is 30s, the reaction pressure is 0.05MPa, and the material flow rate is 0.2m / s. Heptafluoroisobutyronitrile was collected and tested: the purity of heptafluoroisobutyronitrile was 98.2%, and the yield was 92.7%.

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Abstract

The invention discloses a preparation method of heptafluoroisobutyronitrile, the preparation method comprises the following steps: a raw material heptafluoroisobutyramide is subjected to a dehydration reaction under the action of a catalyst to obtain heptafluoroisobutyronitrile, and the catalyst is a molecular sieve catalyst selected from at least one of an HY molecular sieve, a NaY molecular sieve, a beta molecular sieve ZSM-5 molecular sieve, a 3A molecular sieve, a 4A molecular sieve and a 5A molecular sieve. The method has the advantages of high product selectivity, high reaction efficiency, suitability for industrial production and the like.

Description

technical field [0001] The invention relates to the field of insulating gas, in particular to a method for preparing heptafluoroisobutyronitrile through catalytic dehydration of molecular sieves. Background technique [0002] Sulfur hexafluoride is the most widely used insulating gas. It has been used for more than 70 years, but its global warming potential (GWP) is 23600, and its atmospheric life is as high as 3200 years. It is a gas with a very serious greenhouse effect. Heptafluoroisobutyronitrile has a global warming potential (GWP) of 2100 and an atmospheric life of 30 years. It is currently the most potential environmental protection gas to replace sulfur hexafluoride. [0003] At present, the preparation of heptafluoroisobutyronitrile mainly uses heptafluoroisobutyryl fluoride as raw material, first prepares heptafluoroisobutyramide, and then generates heptafluoroisobutyronitrile under the action of dehydrating agent and alkali. PCT patent WO2013151741A1 discloses th...

Claims

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Application Information

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IPC IPC(8): C07C253/34C07C255/10
CPCC07C253/34C07C255/10
Inventor 陈伟蒋强倪航杨汪松
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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