CN101747241A - Method for preparing trifluoromethyl sulfonic acid potassium CF3SO3K by electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F - Google Patents

Method for preparing trifluoromethyl sulfonic acid potassium CF3SO3K by electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F Download PDF

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CN101747241A
CN101747241A CN200810243630A CN200810243630A CN101747241A CN 101747241 A CN101747241 A CN 101747241A CN 200810243630 A CN200810243630 A CN 200810243630A CN 200810243630 A CN200810243630 A CN 200810243630A CN 101747241 A CN101747241 A CN 101747241A
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sulfonic acid
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gas
liquid
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许文林
陶荣辉
王雅琼
李霞
司宗飞
舒亚飞
吴彬
王剑
朱慧
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Yangzhou University
Zhangjiagang Guotai Huarong New Chemical Materials Co Ltd
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Yangzhou University
Zhangjiagang Guotai Huarong New Chemical Materials Co Ltd
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Abstract

The invention relates to a method for preparing trifluoromethyl sulfonic acid potassium CF3SO3K by electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F, the steps of the method are as follows: (1) the gas-phase product of the CH3SO2F electrochemical fluorination is cooled and condensed; (2) gas-liquid separation; (3) the gas-phase material obtained at the last step is added to water solution of potassium hydroxide KOH; (4) gas-liquid separation; (5) the liquid-phase material is evaporated; (6) leaching agent is added to the solid-phase product obtained through evaporation and drying at the last step for leaching operation; (7) solid-liquid separation; (8) the evaporative crystallization of the liquid-phase material obtained at the last step is conducted; (9) solid-liquid separation; (10) solid-phase evaporation and drying is conducted for obtaining the product trifluoromethyl sulfonic acid potassium CF3SO3K. The advantages of the invention are as follows: the process is simple, the energy consumption is less, the quality is good, and the cost is low.

Description

Methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K
Technical field
The present invention relates to a kind of preparation trifluoromethane sulfonic acid potassium CF 3SO 3The method of K, particularly a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K belongs to the fine chemical technology field.
Background technology
Trifluoromethyl sulfonic acid is the important foundation raw material of the novel Chemicals of complex functionality type in the field of fine chemical, it is the important source material of synthetic ionic liquid, fluorine surfactant and lithium-ion electrolyte etc., be with a wide range of applications, new processing method and the gordian technique of exploitation preparation trifluoromethyl sulfonic acid is to construct the important research and development field of functional type, meticulous type, the meticulous fluorine chemical product of high-level efficiency.
Trifluoromethane sulfonic acid potassium, molecular formula are CF 3SO 3K, molecular weight are 188, and fusing point is 230 ℃, and extremely stable below 375 ℃, normal temperature is white solid down.In the soluble in water and second eyeball isopolarity solvent of trifluoromethanesulfonic acid potassium, be soluble in ethanol, acetone, DMC, PC etc., be insoluble in the non-polar solvents such as benzene and ether.Mainly as the high temperature lubricant and the heat-transfer medium of superior performance, also be the synthetic and fine chemistry industry synthetic main raw material of fluorocarbon surfactant.
Methanesulfonyl fluoride, molecular formula are CH 3SO 2F, molecular weight are 98.10, and colourless or little yellow liquid, boiling point are 123-124 ℃, and relative density (water=1) is 1.35, and saturation vapour pressure (80 ℃) is 5.31kPa, and is water insoluble, is dissolved in ethanol, ether and the anhydrous hydrogen fluoride.Methanesulfonyl fluoride stable in properties, flammable, tool severe corrosive, strong and stimulating can cause that human body is burnt, severe toxicity, are subjected to the deleterious corrosive gases hydrogen fluoride of pyrolytic decomposition generation.
Methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product is meant with CH 3SO 2F is a raw material, carries out the electrochemical fluorination reaction in HF solution, generates principal product trifluoromethyl sulfonic acid fluoride CF at anode 3SO 2F generates by product hydrogen H at negative electrode 2, and because the boiling point lower (19.5 ℃) of HF and with CF 3SO 2F and H 2Leave the gas phase mixture of electrochemical fluorination reactor together with gas form, mainly contain CF 3SO 2F, H 2And HF, because water H is arranged 2O and CH 3SO 2F in the electrochemical fluorination process bond rupture and the trace impurity that produces, as oxygen difluoride OF 2, tetrafluoro-methane CF 4Wait the impurity of the difficult liquefaction of some lower boilings.
Summary of the invention
The purpose of this invention is to provide that a kind of technology is simple, consuming little energy, quality is good, cost is low methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K.
Realize that the above-mentioned purpose technical scheme is: a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K is with methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product is a raw material, and described method steps is as follows:
(1) cooling condensation: with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product makes the hydrogen fluoride HF in the gas phase be condensed into liquid-phase fluorination hydrogen;
(2) solution-air is separated: lower the temperature material that condensation obtains of previous step is carried out solution-air and separates, and gas phase enters next step, and liquid phase contains hydrogen fluoride HF further to be recycled;
(3) chemical absorption: in absorption equipment, add the gaseous phase materials that obtains after the previous step solution-air is separated in the potassium hydroxide KOH aqueous solution, to trifluoromethyl sulfonic acid fluoride CF 3SO 2F carries out chemical absorption;
(4) solution-air is separated: the material that the previous step chemical absorption is obtained carries out the solution-air separation, and gas phase contains hydrogen H 2Further recycle, liquid phase enters next step;
(5) evaporation oven dry: the liquid phase material that previous step is obtained evaporates, the water H that the gas-phase product of evaporation obtains through condensation 2O carries out recycle and reuse, and the solid product after the evaporation further enters next step after the oven dry;
(6) leaching: dry the solid product trifluoromethane sulfonic acid potassium CF that obtains in the previous step evaporation 3SO 3Add leaching agent among K, Potassium monofluoride KF and the potassium hydroxide KOH, leach operation;
(7) solid-liquid separates: the material after the previous step leaching is carried out solid-liquid separate, solid phase is further recycled, and liquid phase enters next step;
(8) evaporative crystallization: the liquid phase material that previous step is obtained carries out evaporative crystallization, and the gas phase leaching agent is recycled, trifluoromethane sulfonic acid potassium CF 3SO 3The K crystallization is separated out, and liquid phase and solid-phase material enter next step;
(9) solid-liquid separates: the liquid phase of previous step generation is carried out solid-liquid with solid-phase material separate, liquid phase is returned the leaching recycle of the 6th step, and solid phase enters next step;
(10) evaporation oven dry: solid phase is dried, obtain product trifluoromethane sulfonic acid potassium CF 3SO 3K.
Further, the service temperature of described the first step cooling condensation is-20 ℃～0 ℃, and the operation absolute pressure is 0.1MPa～1.0MPa.
Further, described the 3rd step chemical absorption conversion unit is that the still formula stirs any one in chemical reactor, tubular chemical reactor or the chemical absorption tower, operational condition is 20 ℃～120 ℃ of temperature of reaction, reaction absolute pressure 0.1MPa～1.0MPa, trifluoromethyl sulfonic acid fluoride CF 3SO 2The mol ratio of F and potassium hydroxide KOH is 1.0: 1.2～5.0, and the concentration of the potassium hydroxide KOH aqueous solution is 8.0mol/L～12.0mol/L.
Further, the operational condition of described the 5th step and the evaporation oven dry of the tenth step is 50 ℃～150 ℃ of vaporization temperatures, evaporation absolute pressure 0.01MPa～0.1MPa.
Further, the leaching agent in described the 6th step leaching is any one in acetone, ethanol or the second eyeball.
Chemical equation of the present invention is:
CF 3SO 2F+H 2O→CF 3SO 3H+HF
CF 3SO 3H+KOH→CF 3SO 3K+H 2O
HF+KOH→KF+H 2O
Realize that the main technique equipment that the present invention needs is: chemical absorption conversion unit, leaching equipment, evaporation crystallization equipment, filter plant etc.
Adopt the benefit of technique scheme to be: (1), the present invention are direct as being prepared as raw material with the product of electrochemical reaction, and the product of electrochemical reaction is direct as preparation trifluoromethane sulfonic acid potassium CF 3SO 3The raw material of K helps the economy of the process that improves, and simplifies and separates and operation steps, and raw material is easy to get, and raw materials cost is low, and simplified apparatus reduces facility investment, and operational path is short, and technology is simple; (2), with the separation and purification and the CH of electrochemical reaction process and product 3SO 2The derivatize of F combines, and helps the utilization of energy in the raising process, reduces the consumption of the condensation energy in the gas-phase product sepn process, consuming little energy; (3), make full use of the singularity of product, simplify processing step, reduced production cost, improved the security of technological process; (4), the removal of impurities of gas-phase product and the processing of a tail gas are combined, needn't arrive the later stage just handles and can discharge gas specially, recyclable utilization, realized cleaning production, be convenient to suitability for industrialized production, the no three wastes produce, cleaning, environmental protection, various by products can be recycled, and this has saved cost greatly; (5), the product trifluoromethane sulfonic acid potassium CF of processing method preparation of the present invention 3SO 3The K quality is good, and the yield height adopts high temperature, pressurized conditions in absorption and pyrolytic process, and high temperature helps hydrolysis, and pressurization helps the uptake rate and the efficient of the process that improves.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
The present invention is further detailed explanation below in conjunction with drawings and Examples.
Embodiment one
Major equipment: the still formula stirs chemical reactor, leaching equipment, evaporation crystallization equipment, filter plant.
Main raw material: methanesulfonyl fluoride CH 3SO 2F electrochemical fluorination gas-phase product, potassium hydroxide KOH, leaching agent acetone.
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K is with methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product is a raw material, and described method steps is as follows:
(1) cooling condensation: with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product makes the hydrogen fluoride HF in the gas phase be condensed into liquid-phase fluorination hydrogen, and the service temperature of cooling condensation is 0 ℃, and the operation absolute pressure is 1.0MPa;
(2) solution-air is separated: lower the temperature material that condensation obtains of previous step is carried out solution-air and separates, contain trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrogen H 2Gas phase enter next step, liquid phase contains hydrogen fluoride HF further to be recycled;
(3) chemical absorption: stir in the chemical reactor in the still formula, add the gaseous phase materials that obtains after the previous step solution-air is separated in the potassium hydroxide KOH aqueous solution, to trifluoromethyl sulfonic acid fluoride CF 3SO 2F carries out chemical absorption, and operational condition is 20 ℃ of temperature of reaction, reaction absolute pressure 0.1MPa, trifluoromethyl sulfonic acid fluoride CF 3SO 2The mol ratio of F and potassium hydroxide KOH is 1.0: 1.2, and the concentration of the potassium hydroxide KOH aqueous solution is 8.0mol/L;
(4) solution-air is separated: the material that the previous step chemical absorption is obtained carries out the solution-air separation, and gas phase contains hydrogen H 2Further recycle, contain trifluoromethane sulfonic acid potassium CF 3SO 3The K liquid phase enters next step;
(5) evaporation oven dry: the liquid phase material that previous step is obtained evaporates, and operational condition is 50 ℃ of vaporization temperatures, evaporation absolute pressure 0.01MPa, the water H that the gas-phase product of evaporation obtains through condensation 2O carries out recycle and reuse, contains trifluoromethane sulfonic acid potassium CF after the evaporation 3SO 3The solid product of K and Potassium monofluoride KF further enters next step after the oven dry;
(6) leaching: in leaching equipment, dry the solid product trifluoromethane sulfonic acid potassium CF that obtains in the previous step evaporation 3SO 3Add leaching agent acetone among K, Potassium monofluoride KF and the potassium hydroxide KOH, leach operation;
(7) solid-liquid separates: in filter plant, the material after the previous step leaching is carried out solid-liquid separate, contain Potassium monofluoride KF in the solid phase and potassium hydroxide KOH further recycles, contain trifluoromethane sulfonic acid potassium CF 3SO 3The liquid phase of K enters next step;
(8) evaporative crystallization: in evaporation crystallization equipment, the liquid phase material that previous step is obtained carries out evaporative crystallization, and the gas phase leaching agent is recycled, trifluoromethane sulfonic acid potassium CF 3SO 3The K crystallization is separated out, and liquid phase and solid-phase material enter next step;
(9) solid-liquid separates: in filter plant, the liquid phase of previous step generation is carried out solid-liquid with solid-phase material separate, liquid phase is returned the leaching recycle of the 6th step, and solid phase enters next step;
(10) evaporation oven dry: solid phase is dried, and operational condition is 50 ℃ of vaporization temperatures, and evaporation absolute pressure 0.01MPa obtains product trifluoromethane sulfonic acid potassium CF 3SO 3K.
Embodiment two
Major equipment: tubular chemical reactor, leaching equipment, evaporation crystallization equipment.
Main raw material: methanesulfonyl fluoride CH 3SO 2F electrochemical fluorination gas-phase product, potassium hydroxide KOH, leaching agent ethanol.
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K is with methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product is a raw material, and described method steps is as follows:
(1) cooling condensation: with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product makes the hydrogen fluoride HF in the gas phase be condensed into liquid-phase fluorination hydrogen, and the service temperature of cooling condensation is-10 ℃, and the operation absolute pressure is 0.8MPa;
(2) solution-air is separated: lower the temperature material that condensation obtains of previous step is carried out solution-air and separates, contain trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrogen H 2Gas phase enter next step, liquid phase contains hydrogen fluoride HF further to be recycled;
(3) chemical absorption: in tubular chemical reactor, add the gaseous phase materials that obtains after the previous step solution-air is separated in the potassium hydroxide KOH aqueous solution, to trifluoromethyl sulfonic acid fluoride CF 3SO 2F carries out chemical absorption, and operational condition is 60 ℃ of temperature of reaction, reaction absolute pressure 0.5MPa, trifluoromethyl sulfonic acid fluoride CF 3SO 2The mol ratio of F and potassium hydroxide KOH is 1.0: 3.0, and the concentration of the potassium hydroxide KOH aqueous solution is 10.0mol/L;
(4) solution-air is separated: the material that the previous step chemical absorption is obtained carries out the solution-air separation, and gas phase contains hydrogen H 2Further recycle, contain trifluoromethane sulfonic acid potassium CF 3SO 3The K liquid phase enters next step;
(5) evaporation oven dry: the liquid phase material that previous step is obtained evaporates, and operational condition is 90 ℃ of vaporization temperatures, evaporation absolute pressure 0.08MPa, the water H that the gas-phase product of evaporation obtains through condensation 2O carries out recycle and reuse, contains trifluoromethane sulfonic acid potassium CF after the evaporation 3SO 3The solid product of K and Potassium monofluoride KF further enters next step after the oven dry;
(6) leaching: in leaching equipment, dry the solid product trifluoromethane sulfonic acid potassium CF that obtains in the previous step evaporation 3SO 3Add leaching agent ethanol among K, Potassium monofluoride KF and the potassium hydroxide KOH, leach operation;
(7) solid-liquid separates: in filter plant, the material after the previous step leaching is carried out solid-liquid separate, contain Potassium monofluoride KF in the solid phase and potassium hydroxide KOH further recycles, contain trifluoromethane sulfonic acid potassium CF 3SO 3The liquid phase of K enters next step;
(8) evaporative crystallization: in evaporation crystallization equipment, the liquid phase material that previous step is obtained carries out evaporative crystallization, and the gas phase leaching agent is recycled, trifluoromethane sulfonic acid potassium CF 3SO 3The K crystallization is separated out, and liquid phase and solid-phase material enter next step;
(9) solid-liquid separates: in filter plant, the liquid phase of previous step generation is carried out solid-liquid with solid-phase material separate, liquid phase is returned the leaching recycle of the 6th step, and solid phase enters next step;
(10) evaporation oven dry: solid phase is dried, and operational condition is 90 ℃ of vaporization temperatures, and evaporation absolute pressure 0.08MPa obtains product trifluoromethane sulfonic acid potassium CF 3SO 3K.
Embodiment three
Major equipment: chemical absorption tower, leaching equipment, evaporation crystallization equipment.
Main raw material: methanesulfonyl fluoride CH 3SO 2F electrochemical fluorination gas-phase product, potassium hydroxide KOH, leaching agent second eyeball.
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K is with methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product is a raw material, and described method steps is as follows:
(1) cooling condensation: with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product makes the hydrogen fluoride HF in the gas phase be condensed into liquid-phase fluorination hydrogen, and the service temperature of cooling condensation is-20 ℃, and the operation absolute pressure is 0.1MPa;
(2) solution-air is separated: lower the temperature material that condensation obtains of previous step is carried out solution-air and separates, contain trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrogen H 2Gas phase enter next step, liquid phase contains hydrogen fluoride HF further to be recycled;
(3) chemical absorption: in the chemical absorption tower, add the gaseous phase materials that obtains after the previous step solution-air is separated in the potassium hydroxide KOH aqueous solution, to trifluoromethyl sulfonic acid fluoride CF 3SO 2F carries out chemical absorption, and operational condition is 120 ℃ of temperature of reaction, reaction absolute pressure 1.0MPa, trifluoromethyl sulfonic acid fluoride CF 3SO 2The mol ratio of F and potassium hydroxide KOH is 1.0: 5.0, and the concentration of the potassium hydroxide KOH aqueous solution is 12.0mol/L;
(4) solution-air is separated: the material that the previous step chemical absorption is obtained carries out the solution-air separation, and gas phase contains hydrogen H 2Further recycle, contain trifluoromethane sulfonic acid potassium CF 3SO 3The K liquid phase enters next step;
(5) evaporation oven dry: the liquid phase material that previous step is obtained evaporates, and operational condition is 150 ℃ of vaporization temperatures, evaporation absolute pressure 0.1MPa, the water H that the gas-phase product of evaporation obtains through condensation 2O carries out recycle and reuse, contains trifluoromethane sulfonic acid potassium CF after the evaporation 3SO 3The solid product of K and Potassium monofluoride KF further enters next step after the oven dry;
(6) leaching: in leaching equipment, dry the solid product trifluoromethane sulfonic acid potassium CF that obtains in the previous step evaporation 3SO 3Add leaching agent second eyeball among K, Potassium monofluoride KF and the potassium hydroxide KOH, leach operation;
(7) solid-liquid separates: in filter plant, the material after the previous step leaching is carried out solid-liquid separate, contain Potassium monofluoride KF in the solid phase and potassium hydroxide KOH further recycles, contain trifluoromethane sulfonic acid potassium CF 3SO 3The liquid phase of K enters next step;
(8) evaporative crystallization: in evaporation crystallization equipment, the liquid phase material that previous step is obtained carries out evaporative crystallization, and the gas phase leaching agent is recycled, trifluoromethane sulfonic acid potassium CF 3SO 3The K crystallization is separated out, and liquid phase and solid-phase material enter next step;
(9) solid-liquid separates: in filter plant, the liquid phase of previous step generation is carried out solid-liquid with solid-phase material separate, liquid phase is returned the leaching recycle of the 6th step, and solid phase enters next step;
(10) evaporation oven dry: solid phase is dried, and operational condition is 150 ℃ of vaporization temperatures, and evaporation absolute pressure 0.1MPa obtains product trifluoromethane sulfonic acid potassium CF 3SO 3K.
Embodiment four
Major equipment: the still formula stirs chemical reactor, leaching equipment, evaporation crystallization equipment.
Main raw material: methanesulfonyl fluoride CH 3SO 2F electrochemical fluorination gas-phase product, potassium hydroxide KOH, leaching agent acetone.
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K is with methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product is a raw material, and described method steps is as follows:
(1) cooling condensation: with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product makes the hydrogen fluoride HF in the gas phase be condensed into liquid-phase fluorination hydrogen, and the service temperature of cooling condensation is-5 ℃, and the operation absolute pressure is 0.9MPa;
(2) solution-air is separated: lower the temperature material that condensation obtains of previous step is carried out solution-air and separates, contain trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrogen H 2Gas phase enter next step, liquid phase contains hydrogen fluoride HF further to be recycled;
(3) chemical absorption: stir in the chemical reactor in the still formula, add the gaseous phase materials that obtains after the previous step solution-air is separated in the potassium hydroxide KOH aqueous solution, to trifluoromethyl sulfonic acid fluoride CF 3SO 2F carries out chemical absorption, and operational condition is 40 ℃ of temperature of reaction, reaction absolute pressure 0.3MPa, trifluoromethyl sulfonic acid fluoride CF 3SO 2The mol ratio of F and potassium hydroxide KOH is 1.0: 2.2, and the concentration of the potassium hydroxide KOH aqueous solution is 8.0mol/L;
(4) solution-air is separated: the material that the previous step chemical absorption is obtained carries out the solution-air separation, and gas phase contains hydrogen H 2Further recycle, contain trifluoromethane sulfonic acid potassium CF 3SO 3The K liquid phase enters next step;
(5) evaporation oven dry: the liquid phase material that previous step is obtained evaporates, and operational condition is 70 ℃ of vaporization temperatures, evaporation absolute pressure 0.05MPa, the water H that the gas-phase product of evaporation obtains through condensation 2O carries out recycle and reuse, contains trifluoromethane sulfonic acid potassium CF after the evaporation 3SO 3The solid product of K and Potassium monofluoride KF further enters next step after the oven dry;
(6) leaching: in leaching equipment, dry the solid product trifluoromethane sulfonic acid potassium CF that obtains in the previous step evaporation 3SO 3Add leaching agent acetone among K, Potassium monofluoride KF and the potassium hydroxide KOH, leach operation;
(7) solid-liquid separates: in filter plant, the material after the previous step leaching is carried out solid-liquid separate, contain Potassium monofluoride KF in the solid phase and potassium hydroxide KOH further recycles, contain trifluoromethane sulfonic acid potassium CF 3SO 3The liquid phase of K enters next step;
(8) evaporative crystallization: in evaporation crystallization equipment, the liquid phase material that previous step is obtained carries out evaporative crystallization, and the gas phase leaching agent is recycled, trifluoromethane sulfonic acid potassium CF 3SO 3The K crystallization is separated out, and liquid phase and solid-phase material enter next step;
(9) solid-liquid separates: in filter plant, the liquid phase of previous step generation is carried out solid-liquid with solid-phase material separate, liquid phase is returned the leaching recycle of the 6th step, and solid phase enters next step;
(10) evaporation oven dry: solid phase is dried, and operational condition is 70 ℃ of vaporization temperatures, and evaporation absolute pressure 0.05MPa obtains product trifluoromethane sulfonic acid potassium CF 3SO 3K.
Embodiment five
Major equipment: tubular chemical reactor, leaching equipment, evaporation crystallization equipment.
Main raw material: methanesulfonyl fluoride CH 3SO 2F electrochemical fluorination gas-phase product, potassium hydroxide KOH, leaching agent ethanol.
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K is with methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product is a raw material, and described method steps is as follows:
(1) cooling condensation: with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product makes the hydrogen fluoride HF in the gas phase be condensed into liquid-phase fluorination hydrogen, and the service temperature of cooling condensation is-10 ℃, and the operation absolute pressure is 0.8MPa;
(2) solution-air is separated: lower the temperature material that condensation obtains of previous step is carried out solution-air and separates, contain trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrogen H 2Gas phase enter next step, liquid phase contains hydrogen fluoride HF further to be recycled;
(3) chemical absorption: in tubular chemical reactor, add the gaseous phase materials that obtains after the previous step solution-air is separated in the potassium hydroxide KOH aqueous solution, to trifluoromethyl sulfonic acid fluoride CF 3SO 2F carries out chemical absorption, and operational condition is 80 ℃ of temperature of reaction, reaction absolute pressure 0.6MPa, trifluoromethyl sulfonic acid fluoride CF 3SO 2The mol ratio of F and potassium hydroxide KOH is 1.0: 2.8, and the concentration of the potassium hydroxide KOH aqueous solution is 10.0mol/L;
(4) solution-air is separated: the material that the previous step chemical absorption is obtained carries out the solution-air separation, and gas phase contains hydrogen H 2Further recycle, contain trifluoromethane sulfonic acid potassium CF 3SO 3The K liquid phase enters next step;
(5) evaporation oven dry: the liquid phase material that previous step is obtained evaporates, and operational condition is 100 ℃ of vaporization temperatures, evaporation absolute pressure 0.08MPa, the water H that the gas-phase product of evaporation obtains through condensation 2O carries out recycle and reuse, contains trifluoromethane sulfonic acid potassium CF after the evaporation 3SO 3The solid product of K and Potassium monofluoride KF further enters next step after the oven dry;
(6) leaching: in leaching equipment, dry the solid product trifluoromethane sulfonic acid potassium CF that obtains in the previous step evaporation 3SO 3Add leaching agent ethanol among K, Potassium monofluoride KF and the potassium hydroxide KOH, leach operation;
(7) solid-liquid separates: in filter plant, the material after the previous step leaching is carried out solid-liquid separate, contain Potassium monofluoride KF in the solid phase and potassium hydroxide KOH further recycles, contain trifluoromethane sulfonic acid potassium CF 3SO 3The liquid phase of K enters next step;
(8) evaporative crystallization: in evaporation crystallization equipment, the liquid phase material that previous step is obtained carries out evaporative crystallization, and the gas phase leaching agent is recycled, trifluoromethane sulfonic acid potassium CF 3SO 3The K crystallization is separated out, and liquid phase and solid-phase material enter next step;
(9) solid-liquid separates: in filter plant, the liquid phase of previous step generation is carried out solid-liquid with solid-phase material separate, liquid phase is returned the leaching recycle of the 6th step, and solid phase enters next step;
(10) evaporation oven dry: solid phase is dried, and operational condition is 120 ℃ of vaporization temperatures, and evaporation absolute pressure 0.08MPa obtains product trifluoromethane sulfonic acid potassium CF 3SO 3K.
Embodiment six
Major equipment: chemical absorption tower, leaching equipment, evaporation crystallization equipment.
Main raw material: methanesulfonyl fluoride CH 3SO 2F electrochemical fluorination gas-phase product, potassium hydroxide KOH, leaching agent second eyeball.
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K is with methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product is a raw material, and described method steps is as follows:
(1) cooling condensation: with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product makes the hydrogen fluoride HF in the gas phase be condensed into liquid-phase fluorination hydrogen, and the service temperature of cooling condensation is-15 ℃, and the operation absolute pressure is 0.5MPa;
(2) solution-air is separated: lower the temperature material that condensation obtains of previous step is carried out solution-air and separates, contain trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrogen H 2Gas phase enter next step, liquid phase contains hydrogen fluoride HF further to be recycled;
(3) chemical absorption: in the chemical absorption tower, add the gaseous phase materials that obtains after the previous step solution-air is separated in the potassium hydroxide KOH aqueous solution, to trifluoromethyl sulfonic acid fluoride CF 3SO 2F carries out chemical absorption, and operational condition is 100 ℃ of temperature of reaction, reaction absolute pressure 0.8MPa, trifluoromethyl sulfonic acid fluoride CF 3SO 2The mol ratio of F and potassium hydroxide KOH is 1.0: 2.5, and the concentration of the potassium hydroxide KOH aqueous solution is 12.0mol/L;
(4) solution-air is separated: the material that the previous step chemical absorption is obtained carries out the solution-air separation, and gas phase contains hydrogen H 2Further recycle, contain trifluoromethane sulfonic acid potassium CF 3SO 3The K liquid phase enters next step;
(5) evaporation oven dry: the liquid phase material that previous step is obtained evaporates, and operational condition is 110 ℃ of vaporization temperatures, evaporation absolute pressure 0.09MPa, the water H that the gas-phase product of evaporation obtains through condensation 2O carries out recycle and reuse, contains trifluoromethane sulfonic acid potassium CF after the evaporation 3SO 3The solid product of K and Potassium monofluoride KF further enters next step after the oven dry;
(6) leaching: in leaching equipment, dry the solid product trifluoromethane sulfonic acid potassium CF that obtains in the previous step evaporation 3SO 3Add leaching agent second eyeball among K, Potassium monofluoride KF and the potassium hydroxide KOH, leach operation;
(7) solid-liquid separates: in filter plant, the material after the previous step leaching is carried out solid-liquid separate, contain Potassium monofluoride KF in the solid phase and potassium hydroxide KOH further recycles, contain trifluoromethane sulfonic acid potassium CF 3SO 3The liquid phase of K enters next step;
(8) evaporative crystallization: in evaporation crystallization equipment, the liquid phase material that previous step is obtained carries out evaporative crystallization, and the gas phase leaching agent is recycled, trifluoromethane sulfonic acid potassium CF 3SO 3The K crystallization is separated out, and liquid phase and solid-phase material enter next step;
(9) solid-liquid separates: in filter plant, the liquid phase of previous step generation is carried out solid-liquid with solid-phase material separate, liquid phase is returned the leaching recycle of the 6th step, and solid phase enters next step;
(10) evaporation oven dry: solid phase is dried, and operational condition is 120 ℃ of vaporization temperatures, and evaporation absolute pressure 0.09MPa obtains product trifluoromethane sulfonic acid potassium CF 3SO 3K.
Remove the various embodiments described above, embodiment of the present invention also have a lot, and the technical scheme that all employings are equal to or equivalence is replaced is all within protection scope of the present invention.

Claims (5)

1. methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K is with methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product is a raw material, it is characterized in that described method steps is as follows:
(1) cooling condensation: with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product makes the hydrogen fluoride HF in the gas phase be condensed into liquid-phase fluorination hydrogen;
(2) solution-air is separated: lower the temperature material that condensation obtains of previous step is carried out solution-air and separates, and gas phase enters next step, and liquid phase contains hydrogen fluoride HF further to be recycled;
(3) chemical absorption: in absorption equipment, add the gaseous phase materials that obtains after the previous step solution-air is separated in the potassium hydroxide KOH aqueous solution, to trifluoromethyl sulfonic acid fluoride CF 3SO 2F carries out chemical absorption;
(4) solution-air is separated: the material that the previous step chemical absorption is obtained carries out the solution-air separation, and gas phase contains hydrogen H 2Further recycle, liquid phase enters next step;
(5) evaporation oven dry: the liquid phase material that previous step is obtained evaporates, the water H that the gas-phase product of evaporation obtains through condensation 2O carries out recycle and reuse, and the solid product after the evaporation further enters next step after the oven dry;
(6) leaching: dry the solid product trifluoromethane sulfonic acid potassium CF that obtains in the previous step evaporation 3SO 3Add leaching agent among K, Potassium monofluoride KF and the potassium hydroxide KOH, leach operation;
(7) solid-liquid separates: the material after the previous step leaching is carried out solid-liquid separate, solid phase is further recycled, and liquid phase enters next step;
(8) evaporative crystallization: the liquid phase material that previous step is obtained carries out evaporative crystallization, and the gas phase leaching agent is recycled, trifluoromethane sulfonic acid potassium CF 3SO 3The K crystallization is separated out, and liquid phase and solid-phase material enter next step;
(9) solid-liquid separates: the liquid phase of previous step generation is carried out solid-liquid with solid-phase material separate, liquid phase is returned the leaching recycle of the 6th step, and solid phase enters next step;
(10) evaporation oven dry: solid phase is dried, obtain product trifluoromethane sulfonic acid potassium CF 3SO 3K.
2. methanesulfonyl fluoride CH according to claim 1 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K is characterized in that: the service temperature of described the first step cooling condensation is-20 ℃～0 ℃, and the operation absolute pressure is 0.1MPa～1.0MPa.
3. methanesulfonyl fluoride CH according to claim 1 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K, it is characterized in that: described the 3rd step chemical absorption conversion unit is that the still formula stirs any one in chemical reactor, tubular chemical reactor or the chemical absorption tower, operational condition is 20 ℃～120 ℃ of temperature of reaction, reaction absolute pressure 0.1MPa～1.0MPa, trifluoromethyl sulfonic acid fluoride CF 3SO 2The mol ratio of F and potassium hydroxide KOH is 1.0: 1.2～5.0, and the concentration of the potassium hydroxide KOH aqueous solution is 8.0mol/L～12.0mol/L.
4. methanesulfonyl fluoride CH according to claim 1 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K is characterized in that: the operational condition of described the 5th step and the evaporation oven dry of the tenth step is 50 ℃～150 ℃ of vaporization temperatures, evaporation absolute pressure 0.01MPa～0.1MPa.
5. methanesulfonyl fluoride CH according to claim 1 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid potassium CF 3SO 3The method of K is characterized in that: the leaching agent in described the 6th step leaching is any one in acetone, ethanol or the second eyeball.
CN200810243630A 2008-12-11 2008-12-11 Method for preparing trifluoromethyl sulfonic acid potassium CF3SO3K by electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F Pending CN101747241A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111170898A (en) * 2020-02-13 2020-05-19 内蒙古三爱富万豪氟化工有限公司 Preparation method of potassium perfluorobutane sulfonate
CN114436292A (en) * 2022-02-21 2022-05-06 中船(邯郸)派瑞特种气体股份有限公司 Treatment method of organic sylvite wastewater

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111170898A (en) * 2020-02-13 2020-05-19 内蒙古三爱富万豪氟化工有限公司 Preparation method of potassium perfluorobutane sulfonate
CN114436292A (en) * 2022-02-21 2022-05-06 中船(邯郸)派瑞特种气体股份有限公司 Treatment method of organic sylvite wastewater

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