CN113862707B - Method for preparing trifluoromethyl sulfuryl fluoride by medium-temperature electrolysis method - Google Patents
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Abstract
The invention relates to a method for preparing trifluoromethyl sulfuryl fluoride by a medium-temperature electrolytic method, belonging to the technical field of fine chemical engineering. The method comprises the steps of firstly, mixing HF and more than two alkali metal fluorides according to a specific molar ratio to prepare a complex, heating the complex to obtain molten salt, then heating the molten salt in an electrolytic cell to carry out first electrolytic dehydration, then adding raw materials to carry out second electrolytic dehydration, and finally carrying out electrolytic fluorination at a specific temperature and voltage, so that the preparation of the trifluoromethyl sulfonyl fluoride with high yield at a medium temperature is realized.
Description
Technical Field
The invention relates to a method for preparing trifluoromethyl sulfuryl fluoride by a medium-temperature electrolytic method, belonging to the technical field of fine chemical engineering.
Background
Trifluoromethyl sulfonyl fluoride (CF) 3 SO 2 F) Is an important raw material for synthesizing a surfactant and a lithium ion electrolyte, and is also used for synthesizing trifluoromethanesulfonic acid (CF) 3 SO 3 H) Of (a) thus CF 3 SO 2 F has a very good development prospect. At present, CF 3 SO 2 The preparation method of F comprises a chemical synthesis method and an electrolytic fluorination method:
the main raw material for chemical synthesis is trifluoromethyl sulfonyl chloride CF 3 SO 2 Cl; the main reaction is as follows: CF (compact flash) 3 SO 2 Cl+KF→CF 3 SO 2 F + KCl. The main raw material of the electrolytic fluorination method is methanesulfonyl fluoride CH 3 SO 2 F and anhydrous HF, the main reaction is as follows: HF in the electrolyte can be ionized to form F - And H + (ii) a The anode reaction has two steps: in the first step, the F ion releases electrons to form F radicals: f - -e - → F; the second step is that: reacting the F free radical with the methanesulfonyl fluoride to generate trifluoromethyl sulfonyl fluoride: CH (CH) 3 SO 2 F+6·F→CF 3 SO 2 F +3HF; the cathode reaction is H + Reduction to H 2 。
The by-product of the electrolytic fluorination process is H as opposed to the chemical synthesis process 2 Is more environment-friendly than KCl, has relatively simple process equipment, and is suitable for industrial preparation of CF 3 SO 2 And F, a main method.
At present, the electrolytic fluorination method is CH 3 SO 2 The electrolytic liquid system with F and HF mixed is the core, the first step is to remove HF and CH separately by electrochemical water removal 3 SO 2 Water in F, and then mixing into electrolyte; the second step is to prepare CF by electrolytic fluorination at a low temperature of-10 ℃ to 20 DEG C 3 SO 2 F. This method has a problem of low fluorination efficiency.
Disclosure of Invention
In view of this, the present invention aims to provide a method for preparing trifluoromethyl sulfonyl fluoride by a medium-temperature electrolysis method.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for preparing trifluoromethyl sulfuryl fluoride by a medium-temperature electrolysis method comprises the following steps:
(1) Mixing HF and more than two kinds of alkali metal fluorides (XF) according to a molar ratio of 4;
(2) Carrying out first electrolytic dehydration on the molten salt in the electrolytic bath, wherein the voltage of the first electrolytic dehydration is 4-6V, the temperature of the first electrolytic dehydration is 30-60 ℃, the first electrolytic gas is discharged, and when the current is reduced to 0, the first electrolytic dehydration is finished;
(3) Raw material CH 3 SO 2 Cl or CH 3 SO 2 F is added into an electrolytic bath for the second electrolytic dewatering, the voltage of the second electrolytic dewatering is 4V to 6V, and the temperature of the second electrolytic dewatering is30-60 ℃; emptying the second electrolytic gas, and finishing the second electrolytic water removal when detecting that the second electrolytic gas contains the raw material;
(4) Controlling the electrolysis pressure to be 5V-10V, maintaining the electrolysis temperature at 30-60 ℃, and collecting the electrolytic gas containing the trifluoromethyl sulfonyl fluoride through electrolytic fluorination.
Preferably, the mass fraction of the starting material is 5% to 15% based on 100% of the total mass of HF, alkali metal fluoride (XF) and starting material.
Preferably, the anode in the electrolytic cell is made of nickel or nickel alloy, and the cathode is made of nickel, nickel alloy, stainless steel or carbon steel.
Preferably, in step (1), the alkali metal fluoride (XF) is CsF, liF, naF or KF.
Preferably, in the step (2), a constant-pressure mode is adopted during the first water removal electrolysis.
Preferably, in step (3), the raw material is CH 3 SO 2 F。
Preferably, in the step (3), a constant pressure mode is adopted for the second electrolytic water removal.
Preferably, in the step (4), the current density at the time of electrolytic fluorination is up to 30mA/cm 2 ～80mA/cm 2 。
Advantageous effects
The invention provides a method for preparing trifluoromethyl sulfuryl fluoride by a medium-temperature electrolysis method, which comprises the steps of firstly heating a complex prepared by mixing HF and alkali metal fluoride according to a specific molar ratio to obtain molten salt, then heating the molten salt in an electrolytic bath to carry out first electrolytic dehydration, then adding raw materials to carry out second electrolytic dehydration, and finally carrying out electrolytic fluorination at a specific temperature and voltage, so that the preparation of the trifluoromethyl sulfuryl fluoride with high yield at the medium temperature is realized.
In the method, HF and alkali metal fluoride are mixed to form a complex XF & nHF, on one hand, more than two alkali metal fluorides are added into the electrolyte as a conductive agent, so that the conductivity of the electrolyte can be improved, and further the density of electrolytic current is increased; on the other hand, more than two alkali metal fluorides and anhydrous HF are complexed to form electrolyte,the volatilization amount of HF at the temperature of more than 30 ℃ and the melting temperature of the electrolyte are reduced; the addition ratio of the XF and the nHF is strictly controlled, the melting temperature of the complex XF & nHF is inversely proportional to n, and when the molar ratio of HF to XF is too low, the melting temperature exceeds 80 ℃, and at the moment, the complex system already forms F 2 Formation conditions, during which water removal occurs, F 2 And H 2 The reaction causes a phenomenon of stuffy sound; the molar ratio of HF to XF is too high, so that the conductivity of the electrolyte is insufficient, the current density is not obviously improved, and HF can be greatly volatilized during medium-temperature operation.
In the method of the invention, the first electrolytic water removal is carried out before the raw materials are added, so that the raw materials can be prevented from generating hydrolysis reaction with water to form CH in the presence of alkali metal fluoride 3 SO 2 H, which in turn results in low electrolytic current density and no long-term product recovery.
In the method, during electrolytic fluorination, the electrolytic temperature is kept between 30 and 60 ℃, the temperature is too low, the electrolyte is solidified, and the electrolysis is terminated; excessive temperature, CF 3 SO 2 F yield decreases and there will be F 2 Generation of F 2 And H 2 The reaction is explosive. The electrolytic pressure is maintained between 7V and 10V, the voltage is too low and no CF is generated 3 SO 2 F is generated, and too high a voltage can cause CF 3 SO 2 The yield of F is greatly reduced.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
In the following examples, the cathode and anode of the cell were both nickel plates.
Example 1
(1) Mixing HF, csF and LiF to obtain a complex, heating and melting to obtain a molten salt, and adding the molten salt into an electrolytic cell, wherein the molar ratio of the total amount of HF and the alkali metal fluoride is 7.
(2) And (3) carrying out primary constant-voltage electrolytic dewatering on the molten salt in the electrolytic bath, wherein the voltage of the primary constant-voltage electrolytic dewatering is 5.5V, the temperature of the primary constant-voltage electrolytic dewatering is 45 ℃, the primary constant-voltage electrolytic gas is discharged, and when the current is reduced to 0, the primary constant-voltage electrolytic dewatering is finished.
(3) Raw material CH 3 SO 2 F, adding the mixture into an electrolytic bath, and carrying out secondary constant-voltage electrolytic dewatering at the voltage of 5V and the temperature of 50 ℃; the second time of electrolytic gas emptying, when detecting that the second time of electrolytic gas contains raw materials, the second time of constant voltage electrolysis dewatering is finished; wherein, HF, csF and CH are used 3 SO 2 Total mass of F is 100%, CH 3 SO 2 The mass fraction of F is 10%.
(4) Switching to emptying for collection, increasing the electrolysis pressure to 8.5V, and controlling the current density to 58mA/cm 2 Electrolytic fluorination is carried out at the electrolytic temperature of 45 ℃ to obtain electrolytic gas; the infrared and chromatographic analysis shows that the main component of the electrolytic gas is CF 3 SO 2 F. HF and H 2 CF, based on the total volume of the electrolytic gas being 100% 3 SO 2 The volume fraction of F was 26%.
Example 2
(1) Mixing HF, liF and KF to obtain a complex, and adding molten salt obtained by heating and melting into an electrolytic cell; wherein the molar ratio of HF to LiF is 8, the molar ratio of LiF to KF is 1.
(2) And (3) carrying out primary constant-voltage electrolytic dewatering on the molten salt in the electrolytic bath, wherein the voltage of the primary constant-voltage electrolytic dewatering is 5V, the temperature of the primary constant-voltage electrolytic dewatering is 35 ℃, the primary constant-voltage electrolytic gas is discharged, and when the current is reduced to 0, the primary constant-voltage electrolytic dewatering is finished.
(3) Raw material CH 3 SO 2 Adding Cl into the electrolytic bath, and carrying out secondary constant-voltage electrolytic dewatering at a voltage of 5V and a temperature of 35 ℃; the second time of electrolytic gas emptying, when detecting that the second time of electrolytic gas contains raw materials, the second time of constant voltage electrolysis dewatering is finished; wherein, HF, liF and CH are used 3 SO 2 Total mass of F is 100%, CH 3 SO 2 The mass fraction of Cl was 8%.
(4) Switching to emptying for collection, increasing the electrolysis pressure to 8V, and controlling the current density to 55mA/cm 2 The electrolysis temperature is kept at 35 ℃, and fluorine is electrolyzedDissolving to obtain electrolytic gas; the infrared and chromatographic analysis shows that the main component of the electrolytic gas is CF 3 SO 2 F. HF and H 2 CF, based on the total volume of the electrolytic gas being 100% 3 SO 2 The volume fraction of F was 25%.
Example 3
(1) Mixing HF, liF, naF and KF to obtain a complex, and heating and melting the obtained molten salt to feed the complex into an electrolytic cell, wherein the molar ratio of the total amount of HF and alkali metal fluoride is 9, and the molar ratio of the total amount of LiF, naF and KF is 1.
(2) And (3) carrying out primary constant-voltage electrolytic dewatering on the molten salt in the electrolytic bath, wherein the voltage of the primary constant-voltage electrolytic dewatering is 6V, the temperature of the primary constant-voltage electrolytic dewatering is 30 ℃, the primary constant-voltage electrolytic gas is discharged, and when the current is reduced to 0, the primary constant-voltage electrolytic dewatering is finished.
(3) Raw material CH 3 SO 2 F, adding the mixture into an electrolytic bath, and carrying out secondary constant-voltage electrolytic dewatering at the voltage of 5V and the temperature of 30 ℃; the second time of electrolytic gas emptying, when detecting that the second time of electrolytic gas contains raw materials, the second time of constant voltage electrolysis dewatering is finished; wherein, HF, liF and CH 3 SO 2 Total mass of F is 100%, CH 3 SO 2 The mass fraction of F is 5%.
(4) Switching to emptying for collection, increasing the electrolysis pressure to 10V and the current density to 78mA/cm 2 Electrolytic fluorination is carried out at the electrolytic temperature of 30 ℃ to obtain electrolytic gas; the infrared and chromatographic analysis shows that the main component of the electrolytic gas is CF 3 SO 2 F. HF and H 2 CF, based on the total volume of the electrolytic gas being 100% 3 SO 2 The volume fraction of F was 28%.
Example 4
(1) Mixing HF, liF and NaF to obtain a complex, heating and melting to obtain molten salt, and adding the molten salt into an electrolytic bath, wherein the molar ratio of the total amount of HF and alkali metal fluoride is 4.
(2) And (3) carrying out primary constant-voltage electrolytic dewatering on the molten salt in the electrolytic bath, wherein the voltage of the primary constant-voltage electrolytic dewatering is 4V, the temperature of the primary constant-voltage electrolytic dewatering is 60 ℃, the primary constant-voltage electrolytic gas is discharged, and when the current is reduced to 0, the primary constant-voltage electrolytic dewatering is finished.
(3) Raw material CH 3 SO 2 F, adding the mixture into an electrolytic bath, and carrying out secondary constant-voltage electrolytic dewatering at the voltage of 5V and the temperature of 60 ℃; the second time of electrolytic gas emptying, when detecting that the second time of electrolytic gas contains raw materials, the second time of constant voltage electrolysis dewatering is finished; wherein, HF, liF and CH are used 3 SO 2 Total mass of F is 100%, CH 3 SO 2 The mass fraction of F was 15%.
(4) Switching to emptying for collection, increasing the electrolysis pressure to 5V and the current density to 33mA/cm 2 Maintaining the electrolysis temperature at 60 ℃, and performing electrolytic fluorination to obtain electrolytic gas; the infrared and chromatographic analysis shows that the main component of the electrolytic gas is CF 3 SO 2 F. HF and H 2 CF, based on the total volume of the electrolytic gas being 100% 3 SO 2 The volume fraction of F was 26%.
Comparative example 1
(1) HF and CH 3 SO 2 F, respectively carrying out constant-voltage electrolytic dewatering, wherein the electrolytic voltage is 5.5V, and when the current is reduced to 0, the dewatering is finished.
(2) Removing water from HF and CH 3 SO 2 F is added into an electrolytic cell to be mixed into electrolyte, and the electrolyte is added into the electrolytic cell, and the electrolytic voltage is 6.5V, and the current density is 17mA/cm 2 And electrolytic fluorination is carried out at the electrolytic temperature of 10 ℃ to obtain electrolytic gas. The infrared and chromatographic analysis shows that the main component of the electrolytic gas is CF 3 SO 2 F. HF and H 2 CF, based on the total volume of the electrolytic gas being 100% 3 SO 2 The volume fraction of F was 24%.
Comparative example 2
(1) Mixing HF, liF and KF to obtain a complex, and adding molten salt obtained by heating and melting into an electrolytic cell; wherein the molar ratio of HF to LiF is 6, and the molar ratio of LiF to KF is 1.
(2) And (3) carrying out primary constant-voltage electrolytic dewatering on the molten salt in the electrolytic bath, wherein the voltage of the primary constant-voltage electrolytic dewatering is 5.5V, the temperature of the primary constant-voltage electrolytic dewatering is 50 ℃, the primary constant-voltage electrolytic gas is discharged, and when the current is reduced to 0, the primary constant-voltage electrolytic dewatering is finished.
(3) Raw material CH 3 SO 2 Adding Cl into an electrolytic bath, and carrying out secondary constant-voltage electrolytic dewatering at a voltage of 5V and a temperature of 50 ℃; the second time of electrolytic gas emptying, when detecting that the second time of electrolytic gas contains raw materials, the second time of constant voltage electrolysis dewatering is finished; wherein, HF, KF and CH 3 SO 2 Total mass of Cl, CH, 100% 3 SO 2 The mass fraction of Cl was 8%.
(4) Switching to emptying for collection, increasing the electrolysis pressure to 7V, and controlling the current density to 45mA/cm 2 And the electrolytic temperature is kept at 55 ℃, and electrolytic fluorination is carried out to obtain electrolytic gas. The infrared and chromatographic analysis shows that the main component of the electrolytic gas is CF 3 SO 2 F. HF and H 2 (ii) a When the electrolysis temperature is raised to 80 ℃, CF in the electrolysis gas 3 SO 2 The content of F is reduced, the electrolytic cell has a muffled sound, and the electrolysis is stopped.
Comparative example 3
(1) Mixing HF, liF and NaF to obtain a complex, heating and melting to obtain molten salt, and adding the molten salt into an electrolytic bath, wherein the molar ratio of the total amount of HF and alkali metal fluoride is 4.5.
(2) And (3) carrying out primary constant-voltage electrolytic dewatering on the molten salt in the electrolytic bath, wherein the voltage of the primary constant-voltage electrolytic dewatering is 5.5V, the temperature of the primary constant-voltage electrolytic dewatering is 60 ℃, the primary constant-voltage electrolytic gas is discharged, and when the current is reduced to 0, the primary constant-voltage electrolytic dewatering is finished.
(3) Raw material CH 3 SO 2 F, adding the mixture into an electrolytic bath, and carrying out secondary constant-voltage electrolytic dewatering at the voltage of 5V and the temperature of 50 ℃; the second time of electrolytic gas emptying, when detecting that the second time of electrolytic gas contains raw materials, the second time of constant voltage electrolysis dewatering is finished; wherein the compound is selected from the group consisting of HF, csF andCH 3 SO 2 total mass of F is 100%, CH 3 SO 2 The mass fraction of F was 6%.
(4) Switching to emptying for collection, increasing the electrolysis pressure to 9V, and controlling the current density to 65mA/cm 2 And the electrolysis temperature is kept at 60 ℃, and electrolytic fluorination is carried out to obtain electrolytic gas. The infrared and chromatographic analysis shows that the main component of the electrolytic gas is CF 3 SO 2 F. HF and H 2 (ii) a When the electrolysis voltage is increased to 11V, CF in the electrolysis gas 3 SO 2 The content of F is greatly reduced, and the electrolysis is stopped.
In summary, the invention includes but is not limited to the above embodiments, and any equivalent replacement or local modification made under the spirit and principle of the invention should be considered as being within the protection scope of the invention.
Claims (1)
1. A method for preparing trifluoromethyl sulfuryl fluoride by a medium-temperature electrolysis method is characterized in that: the method comprises the following steps:
(1) Mixing HF and two or more alkali metal fluorides according to a molar ratio of 4;
(2) Carrying out first electrolytic dehydration on the molten salt in the electrolytic bath, wherein the voltage of the first electrolytic dehydration is 4-6V, the temperature of the first electrolytic dehydration is 30-60 ℃, the first electrolytic gas is discharged, and when the current is reduced to 0, the first electrolytic dehydration is finished;
(3) Raw material CH 3 SO 2 Cl or CH 3 SO 2 F, adding the mixture into an electrolytic bath for second electrolytic dewatering, wherein the voltage of the second electrolytic dewatering is 4V-6V, and the temperature of the second electrolytic dewatering is 30-60 ℃; emptying the second electrolytic gas, and finishing the second electrolytic water removal when detecting that the second electrolytic gas contains the raw material;
(4) Controlling the electrolysis pressure to be 5V-10V, maintaining the electrolysis temperature at 30-60 ℃, and collecting the electrolysis gas containing the trifluoromethyl sulfonyl fluoride by electrolytic fluorination
The mass fraction of the raw materials is 5 to 15 percent based on 100 percent of the total mass of the HF and the alkali metal fluoride and the total mass of the raw materials;
the anode in the electrolytic cell is made of nickel or nickel alloy, and the cathode is made of nickel, nickel alloy, stainless steel or carbon steel;
in the step (1), the alkali metal fluoride is CsF, liF, naF or KF;
in the step (2), a constant-pressure mode is adopted during the first time of electrolytic water removal;
in the step (3), the raw material is CH 3 SO 2 F; a constant-pressure mode is adopted during the second electrolytic water removal;
in the step (4), the current density is 30mA/cm during electrolytic fluorination 2 ～80mA/cm 2 。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2732398A (en) * | 1953-01-29 | 1956-01-24 | cafiicfzsojk | |
| CN101748424A (en) * | 2008-12-11 | 2010-06-23 | 张家港市国泰华荣化工新材料有限公司 | Method for preparing trifluoromethyl sulfuryl fluoride CF3SO2F by electrochemical fluorination of methanesulfonyl fluoride CH3SO2F |
| CN112760672A (en) * | 2020-12-15 | 2021-05-07 | 中船重工（邯郸）派瑞特种气体有限公司 | Method for electrochemically preparing trifluoromethyl sulfonyl fluoride from methyl sulfonyl chloride |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2732398A (en) * | 1953-01-29 | 1956-01-24 | cafiicfzsojk | |
| CN101748424A (en) * | 2008-12-11 | 2010-06-23 | 张家港市国泰华荣化工新材料有限公司 | Method for preparing trifluoromethyl sulfuryl fluoride CF3SO2F by electrochemical fluorination of methanesulfonyl fluoride CH3SO2F |
| CN112760672A (en) * | 2020-12-15 | 2021-05-07 | 中船重工（邯郸）派瑞特种气体有限公司 | Method for electrochemically preparing trifluoromethyl sulfonyl fluoride from methyl sulfonyl chloride |
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