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TMSOTf (trimethylsilyl trifluoromethanesulfonate) purifying method

A technology of trimethylsilyl trifluoromethanesulfonate and trimethylsilyl fluoromethanesulfonate, which is applied in the field of purification of trimethylsilyl trifluoromethanesulfonate, to achieve cost reduction and complete impurity recovery and treatment measures Effect

Inactive Publication Date: 2015-01-07
718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In view of the defects in the prior art, the object of the present invention is to provide a method for purifying trimethylsilyl trifluoromethanesulfonate, which can remove trimethylsilyl trifluoromethanesulfonate efficiently and at low cost CF in 3 SO 3 H and HCl impurity gases, while energy consumption is significantly less than multiple distillation, CF can be obtained 3 SO 3 H content below 500ppm and HCl content below 10ppm relatively pure trimethylsilyl trifluoromethanesulfonate product, described method makes up for the deficiency of multiple distillation method, can obtain trifluoromethanesulfonate trimethylsilyl that meets industrial requirements methyl silicon ester

Method used

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Examples

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Embodiment 1

[0031] In the rectification device adopted in this embodiment, the diameter of the rectification tower is 20mm, the height is 2m, and the nickel Pall ring filler is filled inside, and the specific surface area of ​​the filler is 80m 2 / m 3 , the packing form is random.

[0032] A method for purifying trimethylsilyl trifluoromethanesulfonate, the method steps are as follows:

[0033] (1) Removal of light component impurity HCl

[0034] The trimethylsilyl trifluoromethanesulfonate crude product is imported in the HCl-removing rectification tower 1, the pressure of the tower bottom of the said rectification tower 1 is controlled to be -0.098MPa, the temperature of the tower bottom is 40°C, and the temperature of the tower top is 20°C, the feeding amount of the crude product is 5m 3 / h, the reflux ratio is 200, and the gas rich in light component impurity HCl enters condenser A 2 after being discharged from the tower top, and a part of liquid phase is refluxed to described rect...

Embodiment 2

[0041] In the rectification device adopted in this embodiment, the diameter of the rectification tower is 100mm, the height is 10m, and the inside is filled with Monel Pall ring packing, and the specific surface area of ​​the packing is 500m 2 / m 3 , the packing form is random.

[0042] A method for purifying trimethylsilyl trifluoromethanesulfonate, the method steps are as follows:

[0043] (1) Removal of light component impurity HCl

[0044] The trimethylsilyl trifluoromethanesulfonate crude product is introduced into the HCl-removing rectification tower 1, the pressure of the bottom of the distillation tower 1 is controlled to be -0.002MPa, the temperature of the bottom of the tower is 138 ° C, and the temperature of the top of the tower is 120°C, the feeding amount of the crude product is 500m 3 / h, the reflux ratio is 2000, and the gas rich in light component impurity HCl enters condenser A2 after being discharged from the tower top, and a part of liquid phase is reflu...

Embodiment 3

[0051] In the rectification device adopted in this embodiment, the diameter of the rectification tower is 50mm, the height is 5m, and the interior is filled with stainless steel Pall ring packing, and the specific surface area of ​​the packing is 253m 2 / m 3 , the packing form is regular.

[0052] A method for purifying trimethylsilyl trifluoromethanesulfonate, the method steps are as follows:

[0053] (1) Removal of light component impurity HCl

[0054] The trimethylsilyl trifluoromethanesulfonate crude product is imported in the HCl-removing rectification tower 1, the pressure of the bottom of the distillation tower 1 is controlled to be -0.053MPa, the temperature of the bottom of the tower is 98 ° C, and the temperature of the top of the tower is 70°C, the feed amount of the crude product is 210m 3 / h, the reflux ratio is 830, and the gas rich in light component impurity HCl enters condenser A2 after being discharged from the tower top, and a part of liquid phase is refl...

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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

technical field [0001] The invention relates to a method for purifying trimethylsilyl trifluoromethanesulfonate, in particular to a method for purifying trimethylsilyl trifluoromethanesulfonate by continuous rectification, which is suitable for industrial production and belongs to Fine chemical technology field. Background technique [0002] Trimethylsilyl trifluoromethanesulfonate, abbreviated as TMSOTf, molecular formula CF 3 SO 3 Si(CH 3 ) 3 , is a silylation reagent widely used in organic synthesis, mainly used to: protect functional groups, participate in the reaction of carbon-carbon bond formation and growth of carbon chains, and be used as a catalyst in some reactions, with broad market application prospects. But because trifluoromethanesulfonic acid (CF) is used in the preparation process of trimethylsilyl trifluoromethanesulfonate 3 SO 3 H) and methylchlorosilane (CH 3 SiH 2 Cl) and other raw materials contain CF in the product 3 SO 3 Impurities such as H...

Claims

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Application Information

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IPC IPC(8): C07F7/08
Inventor 彭立培黄华璠杨献奎孟祥军郭绪涛商洪涛吕灵华
Owner 718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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