CN108276315A - A kind of purification process of trifluoromethanesulfonic acid - Google Patents
A kind of purification process of trifluoromethanesulfonic acid Download PDFInfo
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- CN108276315A CN108276315A CN201711479006.1A CN201711479006A CN108276315A CN 108276315 A CN108276315 A CN 108276315A CN 201711479006 A CN201711479006 A CN 201711479006A CN 108276315 A CN108276315 A CN 108276315A
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- rectifying column
- light component
- heavy constituent
- trifluoromethanesulfonic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
Abstract
The present invention relates to a kind of purification process of trifluoromethanesulfonic acid, belong to technical field of fine.The method of the invention purifies trifluoromethanesulfonic acid by the way of continuous rectification, easy to operate, efficient, and low energy consumption；Meanwhile condenser is set in the tower top of rectifying column, the light component impurity and product after purification that tower top can be discharged are further purified, in the tower reactor of rectifying column, reboiler is set, a part of material can be made to be utilized as heat source, purifying cost is substantially reduced, improve production capacity；In addition, the technological parameter by regulating and controlling distillation process so that product purity after purification reaches 99.7% or more, H2O content≤400ppm, HF≤9ppm, H2SO4≤ 40ppm is higher than industry quality level.
Description
Technical field
The present invention relates to a kind of purification process of trifluoromethanesulfonic acid, belong to technical field of fine.
Background technology
Trifluoromethanesulfonic acid, molecular formula CF3SO3H, the colourless transparent liquid with intense irritation smell are shown when impure
Yellow or yellowish-brown, in air smoke are a kind of organic super acids, are omnipotent synthetics, are widely used in medicine, chemical industry
Etc. industries.
The classical way for preparing trifluoromethanesulfonic acid is mainly chemical synthesis and electrochemical fluorination.Chemical synthesis be with
Bis trifluoromethyl disulphide is raw material, and trifluoromethanesulfonic acid is synthesized through trimethyl fluoride sulfonyl chlorine route.Electrochemical fluorination is also referred to as
For electrofluorination method, foremost is Simons electrofluorination techniques, it makees raw material with methylsufonyl chloride or methanesulfonyl fluoride,
Fluorinated electrolyte is carried out in anhydrous hydrogen fluoride, obtains the trifluoro Fumette of high yield, later by trifluoro Fumette gas in M
(OH)m(M is alkali or alkaline earth metal, and m is 1 or 2) Transfer in Aqueous Solution becomes fluoroform sulphonate, then sour with dense sulfuric acid treatment
Change can be obtained trifluoromethanesulfonic acid.Electrofluorination method is industrially mostly used at present prepares trifluoromethanesulfonic acid, but prepared trifluoro
Contain H in methylsulphur acid crude2O, HF and H2SO4The specific nature comparison such as table 1 of equal impurity, trifluoromethanesulfonic acid and the impurity.
Table 1
| Molecular formula | Molecular weight (g/mol) | Density (g/cm3) | Fusing point/DEG C | Boiling point/DEG C | No. CAS |
| CF3SO3H | 150.08 | 1.696 | -40 | 168~170 | 1493-13-6 |
| H2O | 18 | 1.00 | 0 | 100 | 7732-18-5 |
| HF | 20.01 | 1.15 | -83.7 | 19.5 | 7664-39-3 |
| H2SO4 | 98.08 | 1.84 | 10.35 | 338 | 7664-93-9 |
As known from Table 1, there were significant differences for the boiling point of trifluoromethanesulfonic acid and its impurity, therefore, it may be considered that using distillation
Method is purified, and qualified trifluoromethanesulfonic acid product is obtained, and the quality index of trifluoromethanesulfonic acid refers to table 2.Trifluoromethanesulfonic acid
Distillation can all be carried out under normal pressure and decompression, but the lower distilling effect of decompression is taken more preferably, this is because with the liter of pressure
Height, the trifluoromethanesulfonic acid elevation of boiling point distill required temperature rise, and side reaction impurity composition showed increased, system is complicated, so
Pressure can namely be reduced by raising vacuum degree to reduce the side reaction in distillation process.In addition, being added in distillation process
The additives such as the concentrated sulfuric acid and silica can distillate rate and return time to improve purification effect, but in reality by control
Technological parameter is strictly controlled in the purifying of border, can just obtain qualified products.
Table 2
Chinese patent CN101402591A is disclosed purifies trifluoromethanesulfonic acid using the method being repeatedly evaporated under reduced pressure, although should
Purification process can also make the purity of trifluoromethanesulfonic acid reach requirement, but the purification process has energy consumption high, the production cycle
Long disadvantage, and in repeatedly turning material distillation process, inevitably product is caused to lose, introduce new impurity, it reduces
Yield.
Invention content
The lower defect of product purity more complex for existing trifluoromethanesulfonic acid purification process technique, and obtaining, this
Invention is designed to provide a kind of purification process of trifluoromethanesulfonic acid, and the method is easy to operate, and the purity of product is higher, at
This is low.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of purification process of trifluoromethanesulfonic acid, the purification process are by de- light component rectifying column and de- heavy constituent essence
Continuous rectification purifying of the tower realization to trifluoromethanesulfonic acid is evaporated, is taken off at the discharge port of light component rectifying column tower top and the exhaust gas of outside
Device connection is managed, the light component impurity of removing is handled, takes off the discharge port and de- heavy constituent essence of light component tower bottom of rectifying tower
The feed inlet connection of tower is evaporated, the discharge port of de- heavy constituent rectifying column tower top is connect with external storage device, for collecting purifying
The discharge port of trifluoromethanesulfonic acid afterwards, de- heavy constituent tower bottom of rectifying tower is connect with external liquid waste treating apparatus, de- for handling
The heavy constituent removed；
Purifying is as follows：
(1) removing light component impurity H2O and HF
Trifluoromethanesulfonic acid crude product is imported from the feed inlet of de- light component rectifying column and is taken off in light component rectifying column, is controlled de- light
The pressure of component tower bottom of rectifying tower is -0.010MPa~-0.099MPa, and the temperature of tower reactor is 40 DEG C~160 DEG C, the temperature of tower top
It it is 20 DEG C~140 DEG C, reflux ratio is 10~200, and the inlet amount of trifluoromethanesulfonic acid crude product is 2m3/ h~200m3/ h, then light component
Impurity H2O, HF and fixed gas are discharged from tower top, remove the trifluoromethanesulfonic acid crude product after light component and stay in tower reactor；
(2) removing heavy constituent impurity H2SO4
Trifluoromethanesulfonic acid crude product after removing light component is recombinated by taking off the discharge port of light component tower bottom of rectifying tower and taking off
The feed inlet of point rectifying column, which imports, to be taken off in heavy constituent rectifying column, control take off the pressure -0.010MPa of heavy constituent tower bottom of rectifying tower~-
The temperature of 0.099MPa, tower reactor are 40 DEG C~180 DEG C, and 20 DEG C~140 DEG C of the temperature of tower top, reflux ratio is 10~100, removing weight
From overhead collection, heavy constituent impurity stays in tower reactor high-purity trifluoromethanesulfonic acid after component.
In step (1) and step (2), 10 DEG C higher than the temperature of tower top of temperature of tower reactor or more.
Further, it takes off in light component rectifying column, the pressure of tower reactor is -0.080MPa~-0.099MPa, the temperature of tower reactor
It it is 120 DEG C~160 DEG C, the temperature of tower top is 80 DEG C~100 DEG C, and reflux ratio is 20~100, the inlet amount of trifluoromethanesulfonic acid crude product
For 100m3/ h~200m3/h；In de- heavy constituent rectifying column, the pressure of tower reactor is -0.080MPa~-0.099MPa, the temperature of tower reactor
Degree is 140 DEG C~180 DEG C, and the temperature of tower top is 120 DEG C~140 DEG C, and reflux ratio is 10~50.
De- light component rectifying column and de- heavy constituent rectifying column are packed tower, and inside is equipped with nickel, stainless steel or Monel one
Kind or more filler；The diameter of de- light component rectifying column and de- heavy constituent rectifying column is each independently 20mm~250mm, and height is respectively
Stand alone as 2m~10m.
The top of de- light component rectifying column can be arranged condenser I, in step (1), from de- light component rectifying column tower top
After the light component that discharge port comes out enters condenser I, a part flowed back into inside de- light component rectifying column from condenser I continue into
Row removing light component purifying, another part enter emission-control equipment；Meanwhile the lower section of de- light component rectifying column can also be arranged
Reboiler I, from the trifluoromethanesulfonic acid crude product part after the removing light component that the discharge port of de- light component tower bottom of rectifying tower comes out
Reboiler I is flowed into, continues to remove light component purifying, another part into light component rectifying column is taken off by being heated as gas
It imports de- heavy constituent rectifying column and carries out removing heavy constituent purifying.
The top of de- heavy constituent rectifying column can be arranged condenser II, in step (2), from de- heavy constituent rectifying column tower top
After trifluoromethanesulfonic acid after the removing heavy constituent that discharge port comes out enters condenser II, a part flows back into de- weight from condenser II
Continue to remove heavy constituent purifying inside component rectifying column, another part is into storage device；Meanwhile de- heavy constituent rectifying column
Reboiler II can also be arranged in lower section, and the heavy constituent part inflow come out from the discharge port of de- heavy constituent tower bottom of rectifying tower is boiled again
Device II continues to remove heavy constituent purifying by being heated as gas into heavy constituent rectifying column is taken off, and another part, which enters, to give up
Liquid processing device.
Advantageous effect：
(1) compared with conventional multiple distillation purifying method, the method for the invention is by the way of continuous rectification to three
Fluorine methanesulfonic acid is purified, easy to operate, and purification efficiency is high, and low energy consumption, reduces production cost so that the purity of product reaches
99.7% or more, impurity H2O content≤400ppm, HF≤9ppm, H2SO4≤ 40ppm is higher than industry quality level.
(2) in purification process of the present invention, by the way that condenser is arranged in rectifying column tower top, tower top can be discharged light
Composition impurity and product after purification are further purified；By the way that reboiler is arranged in tower bottom of rectifying tower, a part of material can be made
It is utilized as heat source, substantially reduces purifying cost, improve production capacity.
Description of the drawings
Fig. 1 is continuous rectification apparatus structural schematic diagram used by being purified in embodiment.
Wherein, 1- takes off light component rectifying column, 2- condensers I, 3- reboilers I, the de- heavy constituent rectifying columns of 4-, 5- condensers
II, 6- reboiler II.
Specific implementation mode
The present invention is further elaborated with reference to the accompanying drawings and detailed description, wherein the method is as without especially
Explanation is conventional method, and the raw material can obtain unless otherwise instructed from open commercial sources.
Rectifier unit employed in following example 1~4 includes de- light component rectifying column 1, condenser I 2, reboiler I
3, heavy constituent rectifying column 4, condenser II 5 and reboiler II 6 are taken off；Peripheral equipment include emission-control equipment, storage device with
And liquid waste treating apparatus；
The discharge port of de- 1 tower top of light component rectifying column is connect with the feed inlet of condenser I 2, the discharge port point of condenser I 2
Do not connect with de- light component rectifying column 1 and emission-control equipment, the discharge port of de- 1 tower reactor of light component rectifying column respectively with boil again
The feed inlet of the feed inlet of device I 3 and de- heavy constituent rectifying column 4 connects, the discharge port of reboiler I 3 and de- light component rectifying column 1
Connection；The discharge port of de- 4 tower top of heavy constituent rectifying column is connect with the feed inlet of condenser II 5, the discharge port difference of condenser II 5
Connect with de- heavy constituent rectifying column 4 and storage device, take off the discharge port of 4 tower reactor of heavy constituent rectifying column respectively with reboiler II 6
Feed inlet and liquid waste treating apparatus connection, the discharge port of reboiler II 6 connect with de- heavy constituent rectifying column 4；
Trifluoromethanesulfonic acid crude product is imported from the feed inlet of de- light component rectifying column 1 and is taken off in light component rectifying column 1, control is de-
The pressure of 1 tower reactor of light component rectifying column is -0.010MPa~-0.099MPa, and the temperature of tower reactor is 40 DEG C~160 DEG C, tower top
Temperature is 20 DEG C~140 DEG C, and reflux ratio is 10~200, and the inlet amount of trifluoromethanesulfonic acid crude product is 2m3/ h~200m3/ h, then gently
Composition impurity H2O, HF and fixed gas enter condenser I 2 after being come out from tower top discharge port, and a part flows back into de- from condenser I 2
Continue to remove light component purifying inside light component rectifying column 1, another part enters emission-control equipment, after removing light component
Trifluoromethanesulfonic acid crude product stay in de- 1 tower reactor of light component rectifying column；It is come out from the discharge port of de- 1 tower reactor of light component rectifying column
Trifluoromethanesulfonic acid crude product after removing light component, a part flow into reboiler I 3, smart into light component is taken off by being heated as gas
It evaporates tower 1 to continue to remove light component purifying, another part imports de- heavy constituent rectifying column 4 and carries out removing heavy constituent purifying；
When de- heavy constituent rectifying column 4 carries out removing heavy constituent purifying, control take off the pressure -0.010MPa of 4 tower reactor of heavy constituent rectifying column~-
The temperature of 0.099MPa, tower reactor are 40 DEG C~180 DEG C, and 20 DEG C~140 DEG C of the temperature of tower top, reflux ratio is 10~100, from tower top
It is a part of from condenser II 5 times after high-purity trifluoromethanesulfonic acid after the removing heavy constituent of discharge port discharge enters condenser II 5
It flows to inside de- heavy constituent rectifying column 4 and continues to remove heavy constituent purifying, another part is into storage device, the heavy constituent of removing
Impurity stays in de- 4 tower reactor of heavy constituent rectifying column；The heavy constituent impurity flowed out from the discharge port of de- 4 tower reactor of heavy constituent rectifying column,
A part flows into reboiler II 6, through being heated as gas enter take off heavy constituent rectifying column 4 continue to remove heavy constituent it is pure
Change, another part enters liquid waste treating apparatus；Wherein, the trifluoromethanesulfonic acid collected in storage device is high-purity after purification
Trifluoromethanesulfonic acid.
In the product collected in storage device, the content of trifluoromethanesulfonic acid is detected using chemical titration；H2O's contains
Amount is measured using karl Fischer moisture teller；Containing F-The content of impurity is measured using Fluoride ion selective electrode method；Containing SO4 2-It is miscellaneous
The content of matter titrates Precipitation Determination using barium chloride.
Embodiment 1
The constituent and its content of trifluoromethanesulfonic acid crude product：CF3SO3The mass fraction of H is 98%, H2O content is
1000ppm, HF content are 1000ppm and H2SO4Content is 18000ppm；De- light component rectifying column 1 and de- heavy constituent rectifying column
4 diameter is 150mm, is highly 6m, inside be respectively arranged with stainless steel helices, it is scattered heap that filler, which loads form,；
The step of being purified to the trifluoromethanesulfonic acid crude product is as follows：
(1) removing light component impurity H2O and HF
Trifluoromethanesulfonic acid crude product is imported and is taken off in light component rectifying column 1, the pressure for taking off 1 tower reactor of light component rectifying column is controlled
For -0.099MPa, the temperature of tower reactor is 120 DEG C, and the temperature of tower top is 90 DEG C, reflux ratio 25, trifluoromethanesulfonic acid crude product into
Doses is 100m3/ h contains a large amount of light component impurity H2O, the gas of HF and fixed gas enters condenser after the discharge of tower top discharge port
I 2, the Partial Liquid Phase formed by condenser I 2, which flows back into inside de- light component rectifying column 1, continues to remove light component purifying,
Another part gas phase enters emission-control equipment, and top gaseous phase light component impurity discharge rate is 75kg/h；After removing light component
Trifluoromethanesulfonic acid crude product stays in tower reactor；
(2) removing heavy constituent impurity H2SO4
The trifluoromethanesulfonic acid crude product after removing light component in de- 1 tower reactor of light component rectifying column, a part flow into reboiler I
3, enter to take off by being heated as gas and continue to remove light component purifying inside light component rectifying column 1, another part imports
In de- heavy constituent rectifying column 4；Control takes off the pressure -0.099MPa of 4 tower reactor of heavy constituent rectifying column, and the temperature of tower reactor is 150 DEG C, tower
130 DEG C of the temperature on top, reflux ratio 20 remove after the trifluoromethanesulfonic acid after heavy constituent comes out from the discharge port of tower top and enter condensation
Device II 5, by condenser II 5 formed a part of liquid-phase reflux to de- heavy constituent rectifying column 4 in continue removing heavy constituent
Purifying, another part gas phase are then collected into storage device；The heavy constituent impurity H of removing2SO4Stay in de- heavy constituent rectifying column 4
Tower reactor, a part flow into reboiler II 6, continue removing recombination into heavy constituent rectifying column 4 is taken off by being heated as gas
Purifying, another part is divided to enter liquid waste treating apparatus.
The trifluoromethanesulfonic acid collected in storage device is high-purity trifluoromethanesulfonic acid after purification, then in storage device
Product carry out composition detection, testing result refers to table 1.
Table 1
Embodiment 2
The constituent and its content of trifluoromethanesulfonic acid crude product：CF3SO3The mass fraction of H is 93%, H2O content is
10000ppm, HF content are 7000ppm and H2SO4Content is 50000ppm；De- light component rectifying column 1 and de- heavy constituent rectifying
The diameter of tower 4 is 150mm, is highly 8m, inside be respectively arranged with nickel Pall ring filler, it is scattered heap that filler, which loads form,；
The step of being purified to the trifluoromethanesulfonic acid crude product is as follows：
(1) removing light component impurity H2O and HF
Trifluoromethanesulfonic acid crude product is imported and is taken off in light component rectifying column 1, the pressure for taking off 1 tower reactor of light component rectifying column is controlled
For -0.095MPa, the temperature of tower reactor is 130 DEG C, and the temperature of tower top is 100 DEG C, reflux ratio 20, trifluoromethanesulfonic acid crude product into
Doses is 150m3/ h contains a large amount of light component impurity H2O, the gas of HF and fixed gas enters condenser after the discharge of tower top discharge port
I 2, the Partial Liquid Phase formed by condenser I 2, which flows back into inside de- light component rectifying column 1, continues to remove light component purifying,
Another part gas phase enters emission-control equipment, and top gaseous phase light component impurity discharge rate is 100kg/h；After removing light component
Trifluoromethanesulfonic acid crude product stays in tower reactor；
(2) removing heavy constituent impurity H2SO4
The trifluoromethanesulfonic acid crude product after removing light component in de- 1 tower reactor of light component rectifying column, a part flow into reboiler I
3, enter to take off by being heated as gas and continue to remove light component purifying inside light component rectifying column 1, another part imports
In de- heavy constituent rectifying column 4；Control takes off the pressure -0.095MPa of 4 tower reactor of heavy constituent rectifying column, and the temperature of tower reactor is 160 DEG C, tower
140 DEG C of the temperature on top, reflux ratio 15 remove after the trifluoromethanesulfonic acid after heavy constituent comes out from the discharge port of tower top and enter condensation
Device II 5, by condenser II 5 formed a part of liquid-phase reflux to de- heavy constituent rectifying column 4 in continue removing heavy constituent
Purifying, another part gas phase are then collected into storage device；The heavy constituent impurity H of removing2SO4Stay in de- heavy constituent rectifying column 4
Tower reactor, a part flow into reboiler II 6, continue removing recombination into heavy constituent rectifying column 4 is taken off by being heated as gas
Purifying, another part is divided to enter liquid waste treating apparatus.
The trifluoromethanesulfonic acid collected in storage device is high-purity trifluoromethanesulfonic acid after purification, then in storage device
Product carry out composition detection, testing result refers to table 2.
Table 2
Embodiment 3
The constituent and its content of trifluoromethanesulfonic acid crude product：CF3SO3The mass fraction of H is 96%, H2O content is
8000ppm, HF content are 1000ppm and H2SO4Content is 30000ppm；De- light component rectifying column 1 and de- heavy constituent rectifying column
4 diameter is 200mm, is highly 8m, inside be respectively arranged with Monel filler, it is scattered heap that filler, which loads form,；
The step of being purified to the trifluoromethanesulfonic acid crude product is as follows：
(1) removing light component impurity H2O and HF
Trifluoromethanesulfonic acid crude product is imported and is taken off in light component rectifying column 1, the pressure for taking off 1 tower reactor of light component rectifying column is controlled
For -0.075MPa, the temperature of tower reactor is 100 DEG C, and the temperature of tower top is 80 DEG C, reflux ratio 100, trifluoromethanesulfonic acid crude product into
Doses is 150m3/ h contains a large amount of light component impurity H2O, the gas of HF and fixed gas enters condenser after the discharge of tower top discharge port
I 2, the Partial Liquid Phase formed by condenser I 2, which flows back into inside de- light component rectifying column 1, continues to remove light component purifying,
Another part gas phase enters emission-control equipment, and top gaseous phase light component impurity discharge rate is 3kg/h；Remove three after light component
Fluorine methylsulphur acid crude stays in tower reactor；
(2) removing heavy constituent impurity H2SO4
The trifluoromethanesulfonic acid crude product after removing light component in de- 1 tower reactor of light component rectifying column, a part flow into reboiler I
3, enter to take off by being heated as gas and continue to remove light component purifying inside light component rectifying column 1, another part imports
In de- heavy constituent rectifying column 4；Control takes off the pressure -0.075MPa of 4 tower reactor of heavy constituent rectifying column, and the temperature of tower reactor is 120 DEG C, tower
100 DEG C of the temperature on top, reflux ratio 70 remove after the trifluoromethanesulfonic acid after heavy constituent comes out from the discharge port of tower top and enter condensation
Device II 5, by condenser II 5 formed a part of liquid-phase reflux to de- heavy constituent rectifying column 4 in continue removing heavy constituent
Purifying, another part gas phase are then collected into storage device；The heavy constituent impurity H of removing2SO4Stay in de- heavy constituent rectifying column 4
Tower reactor, a part flow into reboiler II 6, continue removing recombination into heavy constituent rectifying column 4 is taken off by being heated as gas
Purifying, another part is divided to enter liquid waste treating apparatus.
The trifluoromethanesulfonic acid collected in storage device is high-purity trifluoromethanesulfonic acid after purification, then in storage device
Product carry out composition detection, testing result refers to table 3.
Table 3
Embodiment 4
The constituent and its content of trifluoromethanesulfonic acid crude product：CF3SO3The mass fraction of H is 97%, H2O content is
8000ppm, HF content are 1000ppm and H2SO4Content is 20000ppm；De- light component rectifying column 1 and de- heavy constituent rectifying column
4 diameter is 100mm, is highly 5m, inside be respectively arranged with nickel and stainless steel mixed fillers, it is scattered that filler, which loads form,
Heap；
The step of being purified to the trifluoromethanesulfonic acid crude product is as follows：
(1) removing light component impurity H2O and HF
Trifluoromethanesulfonic acid crude product is imported and is taken off in light component rectifying column 1, the pressure for taking off 1 tower reactor of light component rectifying column is controlled
Temperature for -0.05MPa, tower reactor is 70 DEG C, and the temperature of tower top is 50 DEG C, reflux ratio 50, the charging of trifluoromethanesulfonic acid crude product
Amount is 80m3/ h contains a large amount of light component impurity H2O, the gas of HF and fixed gas enters condenser I 2 after the discharge of tower top discharge port,
The Partial Liquid Phase formed by condenser I 2, which flows back into inside de- light component rectifying column 1, continues to remove light component purifying, separately
A part of gas phase enters emission-control equipment, and top gaseous phase light component impurity discharge rate is 2kg/h；Remove the trifluoro after light component
Methylsulphur acid crude stays in tower reactor；
(2) removing heavy constituent impurity H2SO4
The trifluoromethanesulfonic acid crude product after removing light component in de- 1 tower reactor of light component rectifying column, a part flow into reboiler I
3, enter to take off by being heated as gas and continue to remove light component purifying inside light component rectifying column 1, another part imports
In de- heavy constituent rectifying column 4；Control takes off the pressure -0.05MPa of 4 tower reactor of heavy constituent rectifying column, and the temperature of tower reactor is 90 DEG C, tower top
Temperature 70 C, reflux ratio 50, remove heavy constituent after trifluoromethanesulfonic acid from the discharge port of tower top come out after enter condenser
II 5, by condenser II 5 formed a part of liquid-phase reflux to de- heavy constituent rectifying column 4 in continue removing heavy constituent it is pure
Change, another part gas phase is then collected into storage device；The heavy constituent impurity H of removing2SO4Stay in de- 4 tower of heavy constituent rectifying column
Kettle, a part flow into reboiler II 6, continue to remove heavy constituent into heavy constituent rectifying column 4 is taken off by being heated as gas
Purifying, another part enter liquid waste treating apparatus.
The trifluoromethanesulfonic acid collected in storage device is high-purity trifluoromethanesulfonic acid after purification, then in storage device
Product carry out composition detection, testing result refers to table 4.
Table 4
In conclusion the above is merely preferred embodiments of the present invention, being not intended to limit the scope of the present invention.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (9)
1. a kind of purification process of trifluoromethanesulfonic acid, it is characterised in that：The rectifier unit that the purification process uses includes de- light
Component rectifying column (1) and de- heavy constituent rectifying column (4) take off at the discharge port of light component rectifying column (1) tower top and the exhaust gas of outside
Device connection is managed, the discharge port of de- light component rectifying column (1) tower reactor is connect with the feed inlet of de- heavy constituent rectifying column (4), takes off weight
The discharge port of component rectifying column (4) tower top connect with external storage device, take off heavy constituent rectifying column (4) tower reactor discharge port and
External liquid waste treating apparatus connection；
Purifying is as follows：
Trifluoromethanesulfonic acid crude product is imported from the feed inlet of de- light component rectifying column (1) and is taken off in light component rectifying column (1), light component
Impurity enters emission-control equipment after being come out from de- light component rectifying column (1) tower top, and the trifluoromethanesulfonic acid removed after light component is thick
Product stay in de- light component rectifying column (1) tower reactor；
Trifluoromethanesulfonic acid crude product after removing light component is imported and is taken off in heavy constituent rectifying column (4), the trifluoro after heavy constituent is removed
Methanesulfonic acid enters storage device after being come out from de- heavy constituent rectifying column (4) tower top, and heavy constituent impurity stays in de- heavy constituent rectifying column
(4) in tower reactor；
Wherein, the technological parameter in light component rectifying column (1) is taken off：The pressure of tower reactor is -0.010MPa~-0.099MPa, tower reactor
Temperature be 40 DEG C~160 DEG C, the temperature of tower top is 20 DEG C~140 DEG C, and reflux ratio is 10~200, trifluoromethanesulfonic acid crude product
Inlet amount is 2m3/ h~200m3/ h, and 10 DEG C higher than the temperature of tower top of temperature of tower reactor or more；
Technological parameter in de- heavy constituent rectifying column (4)：Pressure -0.010MPa~-0.099MPa of tower reactor, the temperature of tower reactor are
40 DEG C~180 DEG C, 20 DEG C~140 DEG C of the temperature of tower top, reflux ratio is 10~100, and the temperature of tower reactor is higher than the temperature of tower top
10 DEG C or more.
2. a kind of purification process of trifluoromethanesulfonic acid according to claim 1, it is characterised in that：De- light component rectifying column
(1) technological parameter in：The pressure of tower reactor is -0.080MPa~-0.099MPa, and the temperature of tower reactor is 120 DEG C~160 DEG C, tower
The temperature on top is 80 DEG C~100 DEG C, and reflux ratio is 20~100, and the inlet amount of trifluoromethanesulfonic acid crude product is 100m3/ h~200m3/
h。
3. a kind of purification process of trifluoromethanesulfonic acid according to claim 1, it is characterised in that：De- heavy constituent rectifying column
(4) technological parameter in：The pressure of tower reactor is -0.080MPa~-0.099MPa, and the temperature of tower reactor is 140 DEG C~180 DEG C, tower
The temperature on top is 120 DEG C~140 DEG C, and reflux ratio is 10~50.
4. a kind of purification process of trifluoromethanesulfonic acid according to claim 1, it is characterised in that：De- light component rectifying column
(1) and the inside of de- heavy constituent rectifying column (4) is respectively provided with nickel, stainless steel or Monel more than one fillers.
5. a kind of purification process of trifluoromethanesulfonic acid according to claim 1, it is characterised in that：De- light component rectifying column
(1) and the diameter of de- heavy constituent rectifying column (4) is each independently 20mm~250mm, is highly each independently 2m~10m.
6. a kind of purification process of trifluoromethanesulfonic acid according to claim 1, it is characterised in that：De- light component rectifying column
(1) feed inlet of top setting condenser I (2), the discharge port and condenser I (2) that take off light component rectifying column (1) tower top connects
It connects, the discharge port of condenser I (2) is connect with the emission-control equipment of de- light component rectifying column (1) and outside respectively.
7. a kind of purification process of trifluoromethanesulfonic acid according to claim 1, it is characterised in that：De- light component rectifying column
(1) lower section setting reboiler I (3) takes off the discharge port feed inlet with reboiler I (3) respectively of light component rectifying column (1) tower reactor
And the feed inlet connection of de- heavy constituent rectifying column (4), the discharge port of reboiler I (3) are connect with de- light component rectifying column (1).
8. a kind of purification process of trifluoromethanesulfonic acid according to claim 1, it is characterised in that：De- heavy constituent rectifying column
(4) feed inlet of top setting condenser II (5), the discharge port and condenser II (5) that take off heavy constituent rectifying column (4) tower top connects
It connects, the discharge port of condenser II (5) is connect with the storage device of de- heavy constituent rectifying column (4) and outside respectively.
9. a kind of purification process of trifluoromethanesulfonic acid according to claim 1, it is characterised in that：De- heavy constituent rectifying column
(4) lower section setting reboiler II (6), takes off the discharge port charging with reboiler II (6) respectively of heavy constituent rectifying column (4) tower reactor
Mouth and the connection of the liquid waste treating apparatus of outside, the discharge port of reboiler II (6) are connect with de- heavy constituent rectifying column (4).
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| CN113845446A (en) * | 2021-10-26 | 2021-12-28 | 中船重工（邯郸）派瑞特种气体有限公司 | Preparation method of trifluoromethanesulfonic acid |
| CN114470866A (en) * | 2022-01-26 | 2022-05-13 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for purifying hydrogen fluoride in trifluoromethanesulfonyl fluoride |
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| 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 |
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