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Method and device for preparing fluorine sulfimide acid

A technology of fluorosulfonylimide acid and fluorosulfonylimide salt, which is applied in the field of preparation of fluorosulfonylimide acid, can solve problems such as poor safety, insufficient purity of fluorosulfonylimide acid, and inconvenient operation of the method. Achieve the effects of preventing solidification, improving reaction and distillation efficiency, and reducing the content of impurities

Active Publication Date: 2014-03-26
PERIC SPECIAL GASES CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] In order to overcome the problems that the purity of fluorosulfonylimide acid prepared by the existing method is not high enough, the method is inconvenient to operate, and the safety is poor, the purpose of the present invention is to provide a method and device for preparing fluorosulfonylimide acid, which can effectively reduce the Reduce the content of impurities in fluorosulfonylimide acid, improve the operability in the production process, and improve the purity of fluorosulfonylimide acid

Method used

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  • Method and device for preparing fluorine sulfimide acid
  • Method and device for preparing fluorine sulfimide acid

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Embodiment 1

[0045] 11.4kg (0.116kmol) mass concentration is 100% sulfuric acid, 14.8kg (0.0459kmol) crude product KN (SO 2 CF 3 ) 2 And 1kg of silicon dioxide was put into a 20L reaction vessel for reaction. Stirring was kept during the reaction and distillation process, and nitrogen gas was introduced. The reaction temperature was 85-87°C. The reaction was 4h, and the crude product HN(SO 2 CF 3 ) 2 12.5kg, the yield is 96%. The conditions for feeding nitrogen are: the flow rate is 0.5-0.6L / min, and the pressure is 0-0.1MPa. The crude product KN(SO 2 CF 3 ) 2 And the obtained crude product HN(SO 2 CF 3 ) 2 The mass content of the components is shown in Table 3.

[0046] The mass content table of each material component of table 3 embodiment 1

[0047] component name

[0048] The rectification tower used for purification and the internal connecting pipes of the device are made of stainless steel. The volume of rectification kettle 1 is 10L, the diameter of rectificati...

Embodiment 2

[0050] 212.45kg (2.1245kmol) of sulfuric acid with a mass concentration of 98%, 940kg (4.249kmol) of crude product KN(SO 2 F) 2 And 78.33kg of silicon dioxide was put into a 1000L reaction vessel for reaction. Stirring was kept during the reaction and distillation process, and nitrogen gas was introduced. The reaction temperature was 145-150°C. The reaction was 1h, and the crude product HN(SO 2 F) 2 730kg, the yield is 94.0%, and the conditions for feeding nitrogen are: flow rate 3-6L / min, pressure 0-0.5MPa. The crude product KN(SO 2 F) 2 And the obtained crude product HN(SO 2 F) 2 The mass content of the components is shown in Table 4.

[0051] The mass content table of each material component of table 4 embodiment 2

[0052] component name

[0053] The rectification tower used for purification and the internal connecting pipes of the device are made of stainless steel. The volume of rectification kettle 1 is 1000L, the diameter of rectification column 3 is 2...

Embodiment 3

[0055] 6.628 (71.0185mol) kg of sulfuric acid with a mass concentration of 105%, 10kg (14.2037mol) of crude product Ba[N(SO 2 CF 3 ) 2 ] 2 and 0.4kg of silicon dioxide were put into a 10L reaction vessel, kept stirring during the reaction and distillation process, and nitrogen gas was introduced, the reaction temperature was 90-93°C, the reaction was 2h, and the crude product HN(SO 2 CF 3 ) 2 7.82kg, the yield is 97%. The conditions for feeding nitrogen are: flow rate 1.6-2.0L / min, pressure 0.30-0.33MPa. The crude product Ba[N(SO 2 CF 3 ) 2 ] 2 And the obtained crude product HN(SO 2 CF 3 ) 2 The mass content of the components is shown in Table 5.

[0056] The rectification tower used for purification and the internal connecting pipes of the device are made of stainless steel. The volume of rectification kettle 1 is 10L, the diameter of rectification column 3 is 20mm, and the height is 500mm. . In this rectifying kettle 1, add the crude product HN(SO) of 7.8kg 2...

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Abstract

The invention relates to a method and a device for preparing fluorine sulfimide acid and belongs to the field of fine chemical industries. The method comprises the steps as follows: a crude product of fluorine sulfimide salt reacts with sulfuric acid with the mass concentration in a range of 98-105% with the presence of silicon dioxide at the reaction temperature in a range of 85-150 DEG C for 1-4 h, nitrogen is fed before the reaction, and a crude product of the fluorine sulfimide acid is prepared through atmospheric distillation after the reaction; and then the crude product of the fluorine sulfimide acid is led into a rectifying tower, and the fluorine sulfimide acid is obtained through refinement. According to the method, the content of impurities in the fluorine sulfimide acid is effectively reduced, the operability of the production process is improved, and the purity of the fluorine sulfimide acid is increased.

Description

technical field [0001] The invention relates to a method and a device for preparing fluorosulfonylimide acid, which belong to the field of fine chemical industry. Background technique [0002] Fluorosulfonylimide acid itself is an important acidic substance, and it has very high practical value in chemistry. In organic chemistry, it is mainly used in acid-catalyzed reactions. In inorganic chemistry, it is mainly used to stabilize some inert ions, etc. In addition, fluorosulfonimide acid is an important substance for synthesizing lithium fluorosulfonimide, and its purity determines the purity of lithium fluorosulfonimide. At present, the lithium battery industry has high requirements on the purity of lithium fluorosulfonimide, so it is required to prepare high-purity fluorosulfonimide acid. [0003] As a method for producing fluorosulfonylimide acid, the following methods are known, for example. [0004] U.S. Patent No. 5,874,616 reports that fluoroalkylsulfonyl halides r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/48C07C303/36C01B21/096
Inventor 罗建志杨献奎彭立培商洪涛岳立平宋富财乔蓓蓓
Owner PERIC SPECIAL GASES CO LTD
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