CN104262376A - TMSOTf (trimethylsilyl trifluoromethanesulfonate) purifying method - Google Patents

TMSOTf (trimethylsilyl trifluoromethanesulfonate) purifying method Download PDF

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CN104262376A
CN104262376A CN201410546511.3A CN201410546511A CN104262376A CN 104262376 A CN104262376 A CN 104262376A CN 201410546511 A CN201410546511 A CN 201410546511A CN 104262376 A CN104262376 A CN 104262376A
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tower
trimethylsilyl trifluoromethanesulfonate
hcl
rectifying tower
temperature
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彭立培
黄华璠
杨献奎
孟祥军
郭绪涛
商洪涛
吕灵华
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718th Research Institute of CSIC
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718th Research Institute of CSIC
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Abstract

The invention relates to a TMSOTf (trimethylsilyl trifluoromethanesulfonate) purifying method and belongs to the technical field of fine chemical engineering. The method comprises steps as follows: HCL is removed in an HCL-removing rectifying tower under conditions that the pressure of a tower kettle ranges from -0.098 MPa to -0.002 MPa, the temperature of the tower kettle ranges from 40 DEG C to 138 DEG C, the temperature of the tower top ranges from 20 DEG C to 120 DEG C, the feed quantity ranges from 5 m<3>/h to 500 m<3>/h, and the reflux ratio ranges from 200 to 2000; then CF3SO3H is removed in a CF3SO3H-removing rectifying tower under conditions that the pressure of a tower kettle ranges from -0.099 MPa to -0.008 MPa, the temperature of the tower kettle ranges from 20 DEG C to 100 DEG C, the temperature of the tower top ranges from 0 DEG C to 80 DEG C, and the reflux ratio ranges from 200 to 1000; the temperature of each tower top is lower than that of each tower kettle. The energy consumption of the method is obviously lower than that of a repeated distillation method, impurity recovery measures are complete, impurity gases, namely, the CF3SO3H and the HCL, can be removed in an efficient, low-cost and pollution-free manner, and purer TMSOTf can be obtained.

Description

A kind of purification process of Trimethylsilyl trifluoromethanesulfonate
Technical field
The present invention relates to a kind of purification process of Trimethylsilyl trifluoromethanesulfonate, specifically, relate to a kind of method adopting continuous rectification purifying Trimethylsilyl trifluoromethanesulfonate, be applicable to industrial production, belong to technical field of fine.
Background technology
Trimethylsilyl trifluoromethanesulfonate, english abbreviation is TMSOTf, and molecular formula is CF 3sO 3si (CH 3) 3, be a kind of silylating agent being widely used in organic synthesis, be mainly used in: protection functional group, participate in carbon carbon and become key to increase the reaction of carbochain, in some reaction, be used as catalyzer, market application foreground is wide.But owing to using trifluoromethanesulfonic acid (CF in the preparation process of Trimethylsilyl trifluoromethanesulfonate 3sO 3and methyl chlorosilane (CH H) 3siH 2the raw material such as Cl), in the product just containing CF 3sO 3the impurity such as H and HCl, adopt chemical process to be difficult to be separated, and bring difficulty to subsequent purification.
The crude product of industrial Trimethylsilyl trifluoromethanesulfonate is mainly impure is HCl and CF 3sO 3h, the specific nature of Trimethylsilyl trifluoromethanesulfonate and described impurity is to such as table 1.
Table 1 Trimethylsilyl trifluoromethanesulfonate and wherein contaminant characteristics contrast
As known from Table 1, there were significant differences for the boiling point of Trimethylsilyl trifluoromethanesulfonate and described impurity, utilizes rectification method can separating impurity effectively, obtains qualified Trimethylsilyl trifluoromethanesulfonate product.
In prior art, the method for purifying Trimethylsilyl trifluoromethanesulfonate has a lot, utilizes the difference of impurities physico-chemical property in Trimethylsilyl trifluoromethanesulfonate product gas, some acid gas impurities, directly can adopt the method for alkali liquor absorption; Impurity CF wherein 3sO 3h adopts repeatedly distillation purifying to remove, but wants strict Controlling Technology parameter in actual distillation purifying process, just can obtain qualified product, otherwise product can be caused defective, or yield reduces.
Open Trimethylsilyl trifluoromethanesulfonate product Trimethylsilyl trifluoromethanesulfonate crude product being carried out under a high vacuum distill after obtaining purifying in patent CN1291985A, there is the high and shortcoming that purity is not high of power consumption in described purification process.
Summary of the invention
For the defect that prior art exists, the object of the present invention is to provide a kind of purification process of Trimethylsilyl trifluoromethanesulfonate, described method can CF efficiently, in the removal Trimethylsilyl trifluoromethanesulfonate of low cost 3sO 3h and HCl foreign gas, the consumption of the energy simultaneously is obviously less than repeatedly distillation method, can obtain CF 3sO 3h content is at below 500ppm and HCl content at the purer Trimethylsilyl trifluoromethanesulfonate product of below 10ppm, and described method compensate for repeatedly the deficiency of distillation method, can be met the Trimethylsilyl trifluoromethanesulfonate of industrial requirements.
For realizing object of the present invention, provide following technical scheme.
A purification process for Trimethylsilyl trifluoromethanesulfonate, described method steps is as follows:
(1) light constituent impurity HCl is removed
Imported in de-HCl rectifying tower by Trimethylsilyl trifluoromethanesulfonate crude product, the pressure controlling described tower bottom of rectifying tower is-0.098MPa ~-0.002MPa, and the temperature of tower reactor is 40 DEG C ~ 138 DEG C, and the temperature of tower top is 20 DEG C ~ 120 DEG C, and the inlet amount of described crude product is 5m 3/ h ~ 500m 3/ h, reflux ratio is 200 ~ 2000, and light constituent impurity HCl discharges from tower top, removes the Trimethylsilyl trifluoromethanesulfonate crude product after HCl and stays in tower reactor;
(2) heavy constituent impurity CF is removed 3sO 3h
De-CF is imported by removing the Trimethylsilyl trifluoromethanesulfonate crude product after HCl 3sO 3in H rectifying tower, the pressure controlling described tower bottom of rectifying tower is-0.099MPa ~-0.008MPa, and the temperature of tower reactor is 20 DEG C ~ 100 DEG C, and the temperature of tower top is 0 DEG C ~ 80 DEG C, reflux ratio is 200 ~ 1000, and the Trimethylsilyl trifluoromethanesulfonate after purifying is from overhead collection.
Wherein, described Trimethylsilyl trifluoromethanesulfonate crude product is mixed gas, in described Trimethylsilyl trifluoromethanesulfonate crude product molecular fraction for 100%, wherein, molecular fraction>=80% of Trimethylsilyl trifluoromethanesulfonate, HCl content is 100ppm ~ 8000ppm, CF 3sO 3h content is 20000ppm ~ 60000ppm; The molecular fraction of preferred described Trimethylsilyl trifluoromethanesulfonate is 80% ~ 99%.
The temperature of rectifying tower tower top described in step (1) and (2) is lower than the temperature of tower reactor.
Described rectifying tower is packing tower, and diameter is 20mm ~ 100mm, is highly 2m ~ 10m, and more than one fillers of nickel, stainless steel or Monel are equipped with in inside, and the specific surface area of described filler is 80m 2/ m 3~ 500m 2/ m 3, form of bio-carrier is regular or loose heap.
Preferably condenser is set above described de-HCl rectifying tower, condenser is entered after HCl described in step (1) discharges from de-HCl rectifying tower top, part liquid phase is back to described rectifying tower from overhead condenser and continues purifying, and another part gas phase enters emission-control equipment; Preferably below described de-HCl rectifying tower, arrange reboiler, remove the part of the Trimethylsilyl trifluoromethanesulfonate crude product after HCl in tower reactor and flow into reboiler, enter described rectifying tower provide thermal source through being heated as gas, another part imports de-CF 3sO 3h rectifying tower continues purifying.
Preferably at described de-CF 3sO 3above H rectifying tower, condenser is set, when the Trimethylsilyl trifluoromethanesulfonate after purifying in step (2) is from de-CF 3sO 3enter condenser after H rectifying tower overhead collection, a part of liquid phase is back to described rectifying tower from overhead condenser and continues purifying, and another part gas phase collects from tower top, is the Trimethylsilyl trifluoromethanesulfonate that purity is higher; Preferably at described de-CF 3sO 3below H rectifying tower, reboiler is set, heavy constituent impurity CF in tower reactor 3sO 3a H part flows into reboiler, and enter described rectifying tower provide thermal source through being heated as gas, another part discharges described rectifying tower, can be used as raw material and carries out cycling and reutilization.
Beneficial effect
1. the invention provides a kind of purification process of Trimethylsilyl trifluoromethanesulfonate, described method makes containing CF 3sO 3the Trimethylsilyl trifluoromethanesulfonate raw gas of H and HCl impurity enters rectifying tower, utilize the boiling point difference of Trimethylsilyl trifluoromethanesulfonate and described impurity, each component in described crude product is made to carry out gas-to-liquid contact separation in described rectifying tower, the Trimethylsilyl trifluoromethanesulfonate after purifying is obtained from tower top, purity can reach 99.9%, wherein said impurity HCl content≤10ppm, CF 3sO 3h content≤500ppm;
2. the invention provides a kind of purification process of Trimethylsilyl trifluoromethanesulfonate, define temperature range in described method, if because the temperature of tower reactor is too high, described crude product easily steams from tower top, has little time to be separated with light constituent impurity HCl; If bottom temperature is too low, in described rectifying tower, gas-liquid two-phase cannot be formed;
3. the invention provides a kind of purification process of Trimethylsilyl trifluoromethanesulfonate, described method can be further purified the HCl of tower top discharge and Trimethylsilyl trifluoromethanesulfonate by arranging condenser, a part of material can be made to utilize as thermal source by arranging reboiler, not only highly effective and safe eliminate impurity CF 3sO 3h and HCl, simultaneously described impurity recycling measure is complete, significantly reduces cost and pollution-free.
Accompanying drawing explanation
Fig. 1 is the rectifier unit structural representation adopted in embodiment.
In figure, 1-de-HCl rectifying tower, 2-condenser A, 3-reboiler A, 4-de-CF 3sO 3h rectifying tower, 5-condenser B, 6-reboiler B.
Embodiment
Set forth content of the present invention in more detail below by specific embodiment, except the embodiment mentioned by the present invention, multiple implementation can also be had, do not limited to by the embodiment in the present invention.
The rectifier unit structure adopted in following examples as shown in Figure 1, mainly comprises: de-HCl rectifying tower 1, condenser A 2, reboiler A 3, de-CF 3sO 3h rectifying tower 4, condenser B 5 and reboiler B 6.Wherein, condenser A 2 is positioned at above de-HCl rectifying tower 1, and the bottom of condenser A 2 and middle part are connected to form loop respectively by two pipelines and de-HCl rectifying tower 1 tower top, and the top of condenser A 2 connects a pipeline in order to discharge HCl; Reboiler A 3 is positioned at below de-HCl rectifying tower 1, and the pipeline connected bottom de-HCl rectifying tower 1 is divided into two branch roads, and a branch road is connected with the bottom of reboiler A 3, another branch road and de-CF 3sO 3connect in the middle part of H rectifying tower 4, the top of reboiler A 3 to be connected with de-HCl rectifying tower 1 tower reactor by a pipeline makes itself and de-HCl rectifying tower 1 form loop.Condenser B 5 is positioned at de-CF 3sO 3above H rectifying tower 4, the bottom of condenser B 5 and middle part are respectively by two pipelines and de-CF 3sO 3h rectifying tower 4 tower top is connected to form loop, and the top of condenser B 5 connects a pipeline in order to collect the Trimethylsilyl trifluoromethanesulfonate after purifying; Reboiler B 6 is positioned at de-CF 3sO 3below H rectifying tower 4, de-CF 3sO 3the pipeline connected bottom H rectifying tower 4 is divided into two branch roads, and a branch road is connected with the bottom of reboiler B 6, and CF discharged by another branch road 3sO 3the top of H, reboiler B 6 is by a pipeline and de-CF 3sO 3h rectifying tower 4 tower reactor connects makes itself and de-CF 3sO 3h rectifying tower 4 forms loop.
The detection method of the finished product described in following examples is for adopting chemical titration.
Embodiment 1
In the rectifier unit that the present embodiment adopts, the diameter of rectifying tower is 20mm, is highly 2m, and inner filling nickel Pall ring filler, the specific surface area of filler is 80m 2/ m 3, form of bio-carrier is loose heap.
A purification process for Trimethylsilyl trifluoromethanesulfonate, described method steps is as follows:
(1) light constituent impurity HCl is removed
Imported in de-HCl rectifying tower 1 by Trimethylsilyl trifluoromethanesulfonate crude product, the pressure controlling described rectifying tower 1 tower reactor is-0.098MPa, and the temperature of tower reactor is 40 DEG C, and the temperature of tower top is 20 DEG C, and the inlet amount of described crude product is 5m 3/ h, reflux ratio is 200, and the gas being rich in light constituent impurity HCl enters condenser A 2 after tower top is discharged, and a part of liquid phase is back to described rectifying tower 1 from condenser A 2 and continues purifying, another part gas phase HCl enters HCl emission-control equipment, and top gaseous phase HCl output is 0.1kg/h; Remove the part of the Trimethylsilyl trifluoromethanesulfonate crude product after HCl and flow into reboiler A 3, enter described rectifying tower 1 through being heated as gas thermal source is provided;
(2) heavy constituent impurity CF is removed 3sO 3h
Remove the Trimethylsilyl trifluoromethanesulfonate crude product another part after HCl and import de-CF 3sO 3purifying is continued in H rectifying tower 4, the pressure controlling described rectifying tower 4 tower reactor is-0.099MPa, the temperature of tower reactor is 20 DEG C, the temperature of tower top is 0 DEG C, reflux ratio is 200, and the Trimethylsilyl trifluoromethanesulfonate after purifying enters condenser B 5 after overhead collection, and a part of liquid phase is back to described rectifying tower 4 from condenser B 5 and continues purifying, another part gas phase collects the finished product from tower top, is high purity Trimethylsilyl trifluoromethanesulfonate; Heavy constituent impurity CF in tower reactor 3sO 3a H part flows into reboiler B 6, and enter described rectifying tower 4 provide thermal source through being heated as gas, another part discharges described rectifying tower 4, can be used as reaction raw materials and carries out cycling and reutilization.
Wherein, described Trimethylsilyl trifluoromethanesulfonate crude product is the molecular fraction of Trimethylsilyl trifluoromethanesulfonate be 97%, HCl content is 100ppm, CF 3sO 3h content is the mixed gas of 20000ppm.
The detected result of the finished product described in the present embodiment is as follows:
The finished product contain 8ppm HCl, 315ppm CF 3sO 3h, the purity of Trimethylsilyl trifluoromethanesulfonate is 99.9%.
Embodiment 2
In the rectifier unit that the present embodiment adopts, the diameter of rectifying tower is 100mm, is highly 10m, and inner filling Monel Pall ring filler, the specific surface area of filler is 500m 2/ m 3, form of bio-carrier is loose heap.
A purification process for Trimethylsilyl trifluoromethanesulfonate, described method steps is as follows:
(1) light constituent impurity HCl is removed
Imported in de-HCl rectifying tower 1 by Trimethylsilyl trifluoromethanesulfonate crude product, the pressure controlling described rectifying tower 1 tower reactor is-0.002MPa, and the temperature of tower reactor is 138 DEG C, and the temperature of tower top is 120 DEG C, and the inlet amount of described crude product is 500m 3/ h, reflux ratio is 2000, and the gas being rich in light constituent impurity HCl enters condenser A 2 after tower top is discharged, and a part of liquid phase is back to described rectifying tower 1 from condenser A 2 and continues purifying, another part gas phase HCl enters HCl emission-control equipment, and top gaseous phase HCl output is 1kg/h; Remove the part of the Trimethylsilyl trifluoromethanesulfonate crude product after HCl and flow into reboiler A 3, enter described rectifying tower 1 through being heated as gas thermal source is provided;
(2) heavy constituent impurity CF is removed 3sO 3h
Remove the Trimethylsilyl trifluoromethanesulfonate crude product another part after HCl and import de-CF 3sO 3purifying is continued in H rectifying tower 4, the pressure controlling described rectifying tower 4 tower reactor is-0.008MPa, the temperature of tower reactor is 100 DEG C, the temperature of tower top is 80 DEG C, reflux ratio is 1000, and the Trimethylsilyl trifluoromethanesulfonate after purifying enters condenser B 5 after overhead collection, and a part of liquid phase is back to described rectifying tower 4 from condenser B 5 and continues purifying, another part gas phase collects the finished product from tower top, is high purity Trimethylsilyl trifluoromethanesulfonate; Heavy constituent impurity CF in tower reactor 3sO 3a H part flows into reboiler B 6, and enter described rectifying tower 4 provide thermal source through being heated as gas, another part discharges described rectifying tower 4, can be used as reaction raw materials and carries out cycling and reutilization.
Wherein, described Trimethylsilyl trifluoromethanesulfonate crude product is the molecular fraction of Trimethylsilyl trifluoromethanesulfonate be 93%, HCl content is 8000ppm, CF 3sO 3h content is the mixed gas of 60000ppm.
The detected result of the finished product described in the present embodiment is as follows:
The finished product contain 9ppm HCl, 452ppm CF 3sO 3h, the purity of Trimethylsilyl trifluoromethanesulfonate is 99.9%.
Embodiment 3
In the rectifier unit that the present embodiment adopts, the diameter of rectifying tower is 50mm, is highly 5m, and inner filling stainless steel Pall ring filler, the specific surface area of filler is 253m 2/ m 3, form of bio-carrier is regular.
A purification process for Trimethylsilyl trifluoromethanesulfonate, described method steps is as follows:
(1) light constituent impurity HCl is removed
Imported in de-HCl rectifying tower 1 by Trimethylsilyl trifluoromethanesulfonate crude product, the pressure controlling described rectifying tower 1 tower reactor is-0.053MPa, and the temperature of tower reactor is 98 DEG C, and the temperature of tower top is 70 DEG C, and the inlet amount of described crude product is 210m 3/ h, reflux ratio is 830, and the gas being rich in light constituent impurity HCl enters condenser A 2 after tower top is discharged, and a part of liquid phase is back to described rectifying tower 1 from condenser A 2 and continues purifying, another part gas phase HCl enters HCl emission-control equipment, and top gaseous phase HCl output is 0.46kg/h; Remove the part of the Trimethylsilyl trifluoromethanesulfonate crude product after HCl and flow into reboiler A 3, enter described rectifying tower 1 through being heated as gas thermal source is provided;
(2) heavy constituent impurity CF is removed 3sO 3h
Remove the Trimethylsilyl trifluoromethanesulfonate crude product another part after HCl and import de-CF 3sO 3purifying is continued in H rectifying tower 4, the pressure controlling described rectifying tower 4 tower reactor is-0.051MPa, the temperature of tower reactor is 63 DEG C, the temperature of tower top is 47 DEG C, reflux ratio is 760, and the Trimethylsilyl trifluoromethanesulfonate after purifying enters condenser B 5 after overhead collection, and a part of liquid phase is back to described rectifying tower 4 from condenser B 5 and continues purifying, another part gas phase collects the finished product from tower top, is high purity Trimethylsilyl trifluoromethanesulfonate; Heavy constituent impurity CF in tower reactor 3sO 3a H part flows into reboiler B 6, and enter described rectifying tower 4 provide thermal source through being heated as gas, another part discharges described rectifying tower 4, can be used as reaction raw materials and carries out cycling and reutilization.
Wherein, described Trimethylsilyl trifluoromethanesulfonate crude product is the molecular fraction of Trimethylsilyl trifluoromethanesulfonate be 95%, HCl content is 3000ppm, CF 3sO 3h content is the mixed gas of 40000ppm.
The detected result of the finished product described in the present embodiment is as follows:
The finished product contain 5ppm HCl, 381ppm CF 3sO 3h, the purity of Trimethylsilyl trifluoromethanesulfonate is 99.9%.
The present invention includes but be not limited to above embodiment, every any equivalent replacement of carrying out under the principle of spirit of the present invention or local improvement, all will be considered as within protection scope of the present invention.

Claims (9)

1. a purification process for Trimethylsilyl trifluoromethanesulfonate, is characterized in that: described method steps is as follows:
(1) light constituent impurity HCl is removed
Trimethylsilyl trifluoromethanesulfonate crude product is imported in de-HCl rectifying tower (1), the pressure controlling described rectifying tower (1) tower reactor is-0.098MPa ~-0.002MPa, the temperature of tower reactor is 40 DEG C ~ 138 DEG C, the temperature of tower top is 20 DEG C ~ 120 DEG C, and the inlet amount of described crude product is 5m 3/ h ~ 500m 3/ h, reflux ratio is 200 ~ 2000, and light constituent impurity HCl discharges from tower top, removes the Trimethylsilyl trifluoromethanesulfonate crude product after HCl and stays in tower reactor;
(2) heavy constituent impurity CF is removed 3sO 3h
De-CF is imported by removing the Trimethylsilyl trifluoromethanesulfonate crude product after HCl 3sO 3in H rectifying tower (4), the pressure controlling described rectifying tower (4) tower reactor is-0.099MPa ~-0.008MPa, the temperature of tower reactor is 20 DEG C ~ 100 DEG C, the temperature of tower top is 0 DEG C ~ 80 DEG C, reflux ratio is 200 ~ 1000, and the Trimethylsilyl trifluoromethanesulfonate after purifying is from overhead collection;
Described Trimethylsilyl trifluoromethanesulfonate crude product is molecular fraction>=80% of mixed gas, Trimethylsilyl trifluoromethanesulfonate, and HCl content is 100ppm ~ 8000ppm, CF 3sO 3h content is 20000ppm ~ 60000ppm;
The temperature of rectifying tower tower top described in step (1) and (2) is lower than the temperature of tower reactor;
Described rectifying tower is packing tower, and diameter is 20mm ~ 100mm, is highly 2m ~ 10m, and more than one fillers of nickel, stainless steel or Monel are equipped with in inside, and the specific surface area of described filler is 80m 2/ m 3~ 500m 2/ m 3, form of bio-carrier is regular or loose heap.
2. the purification process of a kind of Trimethylsilyl trifluoromethanesulfonate according to claim 1, is characterized in that: the molecular fraction of described Trimethylsilyl trifluoromethanesulfonate is 80% ~ 99%.
3. the purification process of a kind of Trimethylsilyl trifluoromethanesulfonate according to claim 1 and 2, is characterized in that: arrange condenser in described de-HCl rectifying tower (1) top.
4. the purification process of a kind of Trimethylsilyl trifluoromethanesulfonate according to claim 1 and 2, is characterized in that: arrange reboiler in described de-HCl rectifying tower (1) below.
5. the purification process of a kind of Trimethylsilyl trifluoromethanesulfonate according to claim 4, is characterized in that: arrange condenser in described de-HCl rectifying tower (1) top.
6. the purification process of a kind of Trimethylsilyl trifluoromethanesulfonate according to claim 1 and 2, is characterized in that: at described de-CF 3sO 3h rectifying tower (4) top arranges condenser.
7. the purification process of a kind of Trimethylsilyl trifluoromethanesulfonate according to claim 1 and 2, is characterized in that: at described de-CF 3sO 3h rectifying tower (4) below arranges reboiler.
8. the purification process of a kind of Trimethylsilyl trifluoromethanesulfonate according to claim 7, is characterized in that: at described de-CF 3sO 3h rectifying tower (4) top arranges condenser.
9. the purification process of a kind of Trimethylsilyl trifluoromethanesulfonate according to claim 1 and 2, is characterized in that: arrange condenser in described de-HCl rectifying tower (1) top, below arranges reboiler; At described de-CF 3sO 3h rectifying tower (4) top arranges condenser, and below arranges reboiler.
CN201410546511.3A 2014-10-16 2014-10-16 TMSOTf (trimethylsilyl trifluoromethanesulfonate) purifying method Pending CN104262376A (en)

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Publication number Priority date Publication date Assignee Title
CN108276315A (en) * 2017-12-29 2018-07-13 中国船舶重工集团公司第七八研究所 A kind of purification process of trifluoromethanesulfonic acid
CN110964053A (en) * 2019-11-29 2020-04-07 中船重工(邯郸)派瑞特种气体有限公司 Device and method for purifying trimethylsilyl trifluoromethanesulfonate
CN113109085A (en) * 2021-03-22 2021-07-13 中船重工(邯郸)派瑞特种气体有限公司 Sampling system and method for hazardous liquid negative pressure pipeline
CN113198196A (en) * 2021-04-28 2021-08-03 江西国化实业有限公司 Device for purifying trimethylsilyl trifluoromethanesulfonate

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108276315A (en) * 2017-12-29 2018-07-13 中国船舶重工集团公司第七八研究所 A kind of purification process of trifluoromethanesulfonic acid
CN110964053A (en) * 2019-11-29 2020-04-07 中船重工(邯郸)派瑞特种气体有限公司 Device and method for purifying trimethylsilyl trifluoromethanesulfonate
CN113109085A (en) * 2021-03-22 2021-07-13 中船重工(邯郸)派瑞特种气体有限公司 Sampling system and method for hazardous liquid negative pressure pipeline
CN113198196A (en) * 2021-04-28 2021-08-03 江西国化实业有限公司 Device for purifying trimethylsilyl trifluoromethanesulfonate

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