CN101747240A - Method for preparing trifluoromethyl sulfonic acid CF3SO3H by electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F - Google Patents

Method for preparing trifluoromethyl sulfonic acid CF3SO3H by electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F Download PDF

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CN101747240A
CN101747240A CN200810243629A CN200810243629A CN101747240A CN 101747240 A CN101747240 A CN 101747240A CN 200810243629 A CN200810243629 A CN 200810243629A CN 200810243629 A CN200810243629 A CN 200810243629A CN 101747240 A CN101747240 A CN 101747240A
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sulfonic acid
phase
trifluoromethane sulfonic
gas
fluoride
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许文林
徐晓强
王雅琼
陶荣辉
司宗飞
李霞
丁培兴
方剑慧
王一明
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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 CF3SO3H 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 or sodium hydroxide NaOH or barium hydroxide Ba (OH) 2, the chemical absorption of the trifluoromethyl sulfuryl fluoride CF3SO2F is conducted; (4) gas-liquid separation: (5) liquid-phase evaporation and drying; (6) the solid-phase material is leached; (7) solid-liquid separation; (8) the liquid-phase is added to hydrochloric acid HCL or sulfuric acid H2SO4 for replacement reaction; (9) solid-liquid separation; (10) liquid-phase fractionating is conducted, and the product trifluoromethyl sulfonic acid CF3SO3H is obtained. The advantages of the invention are as follows: the cost is low, the process is simple, the energy consumption is small, the invention is clean and environmental-friendly, and the quality of the product is good.

Description

Methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H
Technical field
The present invention relates to a kind of preparation trifluoromethane sulfonic acid CF 3SO 3The method of H, particularly a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H belongs to the fine chemical technology field.
Background technology
At present, trifluoromethane 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 trifluoromethane 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, molecular formula are CF 3SO 3H, molecular weight are 150.07, and purified trifluoromethane sulfonic acid is the flowable liquid that a kind of water white transparency has irritating smell, color jaundice after sneaking into small amount of impurities.For moisture absorption liquid, have severe corrosive, in damp atmosphere, produce white cigarette, no fire and explosion hazard.Suck or when dropping on skin and eyes and respiratory mucosa, can cause strongly and burn.Density is 1.696.Fusing point is-40 ℃.Boiling point is 162 ℃, and specific refractory power is 1.326-1.33.It is at present known strong acid, and is very easily water-soluble, is soluble in ethanol and ether, also is dissolved in acetoneand ethyl acetate, is slightly soluble in the non-polar solvents such as benzene, hexane.Trifluoromethane sulfonic acid character is highly stable, be widely used in medicinal industry mainly as intermediate, as nucleosides, microbiotic, steroid, protein, join carbohydrate and VITAMIN etc., be a kind of new and effective Friedel-Crafts benzylization and cyclohexyl catalyst for reaction; In the plastics industry, be used for the catalytic chemistry building-up reactions, as a kind of oligomerisation polymerizing catalyst; Also can be used for the silicon rubber modification; In electron chemistry industry, can be used for the production of electron conduction polymkeric substance, as trifluoromethyl sulfonic acid; In the fuel industry, be used as the protonation reaction catalyzer; In the farming industry, be used for synthetic herbicidal formulations and growth regulator etc., it and salt thereof and ester have purposes widely.
The preparation of trifluoromethane sulfonic acid at present mainly contains three kinds of processing methodes: a kind of is to be raw material with dithiocarbonic anhydride, generates trifluoromethyl disulphide with the iodine pentafluoride reaction, then with mercury react trifluoromethylthio mercury (CF 3S) 2Hg, the latter promptly gets trifluoromethane sulfonic acid through the hydrogen peroxide oxidation, and chemical equation is:
Figure G2008102436293D0000021
Second kind is to be raw material with dithiocarbonic anhydride, generates trifluoromethyl disulphide with the iodine pentafluoride reaction, gets the trifluoromethyl SULPHURYL CHLORIDE with chlorine reaction then, and the trifluoromethyl SULPHURYL CHLORIDE promptly gets trifluoromethane sulfonic acid through hydrolysis reaction, and chemical equation is:
Figure G2008102436293D0000022
The third is with trifluoromethane sulfonic acid potassium CF 3SO 3K and excessive oleum H 2SO 4Reaction generates trifluoromethane sulfonic acid CF 3SO 3H, vacuum steams thing and just is trifluoromethane sulfonic acid CF 3SO 3H, yield about 80%.Chemical equation is:
CF 3SO 3K+H 2SO 4→CF 3SO 3H+K 2SO 4
Among these preparation methods, preceding two kinds prepare trifluoromethane sulfonic acid CF 3SO 3The processing method of H exists processing step many, and quantity of three wastes is big, the low and high defective of production cost of quality product; The third preparation trifluoromethane sulfonic acid CF 3SO 3The processing method of H exists the high defective of raw materials cost.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, provide that a kind of technology is simple, consuming little energy, good product quality, methanesulfonyl fluoride CH that production cost is low 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H.
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 CF 3SO 3The method of H 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;
(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 product enters next step, and liquid phase is that hydrogen fluoride HF further recycles;
(3) chemical absorption: in absorption equipment, at potassium hydroxide KOH or sodium hydroxide NaOH or hydrated barta Ba (OH) 2The aqueous solution in add the gaseous phase materials that obtains after the previous step solution-air is separated, 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 material enters next step;
(5) evaporation oven dry: the liquid phase material that previous step is obtained evaporates oven dry, the water H that the gas-phase product of evaporation obtains through condensation 2O recycles, and the solid phase after the evaporation oven dry enters next step;
(6) leaching: the solid-phase material that previous step is produced adds leaching agent, leaches operation;
(7) solid-liquid separates: the material that previous step is produced carries out the solid-liquid separation, and solid phase is further recycled, and liquid phase material enters next step;
(8) replacement(metathesis)reaction: add hydrochloric acid HCl or sulfuric acid H in the liquid phase material that previous step is obtained 2SO 4, carry out replacement(metathesis)reaction, generate product trifluoromethane sulfonic acid CF 3SO 3H and chlorate perhaps generate product trifluoromethane sulfonic acid CF 3SO 3H and vitriol;
(9) solid-liquid separates: the material that previous step is produced carries out the solid-liquid separation, and solid phase is further recycled, and liquid phase enters next step;
(10) rectification under vacuum: the liquid phase material of previous step is carried out rectifying, obtain vapor condensation product trifluoromethane sulfonic acid CF 3SO 3H, leaching agent return the utilization of the 6th step leaching step cycle, and residual solution is further handled.
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 or sodium hydroxide NaOH is 1.0: 2.2～2.8, trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrated barta Ba (OH) 2Mol ratio be 1.0: 1.2～1.8.
Further, the operational condition of described the 5th step evaporation oven dry is 60 ℃～120 ℃ of vaporization temperatures, evaporation absolute pressure 0.01MPa～0.1MPa.
Further, the leaching agent in described the 6th step leaching is any one in the acetone or alcohol.
Further, described the 8th step replacement(metathesis)reaction equipment is that the still formula stirs any one in chemical reactor, tubular chemical reactor or the static mixer.
Further, the operational condition of described the 8th step replacement(metathesis)reaction is 20 ℃～80 ℃ of temperature of reaction, reaction absolute pressure 0.1MPa～1.0MPa, trifluoromethane sulfonic acid potassium CF 3SO 3K or trifluoromethyl sulfonate CF 3SO 3The mol ratio of Na and hydrochloric acid HCl is 1.0: 1.2～1.6, trifluoromethane sulfonic acid potassium CF 3SO 3K or trifluoromethyl sulfonate CF 3SO 3Na and sulfuric acid H 2SO 4Mol ratio be 1.0: 0.6～0.8, or trifluoromethane sulfonic acid barium (CF 3SO 3) 2The mol ratio of Ba and hydrochloric acid HCl is 1.0: 2.4～3.2, or trifluoromethane sulfonic acid barium (CF 3SO 3) 2Ba and sulfuric acid H 2SO 4Mol ratio be 1.0: 1.2～1.6.
Further, the operational condition of described the tenth step rectification under vacuum is 60 ℃～162 ℃ of temperature, absolute pressure 0.001MPa～0.1MPa.
Chemical absorption reaction equation of the present invention is:
CF 3SO 2F+2KOH→CH 3SO 3K+KF+H 2O
CF 3SO 2F+2NaOH→CH 3SO 3Na+NaF+H 2O
CF 3SO 2F+Ba(OH) 2→(CF 3SO 3) 2Ba+BaF 2+H 2O
Employing sulfuric acid metathetical reaction equation of the present invention is:
2CF 3SO 3K+H 2SO 4→2CF 3SO 3H+K 2SO 4
2CF 3SO 3Na+H 2SO 4→2CF 3SO 3H+Na 2SO 4
(CF 3SO 3) 2Ba+H 2SO 4→2CF 3SO 3H+BaSO 4
The reaction equation of employing hydrochloric acid displaces of the present invention is:
CF 3SO 3K+HCl→CF 3SO 3H+KCl
CF 3SO 3Na+HCl→CF 3SO 3H+NaCl
(CF 3SO 3) 2Ba+2HCl→2CF 3SO 3H+BaCl 2
Realize that the main technique equipment that the present invention needs is: chemical absorption reactor, leaching equipment, metathesis reactor, evaporation equipment, cooling apparatus, filter plant etc.
Adopt the benefit of technique scheme to be: (1), the present invention are direct as the preparation raw material with the product of electrochemical reaction, and the product of electrochemical reaction is direct as preparation trifluoromethane sulfonic acid CF 3SO 3The raw material of H 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 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 CF of processing method preparation of the present invention 3SO 3The H 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 assimilated efficiency of the process that improves; (6), with methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product separates and preparation trifluoromethane sulfonic acid CF 3SO 3The preparation of H combines, with potassium hydroxide KOH or sodium hydroxide NaOH or hydrated barta Ba (OH) 2Carry out chemical absorption, generate trifluoromethane sulfonic acid potassium CF 3SO 3K or trifluoromethyl sulfonate CF 3SO 3Na or trifluoromethane sulfonic acid barium (CF 3SO 3) 2The trifluoromethyl sulfonic acid of Ba is again with hydrochloric acid HCl or sulfuric acid H 2SO 4Reaction generates trifluoromethane sulfonic acid CF 3SO 3H can improve trifluoromethane sulfonic acid CF according to the price and the source of these several trifluoromethyl sulfonic acids on the market like this 3SO 3The economy of H reduces production costs; (7), make full use of trifluoromethyl sulfonic acid and be dissolved in characteristic in acetone, ethanol, the ether, alkali is absorbed the trifluoromethyl sulfonic acid that the back generates, adopt the method for leaching to carry out separation and purification, obtain the organic solvent of trifluoromethyl sulfonic acid, use sulfuric acid H then 2SO 4Or hydrochloric acid HCl carries out replacement(metathesis)reaction, obtain trifluoromethane sulfonic acid, the characteristic of further utilizing the chlorate that generates in the replacement(metathesis)reaction or vitriol to be insoluble in organic solvent adopts the isolating method of solid-liquid to remove, and the dissolution characteristics that has made full use of product and by product carries out separation and purification; (8), the organic solvent that obtains is carried out underpressure distillation, obtain trifluoromethane sulfonic acid CF 3SO 3The H product, organic solvent can fully be recycled simultaneously.
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 equipment, cooling apparatus, filter plant.
Main raw material: methanesulfonyl fluoride CH 3SO 2F electrochemical fluorination gas-phase product, potassium hydroxide KOH, leaching agent acetone, hydrochloric acid HCl.
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H 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: in cooling apparatus, with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product, the service temperature of cooling condensation is 0 ℃, the operation absolute pressure is 1.0MPa, 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, contain trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrogen H 2Gas phase enter next step, liquid phase is that hydrogen fluoride HF further recycles;
(3) chemical absorption: stir in the chemical reactor in the still formula, in the aqueous solution of potassium hydroxide KOH, add the gaseous phase materials that obtains after the previous step solution-air is separated, 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: 2.2～2.8, and the concentration of the potassium hydroxide KOH aqueous solution is that 0.1mol/L is to saturation concentration;
(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 is mainly trifluoromethane sulfonic acid potassium CF 3SO 3K, Potassium monofluoride KF, water H 2O, potassium hydroxide KOH contain trifluoromethane sulfonic acid potassium CF 3SO 3The liquid phase of K enters next step;
(5) evaporation oven dry: in evaporation equipment, the liquid phase material that previous step is obtained evaporates oven dry, and operational condition is 60 ℃ of vaporization temperatures, evaporation absolute pressure 0.01MPa, the water H that the gas-phase product of evaporation obtains through condensation 2O recycles, and the solid phase after the evaporation oven dry enters next step;
(6) leaching: in leaching equipment, the solid-phase material that previous step is produced adds leaching agent acetone, leaches operation;
(7) solid-liquid separates: in filter plant, the material that previous step is produced carries out the solid-liquid separation, contains potassium hydroxide KOH and Potassium monofluoride KF in the solid phase, and solid phase is further recycled, and contains trifluoromethane sulfonic acid potassium CF 3SO 3The liquid phase of K enters next step;
(8) replacement(metathesis)reaction: in the still formula stirs chemical reactor, add hydrochloric acid HCl in the liquid phase material that previous step is obtained, carry out replacement(metathesis)reaction, generate product trifluoromethane sulfonic acid CF 3SO 3H and chlorate potassium chloride (KCl), the operational condition of replacement(metathesis)reaction are 20 ℃ of temperature of reaction, reaction absolute pressure 0.1MPa, trifluoromethane sulfonic acid potassium CF 3SO 3The mol ratio of K and hydrochloric acid HCl is 1.0: 1.2～1.6;
(9) solid-liquid separates: in filter plant, the material that previous step is produced carries out the solid-liquid separation, and solid phase is further recycled, and contains trifluoromethane sulfonic acid CF 3SO 3The liquid phase of H enters next step;
(10) rectification under vacuum: the liquid phase material of previous step is carried out rectifying, under the rectification under vacuum condition, at first is to separate out the light constituent leaching agent, then 80 ℃～83 ℃ of temperature, collects trifluoromethane sulfonic acid CF under the absolute pressure 0.005MPa condition 3SO 3H obtains vapor condensation product trifluoromethane sulfonic acid CF 3SO 3H, leaching agent return the utilization of the 6th step leaching step cycle, and residual solution is further handled.
Embodiment two
Major equipment: tubular chemical reactor, leaching equipment, metathesis reactor, evaporation equipment, cooling apparatus, filter plant.
Main raw material: methanesulfonyl fluoride CH 3SO 2F electrochemical fluorination gas-phase product, sodium hydroxide NaOH, leaching agent ethanol, hydrochloric acid HCl.
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H 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: in cooling apparatus, with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product, the service temperature of cooling condensation is-10 ℃, the operation absolute pressure is 0.8MPa, 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, contain trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrogen H 2Gas phase enter next step, liquid phase is that hydrogen fluoride HF further recycles;
(3) chemical absorption: in tubular chemical reactor, in the aqueous solution of sodium hydroxide NaOH, add the gaseous phase materials that obtains after the previous step solution-air is separated, 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 sodium hydroxide NaOH is 1.0: 2.2～2.8, and the concentration of the sodium hydroxide NaOH aqueous solution is that 0.1mol/L is to saturation concentration;
(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 is mainly trifluoromethyl sulfonate CF 3SO 3Na, Sodium Fluoride NaF, water H 2O, sodium hydroxide NaOH contain trifluoromethyl sulfonate CF 3SO 3The liquid phase of Na enters next step;
(5) evaporation oven dry: in evaporation equipment, the liquid phase material that previous step is obtained evaporates oven dry, and operational condition is 80 ℃ of vaporization temperatures, evaporation absolute pressure 0.05MPa, the water H that the gas-phase product of evaporation obtains through condensation 2O recycles, and the solid phase after the evaporation oven dry enters next step;
(6) leaching: in leaching equipment, the solid-phase material that previous step is produced adds leaching agent ethanol, leaches operation;
(7) solid-liquid separates: in filter plant, the material that previous step is produced carries out the solid-liquid separation, contains sodium hydroxide NaOH and Sodium Fluoride NaF in the solid phase, and solid phase is further recycled, and contains trifluoromethyl sulfonate CF 3SO 3The liquid phase of Na enters next step;
(8) replacement(metathesis)reaction: in tubular chemical reactor, add hydrochloric acid HCl in the liquid phase material that previous step is obtained, carry out replacement(metathesis)reaction, generate product trifluoromethane sulfonic acid CF 3SO 3H and chlorate sodium chloride nacl, the operational condition of replacement(metathesis)reaction are 50 ℃ of temperature of reaction, reaction absolute pressure 0.5MPa, trifluoromethyl sulfonate CF 3SO 3The mol ratio of Na and hydrochloric acid HCl is 1.0: 1.2～1.6;
(9) solid-liquid separates: in filter plant, the material that previous step is produced carries out the solid-liquid separation, and solid phase is further recycled, and contains trifluoromethane sulfonic acid CF 3SO 3The liquid phase of H enters next step;
(10) rectification under vacuum: the liquid phase material of previous step is carried out rectifying, under the rectification under vacuum condition, at first is to separate out the light constituent leaching agent, then 90 ℃～92 ℃ of temperature, collects trifluoromethane sulfonic acid CF under the evaporation absolute pressure 0.008MPa condition 3SO 3H obtains vapor condensation product trifluoromethane sulfonic acid CF 3SO 3H, leaching agent return the utilization of the 6th step leaching step cycle, and residual solution is further handled.
Embodiment three
Major equipment: chemical absorption tower, leaching equipment, static mixer, evaporation equipment, cooling apparatus, filter plant.
Main raw material: methanesulfonyl fluoride CH 3SO 2F electrochemical fluorination gas-phase product, hydrated barta Ba (OH) 2, leaching agent acetone, hydrochloric acid HCl.
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H 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: in cooling apparatus, with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product, the service temperature of cooling condensation is-20 ℃, the operation absolute pressure is 0.1MPa, 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, contain trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrogen H 2Gas phase enter next step, liquid phase is that hydrogen fluoride HF further recycles;
(3) chemical absorption: in the chemical absorption tower, at hydrated barta Ba (OH) 2The aqueous solution in add the gaseous phase materials that obtains after the previous step solution-air is separated, 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 2F and hydrated barta Ba (OH) 2Mol ratio be 1.0: 1.2～1.8, hydrated barta Ba (OH) 2The concentration of the aqueous solution is that 0.1mol/L is to saturation concentration;
(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 is mainly trifluoromethane sulfonic acid barium (CF 3SO 3) 2Ba, barium fluoride BaF 2, water H 2O, hydrated barta Ba (OH) 2, contain trifluoromethane sulfonic acid barium (CF 3SO 3) 2The liquid phase of Ba enters next step;
(5) evaporation oven dry: in evaporation equipment, the liquid phase material that previous step is obtained evaporates oven dry, and operational condition is 120 ℃ of vaporization temperatures, evaporation absolute pressure 0.1MPa, the water H that the gas-phase product of evaporation obtains through condensation 2O recycles, and the solid phase after the evaporation oven dry enters next step;
(6) leaching: in leaching equipment, the solid-phase material that previous step is produced adds leaching agent acetone, leaches operation;
(7) solid-liquid separates: in filter plant, the material that previous step is produced carries out the solid-liquid separation, contains hydrated barta Ba (OH) in the solid phase 2With barium fluoride BaF 2, solid phase is further recycled, and contains trifluoromethane sulfonic acid barium (CF 3SO 3) 2The liquid phase of Ba enters next step;
(8) replacement(metathesis)reaction: in static mixer, add hydrochloric acid HCl in the liquid phase material that previous step is obtained, carry out replacement(metathesis)reaction, generate product trifluoromethane sulfonic acid CF 3SO 3H and chlorate bariumchloride Ba (Cl) 2, the operational condition of replacement(metathesis)reaction is 80 ℃ of temperature of reaction, reaction absolute pressure 1.0MPa, trifluoromethane sulfonic acid barium (CF 3SO 3) 2The mol ratio of Ba and hydrochloric acid HCl is 1.0: 2.4～3.2;
(9) solid-liquid separates: in filter plant, the material that previous step is produced carries out the solid-liquid separation, and solid phase is further recycled, and contains trifluoromethane sulfonic acid CF 3SO 3The liquid phase of H enters next step;
(10) rectification under vacuum: the liquid phase material of previous step is carried out rectifying, under the rectification under vacuum condition, at first is to separate out the light constituent leaching agent, then 160 ℃～162 ℃ of temperature, collects trifluoromethane sulfonic acid CF under the absolute pressure 0.1MPa condition 3SO 3H obtains vapor condensation product trifluoromethane sulfonic acid CF 3SO 3H, leaching agent return the utilization of the 6th step leaching step cycle, and residual solution is further handled.
Embodiment four
Major equipment: the still formula stirs chemical reactor, leaching equipment, evaporation equipment, cooling apparatus, filter plant.
Main raw material: methanesulfonyl fluoride CH 3SO 2F electrochemical fluorination gas-phase product, potassium hydroxide KOH, leaching agent ethanol, sulfuric acid H 2SO 4
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H 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: in cooling apparatus, with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product, the service temperature of cooling condensation is-5 ℃, the operation absolute pressure is 0.9MPa, 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, contain trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrogen H 2Gas phase enter next step, liquid phase is that hydrogen fluoride HF further recycles;
(3) chemical absorption: stir in the chemical reactor in the still formula, in the aqueous solution of potassium hydroxide KOH, add the gaseous phase materials that obtains after the previous step solution-air is separated, 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: 2.2～2.8, and the concentration of the potassium hydroxide KOH aqueous solution is that 0.1mol/L is to saturation concentration;
(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 is mainly trifluoromethane sulfonic acid potassium CF 3SO 3K, Potassium monofluoride KF, water H 2O, potassium hydroxide KOH contain trifluoromethane sulfonic acid potassium CF 3SO 3The liquid phase of K enters next step;
(5) evaporation oven dry: in evaporation equipment, the liquid phase material that previous step is obtained evaporates oven dry, and operational condition is 70 ℃ of vaporization temperatures, evaporation absolute pressure 0.03MPa, the water H that the gas-phase product of evaporation obtains through condensation 2O recycles, and the solid phase after the evaporation oven dry enters next step;
(6) leaching: in leaching equipment, the solid-phase material that previous step is produced adds leaching agent ethanol, leaches operation;
(7) solid-liquid separates: in filter plant, the material that previous step is produced carries out the solid-liquid separation, contains potassium hydroxide KOH and Potassium monofluoride KF in the solid phase, and solid phase is further recycled, and contains trifluoromethane sulfonic acid potassium CF 3SO 3The liquid phase of K enters next step;
(8) replacement(metathesis)reaction: in the still formula stirs chemical reactor, add sulfuric acid H in the liquid phase material that previous step is obtained 2SO 4, carry out replacement(metathesis)reaction, generate product trifluoromethane sulfonic acid CF 3SO 3H and vitriol sulfuric acid potassium K 2SO 4, the operational condition of replacement(metathesis)reaction is 40 ℃ of temperature of reaction, reaction absolute pressure 0.3MPa, trifluoromethane sulfonic acid potassium CF 3SO 3K and sulfuric acid H 2SO 4Mol ratio be 1.0: 0.6～0.8;
(9) solid-liquid separates: in filter plant, the material that previous step is produced carries out the solid-liquid separation, and solid phase is further recycled, and contains trifluoromethane sulfonic acid CF 3SO 3The liquid phase of H enters next step;
(10) rectification under vacuum: the liquid phase material of previous step is carried out rectifying, under the rectification under vacuum condition, at first is to separate out the light constituent leaching agent, then 60 ℃～62 ℃ of temperature, collects trifluoromethane sulfonic acid CF under the evaporation absolute pressure 0.001MPa condition 3SO 3H obtains vapor condensation product trifluoromethane sulfonic acid CF 3SO 3H, leaching agent return the utilization of the 6th step leaching step cycle, and residual solution is further handled.
Present embodiment four is basic identical with embodiment one, main different be that the leaching agent of selecting for use in the leaching of the 6th step is an ethanol, the acid of selecting for use in the 8th step replacement(metathesis)reaction is sulfuric acid H 2SO 4
Embodiment five
Major equipment: tubular chemical reactor, leaching equipment, evaporation equipment, cooling apparatus, filter plant.
Main raw material: methanesulfonyl fluoride CH 3SO 2F electrochemical fluorination gas-phase product, sodium hydroxide NaOH, leaching agent acetone, sulfuric acid H 2SO 4
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H 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: in cooling apparatus, with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product, the service temperature of cooling condensation is-10 ℃, the operation absolute pressure is 0.8MPa, 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, contain trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrogen H 2Gas phase enter next step, liquid phase is that hydrogen fluoride HF further recycles;
(3) chemical absorption: in tubular chemical reactor, in the aqueous solution of sodium hydroxide NaOH, add the gaseous phase materials that obtains after the previous step solution-air is separated, 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 sodium hydroxide NaOH is 1.0: 2.2～2.8, and the concentration of the sodium hydroxide NaOH aqueous solution is that 0.1mol/L is to saturation concentration;
(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 is mainly trifluoromethyl sulfonate CF 3SO 3Na, Sodium Fluoride NaF, water H 2O, sodium hydroxide NaOH contain trifluoromethyl sulfonate CF 3SO 3The liquid phase of Na enters next step;
(5) evaporation oven dry: in evaporation equipment, the liquid phase material that previous step is obtained evaporates oven dry, and operational condition is 90 ℃ of vaporization temperatures, evaporation absolute pressure 0.06MPa, the water H that the gas-phase product of evaporation obtains through condensation 2O recycles, and the solid phase after the evaporation oven dry enters next step;
(6) leaching: in leaching equipment, the solid-phase material that previous step is produced adds leaching agent acetone, leaches operation;
(7) solid-liquid separates: in filter plant, the material that previous step is produced carries out the solid-liquid separation, contains sodium hydroxide NaOH and Sodium Fluoride NaF in the solid phase, and solid phase is further recycled, and contains trifluoromethyl sulfonate CF 3SO 3The liquid phase of Na enters next step;
(8) replacement(metathesis)reaction: in tubular chemical reactor, add sulfuric acid H in the liquid phase material that previous step is obtained 2SO 4, carry out replacement(metathesis)reaction, generate product trifluoromethane sulfonic acid CF 3SO 3H and vitriol sulfuric acid sodium Na 2SO 4, the operational condition of replacement(metathesis)reaction is 60 ℃ of temperature of reaction, reaction absolute pressure 0.6MPa, trifluoromethyl sulfonate CF 3SO 3Na and sulfuric acid H 2SO 4Mol ratio be 1.0: 0.6～0.8;
(9) solid-liquid separates: in filter plant, the material that previous step is produced carries out the solid-liquid separation, and solid phase is further recycled, and contains trifluoromethane sulfonic acid CF 3SO 3The liquid phase of H enters next step;
(10) rectification under vacuum: the liquid phase material of previous step is carried out rectifying, under the rectification under vacuum condition, at first is to separate out the light constituent leaching agent, then 90 ℃～92 ℃ of vaporization temperatures, collects trifluoromethane sulfonic acid CF under the evaporation absolute pressure 0.008MPa condition 3SO 3H obtains vapor condensation product trifluoromethane sulfonic acid CF 3SO 3H, leaching agent return the utilization of the 6th step leaching step cycle, and residual solution is further handled.
Present embodiment five is basic identical with embodiment two, main different be that the leaching agent of selecting for use in the leaching of the 6th step is an acetone, the acid of selecting for use in the 8th step replacement(metathesis)reaction is sulfuric acid H 2SO 4
Embodiment six
Major equipment: chemical absorption tower, leaching equipment, static mixer, evaporation equipment, cooling apparatus, filter plant.
Main raw material: methanesulfonyl fluoride CH 3SO 2F electrochemical fluorination gas-phase product, hydrated barta Ba (OH) 2, leaching agent ethanol, sulfuric acid H 2SO 4
As shown in the figure, a kind of methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H 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: in cooling apparatus, with methanesulfonyl fluoride CH 3SO 2The condensation of lowering the temperature of F electrochemical fluorination gas-phase product, the service temperature of cooling condensation is-15 ℃, the operation absolute pressure is 0.5MPa, 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, contain trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrogen H 2Gas phase enter next step, liquid phase is that hydrogen fluoride HF further recycles;
(3) chemical absorption: in the chemical absorption tower, at hydrated barta Ba (OH) 2The aqueous solution in add the gaseous phase materials that obtains after the previous step solution-air is separated, 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 2F and hydrated barta Ba (OH) 2Mol ratio be 1.0: 1.2～1.8, hydrated barta Ba (OH) 2The concentration of the aqueous solution is that 0.1mol/L is to saturation concentration;
(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 is mainly trifluoromethane sulfonic acid barium (CF 3SO 3) 2Ba, barium fluoride BaF 2, water H 2O, hydrated barta Ba (OH) 2, contain trifluoromethane sulfonic acid barium (CF 3SO 3) 2The liquid phase of Ba enters next step;
(5) evaporation oven dry: in evaporation equipment, the liquid phase material that previous step is obtained evaporates oven dry, 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 recycles, and the solid phase after the evaporation oven dry enters next step;
(6) leaching: in leaching equipment, the solid-phase material that previous step is produced adds leaching agent ethanol, leaches operation;
(7) solid-liquid separates: in filter plant, the material that previous step is produced carries out the solid-liquid separation, contains hydrated barta Ba (OH) in the solid phase 2With barium fluoride BaF 2, solid phase is further recycled, and contains trifluoromethane sulfonic acid barium (CF 3SO 3) 2The liquid phase of Ba enters next step;
(8) replacement(metathesis)reaction: in static mixer, add sulfuric acid H in the liquid phase material that previous step is obtained 2SO 4, carry out replacement(metathesis)reaction, generate product trifluoromethane sulfonic acid CF 3SO 3H and vitriol sulfuric acid barium BaSO 4, the operational condition of replacement(metathesis)reaction is 70 ℃ of temperature of reaction, reaction absolute pressure 0.8MPa, trifluoromethane sulfonic acid barium (CF 3SO 3) 2Ba and sulfuric acid H 2SO 4Mol ratio be 1.0: 1.2～1.6;
(9) solid-liquid separates: in filter plant, the material that previous step is produced carries out the solid-liquid separation, and solid phase is further recycled, and contains trifluoromethane sulfonic acid CF 3SO 3The liquid phase of H enters next step;
(10) rectification under vacuum: the liquid phase material of previous step is carried out rectifying, under the rectification under vacuum condition, at first is to separate out the light constituent leaching agent, then 120 ℃～122 ℃ of vaporization temperatures, collects trifluoromethane sulfonic acid CF under the evaporation absolute pressure 0.009MPa condition 3SO 3H obtains vapor condensation product trifluoromethane sulfonic acid CF 3SO 3H, leaching agent return the utilization of the 6th step leaching step cycle, and residual solution is further handled.
Present embodiment six is basic identical with embodiment three, main different be that the leaching agent of selecting for use in the leaching of the 6th step is an acetone, the acid of selecting for use in the 8th step replacement(metathesis)reaction is sulfuric acid H 2SO 4
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 (8)

1. methanesulfonyl fluoride CH 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H 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;
(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 product enters next step, and liquid phase is that hydrogen fluoride HF further recycles;
(3) chemical absorption: in absorption equipment, at potassium hydroxide KOH or sodium hydroxide NaOH or hydrated barta Ba (OH) 2The aqueous solution in add the gaseous phase materials that obtains after the previous step solution-air is separated, 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 material enters next step;
(5) evaporation oven dry: the liquid phase material that previous step is obtained evaporates oven dry, the water H that the gas-phase product of evaporation obtains through condensation 2O recycles, and the solid phase after the evaporation oven dry enters next step;
(6) leaching: the solid-phase material that previous step is produced adds leaching agent, leaches operation;
(7) solid-liquid separates: the material that previous step is produced carries out the solid-liquid separation, and solid phase is further recycled, and liquid phase material enters next step;
(8) replacement(metathesis)reaction: add hydrochloric acid HCl or sulfuric acid H in the liquid phase material that previous step is obtained 2SO 4, carry out replacement(metathesis)reaction, generate product trifluoromethane sulfonic acid CF 3SO 3H and chlorate perhaps generate product trifluoromethane sulfonic acid CF 3SO 3H and vitriol;
(9) solid-liquid separates: the material that previous step is produced carries out the solid-liquid separation, and solid phase is further recycled, and liquid phase enters next step;
(10) rectification under vacuum: the liquid phase material of previous step is carried out rectifying, obtain vapor condensation product trifluoromethane sulfonic acid CF 3SO 3H, leaching agent return the utilization of the 6th step leaching step cycle, and residual solution is further handled.
2. methanesulfonyl fluoride CH according to claim 1 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H 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 CF 3SO 3The method of H, 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 or sodium hydroxide NaOH is 1.0: 2.2～2.8, trifluoromethyl sulfonic acid fluoride CF 3SO 2F and hydrated barta Ba (OH) 2Mol ratio be 1.0: 1.2～1.8.
4. methanesulfonyl fluoride CH according to claim 1 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H is characterized in that: the operational condition of described the 5th step evaporation oven dry is 60 ℃～120 ℃ 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 CF 3SO 3The method of H is characterized in that: the leaching agent in described the 6th step leaching is any one in the acetone or alcohol.
6. methanesulfonyl fluoride CH according to claim 1 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H is characterized in that: described the 8th step replacement(metathesis)reaction equipment is that the still formula stirs any one in chemical reactor, tubular chemical reactor or the static mixer.
7. methanesulfonyl fluoride CH according to claim 1 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H is characterized in that: the operational condition of described the 8th step replacement(metathesis)reaction is 20 ℃～80 ℃ of temperature of reaction, reaction absolute pressure 0.1MPa～1.0MPa, trifluoromethane sulfonic acid potassium CF 3SO 3K or trifluoromethyl sulfonate CF 3SO 3The mol ratio of Na and hydrochloric acid HCl is 1.0: 1.2～1.6, trifluoromethane sulfonic acid potassium CF 3SO 3K or trifluoromethyl sulfonate CF 3SO 3Na and sulfuric acid H 2SO 4Mol ratio be 1.0: 0.6～0.8, or trifluoromethane sulfonic acid barium (CF 3SO 3) 2The mol ratio of Ba and hydrochloric acid HCl is 1.0: 2.4～3.2, or trifluoromethane sulfonic acid barium (CF 3SO 3) 2Ba and sulfuric acid H 2SO 4Mol ratio be 1.0: 1.2～1.6.
8. methanesulfonyl fluoride CH according to claim 1 3SO 2The F electrochemical fluorination gas-phase product prepares trifluoromethane sulfonic acid CF 3SO 3The method of H is characterized in that: the operational condition of described the tenth step rectification under vacuum is 60 ℃～162 ℃ of temperature, absolute pressure 0.001MPa～0.1MPa.
CN200810243629A 2008-12-11 2008-12-11 Method for preparing trifluoromethyl sulfonic acid CF3SO3H by electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F Pending CN101747240A (en)

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