LED LIGHT SOURCE PHOTOCATALYTIC TUBULAR REACTOR AND APPLICATION THEREOF

Abstract

Disclosed is an LED light source photocatalytic tubular reactor and application thereof. The LED light source photocatalytic tubular reactor comprises an LED light source, a temperature control chamber and a transparent reaction pipeline; the transparent reaction pipeline is located in the temperature control chamber; at least one side of the temperature control chamber is a light-transmitting plate; the LED light source provides a light source for the transparent reaction pipeline through the light-transmitting plate; and the transparent reaction pipeline has a diameter-to-length ratio of the inner diameter to the length of 0-0.1, but not 0. The LED light source continuous photocatalytic tubular reactor of the present disclosure can eliminate the scaling up effect, increase the yield and allow continuous production with an advantage of easy to use and low cost. The tubular reaction device of the present disclosure can also realize automatic control, which can effectively reduce personnel costs and improve production safety.

Claims

1. An LED light source photocatalytic tubular reactor, comprises: an LED light source, a temperature control chamber and a transparent reaction pipeline; the transparent reaction pipeline is located in the temperature control chamber; at least one side of the temperature control chamber is a light-transmitting plate; the LED light source provides a light source for the transparent reaction pipeline through the light-transmitting plate; the transparent reaction pipeline has a diameter-to-length ratio of the inner diameter to the length of 0-0.1, but not 0.

2. The LED light source photocatalytic tubular reactor according to claim 1, wherein the LED light source is an LED light source with variable power and wavelength; or, the LED light source is a modular light source group; or, the LED light source is at a distance of 0-5 cm from the light-transmitting plate; or, the LED light source as a whole is designed as an explosion-proof LED light source device.

3. The LED light source photocatalytic tubular reactor according to claim 1, wherein the temperature control chamber are equipped with pressure sensors at its inlet and outlet; or, the light-transmitting plate is a quartz plate or a glass plate; or, the light-transmitting plate has a thickness of 0-50 mm; or, except the part of the light-transmitting plate, the other parts of the temperature control chamber are made from stainless steel or polytetrafluoroethylene; or, the temperature control pipeline of the temperature control chamber has an inner diameter of 1-50 mm; or, the temperature control chamber has a temperature of −50° C.-100° C.; or, the temperature control medium in the temperature control chamber is ethylene glycol or water.

4. The LED light source photocatalytic tubular reactor according to claim 1, wherein a temperature control medium is circulated in the temperature control chamber, or a temperature control pipeline is separately provided in the temperature control chamber; or, the temperature control chamber is provided with an external flow temperature control system; or, the temperature control chamber is in the shape of a cube or a cylinder; or, a bracket is provided in the temperature control chamber for coiling the transparent reaction pipeline.

5. The LED light source photocatalytic tubular reactor according to claim 4, wherein the transparent reaction pipeline is coiled to form a mosquito coil shape, an S shape or a snake shape; when a temperature control pipeline is separately provided in the temperature control chamber, the temperature control pipeline and the transparent reaction pipeline are spirally arranged and coiled; both sides of the temperature control chamber are provided with light-transmitting plates; and the LED light source is located on both sides of the outside of the temperature control chamber; or, a plurality of the temperature control chambers are connected in parallel with the external temperature control chambers.

6. The LED light source photocatalytic tubular reactor according to claim 1, wherein the transparent reaction pipeline has a circular shape; or, the transparent reaction pipeline is made from tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer PFA or perfluoroethylene propylene copolymer FEP; or, the transparent reaction pipeline has a diameter-to-length ratio of the inner diameter to the length of 0-0.0005, but not 0; or, the transparent reaction pipeline has an inner diameter of 0-20 mm, but not 0; or, the transparent reaction pipeline is a plug flow tubular reactor; or, when in use, the transparent reaction pipeline contains liquid, which has a linear velocity of no more than 3 m/s.

7. The LED light source photocatalytic tubular reactor according to claim 1, wherein, a combination of the LED light source photocatalytic tubular reactor in series or in parallel is obtained by connecting interfaces, which are made from tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer PFA, stainless steel or Hastelloy.

8. A photocatalytic reaction device, wherein the photocatalytic reaction device comprises the LED light source photocatalytic tubular reactor according to claim 1.

9. The photocatalytic reaction device according to claim 8, wherein the photocatalytic reaction device comprises a raw material tank, a feed pump, a back pressure valve and a product storage tank connected in sequence; or, the photocatalytic reaction device further comprises a plurality of thermocouples, for example, three thermocouples; or, the photocatalytic reaction device further comprises a plurality of pressure sensors.

10. A method for preparing a trifluoromethyl compound or a brominated compound by using the photocatalytic reaction device according to claim 8, wherein, the method comprises the following steps: S1. continuously supplying reaction raw materials to the transparent reaction pipeline in the photocatalytic reaction device according to claim 8; S2. carrying out photocatalysis to continuously prepare a trifluoromethyl compound or a brominated compound by controlling the reaction temperature using the temperature control chamber under the illumination of the LED light source.

11. A method for preparing a trifluoromethyl compound or a brominated compound by using the photocatalytic reaction device according to claim 9, wherein, the method comprises the following steps: S1. continuously supplying reaction raw materials to the transparent reaction pipeline in the photocatalytic reaction device according to claim 9; S2. carrying out photocatalysis to continuously prepare a trifluoromethyl compound or a brominated compound by controlling the reaction temperature using the temperature control chamber under the illumination of the LED light source.

12. The LED light source photocatalytic tubular reactor according to claim 2, wherein the LED light source is at a distance of 0-5 mm from the light-transmitting plate.

13. The LED light source photocatalytic tubular reactor according to claim 3, wherein the light-transmitting plate has a thickness of 0-20 mm; or, the temperature control pipeline of the temperature control chamber has an inner diameter of 2-20 mm.

14. The LED light source photocatalytic tubular reactor according to claim 13, wherein the light-transmitting plate has a thickness of 2-20 mm.

15. The LED light source photocatalytic tubular reactor according to claim 6, wherein the transparent reaction pipeline has an inner diameter of 0-5 mm, but not 0.

16. The photocatalytic reaction device according to claim 9, wherein the thermocouples are located in a pipeline connecting the transparent reaction pipeline and the back pressure valve, or, in an external flow temperature control system; or, the pressure sensor is located in a pipeline connecting the feed pump and the transparent reaction pipeline, or in the external flow temperature control system.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0058] FIG. 1 shows a schematic diagram of the structure of the LED light source photocatalytic tubular reactor in Example 1.

[0059] FIG. 2 shows an exemplary flow chart of the photocatalytic reaction device in Example 1.

DESCRIPTION OF REFERENCE SIGNS

[0060] Temperature control chamber 1 [0061] Transparent reaction pipeline 2 [0062] LED light source 3 [0063] Integrated sealed box 4 [0064] Thermocouple 5 [0065] Transparent quartz plate 6 [0066] External flow temperature control system 7 [0067] Raw material tank 8 [0068] Feed pump 9 [0069] LED light source photocatalytic tubular reactor 10 [0070] Back pressure valve 11 [0071] Product storage tank 12

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT

[0072] The following examples further illustrate the present disclosure, but the present disclosure is not limited thereto. Unless specified otherwise, the experimental methods in the following examples are selected according to conventional methods and conditions, or according to the commodity specification.

Example 1

[0073] In Example 1, the LED light source photocatalytic tubular reactor 10 comprises an LED light source 3, a temperature control chamber 1 and a transparent reaction pipeline 2 (as shown in FIG. 1).

[0074] The temperature control chamber 1 has a cylindrical shape. Both sides of the temperature control chamber 1 are provided with transparent quartz plates 6. The transparent quartz plate 6 has a thickness of 10 mm Except the part of the transparent quartz plate 6, the other parts of the temperature control chamber 1 are made of stainless steel. The temperature control chamber 1 is provided with an external flow temperature control system 7. The temperature control pipeline of the temperature control chamber 1 has an inner diameter of 10 mm Both the inlet and the outlet of the temperature control chamber 1 are equipped with pressure sensors to monitor the pressure in real time. The temperature of the temperature control chamber 1 is −50° C.-100° C. The temperature control medium in the temperature control chamber 1 is ethylene glycol and water.

[0075] The LED light source 3 is an LED modular light source group with variable power and wavelength, which can change the wavelength and power of the LED by software controlling as required. The LED light source 3 as a whole is designed as an explosion-proof LED light source device, which is commercially available. The LED light source 3 is located on both sides of the outside of the temperature control chamber 1, and provides a light source for the transparent reaction pipeline 2 through the transparent quartz plate 6. The LED light source 3 and the light-transmitting plate has a distance of 1 mm.

[0076] The transparent reaction pipeline 2 is a plug flow tubular reactor. The transparent reaction pipeline 2 has a circular shape, which is commercially available. The transparent reaction pipeline 2 is made from tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer PFA. When in use, the liquid in the transparent reaction pipeline 2 has a linear velocity of no more than 3 m/s.

[0077] The transparent reaction pipeline 2 is located in the temperature control chamber 1. A bracket is provided in the temperature control chamber 1 for coiling the transparent reaction pipeline 2. The transparent reaction pipeline 2 is coiled to form a shape of mosquito coil.

[0078] The inner diameter to the length of the transparent reaction pipeline 2 has a diameter-to-length ratio of the inner diameter to the length of 0.0005. The transparent reaction pipeline 2 has an inner diameter of 5 mm. The height and width of the LED modular light source group correspond to the area occupied by the transparent reaction pipeline 2 which is coiled, thereby providing a uniform light source for the transparent reaction pipeline 2.

[0079] The photocatalytic reaction device in Example 1 comprises the aforementioned LED light source photocatalytic tubular reactor 10 (as shown in FIG. 2).

[0080] The photocatalytic reaction device also includes a raw material tank 8, a feed pump 9, a back pressure valve 11 and a product storage tank 12, which are connected in sequence.

[0081] The photocatalytic reaction device also comprises an integrated sealed box 4, which contains a temperature control chamber 1, an LED light source 3, and a transparent reaction pipeline 2.

[0082] The photocatalytic reaction device further comprises three thermocouples 5, which are located in the pipeline connecting the transparent reaction pipeline 2 and the back pressure valve 11, and in the external flow temperature control system 7.

[0083] The photocatalytic reaction device further comprises a plurality of pressure sensors, which are not only located at the inlet and outlet of the temperature control chamber 1, but also located in the pipeline connecting the feed pump 9 and the transparent reaction pipeline 2.

[0084] In Example 1, when using the aforementioned photocatalytic reaction device to prepare a trifluoromethyl compound or a brominated compound, it comprises the following steps:

[0085] S1. continuously supplying the reaction raw materials to the transparent reaction pipeline 2 in the aforementioned LED light source photocatalytic tubular reactor 10;

[0086] S2. carrying out photocatalysis to continuously prepare a trifluoromethyl compound or a brominated compound by controlling the reaction temperature using the temperature control chamber 1 under the illumination of the LED light source 3.

[0087] The reaction raw materials are the reaction substrate, trifluoromethylation reagent and catalyst; the reaction raw materials were all stored in the raw material tank 8, and the reaction raw materials were pumped into the transparent reaction pipeline 2 through the feed pump 9; after that, under the illumination of the LED light source 3, with the reaction temperature controlled by the temperature control chamber 1, the corresponding trifluoromethyl compounds were continuously prepared by photocatalysis, and the obtained product flowed into the product storage tank 12 through the back pressure valve 11, thereby achieving a convenient continuous production.

EXAMPLE OF EFFECTS

[0088] The scaling up effect can be successfully eliminated by the device of Example 1 and the trifluoromethylation was fed at a flow rate of 200 L/h, and the reaction is complete.

[0089] If the reaction scale is enlarged by a factor of 2, it is only necessary to increase the flow rate by 2 times, and connect the LED light source photocatalytic tubular reactor 10 as described in Example 1 in series or in parallel (connected via the interface made from tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer PFA), with a conversion rate of 100%, and a yield of over 80%; currently, the bromination is realized with 5000 L feed per day, and the yield is over 90%.