High-flux low-energy-consumption tetracycloheptane continuous flow synthesis device and method

A tetracycloheptane, low energy consumption technology, applied in the field of tetracycloheptane continuous flow synthesis device, can solve the problems of low power, low light intensity, small heat release, rapid temperature rise, etc., shorten the reaction time, reduce the unit energy The effect of consumption and increase of surface area

Pending Publication Date: 2022-07-12
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Existing ultraviolet photochemical reaction devices use low-pressure or medium-pressure mercury lamps as light sources. This kind of mercury lamp has defects such as high energy consumption, rapid temperature rise, and the need for external water-cooling equipment. In contrast, ultraviolet LED strips have small heat release, Light monochromaticity and other advantages, but its power and light intensity are low, it is difficult to meet the needs of high-throughput photochemical synthesis

Method used

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  • High-flux low-energy-consumption tetracycloheptane continuous flow synthesis device and method
  • High-flux low-energy-consumption tetracycloheptane continuous flow synthesis device and method
  • High-flux low-energy-consumption tetracycloheptane continuous flow synthesis device and method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] like figure 1 , figure 2 As shown, the tetracycloheptane continuous flow synthesis device of the present embodiment includes a serpentine arrangement capillary continuous flow reactor 2 formed by a serpentine arrangement of stacked capillaries 3, and a ring-shaped arrangement of stacked capillaries 5 formed by an annular arrangement. The capillary continuous flow reactor 4 is arranged, the upper part of the capillary continuous flow reactor 2 and the annular arrangement capillary continuous flow reactor 4 are provided with a high-power panel type UV-LED lamp 1, and the lower part is provided with a reflector 6.

[0032] The capillary continuous flow reactor is made of PFA, the inner diameter is 1mm, and the length is 16m.

[0033] The channels of the capillary continuous flow reactor are arranged in an annular shape and are arranged in a stacked manner, and the number of stacked layers is 2 layers.

[0034] The high-power panel UV-LED lamp emits ultraviolet light wit...

Embodiment 2

[0037] like figure 1 As shown, this embodiment includes a high-power panel UV-LED lamp 1 and a serpentine-arranged capillary continuous flow reactor 2 .

[0038] The capillary continuous flow reactor is made of quartz glass, the inner diameter is 2mm, the wall thickness is 1mm, and the length is 2.26m.

[0039] The capillary continuous flow reactor channels are arranged in a serpentine pattern and placed in a single layer.

[0040] The high-power panel UV-LED lamp emits ultraviolet light with a characteristic wavelength of 365nm and a radiation window of 1200cm 2 , the input power is 500W, and the optical power is 165mW / cm 2 .

[0041] In this example, the above-mentioned system is used to carry out the photosensitized cycloaddition reaction of norbornadiene, the photosensitizer used is tetraethyl Michler's ketone, the mass fraction of the photosensitizer is 0.55%, there is no solvent, and the flow rate of the liquid phase in the capillary is 0.18ml / min, the reaction resi...

Embodiment 3

[0043] This embodiment includes: a high-power panel UV-LED lamp 1 , a continuous flow reactor 2 arranged in a serpentine shape, a laminated capillary tube 3 arranged in a serpentine shape, and a reflector 6 .

[0044] The capillary continuous flow reactor is made of quartz glass, the inner diameter is 2mm, the wall thickness is 1mm, and the length is 22.6m.

[0045] The channels of the capillary continuous flow reactor are arranged in a serpentine shape and are arranged in a stacked manner, and the number of stacked layers is 2.

[0046] The high-power panel UV-LED lamp emits ultraviolet light with a characteristic wavelength of 365nm and a radiation window of 1200cm 2 , the input power is 500W, and the optical power is 165mW / cm 2 .

[0047] A total reflector is placed under the high-power panel UV-LED lamp, and a capillary continuous flow reactor is placed between the high-power panel UV-LED lamp and the reflector.

[0048] In this example, the above-mentioned system is us...

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Abstract

A high-flux low-energy-consumption tetracycloheptane continuous flow synthesis device comprises a fluid conveying device used for conveying reaction raw materials; and the capillary continuous flow reactor is used for reacting the raw materials to generate tetracycloheptane and is arranged between the high-power panel type UV-LED lamp and the reflective mirror. According to the method, tetraethyl michler ketone is used as a photosensitizer, tetraethyl michler ketone is dissolved in norbornadiene to form homogeneous reaction liquid, the homogeneous reaction liquid is irradiated by an ultraviolet light source to react in a capillary continuous flow reactor, and a reaction product is subjected to rotary evaporation separation to obtain tetracycloheptane.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a continuous flow synthesis device and method of tetracycloheptane with high flux and low energy consumption. Background technique [0002] Tetracycloheptane is the product of the photo-sensitized cycloaddition reaction of norbornadiene under ultraviolet light. It has a high-tension cage structure and a large density. It is an efficient rocket propellant and missile attitude control agent, and can be used as a Additives improve the energy density of hydrocarbon fuels and are good solar energy storage materials, which have received extensive attention in the field of solar energy storage. [0003] Traditional batch-pot photoreactors have many limitations, especially in terms of uneven distribution of light intensity, difficulty in amplification, and low utilization efficiency of light energy. Compared with the kettle type photoreactor, the photochemical microreactor has...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/12C07C5/31C07C13/68
CPCB01J19/123C07C5/31C07C2603/86C07C13/68Y02P20/10
Inventor 苏远海王昱翰商敏静
Owner SHANGHAI JIAO TONG UNIV
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