CN210646343U

CN210646343U - Device for preparing trifluoroiodomethane through photocatalysis

Info

Publication number: CN210646343U
Application number: CN201921603164.8U
Authority: CN
Inventors: 金向华; 侯倩; 王新喜; 孙猛; 刘晶; 栗鹏伟; 齐向前
Original assignee: Suzhou Jinhong Gas Co Ltd
Current assignee: Jinhong Gas Co ltd
Priority date: 2019-09-25
Filing date: 2019-09-25
Publication date: 2020-06-02
Anticipated expiration: 2029-09-25

Abstract

The utility model discloses a device of photocatalysis preparation trifluoroiodomethane, supply with the unit including trifluoromethane, oxygen supply with the unit, potassium iodide supply with the unit, the catalyst supply with the unit, photoreaction unit and trifluoroiodomethane receiving element, the photoreaction unit includes import A, import B, import C, import D and export, the exit linkage of trifluoromethane supply with the unit is connected to the import A of photoreaction unit, the exit linkage of oxygen supply with the unit is to photoreaction unit's import B, potassium iodide supply with the exit linkage of unit is to photoreaction unit's import C, the exit linkage of catalyst supply with the unit is to photoreaction unit's import D, photoreaction unit's exit linkage is to the import of trifluoroiodomethane receiving element. The utility model discloses in, can realize this reaction under room temperature ordinary pressure condition, reaction condition is simple, and greatly reduced reaction energy consumption can not cause catalyst carbon deposit phenomenon in the reaction simultaneously, and recycle also can be stabilized to the catalyst.

Description

Device for preparing trifluoroiodomethane through photocatalysis

Technical Field

The utility model relates to a trifluoroiodomethane preparation field, concretely relates to photocatalysis preparation trifluoroiodomethane's device.

Background

The trifluoroiodomethane has the relative molecular mass of 195.9, the potential greenhouse effect (GWP) of <5, the potential Ozone Depletion (ODP) of zero, the density of 2.361g/mL, the freezing point of 110 ℃, the boiling point of-22 ℃, the critical temperature of 123.3 ℃ and the critical pressure of 3.95MPa, can be used for replacing hydrofluorocarbons, hydrochlorofluorocarbons and halon fire extinguishing agents, and can also be used for preparing fluorine-containing intermediates, semiconductor etching, foaming agent compositions, aerosol propellants and the like. Many studies on the synthesis process of trifluoroiodomethane are reported, and the synthesis processes which are industrialized or have industrial prospects mainly comprise a perfluorocarboxylic acid salt thermal decomposition method, a trifluoromethane iodination method and a pentafluoroethane iodination method. Based on the current research reports at home and abroad, the process for synthesizing trifluoroiodomethane by a fluoroalkane iodination method is feasible for industrial application. Among them, the research on the iodotrifluoromethane method is the most extensive, and the Nomera research proposes that CHF3 and I2 are used as raw materials, activated carbon loaded with alkali metal or alkaline earth metal is used as a catalyst, and the iodotrifluoromethane is prepared by gas-phase iodination catalysis, wherein the catalyst shows good catalytic activity, but the catalyst has serious carbon deposition and short service life due to high reaction temperature, and the generated high polymer increases the difficulty of recycling unreacted I2. On the basis, researchers improve the process, and a proper amount of oxygen is added in the reaction process, so that the carbon deposition phenomenon of the catalyst can be reduced to a certain degree, the service life of the catalyst is prolonged, the activated carbon carrier can be prevented from being oxidized, and the purpose of synthesizing the trifluoroiodomethane by the continuous one-step gas-phase catalytic oxidation process is realized.

In conclusion, the synthesis temperature in the existing preparation method of trifluoroiodomethane is high, the carbon deposition phenomenon of the catalyst is difficult to avoid, and the energy consumption is high.

Disclosure of Invention

The utility model aims at providing a device of photocatalysis preparation trifluoroiodomethane, more green, energy-conservation just avoids catalyst carbon deposit phenomenon.

In order to achieve the above purpose, the utility model adopts the technical scheme that: the utility model provides a device of photocatalysis preparation trifluoroiodomethane, includes trifluoromethane supply unit, oxygen supply unit, potassium iodide supply unit, catalyst supply unit, photoreaction unit and trifluoroiodomethane receiving element, the photoreaction unit includes import A, import B, import C, import D and export, the exit linkage of trifluoromethane supply unit is connected to the import A of photoreaction unit, the exit linkage of oxygen supply unit is connected to the import B of photoreaction unit, the exit linkage of potassium iodide supply unit is connected to the import C of photoreaction unit, the exit linkage of catalyst supply unit is connected to the import D of photoreaction unit, the exit linkage of photoreaction unit is to the import of trifluoroiodomethane receiving element.

Further, the trifluoromethane supply unit is a trifluoromethane gas cylinder.

Further, the oxygen supply unit is an oxygen cylinder.

Further, the potassium iodide supply unit is a potassium iodide solution storage tank.

Further, the catalyst supply unit is a carbon nitride storage tank.

Further, the photoreaction unit includes a reactor and a light source irradiating a light source solution inside the reactor.

Further, the reactor includes bottom, lateral wall and top, the bottom with the lateral wall is the polytetrafluoroethylene material, the top is the quartz material, and it is used for seeing through the light that the light source sent.

Further, the light source is a 1000W xenon lamp light source.

Further, the trifluoroiodomethane receiving unit is a gas chromatograph.

Because of the application of the technical scheme, compared with the prior art, the utility model has the following advantages: the utility model discloses a device of photocatalysis preparation trifluoroiodomethane through photocatalysis's method to trifluoromethane, oxygen, potassium iodide are raw materials preparation trifluoroiodomethane, can realize this reaction under room temperature ordinary pressure condition, and reaction conditions is simple, and greatly reduced reaction energy consumption can not cause catalyst carbon deposit phenomenon in the reaction simultaneously, and recycle also can be stabilized to the catalyst.

Drawings

Fig. 1 is a schematic composition diagram of the device for preparing trifluoroiodomethane by photocatalysis disclosed by the utility model.

Wherein, 10, a trifluoromethane supply unit; 20. an oxygen supply unit; 30. a potassium iodide supply unit; 40. a catalyst supply unit; 50. a photoreaction unit; 51. a reactor; 52. a light source; 60. a trifluoroiodomethane receiving unit.

Detailed Description

The invention will be further described with reference to the accompanying drawings and examples:

referring to fig. 1, as shown in the figure, an apparatus for preparing trifluoroiodomethane by photocatalysis comprises a trifluoromethane supply unit 10, an oxygen supply unit 20, a potassium iodide supply unit 30, a catalyst supply unit 40, a photoreaction unit 50 and a trifluoroiodomethane receiving unit 60, wherein the photoreaction unit 50 comprises an inlet a, an inlet B, an inlet C, an inlet D and an outlet, the outlet of the trifluoromethane supply unit 10 is connected to the inlet a of the photoreaction unit 50, the outlet of the oxygen supply unit 20 is connected to the inlet B of the photoreaction unit 50, the outlet of the potassium iodide supply unit 30 is connected to the inlet C of the photoreaction unit 50, the outlet of the catalyst supply unit 40 is connected to the inlet D of the photoreaction unit 50, and the outlet of the photoreaction unit 50 is connected to the inlet of the trifluoroiodomethane receiving unit 60.

In the preferred embodiment of this embodiment, the trifluoromethane supply unit 10 is a trifluoromethane gas cylinder, and the trifluoromethane is supplied to the reactor by opening a valve in the pipe.

In the preferred embodiment of this embodiment, the oxygen supply unit 20 is an oxygen cylinder, and oxygen is supplied to the reactor by opening a valve on the pipeline.

In a preferred embodiment of this embodiment, the potassium iodide supply unit 30 is a potassium iodide solution storage tank, and the potassium iodide solution is delivered to the reactor by opening a liquid inlet pump or opening a valve.

In the preferred embodiment of this embodiment, the catalyst supply unit 40 is a carbon nitride storage tank, and the carbon nitride is transferred to the reactor by its own weight by opening a valve.

In a preferred embodiment of this embodiment, the photoreaction unit 50 includes a reactor 51 and a light source 52 for irradiating the inside of the reactor 51.

In the preferred embodiment of the present invention, the reactor 51 comprises a bottom, a sidewall and a top, wherein the bottom and the sidewall are made of teflon, and the top is made of quartz, which is used to transmit the light emitted from the light source 52.

In a preferred embodiment of this embodiment, the light source 52 is a 1000W xenon lamp light source.

In a preferred embodiment of this embodiment, the trifluoroiodomethane receiving unit 60 is a gas chromatograph.

Firstly, conveying a potassium iodide solution into a reactor;

then, delivering carbon nitride into the reactor, and dispersing the carbon nitride in a potassium iodide solution;

then, conveying the trifluoromethane and the oxygen serving as reaction raw material gases into the reactor after decompression;

finally, the product trifluoroiodomethane was analyzed by gas chromatography.

Regarding the photocatalyst, which is a conventional raw material, the preparation method thereof is briefly described here: 10g of urea is placed in a crucible, heated to 550 ℃ at the heating rate of 5 ℃/min under the condition of nitrogen, kept at the constant temperature for 2h, and ground to obtain light yellow carbon nitride powder. 5.3g of magnesium nitrate hexahydrate is dissolved in 100mL of isopropanol and subjected to ultrasonic treatment for 1h, then 0.5g of the prepared carbon nitride powder is added into the solution and then ultrasonic treatment is continued for 24h, then the solution is subjected to rotary evaporation to remove the solvent, the obtained solid is heated to 400 ℃ at the heating rate of 5 ℃/min under the condition of nitrogen, and then the temperature is kept for 4h at constant temperature, so that the photocatalyst is MgO @ g-C3N 4.

For the preparation of trifluoroiodomethane: adding 100mL of saturated aqueous solution of potassium iodide into a photoreactor, adding 0.2g of MgO @ g-C3N4 catalyst, continuously stirring, introducing trifluoromethane and oxygen for 30min under dark conditions, turning on a light source, carrying out light reaction for 24h, and analyzing the purity of trifluoroiodomethane to be 99.6% by gas chromatography.

The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. The device for preparing trifluoroiodomethane through photocatalysis is characterized by comprising a trifluoromethane supply unit, an oxygen supply unit, a potassium iodide supply unit, a catalyst supply unit, a photoreaction unit and a trifluoroiodomethane receiving unit, wherein the photoreaction unit comprises an inlet A, an inlet B, an inlet C, an inlet D and an outlet, the outlet of the trifluoromethane supply unit is connected to the inlet A of the photoreaction unit, the outlet of the oxygen supply unit is connected to the inlet B of the photoreaction unit, the outlet of the potassium iodide supply unit is connected to the inlet C of the photoreaction unit, the outlet of the catalyst supply unit is connected to the inlet D of the photoreaction unit, and the outlet of the photoreaction unit is connected to the inlet of the trifluoroiodomethane receiving unit.

2. The apparatus for photocatalytic production of trifluoroiodomethane according to claim 1, wherein the trifluoromethane supply unit is a trifluoromethane cylinder.

3. The apparatus for photocatalytic production of trifluoroiodomethane according to claim 1, wherein the oxygen supply unit is an oxygen cylinder.

4. The apparatus for photocatalytic production of trifluoroiodomethane according to claim 1, wherein the potassium iodide supply unit is a potassium iodide solution tank.

5. The apparatus for photocatalytic production of trifluoroiodomethane according to claim 1, wherein the catalyst supply unit is a carbon nitride storage tank.

6. The apparatus for photocatalytic production of trifluoroiodomethane according to claim 1, wherein the photoreaction unit comprises a reactor and a light source that irradiates a light source solution inside the reactor.

7. The apparatus of claim 6, wherein the reactor comprises a bottom, a sidewall and a top, the bottom and the sidewall are made of Teflon, and the top is made of quartz and is used for transmitting light emitted from the light source.

8. The apparatus for photocatalytic preparation of trifluoroiodomethane according to claim 6, wherein the light source is a 1000W xenon lamp light source.

9. The apparatus for photocatalytic production of trifluoroiodomethane according to claim 1, wherein the trifluoroiodomethane receiving unit is a gas chromatograph.