A purification device and method for trimethylsilyl trifluoromethanesulfonate

Abstract

The application provides a purification device for trimethylsilyl trifluoromethanesulfonate, which comprises a reaction kettle, a uniform feeding mechanism arranged on the outer wall of the reaction kettle, a stirring device installed at the upper end of the reaction kettle, a rectifying column connected to the upper end of the reaction kettle, a filler mechanism arranged in the rectifying column, a reflux tank installed at the upper end of the rectifying column, a material conveying pipe connected to the upper end of the reflux tank, a condenser installed on the material conveying pipe, and a product receiving tank connected to one end of the material conveying pipe; and the application also provides a method for purifying trimethylsilyl trifluoromethanesulfonate by using the above-mentioned purification device, which comprises the following steps: introducing crude trimethylsilyl trifluoromethanesulfonate into the reaction kettle through the uniform feeding mechanism, vacuumizing the purification device from the top of the rectifying column, heating the reaction kettle, and refluxing to obtain high-purity trimethylsilyl trifluoromethanesulfonate. The application can effectively improve the mixing and stirring speed of raw materials, can fully and quickly absorb in the rectification stage, can reduce product loss, and can improve production efficiency.

Description

TECHNICAL FIELD

[0001] The present application relates to the chemical technology field, specifically relates to a purification device and method of trifluoromethanesulfonic acid trimethyl silyl ester. BACKGROUND

[0002] Currently, in chemical production, trifluoromethanesulfonic acid trimethyl silyl ester is generally prepared from trifluoromethanesulfonic acid and trimethylchlorosilane, and the whole preparation process includes the following steps: 1. In the reactor, trimethylchlorosilane is reacted with trifluoromethanesulfonic acid in a dropwise manner to generate main product trifluoromethanesulfonic acid trimethyl silyl ester crude product and byproduct hydrogen chloride; 2. After the reaction is completed, the trifluoromethanesulfonic acid trimethyl silyl ester crude product is pretreated (preliminary purification) in the reactor; 3. The trifluoromethanesulfonic acid trimethyl silyl ester crude product is purified by multiple distillation or two-stage rectification to obtain trifluoromethanesulfonic acid trimethyl silyl ester product. The above process has the following disadvantages: 1. The product needs to be distilled multiple times to obtain qualified product, the process is complex, and the production efficiency is low; 2. By adopting multiple distillation or two-stage rectification, the material is transferred in multiple devices, and there is loss in different degrees, so the product yield is low; 3. By adopting multiple distillation or two-stage rectification, more heating devices are involved, and the energy consumption is large.

[0003] Therefore, a purification device and method of trifluoromethanesulfonic acid trimethyl silyl ester are provided to solve the above problems. SUMMARY

[0004] The technical problem to be solved by the present application is to provide a purification device and method of trifluoromethanesulfonic acid trimethyl silyl ester, which can effectively improve the mixing and stirring speed of raw materials, and can quickly absorb in the rectification stage, while reducing product loss.

[0005] To solve the above technical problems, the technical scheme adopted by the present application is as follows: a purification device of trifluoromethanesulfonic acid trimethyl silyl ester, comprising a reaction kettle, a uniform feeding mechanism is arranged on the outer side wall of the reaction kettle, a stirring mechanism is arranged at the upper end of the reaction kettle, a rectification column is also arranged at the upper end of the reaction kettle, a packing mechanism is arranged in the rectification column, the upper end of the rectification column penetrates through the bottom end of a reflux tank and extends into the reflux tank, a reflux pipe is arranged on the outer side wall of the lower part of the reflux tank, one end of the reflux pipe is connected with the rectification column, a connecting head is connected with the upper end of the reflux tank, a tower top thermometer is arranged on the upper end of the connecting head, a material conveying pipe vacuum pipeline is connected with one side end of the connecting head, a material conveying pipe is connected with the other side end of the connecting head, a condenser is installed on the material conveying pipe, a product receiving tank is connected with one end of the material conveying pipe, and a receiving tank vacuum pipeline is connected with the upper end of the product receiving tank.

[0006] The uniform feeding mechanism comprises an annular connecting pipe mounted on the outer sidewall of the reaction kettle, a plurality of spray heads are equidistantly arranged on the inner sidewall of the annular connecting pipe, one end of each of the spray heads penetrates the sidewall of the reaction kettle and extends into the reaction kettle, a delivery pump is arranged on one side of the reaction kettle, the delivery pump is connected with the annular connecting pipe through a delivery pipe, the packing mechanism comprises a spiral baffle arranged on the bottom of the rectifying column, and a packing layer is arranged between the spiral baffles, the stirring mechanism comprises a motor mounting support mounted on the upper end of the reaction kettle, a driving motor is mounted on the motor mounting support, a stirring rod is connected with the output shaft of the driving motor through a shaft coupling, and the lower end of the stirring rod extends into the reaction kettle.

[0007] Preferably, a reflux valve is mounted on the reflux pipe.

[0008] Preferably, the rectifying column is made of enamel, titanium or super stainless steel 254SMO.

[0009] Preferably, a tower top vacuum valve is arranged on the delivery pipe vacuum line.

[0010] Preferably, a receiving tank vacuum valve is arranged on the receiving tank vacuum line, one end of the tower top thermometer is connected with the tower top vacuum valve, and the other end of the tower top thermometer is connected with the receiving tank vacuum valve.

[0011] Preferably, a receiving tank feeding valve is arranged on the delivery pipe between the condenser and the product receiving tank.

[0012] The application also provides a method for purifying trimethylsilyl triflate by using the above-mentioned purification device, which comprises the following steps:

[0013] S1, introducing the crude trimethylsilyl triflate into the reaction kettle through the uniform feeding mechanism;

[0014] S2, opening the tower top vacuum valve, vacuumizing the purification device through the delivery pipe vacuum line from the top of the rectifying column, heating and warming the reaction kettle when the vacuum is stable, keeping the temperature of the top of the rectifying column at 55-75 DEG C, and making the reflux tank in full reflux; when the temperature of the reaction kettle is 75-90 DEG C and the temperature of the top of the rectifying column is 65-85 DEG C, closing the tower top vacuum valve, vacuumizing the reaction kettle through the product receiving tank, and keeping the reflux ratio of the reflux tank at 6-8;

[0015] S3, when the temperature of the reaction kettle is greater than or equal to 105 DEG C, stopping product collection, heating and vacuumizing, opening the reflux valve, pouring the liquid in the reflux tank into the reaction kettle, and ending the rectification, so that high-purity trimethylsilyl triflate is obtained in the product receiving tank.

[0016] Preferably, the pressure of the vacuum in S2 is -0.095MPa to -0.092MPa.

[0017] Compared with the prior art, the present application has the following advantages:

[0018] The present application can effectively improve the mixing and stirring speed of raw materials, and can fully and quickly absorb in the rectification stage, reduce product loss, facilitate equipment maintenance, improve production efficiency, reduce production procedures, and improve operation safety and practicality.

[0019] The present application will be further described in detail below in combination with the accompanying drawings and examples. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 is a schematic diagram of the internal structure of the present application.

[0021] Figure 2 is a schematic diagram of the external structure of the present application.

[0022] Figure 3 is a schematic diagram of the structure of the annular connecting pipe in the present application.

[0023] Figure 4 is Figure 1 is an enlarged view of structure A in the present application.

[0024] BRIEF DESCRIPTION OF DRAWINGS

[0025] 1 - delivery pump; 2 - delivery pipe; 3 - annular connecting pipe; 4 - reaction kettle; 5 - rectification column; 6 - reflux valve; 7 - spiral baffle; 8 - reflux tank; 9 - overhead vacuum valve; 10 - overhead temperature gauge; 11 - connecting head; 12 - reflux pipe; 13 - driving motor; 14 - condenser; 15 - material delivery pipe; 16 - receiving tank feed valve; 17 - receiving tank vacuum valve; 18 - receiving tank vacuum pipe line; 19 - product receiving tank; 20 - stirring rod; 21 - spray head; 22 - packing layer. DETAILED DESCRIPTION

[0026] The technical solutions in the embodiments of the present application will be described clearly and completely below in combination with the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments.

[0027] As Figure 1As shown, the purification device of the present application for trimethylsilyl trifluoromethanesulfonate comprises a reaction kettle 4, the outer wall of which is provided with a uniform feeding mechanism, the upper end of the reaction kettle 4 is provided with a stirring mechanism, and the upper end of the reaction kettle 4 is also provided with a rectifying column 5, the rectifying column 5 is provided with a packing mechanism, the upper end of the rectifying column 5 penetrates the bottom end of a reflux tank 8 and extends into the reflux tank 8, the outer wall of the lower part of the reflux tank 8 is provided with a reflux pipe 12, one end of the reflux pipe 12 is connected with the rectifying column 5, the upper end of the reflux tank 8 is connected with a connecting head 11, the upper end of the connecting head 11 is provided with a top temperature gauge 10, one side end of the connecting head 11 is connected with a material conveying pipe vacuum pipeline, the other side end of the connecting head 11 is connected with a material conveying pipe 15, the material conveying pipe 15 is provided with a condenser 14, one end of the material conveying pipe 15 is connected with a product receiving tank 19, and the upper end of the product receiving tank 19 is connected with a receiving tank vacuum pipeline 18.

[0028] The uniform feeding mechanism comprises an annular connecting pipe 3 installed on the outer wall of the reaction kettle 4, a plurality of spray heads 21 are equidistantly arranged on the inner wall of one side of the annular connecting pipe 3, and one end of each spray head 21 penetrates the side wall of the reaction kettle 4 and extends into the reaction kettle 4; one side of the reaction kettle 4 is provided with a conveying pump 1 connected with the annular connecting pipe 3 through a conveying pipe.

[0029] The packing mechanism comprises a spiral baffle 7 arranged on the bottom of the rectifying column 5, and a packing layer 22 is arranged between the spiral baffles 7, and the packing layer 22 is stainless steel Pall ring packing or stepped ring packing, etc.; the packing layer 22 provides sufficient contact surface for gas and liquid phases, and creates conditions for improving the turbulence degree of the gas phase, so as to facilitate mass transfer and heat transfer, so that the light component (HCl) is continuously enriched and rises, and the heavy component (CF3SO3H) is continuously concentrated and falls, thereby achieving the purpose of purifying the product.

[0030] The stirring mechanism comprises a motor mounting support installed on the upper end of the reaction kettle 4, a driving motor 13 is installed on the motor mounting support, a stirring rod 20 is connected with the output shaft of the driving motor 13 through a shaft coupling, and the lower end of the stirring rod 20 extends into the reaction kettle 4.

[0031] In this embodiment, the reflux valve 6 is installed on the reflux pipe 12; the rectifying column 5 is made of enamel, titanium material or super stainless steel 254SMO material.

[0032] In this embodiment, the feed pipe 15 between the condenser 14 and the product receiving tank 19 is provided with a receiving tank feed valve 16; the overhead vacuum valve 9 is provided on the feed pipe vacuum line, the receiving tank vacuum valve 17 is provided on the receiving tank vacuum line 18, one end of the overhead thermometer 10 is connected with the overhead vacuum valve 9, and the other end of the overhead thermometer 10 is connected with the receiving tank vacuum valve 17.

[0033] Example 2

[0034] The method for purifying trimethylsilyl triflate using the purification device in Example 1 comprises the following steps:

[0035] S1, the crude trimethylsilyl triflate is introduced into the reaction kettle 4 through the delivery pipe 2 and the annular connecting pipe 3 in the uniform feeding mechanism; the component content of the crude trimethylsilyl triflate is shown in Table 1;

[0036] S2, the overhead vacuum valve 9 is opened, the entire purification device is vacuumed through the feed pipe vacuum line from the top of the rectification column 5, at this time, the light component impurities (HCl) in the purification device are directly removed from the top of the rectification column 5, after the vacuum is stable, the liquid in the reaction kettle 4 is gradually heated and warmed, the temperature of the top of the rectification column 5 is maintained at 55℃, and the reflux tank 8 is in full reflux;

[0037] When the temperature of the reaction kettle 4 is 75℃ and the temperature of the top of the rectification column 5 is 65℃, the overhead vacuum valve 9 is closed, the receiving tank vacuum valve 17 is opened, the reaction kettle 4 is vacuumed through the product receiving tank 19, the reflux ratio of the reflux tank 8 is 6, and the product is collected; the pressure of the vacuuming is all-0.095MPa;

[0038] S3, when the kettle temperature of the reaction kettle 4 is ≥105℃, the product collection is stopped, the heating is stopped, the vacuuming is stopped, the reflux valve 6 is opened, the liquid in the reflux tank 8 is poured into the reaction kettle 4, the rectification is ended, and the high-purity trimethylsilyl triflate is obtained in the product receiving tank 19.

[0039] The component content of the high-purity trimethylsilyl triflate obtained in this embodiment is shown in Table 1.

[0040] Example 3

[0041] The method for purifying trimethylsilyl triflate using the purification device in Example 1 comprises the following steps:

[0042] S1, the crude trimethylsilyl triflate is introduced into the reaction kettle 4 through the delivery pipe 2 and the annular connecting pipe 3 in the uniform feeding mechanism; the component content of the crude trimethylsilyl triflate is shown in Table 1;

[0043] S2, open the overhead vacuum valve 9, and vacuum the entire purification device through the feed pipe vacuum line from the top of the rectification column 5, at which time the light component impurities in the purification device are directly removed from the top of the rectification column 5, and after the vacuum is stable, the liquid in the reaction kettle 4 is heated and warmed, the temperature of the top of the rectification column 5 is kept at 75°C, and the reflux tank 8 is in total reflux;

[0044] When the temperature of the reaction kettle 4 is 90°C and the temperature of the top of the rectification column 5 is 85°C, the overhead vacuum valve 9 is closed, the receiving tank vacuum valve 17 is opened, the reaction kettle 4 is vacuumed through the product receiving tank 19, the reflux ratio of the reflux tank 8 is 8, and product collection is performed; the vacuuming pressure is all -0.092 MPa;

[0045] S3, when the kettle temperature of the reaction kettle 4 is ≥ 105°C, stop product collection, stop heating, stop vacuuming, open the reflux valve 6, and pour the liquid in the reflux tank 8 into the reaction kettle 4, and the distillation is completed, and the product receiving tank 19 obtains high-purity trimethylsilyl triflate.

[0046] The component content of the high-purity trimethylsilyl triflate obtained in this example is shown in Table 1.

[0047] Example 4

[0048] The method for purifying trimethylsilyl triflate using the purification device in Example 1 includes the following steps:

[0049] S1, the crude trimethylsilyl triflate is introduced into the reaction kettle 4 through the feed pipe 2 and the annular connecting pipe 3 in the uniform feeding mechanism; the component content of the crude trimethylsilyl triflate is shown in Table 1;

[0050] S2, open the overhead vacuum valve 9, and vacuum the entire purification device through the feed pipe vacuum line from the top of the rectification column 5, at which time the light component impurities in the purification device are directly removed from the top of the rectification column 5, and after the vacuum is stable, the liquid in the reaction kettle 4 is heated and warmed, the temperature of the top of the rectification column 5 is kept at 65°C, and the reflux tank 8 is in total reflux;

[0051] When the temperature of the reaction kettle 4 is 85°C and the temperature of the top of the rectification column 5 is 75°C, the overhead vacuum valve 9 is closed, the receiving tank vacuum valve 17 is opened, the reaction kettle 4 is vacuumed through the product receiving tank 19, the reflux ratio of the reflux tank 8 is 7, and product collection is performed; the vacuuming pressure is all -0.093 MPa;

[0052] S3, when the temperature of the reactor 4 is ≥ 105℃, stop collecting the product, stop heating, stop vacuumizing, open the reflux valve 6, pour the liquid in the reflux tank 8 into the reactor 4, and the distillation is finished, the high-purity trimethylsilyl trifluoromethanesulfonate is obtained in the product receiving tank 19.

[0053] The component content of the high-purity trimethylsilyl trifluoromethanesulfonate obtained in the example is shown in Table 1.

[0054] Table 1 Component content of the crude trimethylsilyl trifluoromethanesulfonate and the high-purity trimethylsilyl trifluoromethanesulfonate in Examples 2-4

[0055]

[0056] As shown in Table 1, the device of the present application includes the whole process of product synthesis and distillation, and the purity of the crude trimethylsilyl trifluoromethanesulfonate is increased from 92%-95% to ≥ 99.0%; compared with the existing process of multiple distillation, the product yield is increased from about 90% to more than 98%; compared with the existing process, the single-pot operation period (from starting feeding to product packaging) of the method of the present application is shortened from 120h to 72h, and it can be seen that the production efficiency of the method of the present application is higher than that of the prior art, and the product loss is reduced, the equipment is convenient to maintain, and the safety of operation is improved.

[0057] The above is only the preferred embodiment of the present application, and does not limit the present application. Any simple modification, change and equivalent change made according to the technical essence of the present application to the above embodiment are still within the protection scope of the technical solution of the present application.

Claims

1. A purification apparatus for trimethylsilyl triflate comprising a reaction vessel (4), characterized in that, The outer side wall of the reaction kettle (4) is provided with a uniform feeding mechanism, the upper end of the reaction kettle (4) is provided with a stirring mechanism, the upper end of the reaction kettle (4) is also provided with a rectifying column (5), the rectifying column (5) is provided with a packing mechanism, the upper end of the rectifying column (5) penetrates the bottom end of the reflux tank (8) and extends into the reflux tank (8), the lower part of the outer side wall of the reflux tank (8) is provided with a reflux pipe (12), one end of the reflux pipe (12) is connected with the rectifying column (5), the upper end of the reflux tank (8) is connected with a connecting head (11), the upper end of the connecting head (11) is provided with a tower top thermometer (10), one side end of the connecting head (11) is connected with a material conveying pipe vacuum pipeline, the other side end of the connecting head (11) is connected with a material conveying pipe (15), the material conveying pipe (15) is provided with a condenser (14), one end of the material conveying pipe (15) is connected with a product receiving tank (19), the upper end of the product receiving tank (19) is connected with a receiving tank vacuum pipeline (18); The uniform feeding mechanism comprises an annular connecting pipe (3) installed on the outer side wall of the reaction kettle (4), a plurality of spray heads (21) are equidistantly arranged on the inner side wall of one side of the annular connecting pipe (3), and one end of each spray head (21) penetrates the side wall of the reaction kettle (4) and extends into the reaction kettle (4); a conveying pump (1) is arranged on one side of the reaction kettle (4), and the conveying pump (1) is connected with the annular connecting pipe (3) through a conveying pipe (2); the packing mechanism comprises a spiral baffle (7) arranged on the bottom of the rectifying column (5), and a packing layer (22) is arranged between the spiral baffles (7); the stirring mechanism comprises a motor mounting support installed on the upper end of the reaction kettle (4), a driving motor (13) is installed on the motor mounting support, a stirring rod (20) is connected with the output shaft of the driving motor (13) through a shaft coupling, and the lower end of the stirring rod (20) extends into the reaction kettle (4).

2. The device for purifying trimethylsilyl triflate according to claim 1, wherein The reflux valve (6) is installed on the reflux pipe (12).

3. The device for purifying trimethylsilyl triflate according to claim 1, wherein The rectifying column (5) is made of enamel, titanium material or super stainless steel 254SMO material.

4. The device for purifying trimethylsilyl triflate according to claim 1, wherein The overhead vacuum valve (9) is arranged on the material conveying pipe vacuum pipeline.

5. A device for purifying trimethylsilyl triflate according to claim 4, characterized in that, The receiving tank vacuum valve (17) is arranged on the receiving tank vacuum pipeline (18), one end of the tower top thermometer (10) is connected with the overhead vacuum valve (9), and the other end of the tower top thermometer (10) is connected with the receiving tank vacuum valve (17).

6. The device for purifying trimethylsilyl triflate according to claim 1, wherein The receiving tank feeding valve (16) is arranged on the material conveying pipe (15) between the condenser (14) and the product receiving tank (19).

7. A process for purifying trimethylsilyl triflate using the purification apparatus according to any one of claims 1 to 6, characterized in that, The method comprises the following steps: S1, the crude product of trimethylsilyl triflate is introduced into the reaction kettle (4) through the uniform feeding mechanism; S2, open the overhead vacuum valve (9), vacuum the purification device from the top of the rectification column (5) through the feed tube vacuum pipeline, after the vacuum is stable, heat the reaction kettle (4), keep the temperature of the top of the rectification column (5) at 55-75℃, and the reflux tank (8) is in total reflux; when the temperature of the reaction kettle (4) is 75-90℃ and the temperature of the top of the rectification column (5) is 65-85℃, close the overhead vacuum valve (9), vacuum the reaction kettle (4) through the product receiving tank (19), the reflux ratio of the reflux tank (8) is 6-8, and the product is collected; S3, when the temperature of the reaction kettle (4) is greater than or equal to 105℃, stop collecting the product, stop heating, stop vacuumizing, open the reflux valve (6), pour the liquid in the reflux tank (8) into the reaction kettle (4), and the rectification is finished. The product receiving tank (19) obtains high-purity trimethylsilyl triflate.

8. The method of purifying trimethylsilyl triflate according to claim 7, wherein The pressure of the vacuum in S2 is-0.095MPa~ -0.092MPa.

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