Patent ID: 12186727

DESCRIPTION OF REFERENCE SIGNS

Temperature control chamber1Transparent reaction pipeline2LED light source3Integrated sealed box4Thermocouple5Transparent quartz plate6External flow temperature control system7Raw material tank8Feed pump9LED light source photocatalytic tubular reactor10Back pressure valve11Product storage tank12

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT

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

In Example 1, the LED light source photocatalytic tubular reactor10comprises an LED light source3, a temperature control chamber1and a transparent reaction pipeline2(as shown inFIG.1).

The temperature control chamber1has a cylindrical shape. Both sides of the temperature control chamber1are provided with transparent quartz plates6. The transparent quartz plate6has a thickness of 10 mm Except the part of the transparent quartz plate6, the other parts of the temperature control chamber1are made of stainless steel. The temperature control chamber1is provided with an external flow temperature control system7. The temperature control pipeline of the temperature control chamber1has an inner diameter of 10 mm Both the inlet and the outlet of the temperature control chamber1are equipped with pressure sensors to monitor the pressure in real time. The temperature of the temperature control chamber1is −50° C.-100° C. The temperature control medium in the temperature control chamber1is ethylene glycol and water.

The LED light source3is 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 source3as a whole is designed as an explosion-proof LED light source device, which is commercially available. The LED light source3is located on both sides of the outside of the temperature control chamber1, and provides a light source for the transparent reaction pipeline2through the transparent quartz plate6. The LED light source3and the light-transmitting plate has a distance of 1 mm.

The transparent reaction pipeline2is a plug flow tubular reactor. The transparent reaction pipeline2has a circular shape, which is commercially available. The transparent reaction pipeline2is made from tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer PFA. When in use, the liquid in the transparent reaction pipeline2has a linear velocity of no more than 3 m/s.

The transparent reaction pipeline2is located in the temperature control chamber1. A bracket is provided in the temperature control chamber1for coiling the transparent reaction pipeline2. The transparent reaction pipeline2is coiled to form a shape of mosquito coil.

The inner diameter to the length of the transparent reaction pipeline2has a diameter-to-length ratio of the inner diameter to the length of 0.0005. The transparent reaction pipeline2has 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 pipeline2which is coiled, thereby providing a uniform light source for the transparent reaction pipeline2.

The photocatalytic reaction device in Example 1 comprises the aforementioned LED light source photocatalytic tubular reactor10(as shown inFIG.2).

The photocatalytic reaction device also includes a raw material tank8, a feed pump9, a back pressure valve11and a product storage tank12, which are connected in sequence.

The photocatalytic reaction device also comprises an integrated sealed box4, which contains a temperature control chamber1, an LED light source3, and a transparent reaction pipeline2.

The photocatalytic reaction device further comprises three thermocouples5, which are located in the pipeline connecting the transparent reaction pipeline2and the back pressure valve11, and in the external flow temperature control system7.

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 chamber1, but also located in the pipeline connecting the feed pump9and the transparent reaction pipeline2.

In Example 1, when using the aforementioned photocatalytic reaction device to prepare a trifluoromethyl compound or a brominated compound, it comprises the following steps:S1. continuously supplying the reaction raw materials to the transparent reaction pipeline2in the aforementioned LED light source photocatalytic tubular reactor10;S2. carrying out photocatalysis to continuously prepare a trifluoromethyl compound or a brominated compound by controlling the reaction temperature using the temperature control chamber1under the illumination of the LED light source3.

The reaction raw materials are the reaction substrate, trifluoromethylation reagent and catalyst; the reaction raw materials were all stored in the raw material tank8, and the reaction raw materials were pumped into the transparent reaction pipeline2through the feed pump9; after that, under the illumination of the LED light source3, with the reaction temperature controlled by the temperature control chamber1, the corresponding trifluoromethyl compounds were continuously prepared by photocatalysis, and the obtained product flowed into the product storage tank12through the back pressure valve11, thereby achieving a convenient continuous production.

EXAMPLE OF EFFECTS

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.

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 reactor10as 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%.