Method and equipment for producing trimethylsilyl trifluoromethanesulfonate

A trimethylsilyl trifluoromethanesulfonate and production equipment technology, which is applied in the field of trimethylsilyl trifluoromethanesulfonate production, can solve the problems of violent reaction, insufficient reaction, and difficult control, and achieve stirring The effect of sufficient reaction, high purity and less impurities

Active Publication Date: 2020-12-18
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, the production method of trimethylsilyl trifluoromethanesulfonate is usually to directly add trimethylchlorosilane into trifluoromethanesulfonic acid, the reaction is violent and difficult to control and is prone to insufficient reaction
In addition, a reactor will be used in the production process of trifluoromethanesulfonic acid, but the existing reactor is not sufficiently stirred, and there is no special titration device, so the addition of trimethylchlorosilane cannot be accurately controlled

Method used

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  • Method and equipment for producing trimethylsilyl trifluoromethanesulfonate
  • Method and equipment for producing trimethylsilyl trifluoromethanesulfonate
  • Method and equipment for producing trimethylsilyl trifluoromethanesulfonate

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Such as Figure 1~3 As shown, a trimethylsilyl trifluoromethanesulfonate production equipment, the equipment includes a reactor 1 and a quantitative tank 15.

[0026] The middle part of the reaction kettle 1 is fixedly connected with the fixed plate 3, the top of the rotating rod 2 protrudes from the fixed plate 3 and is rotatably connected with the fixed plate 3, the bottom of the rotating rod 2 protrudes from the bottom of the reaction kettle 1, and is fixed to the outside of the bottom of the reaction kettle 1 The motor 10 is connected; the outer wall of the rotating rod 2 is provided with two sets of symmetrical stirring mechanisms.

[0027] Each group of stirring mechanisms includes a device cylinder 6 fixed on the outer wall of the rotating rod 2. There are four device cylinders 6, and every two are symmetrically placed as a group, and the two groups are arranged up and down; The inner wall of the plate and the inner wall of the device cylinder 6 are elastically ...

Embodiment 2

[0033] A method for producing trimethylsilyl trifluoromethanesulfonate, the method steps are as follows:

[0034]Add trifluoromethanesulfonic acid in reactor 1, add trimethylchlorosilane dropwise in reactor 1 to react, the rate of addition is 5mm / min, the pressure of reactor 1 is 0.002MPa, and the reaction temperature is 20°C. The time was 8.5 hours; after the reaction was completed, distillation under reduced pressure was carried out, and the fraction at 125°C was collected to obtain the final product, trimethylsilyl trifluoromethanesulfonate, with a yield of 98.1%.

[0035] The final product that present embodiment is made detects as follows:

[0036] It can be known that the final product is trimethylsilyl trifluoromethanesulfonate with a purity of 99.97% through Fourier transform infrared spectroscopy and nuclear magnetic resonance detection.

Embodiment 3

[0038] A method for producing trimethylsilyl trifluoromethanesulfonate, the method steps are as follows:

[0039] Add trifluoromethanesulfonic acid in reactor 1, drop trimethylchlorosilane in reactor 1 to react, the rate of addition is 8mm / min, the pressure of reactor 1 is 0.002MPa, and the reaction temperature is 25°C. The time was 9 hours; after the reaction was completed, the reaction was distilled under reduced pressure, and the fraction at 130°C was collected to obtain the final product, trimethylsilyl trifluoromethanesulfonate, with a yield of 98.3%.

[0040] The final product that present embodiment is made detects as follows:

[0041] It can be known that the final product is trimethylsilyl trifluoromethanesulfonate with a purity of 99.98% through Fourier transform infrared spectroscopy and nuclear magnetic resonance detection.

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Abstract

The invention relates to a method and equipment for producing trimethylsilyl trifluoromethanesulfonate, which belongs to the technical field of trimethylsilyl trifluoromethanesulfonate production. Themethod comprises the following steps of adding trifluoromethanesulfonic acid into a reaction kettle, dropwisely adding trimethylchlorosilane, reacting at 20-30 DEG C under 0.002-0.003 MPa for 8.5-10hours, carrying out reduced pressure distillation, and collecting 125-135 DEG C fractions, thereby obtaining the trimethylsilyl trifluoromethanesulfonate. The equipment comprises a reaction kettle anda quantitative tank, a fixed plate is fixed in the reaction kettle, a rotating rod is rotatably connected to the fixed plate, a motor fixed to the rotating rod is installed at the bottom of the reaction kettle, a stirring mechanism is arranged on the outer side of the rotating rod, and a titration opening is formed in the top of the reaction kettle and connected with a titration mechanism in a liquid inlet pipe at the bottom of the quantitative tank; astrip-shaped cavity is arranged on one side wall of thequantitative tank; a control mechanism connected with the titration mechanism is arranged in the strip-shaped cavity, and an injection port and a nitrogen filling port are formed in the other side wall of the strip-shaped cavity. The equipment can accurately control the trimethylchlorosilane titration speed, and the product purity is higher.

Description

technical field [0001] The invention relates to a production method and equipment of trimethylsilyl trifluoromethanesulfonate, belonging to the technical field of trimethylsilyl trifluoromethanesulfonate production. Background technique [0002] Trimethylsilyl trifluoromethanesulfonate (CF 3 SO 3 Si(CH 3 ) 3 ) is an important trifluoromethanesulfonic acid derivative, which has a wide range of applications in organic synthesis: it is a very effective methyl silylation reagent, which can be used for the transformation and protection of functional groups (can be used as alcohol, carboxyl acid, carbonyl compound, thiol and nitro compound); participate in the reaction of organic compound C-C bond formation and carbon chain growth; used as Lewis acid catalyst; used for removal of protective group; as cationic polymerization initiator etc. [0003] In the prior art, the production method of trimethylsilyl trifluoromethanesulfonate is usually to directly add trimethylchlorosila...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08C07F7/20B01J4/00B01J19/18
CPCC07F7/0834C07F7/20B01J19/18B01J4/008B01J4/001
Inventor 林坤吕灵华商洪涛王少波罗建志马朝选孙秋丽赵庆伟
Owner PERIC SPECIAL GASES CO LTD
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