CN103450050A - Purification method of trifluoromethanesulfonic anhydride - Google Patents
Purification method of trifluoromethanesulfonic anhydride Download PDFInfo
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Abstract
The invention discloses a purification method of trifluoromethanesulfonic anhydride, and belongs to the field of fine chemicals. The method comprises the following steps: introducing a trifluoromethanesulfonic anhydride crude product into a rectification kettle with a rectification tower, vaccumizing a rectification system, starting to heat the rectification kettle after the vacuum degree is stable, and performing total reflux for 1-5 hours; collecting a front fraction at the reflux ratio of 10-15 when the temperature of the rectification kettle is 50-65 DEG C and the temperature at the tower top of the rectification tower is 40-60 DEG C; collecting a medium fraction at the reflux ratio of 4-6 when the temperature of the rectification kettle is 65-70 DEG C and the temperature at the tower top of the rectification tower is 60-68 DEG C; collecting a back fraction at the reflux ratio of 6-8 when the temperature of the rectification kettle increases by 2 DEG C and the temperature at the tower top of the rectification tower is 66-71 DEG C; stopping the collection of the back fraction, stopping heating, stopping vaccumizing and finishing rectification when the temperature of the rectification kettle is not less than 120 DEG C, wherein the medium fraction is a trifluoromethanesulfonic anhydride fine product. The method has the advantages of simplicity in operation and higher product purity.
Description
Technical field
The present invention relates to a kind of purification process of trifluoromethanesulfanhydride anhydride, be applicable to take trifluoromethanesulfonic acid and Vanadium Pentoxide in FLAKES as raw material prepares the suitability for industrialized production of trifluoromethanesulfanhydride anhydride, belong to field of fine chemical.
Background technology
Trifluoromethanesulfanhydride anhydride ((CF
3sO
2)
2o) be the derivative of trifluoromethanesulfonic acid, of many uses: as to be intermediate commonly used in pharmaceutical industry, can be used for synthetic nucleosides, microbiotic, steroid, protein, VITAMIN etc.Can be used as again the catalyzer of the reactions such as polymerization, esterification, alkylation, be widely used in the fields such as plastics industry, electron chemistry industry, sugar-refining industry.
Trifluoromethanesulfanhydride anhydride has multiple preparation method: trifluoromethanesulfonic acid and Vanadium Pentoxide in FLAKES reaction method; Trifluoromethanesulfonic acid and phosphorus pentachloride, trifluoromethanesulfonic acid and phosphorus trichloride and chlorine reaction method; The lithium of trifluoromethanesulfchloride chloride and trifluoromethanesulfonic acid, sodium, sylvite reaction method etc.The industrial method for preparing trifluoromethanesulfanhydride anhydride is mainly to adopt trifluoromethanesulfonic acid to react with Vanadium Pentoxide in FLAKES, and reaction equation is shown as follows.
6CF
3SO
3H+P
2O
5→3(CF
3SO
2)
2O+2H
3PO
4
The impurity that trifluoromethanesulfanhydride anhydride reacts with Vanadium Pentoxide in FLAKES in the trifluoromethanesulfanhydride anhydride made mainly comprises trifluoromethanesulfonic acid (CF
3sO
3h), trifluoromethanesulfonic acid trifluoro methyl esters (CF
3sO
2oCF
3), tetra-sodium (H
4p
2o
7), fluorion (F
-), sulfate ion (SO
4 2-) etc.The main physical property of trifluoromethanesulfanhydride anhydride and impurity thereof is in Table 1.
The main physical property of table 1 trifluoromethanesulfanhydride anhydride and impurity thereof
As can be seen from Table 1, the boiling point difference of the boiling point of trifluoromethanesulfanhydride anhydride and its impurity is large (>=38 ℃), therefore can adopt the method for distillation to be purified.The distillation of trifluoromethanesulfanhydride anhydride all can be carried out under normal pressure and decompression, but the lower distilling effect of taking to reduce pressure is better, and this is because, on the one hand along with the rising of pressure, polymerization can occur trifluoromethanesulfanhydride anhydride, makes F
-concentration rises, and product yield descends; On the other hand, along with the rising of pressure, the trifluoromethanesulfanhydride anhydride elevation of boiling point, distill required temperature and rise, the trifluoromethanesulfonic acid trifluoro methyl esters (CF that side reaction generates
3sO
3cF
3) showed increased, therefore can reduce the side reaction in still-process by gas clean-up.
The quality index of table 2 trifluoromethanesulfanhydride anhydride
Although the purification process of distillation also can make the purity of trifluoromethanesulfanhydride anhydride reach requirement, but the efficiency of purifying is lower, even need repeatedly to distill and just can reach quality index (in Table 2), in still-process repeatedly, inevitably can cause product loss, introduce new impurity, and reduce productive rate.
In addition, the reaction distillation method also can the purifying trifluoromethanesulfanhydride anhydride.Japanese Patent JP2002088050 report adds a certain amount of Vanadium Pentoxide in FLAKES in the trifluoromethanesulfanhydride anhydride crude product, by reaction distillation, removes trifluoromethanesulfonic acid and the sulfate ion in trifluoromethanesulfanhydride anhydride.Russ P RU2282620 report adds appropriate Vanadium Pentoxide in FLAKES and silicon-dioxide in three fluorosulfonic anhydride, removes respectively trifluoromethanesulfonic acid and fluorion.The reaction distillation method can reduce the content of impurity, but reaction process needs the regular hour, in reaction, also side reaction can occur, and reaction relates to the problem of distillation equally after finishing, and the reagent that need to add has improved the purifying cost.
Summary of the invention
More complicated for existing trifluoromethanesulfanhydride anhydride purification process technique, and the lower defect of the product purity obtained, the object of the present invention is to provide a kind of purification process of trifluoromethanesulfanhydride anhydride, described method is simple to operate, and the purity of product is higher.
Purpose of the present invention is realized by following technical scheme:
A kind of purification process of trifluoromethanesulfanhydride anhydride, described method is as follows:
The trifluoromethanesulfanhydride anhydride crude product is imported in the rectifying still with rectifying tower, distillation system is vacuumized, after vacustat, start to heat rectifying still, total reflux 1～5h, make boiling point lower than the trifluoromethanesulfanhydride anhydride impurity composition in the enrichment of rectifying tower tower top; When the rectifying still temperature is 50～65 ℃, when rectifying tower tower top temperature is 40～60 ℃, the reflux ratio with 10～15 is collected front-end volatiles, and condensation is reclaimed; When the rectifying still temperature is 65～70 ℃, when rectifying tower tower top temperature is 60～68 ℃, with cut in 4～6 reflux ratio collection, and condensation is reclaimed; When the rectifying still temperature rises 2 ℃, temperature is 67～72 ℃, and when rectifying tower tower top temperature is 66～71 ℃, the reflux ratio with 6～8 is collected after cut, and condensation is reclaimed; When the rectifying still temperature is more than or equal to 120 ℃, stop collecting after cut, stop heating, stop vacuumizing, rectifying finishes; Described middle cut is the trifluoromethanesulfanhydride anhydride elaboration;
Described trifluoromethanesulfanhydride anhydride crude product is by trifluoromethanesulfanhydride anhydride, with Vanadium Pentoxide in FLAKES, to react to make, and trifluoromethanesulfanhydride anhydride purity is more than or equal to 90%; Impurity in the trifluoromethanesulfanhydride anhydride crude product mainly comprises trifluoromethanesulfonic acid (CF
3sO
3h), fluorion (F
-) and sulfate ion (SO
4 2-), wherein, trifluoromethanesulfonic acid content≤5%, content of fluoride ion≤1000ppm, sulfate ion content≤300ppm;
Described rectifying still volume is 1～1000L, and the rectifying tower internal diameter is 25～300mm, and stage number is 10～30;
Described rectifying tower is packing tower, and filler used is Stainless Steel Helices, is preferably stainless steel Dixon ring filler;
Described vacuum tightness is-0.01～-0.07MPa, be preferably-0.025～-0.065MPa;
Described rectifying tower is positioned at the rectifying still top, and in whole rectifying, the temperature of rectifying still and rectifying tower all constantly raises, and rectifying tower tower top temperature is all the time lower than the rectifying still temperature.
Beneficial effect
The purification process of trifluoromethanesulfanhydride anhydride of the present invention, by the mode of the vacuum batch distillation trifluoromethanesulfanhydride anhydride of purifying, simple to operate, purification efficiency is high, effectively reduces the content of impurity in product, makes the purity of product reach more than 99.5%.In addition, the front and back cut that rectifying is collected, all can recycle again, greatly improved economic benefit.
The accompanying drawing explanation
Fig. 1 is the device that purification process of the present invention adopts;
Wherein, 1-rectifying still, 2-rectifying tower, 3-return channel, 4-condenser, 5-front-end volatiles receiving tank, 6-middle cut receiving tank, 7-after cut receiving tank.
Embodiment
Below in conjunction with specific embodiment in detail the present invention is described in detail, but is not limited to this.
The rectifier unit that following examples adopt as shown in Figure 1, comprising: rectifying still 1, rectifying tower 2, return channel 3, condenser 4, front-end volatiles receiving tank 5, middle cut receiving tank 6 and after cut receiving tank 7.Wherein, rectifying tower 2 is placed in rectifying still 1 top, and return channel 3 is placed in rectifying tower 2 tops, and rectifying still 1, rectifying tower 2, return channel 3 and condenser 4 are connected successively, and front-end volatiles receiving tank 5, middle cut receiving tank 6 and after cut receiving tank 7 all are connected with condenser 4.
Raw material: the trifluoromethanesulfanhydride anhydride crude product is that trifluoromethanesulfonic acid reacts and obtains with Vanadium Pentoxide in FLAKES, and its main component is in Table 3.
Table 3 trifluoromethanesulfanhydride anhydride crude product component list
Rectifier unit: rectifying still 1 is the 1000ml round-bottomed flask, and glass rectifying tower 2 internal diameters are 25mm, in-built 3mm * 3mm Dixon ring filler, 10 of stage number.
Rectifying: 1200g trifluoromethanesulfanhydride anhydride crude product (it forms in Table 3) is joined in round-bottomed flask, distillation system is vacuumized, make pressure be-0.025MPa, start heating, and the water coolant of opening return channel 3 starts total reflux, the total reflux time is 1h, make boiling point lower than the trifluoromethanesulfanhydride anhydride impurity composition in rectifying tower 2 tower top enrichments.Then, when rectifying still 1 temperature is 65 ℃, rectifying tower 2 tower top temperatures are 60 ℃, collect front-end volatiles with reflux ratio 15, and are recovered in front-end volatiles receiving tank 5 by the phlegma in condenser 4; When rectifying still 1 temperature arrives 70 ℃, rectifying tower 2 tower top temperatures arrive 68 ℃, and the reflux ratio 4 of take is collected the cut of rectifying still 1 temperature in 70～72 ℃, in cut, and be recovered in middle cut receiving tank 6 by phlegma; When rectifying still 1 temperature reaches 72 ℃, rectifying tower 2 tower top temperatures reach 71 ℃, collect after cut with reflux ratio 6, and are recovered in after cut receiving tank 7 by phlegma; When rectifying still 1 temperature reaches 120 ℃, stop collecting after cut, stop heating, stop vacuumizing, rectifying finishes.Finally obtain, front-end volatiles 183.5g, account for 15.3% of described crude product quality; Middle cut 882g, account for 73.5% of described crude product quality; After cut 108g, account for 9% of described crude product quality; Rectifying still 1 raffinate 19.3g.
Wherein, described phlegma is refrigerant, and temperature is-20～-25 ℃.
The centering cut carries out analyzing and testing, and method is: utilize fluorine spectrum nucleus magnetic resonance (
19f NMR) detect (CF
3sO
2)
2o and CF
3sO
3the content of H; Utilize Fluoride ion selective electrode method to measure F
-content; Utilize bariumchloride titration Precipitation Determination SO
4 2-content.
After testing, middle cut is the trifluoromethanesulfanhydride anhydride elaboration, and its composition is as shown in table 4:
Fraction compositions table in table 4
Raw material: with embodiment 1
Rectifier unit: rectifying still 1000ml round-bottomed flask, glass rectifying tower 2 internal diameter 25mm, in-built 3mm * 3mm Dixon ring filler, 30 of stage number.
Rectifying: 1200g trifluoromethanesulfanhydride anhydride crude product (it forms in Table 3) is joined in round-bottomed flask, distillation system is vacuumized, make pressure be-0.065MPa, start heating, and the water coolant of opening return channel 3 starts total reflux, the total reflux time is 5h, make boiling point lower than the trifluoromethanesulfanhydride anhydride impurity composition in rectifying tower 2 tower top enrichments.Then, when rectifying still 1 temperature is 50 ℃, rectifying tower 2 tower top temperatures are 40 ℃, collect front-end volatiles with reflux ratio 10, and are recovered in front-end volatiles receiving tank 5 by the phlegma in condenser 4; When rectifying still 1 temperature arrives 65 ℃, rectifying tower 2 tower top temperatures arrive 60 ℃, and the reflux ratio 6 of take is collected the cut of rectifying still 1 temperature in 65～67 ℃, in cut, and be recovered in middle cut receiving tank 6 by phlegma; When rectifying still 1 temperature reaches 67 ℃, rectifying tower 2 tower top temperatures reach 66 ℃, collect after cut with reflux ratio 8, and are recovered in after cut receiving tank 7 by phlegma; When rectifying still 1 temperature reaches 120 ℃, stop collecting after cut, stop heating, stop vacuumizing, rectifying finishes.Finally obtain, front-end volatiles 218.4g, account for 18.2% of described crude product quality; Middle cut 891.6g, account for 74.3% of described crude product quality; After cut 74.4g, account for 6.2% of described crude product quality; Rectifying still 1 raffinate 11.7g.
Wherein, described phlegma is refrigerant, and temperature is-20～-25 ℃.
According to the method in embodiment 1, the middle cut obtained is detected, the result obtained is as shown in table 5
Fraction compositions table in table 5
Raw material: with embodiment 1
Rectifier unit: rectifying still 1000ml round-bottomed flask, glass rectifying tower 2 internal diameter 25mm, in-built 3mm * 3mm Dixon ring filler, 20 of stage number.
Rectifying: 1200g trifluoromethanesulfanhydride anhydride crude product (it forms in Table 3) is joined in round-bottomed flask, distillation system is vacuumized, make pressure be-0.05MPa, start heating, and the water coolant of opening return channel 3 starts total reflux, the total reflux time is 3h, make boiling point lower than the trifluoromethanesulfanhydride anhydride impurity composition in rectifying tower 2 tower top enrichments.Then, when rectifying still 1 temperature is 55 ℃, rectifying tower 2 tower top temperatures are 50 ℃, collect front-end volatiles with reflux ratio 12, and are recovered in front-end volatiles receiving tank 5 by the phlegma in condenser 4; When rectifying still 1 temperature arrives 68 ℃, rectifying tower 2 tower top temperatures arrive 65 ℃, and the reflux ratio 5 of take is collected the cut of rectifying still 1 temperature in 68～70 ℃, in cut, and be recovered in middle cut receiving tank 6 by phlegma; When rectifying still 1 temperature reaches 70 ℃, rectifying tower 2 tower top temperatures reach 69 ℃, collect after cut with reflux ratio 7, and are recovered in after cut receiving tank 7 by phlegma; When rectifying still 1 temperature reaches 120 ℃, stop collecting after cut, stop heating, stop vacuumizing, rectifying finishes.Finally obtain, front-end volatiles 147.6g, account for 12.3% of described crude product quality; Middle cut 822g, account for 68.5% of described crude product quality; After cut 189.2g, account for 15.7% of described crude product quality; Rectifying still 1 raffinate 23.7g.
Wherein, described phlegma is refrigerant, and temperature is-20～-25 ℃.
According to the method in embodiment 1, the middle cut obtained is detected, the result obtained is as shown in table 6.
Fraction compositions table in table 6
Raw material: the trifluoromethanesulfanhydride anhydride crude product is that trifluoromethanesulfonic acid reacts and obtains with Vanadium Pentoxide in FLAKES, and its main component is in Table 7.
Table 7 trifluoromethanesulfanhydride anhydride crude product component list
Rectifier unit: rectifying still 1 is 50L stainless steel still, and stainless steel rectifying tower 2 internal diameters are 125mm, in-built 10mm * 10mm Dixon ring filler, 10 of stage number.
Rectifying: 70kg trifluoromethanesulfanhydride anhydride crude product (it forms in Table 7) is joined in round-bottomed flask, distillation system is vacuumized, make pressure be-0.025MPa, start heating, and the water coolant of opening return channel 3 starts total reflux, the total reflux time is 1h, make boiling point lower than the trifluoromethanesulfanhydride anhydride impurity composition in rectifying tower 2 tower top enrichments.Then, when rectifying still 1 temperature is 65 ℃, rectifying tower 2 tower top temperatures are 58 ℃, collect front-end volatiles with reflux ratio 15, and are recovered in front-end volatiles receiving tank 5 by the phlegma in condenser 4; When rectifying still 1 temperature arrives 70 ℃, rectifying tower 2 tower top temperatures arrive 67 ℃, and the reflux ratio 4 of take is collected the cut of rectifying still 1 temperature in 70～72 ℃, in cut, and be recovered in middle cut receiving tank 6 by phlegma; When rectifying still 1 temperature reaches 72 ℃, rectifying tower 2 tower top temperatures reach 71 ℃, collect after cut with reflux ratio 6, and are recovered in after cut receiving tank 7 by phlegma; When rectifying still 1 temperature reaches 120 ℃, stop collecting after cut, stop heating, stop vacuumizing, rectifying finishes.Finally obtain, front-end volatiles 7.5kg, account for 10.7% of described crude product quality; Middle cut 50.6kg, account for 72.3% of described crude product quality; After cut 10.1kg, account for 14.4% of described crude product quality.
Wherein, described phlegma is refrigerant, and temperature is-22 ℃.
According to the method in embodiment 1, the middle cut obtained is detected, the result obtained is as shown in table 8.
Fraction compositions table in table 8
Embodiment 5
Raw material: with embodiment 4
Rectifier unit: rectifying still 1 is 50L stainless steel still, and stainless steel rectifying tower 2 internal diameters are 125mm, in-built 10mm * 10mm Dixon ring filler, and stage number is 30.
Rectifying: 70kg trifluoromethanesulfanhydride anhydride crude product (it forms in Table 7) is joined in round-bottomed flask, distillation system is vacuumized, make pressure be-0.065MPa, start heating, and the water coolant of opening return channel 3 starts total reflux, the total reflux time is 5h, make boiling point lower than the trifluoromethanesulfanhydride anhydride impurity composition in rectifying tower 2 tower top enrichments.Then, when rectifying still 1 temperature is 60 ℃, rectifying tower 2 tower top temperatures are 55 ℃, collect front-end volatiles with reflux ratio 10, and are recovered in front-end volatiles receiving tank 5 by the phlegma in condenser 4; When rectifying still 1 temperature arrives 65 ℃, rectifying tower 2 tower top temperatures arrive 60 ℃, and the reflux ratio 5 of take is collected the cut of rectifying still 1 temperature in 65～67 ℃, in cut, and be recovered in middle cut receiving tank 6 by phlegma; When rectifying still 1 temperature reaches 67 ℃, rectifying tower 2 tower top temperatures reach 66 ℃, collect after cut with reflux ratio 8, and are recovered in after cut receiving tank 7 by phlegma; When rectifying still 1 temperature reaches 120 ℃, stop collecting after cut, stop heating, stop vacuumizing, rectifying finishes.Finally obtain, front-end volatiles 12.7kg, account for 18.1% of described crude product quality; Middle cut 47.9kg, account for 68.4% of described crude product quality; After cut 8.3kg, account for 11.9% of described crude product quality.
Wherein, described phlegma is refrigerant, and temperature is-23 ℃.
According to the method in embodiment 1, the middle cut obtained is detected, the result obtained is as shown in table 9.
Fraction compositions table in table 9
Embodiment 6
Raw material: with embodiment 4
Rectifier unit: rectifying still 1 is 50L stainless steel still, and stainless steel rectifying tower 2 internal diameters are 125mm, in-built 10mm * 10mm Dixon ring filler, 20 of stage number.
Rectifying: 70kg trifluoromethanesulfanhydride anhydride crude product (it forms in Table 7) is joined in round-bottomed flask, distillation system is vacuumized, make pressure be-0.04MPa, start heating, and the water coolant of opening return channel 3 starts total reflux, the total reflux time is 2h, make boiling point lower than the trifluoromethanesulfanhydride anhydride impurity composition in rectifying tower 2 tower top enrichments.Then, when rectifying still 1 temperature is 58 ℃, rectifying tower 2 tower top temperatures are 48 ℃, collect front-end volatiles with reflux ratio 13, and are recovered in front-end volatiles receiving tank 5 by the phlegma in condenser 4; When rectifying still 1 temperature arrives 67 ℃, rectifying tower 2 tower top temperatures arrive 65 ℃, and the reflux ratio 4 of take is collected the cut of rectifying still 1 temperature in 67～69 ℃, in cut, and be recovered in middle cut receiving tank 6 by phlegma; When rectifying still 1 temperature reaches 69 ℃, rectifying tower 2 tower top temperatures reach 68 ℃, collect after cut with reflux ratio 7, and are recovered in after cut receiving tank 7 by phlegma; When rectifying still 1 temperature reaches 120 ℃, stop collecting after cut, stop heating, stop vacuumizing, rectifying finishes.Finally obtain, front-end volatiles 11.3kg, account for 16.1% of described crude product quality; Middle cut 50.9kg, account for 72.7% of described crude product quality; After cut 6.2kg, account for 8.9% of described crude product quality; .
Wherein, described phlegma is refrigerant, and temperature is-21 ℃.
According to the method in embodiment 1, the middle cut obtained is detected, the result obtained is as shown in table 10.
Fraction compositions table in table 10
Embodiment 7
Raw material: the trifluoromethanesulfanhydride anhydride crude product is that trifluoromethanesulfonic acid reacts and obtains with Vanadium Pentoxide in FLAKES, and its main component is in Table 11.
Table 11 trifluoromethanesulfanhydride anhydride crude product component list
Rectifier unit: rectifying still 1 is 1000L stainless steel still, and stainless steel rectifying tower 2 internal diameters are 300mm, in-built 25mm * 25mm Dixon ring filler, 20 of stage number.
Rectifying: 1200kg trifluoromethanesulfanhydride anhydride crude product (it forms in Table 11) is joined in round-bottomed flask, distillation system is vacuumized, make pressure be-0.05MPa, start heating, and the water coolant of opening return channel 3 starts total reflux, the total reflux time is 3h, make boiling point lower than the trifluoromethanesulfanhydride anhydride impurity composition in rectifying tower 2 tower top enrichments.Then, when rectifying still 1 temperature is 55 ℃, rectifying tower 2 tower top temperatures are 50 ℃, collect front-end volatiles with reflux ratio 14, and are recovered in front-end volatiles receiving tank 5 by the phlegma in condenser 4; When rectifying still 1 temperature arrives 68 ℃, rectifying tower 2 tower top temperatures arrive 65 ℃, and the reflux ratio 4 of take is collected the cut of rectifying still 1 temperature in 68～70 ℃, in cut, and be recovered in middle cut receiving tank 6 by phlegma; When rectifying still 1 temperature reaches 70 ℃, rectifying tower 2 tower top temperatures reach 69 ℃, collect after cut with reflux ratio 7, and are recovered in after cut receiving tank 7 by phlegma; When rectifying still 1 temperature reaches 120 ℃, stop collecting after cut, stop heating, stop vacuumizing, rectifying finishes.Finally obtain, front-end volatiles 182.4kg, account for 15.2% of described crude product quality; Middle cut 845.1kg, account for 70.4% of described crude product quality; After cut 163.6kg, account for 13.6% of described crude product quality.
Wherein, described phlegma is refrigerant, and temperature is-24 ℃.
According to the method in embodiment 1, the middle cut obtained is detected, the result obtained is as shown in table 12.
Fraction compositions table in table 12
The trifluoromethanesulfanhydride anhydride elaboration obtained in above embodiment has all reached the quality index shown in table 2, and purity is higher, has reached more than 99.5%.
The present invention includes but be not limited to above embodiment, every any being equal to of carrying out under the principle of spirit of the present invention, replace or local improvement, all will be considered as within protection scope of the present invention.
Claims (3)
1. the purification process of a trifluoromethanesulfanhydride anhydride, is characterized in that, described method is as follows:
The trifluoromethanesulfanhydride anhydride crude product is imported in the rectifying still with rectifying tower, distillation system is vacuumized, after vacustat, start to heat rectifying still, total reflux 1～5h, make boiling point lower than the trifluoromethanesulfanhydride anhydride impurity composition in the enrichment of rectifying tower tower top; When the rectifying still temperature is 50～65 ℃, when rectifying tower tower top temperature is 40～60 ℃, the reflux ratio with 10～15 is collected front-end volatiles, and condensation is reclaimed; When the rectifying still temperature is 65～70 ℃, when rectifying tower tower top temperature is 60～68 ℃, with cut in 4～6 reflux ratio collection, and condensation is reclaimed; When the rectifying still temperature rises 2 ℃, when rectifying tower tower top temperature is 66～71 ℃, the reflux ratio with 6～8 is collected after cut, and condensation is reclaimed; When the rectifying still temperature is more than or equal to 120 ℃, stop collecting after cut, stop heating, stop vacuumizing, rectifying finishes; Described middle cut is the trifluoromethanesulfanhydride anhydride elaboration;
Described trifluoromethanesulfanhydride anhydride crude product is by trifluoromethanesulfanhydride anhydride, with Vanadium Pentoxide in FLAKES, to react to make, and trifluoromethanesulfanhydride anhydride purity is more than or equal to 90%; Impurity in the trifluoromethanesulfanhydride anhydride crude product mainly comprises trifluoromethanesulfonic acid, fluorion and sulfate ion, wherein, and trifluoromethanesulfonic acid content≤5%, content of fluoride ion≤1000ppm, sulfate ion content≤300ppm;
Described rectifying still volume is 1～1000L, and the rectifying tower internal diameter is 25～300mm, and stage number is 10～30;
Described rectifying tower is packing tower, and filler used is Stainless Steel Helices;
Described vacuum tightness is-0.01～-0.07MPa;
Described rectifying tower is positioned at the rectifying still top, and in whole rectifying, the temperature of rectifying still and rectifying tower all constantly raises, and rectifying tower tower top temperature is all the time lower than the rectifying still temperature.
2. the purification process of a kind of trifluoromethanesulfanhydride anhydride according to claim 1, is characterized in that, described filler is stainless steel Dixon ring filler.
3. the purification process of a kind of trifluoromethanesulfanhydride anhydride according to claim 1, is characterized in that, described vacuum tightness is-0.025～-0.065MPa.
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| CN114174258B (en) * | 2019-08-07 | 2024-01-16 | 巴斯夫欧洲公司 | Recovery of anhydrous methanesulfonic acid from distillation column bottoms stream |
| CN114174258A (en) * | 2019-08-07 | 2022-03-11 | 巴斯夫欧洲公司 | Recovery of anhydrous methanesulfonic acid from a distillation column bottom stream |
| CN112321464A (en) * | 2020-08-11 | 2021-02-05 | 中国科学院上海有机化学研究所 | Method for purifying crude product of trifluoromethanesulfonic anhydride or its analogue |
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| CN114470826B (en) * | 2022-02-17 | 2023-03-14 | 中船(邯郸)派瑞特种气体股份有限公司 | Purification device and method of bis (trifluoromethanesulfonyl) imide |
| CN114949897A (en) * | 2022-06-22 | 2022-08-30 | 安徽佳先功能助剂股份有限公司 | Continuous dehydration distillation plant of nylon acid diisobutyl ester |
| CN114949897B (en) * | 2022-06-22 | 2023-06-27 | 安徽佳先功能助剂股份有限公司 | Continuous dehydration distillation device for diisobutyl nylon acid |
| CN115400714A (en) * | 2022-09-21 | 2022-11-29 | 中船(邯郸)派瑞特种气体股份有限公司 | Production device and method of trifluoromethanesulfonic acid |
| CN115400714B (en) * | 2022-09-21 | 2024-07-05 | 中船(邯郸)派瑞特种气体股份有限公司 | Production device and method of trifluoromethanesulfonic acid |
| CN115504912A (en) * | 2022-10-14 | 2022-12-23 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for preparing high-purity trifluoromethanesulfonic anhydride by using batch distillation kettle |
| CN115504912B (en) * | 2022-10-14 | 2023-08-18 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for preparing high-purity trifluoromethanesulfonic anhydride by using batch still |
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