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Methods and systems for preparing SOF2 gas and SOF4 gas

A SOF4 and SOF2 technology, applied in chemical instruments and methods, sulfur and halogen compounds, thionyl fluoride, etc., can solve the problems of expensive and difficult to obtain reaction raw materials, less production at one time, harsh reaction conditions, etc., and achieve mild reaction conditions , Simple production process and simple preparation system

Active Publication Date: 2018-06-08
中宏鑫投资控股(深圳)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is that existing preparation SOF 4 The gas method, due to the harsh reaction conditions, expensive and difficult to obtain reaction raw materials, and the prepared SOF 4 The reasons such as low gas purity and a small amount of one-time production limit its further scale-up production

Method used

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  • Methods and systems for preparing SOF2 gas and SOF4 gas
  • Methods and systems for preparing SOF2 gas and SOF4 gas
  • Methods and systems for preparing SOF2 gas and SOF4 gas

Examples

Experimental program
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preparation example Construction

[0032] The invention provides a SOF 2 The gas preparation method is as follows:

[0033] Step 1-1: Mix the fluorinating reagent, thionyl chloride and solvent evenly and add to SOF 2 In the reaction kettle 2, heat and reflux and stir to prepare SOF 2 solution, wherein the temperature of the condenser tube 42 is controlled at -20°C to -50°C, and SOF is obtained 2 gas. Preferably, the solvent is acetonitrile (CH 3 CN); the molar ratio of the fluorinating reagent, the thionyl chloride and the solvent is 6:0.838:5.5.

[0034] Preferably, 50L of glass SOF 2 The reaction kettle 2 is connected with the heating water bath circulation pump 3; the low temperature circulation pump 5 is connected with the condensation pipe 42 in the condensation device 4; the condensation pipe 42 is connected with the SOF through a rubber tube 2 Reactor 2 is connected. After connecting the equipment in sequence, heat the heating water bath circulation pump 3 to 60°C and circulate it to keep the airt...

Embodiment 1

[0049] This embodiment provides a SOF 2 Gas preparation method.

[0050] Step 1-1: First, the SOF 2 Nitrogen gas was passed into the reaction kettle 2 for 30 minutes, and the air in the whole system was discharged. To 50L glass SOF 2 Add 15kg of sodium fluoride and 12kg of acetonitrile solution to the reaction kettle 2 and stir evenly, add 5.5kg of thionyl chloride solution to the constant pressure dropping funnel 1, and add thionyl chloride dropwise to the reaction kettle , wherein, the time of dropping is 3 hours.

[0051] Secondly, heating and reflux stirring to prepare SOF 2 During the collection of the solution, the temperature in the condenser tube 42 is always kept at -35°C to -40°C. After 6 hours of complete reaction, a colorless and transparent solution can be collected in the glass cold well 43 as SOF 2 Liquid, produce at least 3kg of SOF at a time 2 Liquid, 87% yield.

[0052] Step 1-2: Put the SOF in the cold well 43 2 Solution transferred to 10L SOF 2 Pur...

Embodiment 2

[0054] This embodiment provides a SOF 2 Gas preparation method.

[0055] The difference between this embodiment and implementation 1 is:

[0056] Step 1-1: First, the SOF 2 Nitrogen gas was passed into the reaction kettle 2 for 30 minutes, and the air in the whole system was discharged. to SOF 2 Add 20.7kg of potassium fluoride and 12kg of acetonitrile solution in turn to the reaction kettle 2 and stir evenly, add 5.5kg of thionyl chloride solution into the constant pressure dropping funnel 1, and dropwise add dichloromethane For sulfone, the dropwise addition takes 3 hours.

[0057] Heating to reflux and stirring to produce SOF 2 During the collection of the solution, the temperature in the condenser tube 42 is always kept at -35°C to -40°C. After 6 hours of complete reaction, a colorless and transparent solution can be collected in the glass cold well 43 as SOF 2 Liquid, produce at least 3kg of SOF at a time 2 Liquid, 88% yield.

[0058] Step 1-2: Put the SOF in the ...

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Abstract

The invention relates to the technical field of industrial chemical production, and discloses methods and systems for preparing SOF2 gas and SOF4 gas. The system for preparing the SOF4 gas includes anSOF2 gas inlet pipeline, a fluorine pipeline, an SOF4 reaction kettle and a temperature control device, and the method for preparing the SOF4 gas includes the following steps of: step 1, introducingthe SOF2 gas into the SOF4 reaction kettle; step 2, introducing an appropriate amount of fluorine gas into the SOF4 reaction kettle under a condition of low temperature; and step 3, raising the temperature of the SOF4 reaction kettle to room temperature, and performing a reaction for a certain period of time so as to obtain the SOF4 gas, wherein the sequence of the step 1 and step 2 can be interchangeable. The methods and systems for preparing the SOF2 gas and SOF4 gas have the following advantages that: the methods and systems which have low cost and facilitate mass production and preparationof the high-purity SOF2 gas and high-purity SOF4 gas are proposed for the first time, preparation of kilogram-level SOF4 gas can be realized in the reaction kettle at room temperature, and the gas phase purity of the product can reach 99.5%.

Description

technical field [0001] The invention relates to the technical field of industrial chemical production, in particular to a SOF 2 gas and sulfur oxytetrafluoride (SOF 4 ) gas preparation method and system thereof. Background technique [0002] Those skilled in the art know that sulfur oxytetrafluoride (SOF 4 ) is a colorless gas with a pungent odor at room temperature. SOF 4 It has extensive potential research value and good application prospects in biochemistry, drug preparation and polymer materials (S.Li, P.Wu, J.E.Moses, K.B.Sharpless, Angew.Chem.Int.Ed.2017,56,2903 -2908. Therefore, SOF can be prepared in large quantities, with high purity and at low cost 4 is of great significance. [0003] However, SOF 4 There are very few preparation methods, and the literature that can be used for reference is only very early foreign literature, and it can only be prepared theoretically, or can only be prepared on a small scale. [0004] Theoretically, SOF 4 can be found by S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/45
CPCC01B17/4561C01B17/4569
Inventor 董佳家柯森李苏华
Owner 中宏鑫投资控股(深圳)有限公司
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