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Continuous preparation device and method of trifluoroacetyl chloride

A technology of trifluoroacetyl chloride and preparation device, which is applied in the preparation of acid halide, preparation of acid halide, preparation of organic compounds, etc., can solve the problems of fluoride ion corrosion equipment, glass optical trap corrosion, etc., which are difficult to solve, and achieve suppressed fracture. , The effect of inhibiting corrosion and accelerating the reaction

Pending Publication Date: 2022-05-17
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The R123 photooxidation route generally produces fluoride ions in the reaction, which will cause corrosion to the reactor, especially the glass optical trap.
The above-mentioned patents suppress fluorine ion corrosion by controlling the wavelength of the light source and using light-shielding components, which are more effective in the laboratory research stage. Once industrialized production is carried out, it is difficult to solve the situation of fluoride ion corrosion equipment

Method used

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  • Continuous preparation device and method of trifluoroacetyl chloride
  • Continuous preparation device and method of trifluoroacetyl chloride
  • Continuous preparation device and method of trifluoroacetyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0075] This embodiment provides a continuous preparation device for trifluoroacetyl chloride, figure 1 , figure 2 Schematically gives the structure diagram of the continuous preparation device of trifluoroacetyl chloride, as figure 1 , figure 2 Shown, described continuous preparation device comprises:

[0076] Side circulation unit, described side circulation unit comprises circulation pump 13, gas injector 11 and static mixer 12 connected in sequence, the material of reaction unit enters gas injector through circulation pump, and feed gas (oxygen and chlorine) in gas injection Mix in the container, and then return to the reaction unit to carry out the photooxidation reaction after being further mixed evenly by the static mixer;

[0077] A reaction unit, the reaction unit includes a reactor 21, a cold trap 22 placed in the reactor, a mercury lamp 23 placed in the cold trap, and a raw material storage container 24 for adding raw material R123 to the reactor, the cold The ...

Embodiment 2

[0083] This embodiment provides a continuous production method of trifluoroacetyl chloride, the continuous production method adopts the continuous production device described in Example 1, specifically: a 100L reactor is used, the mercury lamp is a 2000w high-pressure mercury lamp, and the ETFE The coating thickness of the film is 50 μm, and the rotation speed of the circulation pump is 1500 r / min.

[0084] The reaction process is as follows:

[0085] Add 80L of liquid raw material R123 into the reactor, continuously feed oxygen and chlorine under stirring, the oxygen flow rate is 1000ml / min, the chlorine flow rate is 100ml / min, and the liquid level in the reactor is kept stable by continuously adding R123. The reaction pressure was controlled at 0.1MPa, the reaction temperature was controlled at 48°C through the reactor jacket, and the reactants were continuously discharged from the gas phase outlet of the reactor in the form of gas phase.

[0086] After reacting for 24 hour...

Embodiment 3

[0090] The operation of this embodiment is the same as that of Embodiment 2, the only difference being: the Teflon AF film sprayed on the outer surface of the cold trap.

[0091] After reacting for 100 hours, the calculated TFAC content was 66.4%, the R123 content was 32.8%, the R113a content was 0.8%, and the fluoride ion content was detected to be 7ppm.

[0092] After the reaction was stopped and the cold trap was removed, it was found that there was no corrosion phenomenon on the surface of the cold trap, and no white powdery film was attached, and the light transmittance was 94%.

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Abstract

The invention discloses a continuous preparation device and method of trifluoroacetyl chloride, the continuous preparation device comprises: a side circulation unit comprising a gas injector provided with a liquid inlet, a gas inlet and an injection orifice, a material of a reaction unit and a raw material gas being mixed in the gas injector and then returning to the reaction unit through the injection orifice; the reaction unit comprises a reactor, a cold trap arranged in the reactor and a mercury lamp arranged in the cold trap, and the outer surface of the cold trap is coated with a thermal shrinkage fluororesin material; the separation unit comprises a coarse separation tower, a compressor, a flexible separation tower, a dechlorination tower and a TFAC product tower which are connected in sequence, the tower top of the coarse separation tower is connected with an inlet of the compressor, a tower kettle of the flexible separation tower is connected with the dechlorination tower, a tower kettle of the dechlorination tower is connected with the TFAC product tower, and a trifluoroacetyl chloride product is obtained at the tower top of the TFAC product tower. The method has the advantages of low equipment corrosion, high reaction yield, capability of selectively preparing products, suitability for industrial production and the like.

Description

technical field [0001] The invention relates to the preparation of fluorine-containing intermediates, in particular to a continuous preparation device and method for trifluoroacetyl chloride, and a co-production device and method for trifluoroacetyl chloride and trifluoroacetic acid. Background technique [0002] Trifluoroacetyl chloride, referred to as TFAC, is a volatile, colorless liquid with a pungent odor, easily hydrolyzed, easily soluble in organic solvents, and is mainly used for the synthesis of trifluoroacetic acid or other derivatives. important raw material. [0003] At present, the preparation route of trifluoroacetyl chloride mainly includes: [0004] 1) R113a catalytic oxidation route [0005] Using R113a as raw material and fuming sulfuric acid as oxidant, trifluoroacetyl chloride was prepared by catalytic oxidation under the action of mercury-based catalyst. [0006] Patent US3160659A discloses R113a and SO 3 in HgSO 4 / Hg 2 SO 4 The method for prepar...

Claims

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Application Information

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IPC IPC(8): B01J19/24C07C51/58C07C51/64C07C53/48C07C51/04C07C53/18
CPCB01J19/24C07C51/58C07C51/64C07C51/04C07C53/48C07C53/18
Inventor 王术成郑瑞朋刘武灿周飞翔吴江平吕正璋刘建鹏吴建徐波朱梦宇
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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