Light reaction equipment adaptive to side illumination type light source

Abstract

The utility model relates to the technical field of photoreaction equipment, in particular to photoreaction equipment adaptive to a side illumination type light source. The photoreaction equipment comprises a photoreactor used for containing photoreaction liquid and providing a place for the photoreaction liquid to react; the light source is used for providing light energy required by reaction for the light reaction liquid, and the light source is a side illumination type light source; and the light beam shaper is positioned between the light source and the photoreactor and is used for adjusting the light beam of the irradiation light emitted by the light source, so that the size and the shape of the light spot reaching the photoreactor are matched with those of the reactor, and the spatial distribution of the light intensity irradiated to the photoreactor is uniform. The photoreaction equipment disclosed by the utility model can improve the utilization efficiency of photons, so that the photoreaction liquid in the reaction equipment is uniformly illuminated, and the yield of a target product is improved.

Description

Technical Field

[0001] The utility model relates to the technical field of photoreaction equipment, in particular to a photoreaction device adapted to a side-illuminated light source. Background Art

[0002] Photochemical reactions can achieve the synthesis of important chemical products with high selectivity and high yield under mild conditions, and are one of the important technologies for realizing green chemistry in the future. The light source and the photoreactor are indispensable core components in photochemical reactions, and the matching degree between the two determines the yield of the synthesis product in photochemical reactions. The current photoreactors are mainly of tubular or kettle type structures, and are mostly adapted to traditional strip or columnar light sources. For example, the light strip spirally wound outside the tubular reaction tube disclosed in the patent document CN218077848U, and the light source with multiple curved outer layers disclosed in the patent document CN209222092U.

[0003] With the development of optical technologies, more and more new types of light sources, such as side-illuminated parallel and quasi-parallel light sources like laser light sources and LED light sources, have emerged and are applied in photochemical reactions. When using a side-illuminated light source and a traditional tubular or kettle-type photoreactor for photochemical reactions, at the interface of the photoreactor, the incident light enters the photoreactor at any angle, and the light refraction and reflection losses are serious. On the one hand, it leads to light energy loss, reduces the utilization efficiency of photons, and affects the photochemical reaction efficiency; on the other hand, the light intensities received by the photoreaction liquid in different regions of the photoreactor vary greatly. The photoreaction liquid in some regions is over-illuminated, and the photoreaction liquid in some regions is not fully illuminated, resulting in uneven mass transfer and heat transfer in the whole reaction, an increase in side reactions, and a reduction in the product yield. Summary of the Utility Model

[0004] To improve the deficiencies of the prior art, the purpose of the present utility model is to provide a photoreaction device adapted to a side-illuminated light source, and the photoreaction device can improve at least one of the following problems: improve the utilization efficiency of photons, make the photoreaction liquid in the reaction device receive light evenly, and improve the yield of the target product.

[0005] In a first aspect, the present utility model provides a photoreaction device adapted to a side-illuminated light source, comprising:

[0006] A photoreactor for accommodating the photoreaction liquid and providing a place for the photoreaction liquid to react;

[0007] A light source for providing the light energy required for the reaction to the photoreaction liquid, and the light source is a side-illuminated light source;

[0008] A beam shaper located between the light source and the photoreactor, for adjusting the light spot of the irradiation light emitted by the light source, so that the size of the light spot reaching the photoreactor matches the reactor, and the light energy of each point of the light spot irradiating the photoreactor is the same.

[0009] According to an embodiment of the present utility model, the photoreactor includes a light receiving side for receiving light illumination, the light source is disposed opposite to the light receiving side, and the light beam emitted by the light source perpendicularly enters the light receiving side.

[0010] In some embodiments of the present utility model, the photoreactor has a flat plate structure, for example, a flat plate photoreactor in a flat shape.

[0011] In some embodiments of the present utility model, the thickness of the internal cavity (where the photoreaction liquid is accommodated) of the flat plate photoreactor is less than or equal to 10 cm, preferably the thickness of the internal cavity of the flat plate photoreactor is less than or equal to 8 cm.

[0012] In some embodiments of the present utility model, a reflective coating is applied to the non-light receiving surface of the photoreactor.

[0013] According to an embodiment of the present utility model, the light source includes a light source capable of emitting parallel light, quasi-parallel light or non-parallel light. Preferably, the light sources emitting parallel light and quasi-parallel light are laser light sources and LED light sources, and preferably the light source emitting non-parallel light is a spherical light source.

[0014] In some embodiments of the present utility model, the light source is one or more of a laser light source, an LED light source, a xenon light source, a mercury light source, a sodium light source, a halogen light source, etc.

[0015] In some embodiments of the present utility model, the beam shaper includes a spot homogenization component, and the spot homogenization component is used to make the light intensity of the spot entering the photoreactor equal everywhere.

[0016] In some embodiments of the present utility model, the beam shaper includes a beam expanding or contracting component, and the beam expanding or contracting component is used to timely adjust the shape and size of the beam cross-section (i.e., the spot) according to the light emission pattern of the light source and the size of the photoreactor.

[0017] In some embodiments of the present utility model, the beam shaper includes a beam collimation component, and the beam collimation component is used to make the light after beam expanding or contracting propagate along a parallel path.

[0018] In some embodiments of the present utility model, the beam shaper includes a beam universal turning component, and the beam universal turning component is used to change the beam irradiation direction according to the relative position between the light source and the photoreactor.

[0019] According to an embodiment of the present utility model, the beam shaper can achieve one or several functions of homogenizing the light intensity, changing the spot shape and size, and adjusting the optical path direction.

[0020] As a preferred embodiment of the present utility model, the beam shaper shapes a beam with a relatively narrow linewidth having a full width at half maximum less than or equal to 30 nanometers.

[0021] According to an embodiment of the present utility model, the reaction device further includes a perturbation type constant temperature circulation kettle, which is connected to the photoreactor. The photoreaction liquid can circulate between the photoreactor and the perturbation type constant temperature circulation kettle at a certain flow rate. Under the condition of cyclic perturbation, the photoreaction liquid is fully mixed and the light irradiation is uniform.

[0022] According to an embodiment of the present utility model, the reaction device further includes a raw material mixing constant temperature stirring kettle, which is used to provide the initial photoreaction liquid. The raw material mixing constant temperature stirring kettle is connected to the photoreactor and is used to introduce the initial photoreaction liquid into the photoreactor.

[0023] According to an embodiment of the present utility model, the reaction device further includes a product purification variable temperature kettle, which is connected to the perturbation type constant temperature circulation kettle and is used to receive the photoreaction product.

[0024] According to an embodiment of the present utility model, the photoreactor is a flat three-dimensional structure, and the plane with the largest area is placed perpendicular to the optical path.

[0025] According to an embodiment of the present utility model, the main body of the photoreactor is composed of two nested three-dimensional structures inside and outside. A hollow sandwich is formed between the two three-dimensional structures. The photoreaction liquid is placed in the inner cavity of the inner three-dimensional structure, and the sandwich is used to store the condensate (such as condensed water).

[0026] According to an embodiment of the present utility model, the photoreactor is made of a transparent material, such as quartz, borosilicate glass, etc.

[0027] According to an embodiment of the present utility model, a condenser is provided above the photoreactor.

[0028] As an example, a gas-fluid outlet is provided at the upper end of the condenser. The condenser is used to cool the gas flowing out of the top of the photoreactor, so that the solvent of the photoreaction liquid in it condenses and flows back into the photoreactor, reducing the solvent loss.

[0029] According to an embodiment of the present utility model, a photoreaction liquid flow outlet is provided at the top of the photoreactor. The photoreactor is connected to the perturbation type constant temperature circulation kettle through the photoreaction liquid flow outlet.

[0030] According to the implementation scheme of the utility model, a photoreaction liquid inlet one and a photoreaction liquid inlet two are arranged below the photoreactor. The reactor is connected to a raw material mixing constant temperature stirring kettle through the photoreaction liquid inlet one to introduce the initial photoreaction liquid into the photoreactor. The photoreactor is connected to a disturbance type constant temperature circulation kettle through the photoreaction liquid inlet two.

[0031] According to the implementation scheme of the utility model, the lower end of the photoreactor is equipped with a gas-liquid mixing valve and a gas inlet one, the photoreaction liquid flows in from the photoreaction liquid inlet one, the gas flows in from the gas inlet one, the photoreaction liquid and the gas are mixed at the gas-liquid mixing valve and then flow into the photoreactor, the inflowing gas forms uniform bubbles, which fully disturbs the photoreaction liquid, so that the photoreaction system can achieve efficient mass transfer and heat transfer, greatly improving the photoreaction efficiency.

[0032] According to the implementation scheme of the utility model, a paddle stirrer is arranged in the disturbance-type constant temperature circulation kettle to fully disturb the photoreaction liquid, mix it evenly, and improve the photoreaction yield.

[0033] According to the implementation scheme of the utility model, the top of the disturbance-type constant temperature circulation kettle is provided with a photoreaction liquid inlet and an inert gas inlet two, and the inert gas inlet two is used to blow inert gas into the disturbance-type constant temperature circulation kettle, so as to effectively inhibit the oxidation of photoreaction raw materials and photoreaction products and improve the yield of target products.

[0034] According to the implementation scheme of the utility model, the second photoreaction liquid inlet is connected to the photoreaction liquid outlet on the photoreactor, and the second inert gas inlet is used to introduce inert gas.

[0035] According to the implementation scheme of the utility model, a three-way valve two is arranged at the bottom of the disturbance type constant temperature circulation kettle, and a photoreaction liquid outflow outlet three and a photoreaction liquid outflow outlet four are arranged on the three-way valve two. The disturbance type constant temperature circulation kettle is connected with the photoreaction liquid outflow inlet two of the photoreactor through the photoreaction liquid outflow outlet three, and is used for circulating the photoreaction liquid in the photoreactor with the photoreaction liquid in the disturbance type constant temperature circulation kettle together with the photoreactor; the disturbance type constant temperature circulation kettle is connected with the purification variable temperature kettle through the photoreaction liquid outflow outlet four, and is used for conducting the reactants into the purification variable temperature kettle for purification.

[0036] According to the implementation scheme of the utility model, a delivery pump 2 and a flow meter 2 are arranged between the photoreaction liquid flow outlet 3 and the photoreaction liquid flow inlet 2 of the disturbance-type constant temperature circulation kettle. The photoreaction liquid flow outlet 3, the delivery pump 2, the flow meter 2 and the photoreaction liquid flow inlet 2 are connected through a pipeline to form a photoreaction liquid circulation system. The photoreaction liquid flow outlet 3 is connected to the photoreaction flow inlet 2 of the photoreactor through the delivery pump 2 and the flow meter 2.

[0037] According to the implementation scheme of the utility model, a sampling valve is provided at the bottom of the disturbance type constant temperature circulation kettle for obtaining the photoreaction liquid sample in the disturbance type constant temperature circulation kettle, and performing real-time monitoring of the photoreaction, thereby monitoring the progress of the photoreaction.

[0038] According to the implementation scheme of the utility model, the disturbance-type constant temperature circulation kettle is provided with a heat preservation layer 1 on the outside, and the heat preservation layer 1 is connected to the constant temperature system to control the temperature of the photoreaction system while suppressing the thermal isomerization reaction.

[0039] According to the implementation scheme of the utility model, the raw material mixing constant temperature stirring kettle is used to prepare the photoreactive material.

[0040] According to the implementation scheme of the utility model, the mixing constant temperature stirring kettle is provided with a feed port and an inert gas inlet, and a paddle stirrer is provided inside. The photoreaction material is added into the kettle through the feed port, and the paddle stirrer is used to fully mix and dissolve the photoreaction material.

[0041] According to the implementation scheme of the utility model, the bottom end of the raw material mixing constant temperature stirring kettle is provided with a second photoreaction liquid outflow port, which is connected to the first photoreaction liquid inflow port of the photoreactor through a delivery pump and a flow meter in sequence.

[0042] According to the implementation scheme of the utility model, an inert gas inlet one is provided at the top of the raw material mixing constant temperature stirring kettle, which is used to blow inert gas into the raw material mixing constant temperature stirring kettle to inhibit oxidation of the raw materials.

[0043] According to the implementation scheme of the utility model, a second insulation layer is arranged outside the raw material mixing constant temperature stirring kettle, and the second insulation layer is connected to the temperature control system.

[0044] According to the implementation scheme of the utility model, a light reaction liquid inlet five is arranged at the top of the product purification variable temperature kettle, and the light reaction liquid inlet five is connected to the light reaction liquid outlet four of the disturbance type constant temperature circulation kettle through a conveying pipeline.

[0045] According to the implementation scheme of the utility model, a third insulation layer is arranged outside the product purification temperature-variable kettle, and the third insulation layer is connected to the temperature control system.

[0046] In a second aspect, the utility model provides an application of the above-mentioned photoreaction device in a photochemical reaction.

[0047] In a third aspect, the present invention further provides a method for performing a photoreaction using the above-mentioned photoreaction device, comprising the following steps:

[0048] Firstly, the raw materials and the solvent are added into a raw material mixing constant temperature stirring kettle to mix and prepare a starting photoreaction liquid, and then the photoreaction liquid is introduced into a flat-plate photoreactor, and the light source is turned on to react.

[0049] According to the embodiments of the present utility model, in the reaction, the agitated thermostatic circulation kettle is connected to the flat-plate photoreactor. During the photoreaction process, the photoreaction liquid reciprocally circulates between the flat-plate photoreactor and the agitated thermostatic circulation kettle.

[0050] Beneficial effects

[0051] 1) The photoreaction device in the present utility model includes a side-illuminated light source, a beam shaper, and a photoreactor. The side-illuminated light source has the characteristic of single-sided light emission, and its emitted light converges on the beam shaper; the beam shaper is placed between the side-illuminated light source and the photoreactor to perform energy homogenization and shape adjustment on the parallel light, quasi-parallel light, or non-parallel light emitted by the side-illuminated light source, forming a light spot that perfectly matches the size and shape of the photoreactor; the photoreactor is a flat double-layer jacket, and the plane with the largest area is placed perpendicular to the emission direction of the shaped light beam.

[0052] 2) The photoreaction device in the present utility model further includes an agitated thermostatic circulation kettle. The agitated thermostatic circulation kettle is connected to the photoreactor, and the photoreaction liquid circulates between the photoreactor and the agitated thermostatic circulation kettle, enabling the photoreaction liquid to perform a homogeneous reaction under circulation conditions.

[0053] 3) By adapting the light spot to the photoreactor, the present utility model uses the beam shaper to converge or diverge the light beam of the side-illuminated light source, homogenize the energy, and shape the light spot, making the light spot perfectly match the photoreactor, solving the problem of mismatch between the new side-illuminated light source and the traditional tubular and kettle-type photoreactors in the prior art, and greatly improving the utilization efficiency of photons; at the same time, by using the photoreactor and the agitated thermostatic circulation kettle, the photoreaction liquid is circulated, the photoreaction is fully agitated, and the mass transfer and heat transfer of the photoreaction are made uniform and efficient, achieving the purpose of increasing the yield of the target product. Description of the drawings

[0054] Figure 1 It is a schematic structural diagram of the photoreactor in the present utility model;

[0055] Figure 2 It is a schematic structural diagram of the photoreaction device in the present utility model.

[0056] In the figure: 1. Flat-plate photoreactor; 2. Side-illuminating light source; 3. Beam shaper; 4. Stirring type constant-temperature circulation kettle; 5. Raw material mixing constant-temperature stirring kettle; 6. Product purification variable-temperature kettle; 10. Condenser; 11. Delivery pump I; 12. Flowmeter I; 13. Delivery pump II; 14. Flowmeter II; 15. Gas-liquid mixing valve; 16. Interlayer; 17. Thermal insulation layer I; 18. Thermal insulation layer II; 19. Thermal insulation layer III; 20. Blade stirrer I; 21. Blade stirrer II; 22. Three-way valve I; 23. Three-way valve II; 101. Photoreaction liquid inlet I; 102. Photoreaction liquid outlet I; 103. Condensate water inlet; 104. Condensate water outlet; 105. Gas inlet; 106. Gas outlet; 107. Photoreaction inlet II; 108. Photoreaction liquid outlet II; 109. Feeding port; 110. Inert gas inlet I; 111. Photoreaction liquid outlet III; 112. Photoreaction liquid outlet IV; 113. Photoreaction liquid inlet III; 114. Inert gas inlet II; 115. Product outlet; 116. Photoreaction liquid inlet V. Detailed implementation mode

[0057] The following will further elaborate on the equipment, methods, and applications of the present utility model in combination with specific embodiments. It should be understood that the following embodiments are only for illustrative explanation of the present utility model and should not be construed as limiting the protection scope of the present utility model. All technologies implemented based on the above content of the present utility model are covered within the scope intended to be protected by the present utility model.

[0058] Unless otherwise specified, the raw materials and reagents used in the following embodiments are all commercially available products or can be prepared by known methods.

[0059] Embodiment 1

[0060] A photoreaction device adapted to a side-illuminating light source provided in this embodiment, as Figure 1 - Figure 2 shown, includes a flat-plate photoreactor 1, a side-illuminating light source 2, a beam shaper 3, a stirring type constant-temperature circulation kettle 4, a raw material mixing constant-temperature stirring kettle 5, and a product purification variable-temperature kettle 6.

[0061] The flat-plate photoreactor 1 is used to accommodate the photoreaction liquid and provide a place for the photoreaction liquid to react; the side-illuminating light source 2 is arranged outside the flat-plate photoreactor 1 and is used to provide the irradiation light required for the reaction to the flat-plate photoreactor 1.

[0062] The beam shaper 3 is located between the side-illuminating light source 2 and the flat-plate photoreactor 1 and is used to converge or diffuse and shape the light beam emitted by the side-illuminating light source 2 so that the spot size received by the light-receiving side surface of the flat-plate photoreactor 1 is matched and the energy is uniform.

[0063] The perturbation type constant temperature circulation kettle 4 is connected to the flat plate type photoreactor 1, and the photoreaction liquid can circulate between the flat plate type photoreactor 1 and the perturbation type constant temperature circulation kettle 4, so that the photoreaction liquid undergoes a homogeneous reaction under the circulation condition.

[0064] The raw material mixing constant temperature stirring kettle 5 is used to provide the starting photoreaction liquid. The raw material mixing constant temperature stirring kettle 5 is connected to the flat plate type photoreactor 1 and is used to introduce the starting photoreaction liquid into the flat plate type photoreactor 1.

[0065] The product purification variable temperature kettle 6 is connected to the perturbation type constant temperature circulation kettle 4 and is used to receive the photoreaction product.

[0066] Specifically, the irradiation light emitted by the side illumination type light source 2 is subjected to energy homogenization and shape adjustment by the beam shaper 3 to form a light spot that completely matches the size and shape of the light receiving side surface of the flat plate type photoreactor 1 and has uniform energy at each point. The light spot finally irradiates on the light receiving side surface of the flat plate type photoreactor 1 to provide light energy for the photochemical reaction. Among them, the size, structure, and position of the light receiving side surface are set according to actual needs. For example, it can be the side surface opposite to the side illumination type light source 2, and this side surface is set as a horizontal structure; in actual use, this side surface can also be other structures. When it is other structures, the light spot energy at different positions on the side surface after the beam shaper 3 adjusts is the same.

[0067] Among them, the selection of the side illumination type light source 2 is not restricted and can be a parallel light source, a quasi-parallel light source, or a non-parallel light source. For example, it can be an LED light source, a laser light source, etc. It is a laser that emits parallel light or a laser light source, an LED light source that emits quasi-parallel light; the non-parallel light source is selected from spherical light sources. For example, the non-parallel light source can be at least one of a xenon lamp light source, a mercury lamp light source, a sodium lamp light source, and a halogen lamp light source; when it is a non-parallel light source, a condensing component can be arranged between the side illumination type light source 2 and the beam shaper 3, and the condensing component is used to adjust the non-parallel light path so that it propagates along a parallel or quasi-parallel path.

[0068] A condenser 10 is equipped above the flat plate type photoreactor 1. An air-fluid outlet 106 is arranged at the upper end of the condenser 10. The condenser 10 cools the gas flowing out from the top of the flat plate type photoreactor 1, so that the photoreaction solvent in it condenses and then flows back into the flat plate type photoreactor 1 to reduce solvent loss; a photoreaction liquid flow outlet 102 is arranged at the top of the flat plate type photoreactor 1, and the flat plate type photoreactor 1 is connected to the perturbation type constant temperature circulation kettle 4 through the photoreaction liquid flow outlet 102.

[0069] A photoreaction liquid inlet 101 and a photoreaction liquid inlet 2 107 are arranged below the flat-plate photoreactor 1. The flat-plate photoreactor 1 is connected to the raw material mixing constant temperature stirring kettle 5 through the photoreaction liquid inlet 101, which is used to introduce the initial photoreaction liquid into the flat-plate photoreactor 1. The flat-plate photoreactor 1 is connected to the disturbance type constant temperature circulation kettle 4 through the photoreaction liquid inlet 2 107.

[0070] The lower end of the flat-plate photoreactor 1 is equipped with a gas-liquid mixing valve 15, a gas inlet 105, and a three-way valve 22. The photoreaction liquid flows in from the photoreaction liquid inlet 101, and the gas flows in from the gas inlet 105. The photoreaction liquid and the gas are mixed at the gas-liquid mixing valve 15 and then flow into the flat-plate photoreactor 1. The inflowing gas forms uniform and fine bubbles, which fully disturbs the photoreaction liquid, so that the photoreaction has efficient mass and heat transfer, and the photoreaction efficiency is greatly improved.

[0071] The flat-plate photoreactor 1 is composed of two transparent three-dimensional structures stacked inside and outside, and a hollow interlayer 16 is formed between the two three-dimensional structures. A condensed water outlet 104 is provided at the upper part of the interlayer 16, and a condensed water inlet 103 is provided at the lower part. Condensed water is introduced into the interlayer 16 through the condensed water inlet 103 and discharged through the condensed water outlet 104. The temperature of the photoreaction system in the flat-plate photoreactor 1 is controlled by adjusting the temperature of the condensed water, thereby effectively suppressing the thermal isomerization side reaction and improving the photoreaction yield.

[0072] The disturbance type constant temperature circulation kettle 4 in this embodiment is provided with a paddle stirrer 20 to fully disturb the photoreaction liquid, mix it evenly, and improve the photoreaction yield. The top of the disturbance type constant temperature circulation kettle 4 is provided with a photoreaction liquid inlet 113 and an inert gas inlet 114. The inert gas inlet 114 is used to blow inert gas into the disturbance type constant temperature circulation kettle 4 to effectively inhibit the oxidation of the photoreaction raw materials and the photoreaction products and improve the yield of the target product.

[0073] Among them, the photoreaction liquid inlet 113 is connected with the photoreaction liquid outlet 102 on the flat-plate photoreactor 1, and the inert gas inlet 2 114 is used to introduce inert gas; a three-way valve 2 23 is provided at the bottom of the disturbance type constant temperature circulation kettle 4, and a photoreaction liquid outlet 3 111 and a photoreaction liquid outlet 4 112 are provided on the three-way valve 23, wherein the disturbance type constant temperature circulation kettle 4 is connected with the photoreaction liquid inlet 2 107 of the flat-plate photoreactor 1 through the photoreaction liquid outlet 3 111, which is used to guide the incompletely reacted photoreaction liquid back to the flat-plate photoreactor 1 for further reaction; the disturbance type constant temperature circulation kettle 4 is connected with the purification variable temperature kettle 6 through the photoreaction liquid outlet 4 112, which is used to guide the reactants into the purification variable temperature kettle 6 for purification.

[0074] A transfer pump II 13 and a flowmeter II 14 are arranged between the photoreaction liquid flow outlet III 111 and the photoreaction liquid flow inlet II 107 of the perturbation type constant temperature circulation kettle 4. They are connected by pipelines to form a photoreaction liquid circulation system. The photoreaction liquid flow outlet III 111 is connected to the photoreaction flow inlet 107 II of the flat plate photoreactor 1 through the transfer pump II 13 and the flowmeter II 14. When the volumes of the photoreaction liquid in the flat plate photoreactor 1 and the perturbation type constant temperature circulation kettle 4 reach the requirements, the three-way valve 23 for the photoreaction liquid flow outlet III 111 is opened, and the three-way valve 22 for the photoreaction liquid flow inlet II 107 is opened. At this time, the photoreaction liquid only circulates between the flat plate photoreactor 1 and the perturbation type constant temperature circulation kettle 4.

[0075] The photoreaction liquid undergoes a light reaction in the flat plate photoreactor 1 at a certain flow rate, then flows into the perturbation type constant temperature circulation kettle 4. After being fully mixed, it flows back into the flat plate photoreactor 1. This cycle repeats until the photoreaction reaches an ideal yield. For example, a sampling port (not shown in the figure) is provided at the bottom of the perturbation type constant temperature circulation kettle 4. Sampling is carried out through this sampling port to monitor the reaction in real time.

[0076] An insulation layer I 17 is provided outside the perturbation type constant temperature circulation kettle 4 and is connected to the constant temperature system to control the temperature of the photoreaction system while suppressing thermal isomerization reactions.

[0077] In this embodiment, the raw material mixing constant temperature stirring kettle 5 is used to prepare the photoreaction materials. A feeding port 109 and an inert gas flow inlet I 110 are provided on the raw material mixing constant temperature stirring kettle 5. A paddle stirrer I 20 is arranged inside. The photoreaction materials are added into the kettle through the feeding port 109, and the paddle stirrer I 20 is used to fully mix and dissolve the photoreaction materials. A photoreaction liquid flow outlet II 108 is provided at the bottom end of the raw material mixing constant temperature stirring kettle 5. The photoreaction liquid flow outlet II 108 is connected in series with the photoreaction liquid flow inlet I 101 of the flat plate photoreactor 1 through a transfer pump I 11 and a flowmeter I 12. At the initial stage of the photoreaction, the photoreaction liquid flow inlet I 101 of the three-way valve I 22 and the photoreaction flow outlet 111 of the three-way valve II 23 are opened. At this time, the photoreaction materials are pumped into the flat plate photoreactor 1 and the perturbation type constant temperature circulation kettle 4 at a certain speed through the transfer pump I 11.

[0078] An inert gas flow inlet I 110 is provided at the top of the raw material mixing constant temperature stirring kettle 5. Inert gas is introduced into the raw material mixing constant temperature stirring kettle 5 through this inert gas flow inlet to inhibit the oxidation of the raw materials. An insulation layer II 18 is provided outside the raw material mixing constant temperature stirring kettle 5 and is connected to the temperature control system to set the corresponding dissolution temperature of the materials and increase the solubility of the materials.

[0079] The product purification variable-temperature kettle 6 is used for enriching and purifying the photochemical reaction products. At the top of the product purification variable-temperature kettle 6, there is a fifth photochemical reaction liquid inlet 116. The fifth photochemical reaction liquid inlet 116 is connected to the fourth photochemical reaction liquid outlet 112 of the agitated constant-temperature circulation kettle 4 through a conveying pipeline. When the conversion rate of the photochemical reaction raw materials and the yield of the products reach an ideal state, the fourth photochemical reaction liquid outlet 112 of the agitated constant-temperature circulation kettle 4 is opened, and the photochemical reaction products flow into the product purification variable-temperature kettle 6 through the fifth photochemical reaction liquid inlet 116. At this time, the first photochemical reaction liquid inlet 101 of the flat-plate photoreactor 1 is opened, and the new photochemical reaction raw materials enter the flat-plate photoreactor 1 from the raw material mixing constant-temperature stirring kettle 5 through the second photochemical reaction liquid outlet 108 and the conveying pipe, thus realizing continuous production; at the lower end of the product purification variable-temperature kettle 6, there is a product outlet 115, and the products are removed from the photochemical reaction equipment through the product outlet 115.

[0080] A third heat-insulating layer 19 is arranged outside the product purification variable-temperature kettle 6. The third heat-insulating layer 19 is connected to the temperature control system. Setting an appropriate constant temperature or programmed heating and programmed cooling is beneficial to the precipitation of the products.

[0081] Example 2

[0082] This example provides a method for carrying out a photochemical reaction using the above-mentioned photochemical reaction equipment:

[0083] In the first step, an inert gas is introduced into the raw material mixing constant-temperature stirring kettle 5 through the first inert gas inlet 110 at the top of the raw material mixing constant-temperature stirring kettle 5. After the gas replacement is complete, the reaction solvent and the materials are put into the raw material mixing constant-temperature stirring kettle 5 through the feeding port 109, and the paddle stirrer 21 and the constant-temperature system are turned on to dissolve the materials to prepare the photochemical reaction liquid.

[0084] Step 2: After the materials are completely dissolved, open the second photoreaction liquid outlet 108 at the bottom of the raw material mixing and constant temperature stirring kettle 5, the first photoreaction liquid inlet 101, the first photoreaction liquid outlet 102 of the flat photoreactor 1, the gas inlet 105, the condensed water circulation system, and the condenser 10. Start the first transfer pump 11 and the first flowmeter 12, and then open the third photoreaction liquid inlet 113 of the perturbed constant temperature circulation kettle 4 and start the heat preservation system of the perturbed constant temperature circulation kettle 4. The reaction materials flow into the flat photoreactor 1 under the action of the transfer pump. The flow rate of the materials can be controlled by adjusting the flow rate of the first transfer pump 11, thereby adjusting the residence time of the materials in the flat photoreactor 1. After all the first batch of materials are pumped into the flat photoreactor 1 and the perturbed constant temperature circulation kettle 4, turn off the first transfer pump 11 and the first flowmeter 12, close the second photoreaction liquid outlet 108 at the bottom of the raw material mixing and constant temperature stirring kettle 5 and the first photoreaction liquid inlet 101 of the flat photoreactor 1, and the raw material mixing and constant temperature stirring kettle 5 prepares for the second batch of batching. Open the second inert gas inlet and the third photoreaction liquid outlet 111 of the perturbed constant temperature circulation kettle 4, start the second transfer pump 11 and the second flowmeter 12, and make the photoreaction liquid circulate between the flat photoreactor 1 and the perturbed constant temperature circulation kettle 4 until the circulation is stable.

[0085] Step 3: Turn on the side-illuminated light source 2 and the beam shaper 3, and start the photoreaction. During the photoreaction, the photoreaction liquid circulates stably between the flat photoreactor 1 and the perturbed constant temperature circulation kettle 4.

[0086] Step 4: At the end of the photoreaction, close the third photoreaction liquid outlet 111 of the perturbed constant temperature circulation kettle 4, open the fourth photoreaction liquid outlet 112, and open the fifth photoreaction liquid inlet 116 of the product purification variable temperature kettle 6 to make the photoreaction liquid flow into the product purification variable temperature kettle 6.

[0087] Step 5: While performing the operation in Step 4, start the material conveying system of the raw material mixing and constant temperature stirring kettle 5, convey a new batch of materials into the flat photoreactor 1, and start a new round of photoreaction. Repeat this process to carry out continuous photoreaction.

[0088] Step 6: Take out the product from the product purification variable temperature kettle 6 and perform subsequent treatment.

[0089] Example 3 Preparation of vitamin D2 using the photoreaction equipment in Example 1

[0090] Step 1: Set the temperature of the raw material mixing and constant temperature stirring kettle to 25°C. After introducing nitrogen into the stirring kettle for 10 minutes, add 8 liters of a mixed solvent of n-hexane and methanol (the volume ratio of n-hexane to methanol is 6:1) to the stirring kettle, then add 200 grams of ergosterol and 100 milligrams of tert-butylhydroxyanisole, start the paddle stirrer, and stir at a constant temperature for 30 minutes to completely dissolve the ergosterol.

[0091] Step 2: Set the temperatures of the flat-plate photoreactor and the agitated thermostatic circulation kettle to 25°C. After introducing nitrogen for 10 minutes, start the transfer pump between the raw material mixing thermostatic stirring kettle and the flat-plate photoreactor, and transfer all the ergosterol photoreaction solution from the thermostatic stirring kettle to the photoreactor and the circulation kettle. Then, start the transfer pump between the photoreactor and the circulation kettle to make the photoreaction solution circulate smoothly between the photoreactor and the circulation kettle at a flow rate of 4 liters per minute.

[0092] Step 3: Start the LED side-illuminated light source with a central wavelength of 280 nm and a power of 1 kW, and adjust the beam shaper so that the shaped light spot uniformly irradiates the photoreaction solution in the flat-plate photoreactor for a light irradiation reaction for 30 minutes.

[0093] Step 4: Set the temperature of the product purification variable-temperature kettle to 25°C. After introducing nitrogen for 10 minutes, transfer all the photoreaction solution after the light irradiation reaction from the photoreactor and the circulation kettle to the product purification variable-temperature kettle.

[0094] Step 5: While performing the operation in Step 4, turn on the material delivery system of the raw material mixing thermostatic stirring kettle, transfer the initial photoreaction solution of a new batch of ergosterol to the flat-plate photoreactor and the agitated thermostatic circulation kettle, and start the second-round light irradiation reaction.

[0095] Step 6: Remove the photoreaction product from the product purification variable-temperature kettle, concentrate it, perform recrystallization, and recover the unreacted ergosterol to obtain a pre-vitamin D2 solution of the light irradiation product, with a conversion rate of ergosterol of 54.4%.

[0096] After the pre-vitamin D2 undergoes a thermal isomerization reaction, crude vitamin D2 is obtained, and the molar percentage content of vitamin D2 in the crude vitamin D2 is 76.3%.

[0097] Comparative Example 1

[0098] Compared with Example 3, the equipment used in this comparative example is the same as that in Example 1 except that there is no beam shaper, and other reaction conditions are exactly the same as those in Example 3.

[0099] After the light irradiation reaction, remove the photoreaction product from the product purification variable-temperature kettle, concentrate it, perform recrystallization, and recover the unreacted ergosterol to obtain a pre-vitamin D2 solution of the light irradiation product, with a conversion rate of ergosterol of 31.7%.

[0100] After the pre-vitamin D2 undergoes a thermal isomerization reaction, crude vitamin D2 is obtained, and the molar percentage content of vitamin D2 in the crude vitamin D2 is 52.1%.

[0101] Comparative Example 2

[0102] Compared with Example 3, the equipment used in this comparative example is the same as that in Example 1 except that a traditional tubular photoreactor is used, and other reaction conditions are exactly the same as those in Example 3.

[0103] After the photoreaction, the photoreaction product was removed from the product purification temperature-changing kettle, concentrated, recrystallized, and the unreacted ergosterol was recovered to obtain a pre-vitamin D2 solution of the photoreaction product, and the conversion rate of ergosterol was 23.2%.

[0104] After the pre-vitamin D2 was subjected to a thermal isomerization reaction, crude vitamin D2 was obtained, and the molar percentage content of vitamin D2 in the crude vitamin D2 was 38.7%.

[0105] The above are only the preferred embodiments of the present utility model, but the protection scope of the present utility model is not limited thereto. Any person skilled in the art can make several deformations and improvements without departing from the creative concept of the present utility model, and all of them should be covered by the protection of the present utility model. The above describes the embodiments of the present utility model. However, the present utility model is not limited to the above embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present utility model shall be included in the protection scope of the present utility model.

Claims

1. A light reaction device adapted to a side-lit light source, characterized in that: include: A photoreactor, used for containing a photoreaction liquid and providing a place for the photoreaction liquid to react; A light source, used to provide the light energy required for the reaction to the photoreaction liquid, wherein the light source is a side-illuminated light source; The beam shaper is located between the light source and the photoreactor. It is used to adjust the light beam emitted by the light source so that the size and shape of the light spot reaching the light receiving surface of the photoreactor match the reactor, and the light intensity irradiating the photoreactor is evenly distributed everywhere.

2. The photo-reactive device adapted to a side-lit light source according to claim 1, characterized in that: The photoreactor body is composed of two stacked three-dimensional structures, the inner three-dimensional structure is a hollow internal cavity, and the internal cavity is used to accommodate the photoreaction liquid; a sandwich is formed between the two three-dimensional structures, and the sandwich is used to store condensate.

3. The photo-reactive device adapted to a side-lit light source according to claim 2, characterized in that: The photoreactor comprises a light receiving side for receiving light, the light source is arranged opposite to the light receiving side, and the light emitted by the light source is placed perpendicular to the light receiving side of the photoreactor.

4. The photo-reactive device adapted to a side-lit light source according to claim 2, characterized in that: The photoreactor is a flat plate structure.

5. The photo-reactive device adapted to a side-lit light source according to claim 1, characterized in that: The beam shaper comprises a light spot homogenizing component, and the light spot homogenizing component is used to make the light intensity distribution of the light beam emitted by the light source uniform.

6. The photo-reactive device adapted to a side-lit light source according to claim 1, characterized in that: The beam shaper comprises a beam expansion or contraction component, and the beam expansion or contraction component is used to timely adjust the beam size according to the shape of light emitted by the light source and the size of the photoreactive device.

7. The photoreactive device adapted to a side-illuminated light source according to any one of claims 1 to 3, characterized in that: The reaction equipment also includes a disturbance type constant temperature circulation kettle, which is connected to the photoreactor. The photoreaction liquid can circulate between the photoreactor and the disturbance type constant temperature circulation kettle at a certain flow rate, so that the photoreaction liquid can undergo a homogeneous reaction under circulation conditions.

8. The photo-reactive device adapted to a side-lit light source according to claim 7, characterized in that: The top of the photoreactor is provided with a light reaction liquid outflow outlet, the bottom of the photoreactor is provided with a light reaction liquid inflow inlet, and the photoreactor is connected with the disturbance type constant temperature circulation kettle through the light reaction liquid outflow outlet and the light reaction liquid inflow inlet.

9. The photo-reactive device adapted to a side-lit light source according to claim 1, characterized in that: The reaction equipment also includes a raw material mixing constant temperature stirring kettle, which is used to provide a starting photoreaction liquid. The raw material mixing constant temperature stirring kettle is connected to the photoreactor and is used to introduce the starting photoreaction liquid into the photoreactor.

10. The photo-reactive device adapted to a side-lit light source according to claim 7, characterized in that: The reaction equipment also includes a product purification temperature-variable kettle, which is connected to the disturbance-type constant temperature circulation kettle and is used to receive the photoreaction product.

11. The photoreactive device adapted to a side-lit light source according to any one of claims 1 to 3, characterized in that: The lower end of the photoreactor is equipped with a gas-liquid mixing valve and a gas inlet 1. The photoreaction liquid flows in from the photoreaction liquid inlet 1, and the gas flows in from the gas inlet 1. The photoreaction liquid and the gas are mixed at the gas-liquid mixing valve and then flow into the photoreactor, and the inflowing gas forms uniform bubbles.

12. The photo-reactive device adapted to a side-lit light source according to claim 7, characterized in that: The top of the disturbance-type constant temperature circulation kettle is provided with a photoreaction liquid inlet, a photoreaction liquid outlet, and a second inert gas inlet. The photoreaction liquid inlet and the outlet are used to communicate with the photoreactor, and the second inert gas inlet is used to blow inert gas into the disturbance-type constant temperature circulation kettle.

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