CN214183030U - Photochemical reaction kettle - Google Patents

Photochemical reaction kettle Download PDF

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Publication number
CN214183030U
CN214183030U CN202022959635.8U CN202022959635U CN214183030U CN 214183030 U CN214183030 U CN 214183030U CN 202022959635 U CN202022959635 U CN 202022959635U CN 214183030 U CN214183030 U CN 214183030U
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Prior art keywords
photochemical reaction
gas distributor
gas
photochemical
feed inlet
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CN202022959635.8U
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梁荣超
邓清田
刘皓
周家发
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Chengdu Chenguang Boda New Material Co.,Ltd.
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Chenguang Fluoro & Silicone Elastomers Co ltd
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Abstract

The utility model discloses a photochemical reaction cauldron, including the photochemical reaction cauldron that is equipped with ultraviolet generator and agitator, liquid phase feed inlet, gaseous phase feed inlet and gaseous phase export are established on photochemical reaction cauldron upper portion, and the liquid phase discharge gate is established to photochemical reaction cauldron lower part, establishes gas distributor in the photochemical reaction cauldron, and gas distributor intercommunication gaseous phase feed inlet forms the oxygen passageway, and the agitator is located the below of gas distributor export. Through the cooperation of the gas distributor and the stirrer, the uniform dispersion and the efficient mass transfer of gas in the gas-liquid two-phase type photochemical reaction process can be realized, and the reaction efficiency is improved.

Description

Photochemical reaction kettle
Technical Field
The utility model relates to a photochemical reaction cauldron, concretely relates to reation kettle of gas-liquid heterogeneous photochemical reaction process control belongs to the photochemical reaction equipment field.
Background
At present, the photochemical reaction process is generally carried out under a positive pressure condition, and a light source irradiates reaction materials to promote the reaction. The wavelength of the light source, the irradiation intensity, etc. may affect the chemical reaction. In order to facilitate the transmission of light waves, glass materials are generally used as the light source housing for protection. Meanwhile, when the reaction system is a heterogeneous reaction system, especially a gas-liquid two-phase reaction process, uniform dispersion of gas in liquid-phase reactants and high mass transfer efficiency are very important, and the reaction initiation and the reaction process are possibly greatly influenced. If the diameter of the gas-phase bubble is too large, dispersion and mass transfer are not facilitated, and the ultraviolet ray is easy to refract, so that optical loss is caused.
If the reaction system contains or gradually produces materials which are corrosive to glass, chemical and chemical reaction processes involving fluorine often accompany with compounds which are corrosive to glass materials, such as acyl fluoride groups and/or HF. The corrosion is intensified along with the time, the surface of the glass is blurred, and the light efficiency is influenced by the diffuse reflection of ultraviolet light. Therefore, when reaction equipment is designed, the problem of corrosivity needs to be considered, materials are prevented from being directly contacted with the light emitter through special design, or protective design is adopted, and the influence caused by corrosion is eliminated through measures such as replacing the protective sleeve regularly.
The method aims to solve the problems existing in the photochemical reaction process, particularly the problems of uniform dispersion and high-efficiency mass transfer of gas-phase materials existing in the heterogeneous gas-liquid two-phase photochemical reaction system process, corrosive influence of corrosive materials on light source glass and the like. In the prior art, CN109603708A discloses a m-xylene photo-chlorination reaction kettle capable of automatically controlling temperature, wherein a gas distributor is used in the kettle to disperse the input chlorine gas, and a circulating flow is formed in the reaction kettle through a guide cylinder, so that the chlorine gas and the m-xylene solution are more fully contacted, which is beneficial to improving the reaction efficiency when p-chlorophenol is synthesized, in addition, an electrodeless ultraviolet lamp is used as a light source, and the radiation intensity of short-wave ultraviolet light (254 mm) of the electrodeless ultraviolet lamp can be improved by 10 times compared with that of a traditional light source, and the service life of the electrodeless ultraviolet lamp is long.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a photochemical reaction cauldron, through the cooperation of gas distributor and agitator, can realize gaseous homodisperse and the high-efficient mass transfer in gas-liquid double-phase formula photochemical reaction process, improves reaction efficiency.
The utility model discloses a following technical scheme realizes: a photochemical reaction kettle is characterized in that: the device comprises a photochemical reaction kettle provided with an ultraviolet generator and a stirrer, wherein a liquid-phase feed inlet, a gas-phase feed inlet and a gas-phase outlet are arranged at the upper part of the photochemical reaction kettle, a liquid-phase discharge outlet is arranged at the lower part of the photochemical reaction kettle, a gas distributor is arranged in the photochemical reaction kettle, the gas distributor is communicated with the gas-phase feed inlet to form an oxygen channel, and the stirrer is positioned below the outlet of the gas distributor.
The gas distributor is positioned at the lower part of the photochemical reaction kettle, and the stirrer is arranged for stirring.
The gas distributor is a metal coil pipe with micropores, and the pore size of each micropore is 0.5-10 mu m.
The ultraviolet light generator is provided with a detachable glass sealing tube, and the ultraviolet light irradiation light source is sleeved in the glass sealing tube.
The photochemical reaction kettle is provided with a jacket, and the jacket is provided with a refrigerant inlet and a refrigerant outlet.
Compared with the prior art, the utility model, following advantage and beneficial effect have:
(1) the utility model discloses the setting is taken microporous metal coil pipe formula gas distributor, and the gas material can form the microbubble through this distributor, mixes under the combination and can realize high-efficient homodisperse and the mass transfer of gas in reaction system.
(2) The utility model discloses adopt the loose joint formula with ultraviolet lamp irradiation light source to connect, set up in glass sealed tube, the material does not take place direct contact with the light source, and the glass material that outer sealed tube adopted does not cause the influence to the propagation of irradiation light, designs to can dismantle the form, the periodic replacement of being convenient for.
(3) The utility model discloses a set up gas distributor and agitator in photochemical reaction cauldron and cooperate, can provide the reaction efficiency of homodisperse and high-efficient mass transfer for gas-liquid heterogeneous formula photochemical reaction process to ensure light source irradiation efficiency, intensity stability, can satisfy the stable production technology technical requirement of scale.
Drawings
Fig. 1 is a schematic structural diagram of the photochemical reaction kettle of the present invention.
Fig. 2 is a schematic diagram of the structure of the ultraviolet light generator of the present invention.
The device comprises 1-an ultraviolet light generator, 2-a stirrer, 3-a photochemical reaction kettle, 4-a liquid phase feed inlet, 5-a gas phase feed inlet, 6-a gas phase outlet, 7-a liquid phase discharge outlet, 8-a gas distributor, 9-a refrigerant inlet, 10-a refrigerant outlet, 11-a glass sealing tube, 12-a flange component and 13-a condenser liquid return port.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited thereto.
Example 1:
this example presents a photochemical reaction kettle.
As shown in fig. 1, this photochemical reaction cauldron 3 is the jacketed kettle body, is applicable to the heterogeneous formula photochemical reaction process of gas-liquid, and upper portion is equipped with ultraviolet generator 1, liquid phase feed inlet 4, gaseous phase feed inlet 5 and gaseous phase export 6 in the cauldron, and agitator 2, gas distributor 8 and liquid phase discharge gate 7 are established to the lower part in the cauldron, and gas distributor 8 intercommunication gaseous phase feed inlet 5 forms the oxygen passageway, and agitator 2 sets up to stir down, is located the below that 8 exports of gas distributor.
The gas distributor 8 can be arranged as a metal coil with micropores, the pore size of which is set between 0.5 to 10 [ mu ] m, for example, in one embodiment, the pore size of which is 2 [ mu ] m. When the device is used, liquid materials are fed into the photochemical reaction kettle 3 from the liquid-phase feed inlet 4, the temperature in the kettle is controlled by a jacket, for example, in one embodiment, the temperature is controlled by the jacket through a refrigerant, the jacket is provided with a refrigerant inlet 9 and a refrigerant outlet 10, gas-phase materials are continuously fed into the photochemical reaction kettle 3 through micropores on a metal coil, the gas-phase materials are uniformly dispersed and efficiently transferred in the liquid materials through the cooperation of the gas distributor 8 and the stirrer 2, the photochemical reaction is carried out under the irradiation of ultraviolet light, reaction products can be fed out through the liquid-phase discharge outlet 7 after the reaction is finished, unreacted monomers are fed into a condenser through the gas-phase outlet 6 and are recycled into the storage tank, and the top of the photochemical reaction kettle 3 is provided with a condenser liquid return port 13.
In consideration of the corrosion problem of the ultraviolet light generator 1, in a possible embodiment, a movably connected glass sleeve type ultraviolet light generator is provided, and the original mode that the ultraviolet light generator 1 and the glass sealing tube 11 are fixedly connected is replaced by a detachable mode. As shown in fig. 2, one end of the glass sealing tube 11 is closed, the ultraviolet irradiation light source is sleeved in the glass sealing tube 11, the flange assembly 12 arranged on the ultraviolet generator 1 is used for realizing the detachable connection of the glass sealing tube 11, and in order to enhance the sealing effect of the glass sealing tube 11, a sealing gasket can be arranged on the flange assembly 12, and the specific structure can be referred to the glass tube sealing device of CN 202343187U.
Example 2:
this example is a specific process for synthesizing a peroxide-containing perfluoropolyether product by using the photochemical reaction kettle 3 described in example 1 to photopolymerize a pesticide with hexafluoropropylene and oxygen under ultraviolet irradiation.
The photochemical reaction kettle 3 is vacuumized by nitrogen replacement, a jacket is circularly cooled to-30 ℃ by introducing a refrigerant, 15kg of hexafluoropropylene is added for cooling and liquefaction, and the temperature of the materials is controlled to be-30 ℃ in the polymerization process. Oxygen is continuously fed through the gas phase feed port 5, fine bubbles are formed through the gas distributor 8 and are dispersed and uniformly mixed with liquid hexafluoropropylene, the feeding speed of the oxygen is 2g/min, and the continuous aeration time is 8.5 h. While oxygen was being ventilated, the ultraviolet light source was continuously irradiated with an irradiation power of 500W, an irradiation wavelength of 300nm, and a stirring rate of 100 rpm. After the reaction is stopped, the temperature of the reaction product is gradually raised to normal temperature, unreacted monomer hexafluoropropylene is condensed and recycled into a storage tank, and 9.5kg of liquid peroxide product is obtained by collection, wherein the yield is 63.3% according to the amount of hexafluoropropylene fed.
The above is only the preferred embodiment of the present invention, not to the limitation of the present invention in any form, all the technical matters of the present invention all fall into the protection scope of the present invention to any simple modification and equivalent change of the above embodiments.

Claims (5)

1. A photochemical reaction kettle is characterized in that: including photochemical reaction cauldron (3) that are equipped with ultraviolet generator (1) and agitator (2), liquid phase feed inlet (4), gaseous phase feed inlet (5) and gaseous phase export (6) are established on photochemical reaction cauldron (3) upper portion, liquid phase discharge gate (7) are established to photochemical reaction cauldron (3) lower part, establish gas distributor (8) in photochemical reaction cauldron (3), gas distributor (8) intercommunication gaseous phase feed inlet (5) form the oxygen passageway, agitator (2) are located the below of gas distributor (8) export.
2. A photochemical reactor as claimed in claim 1, wherein: the gas distributor (8) is positioned at the lower part of the photochemical reaction kettle (3), and the stirrer (2) is arranged for stirring.
3. A photochemical reactor as claimed in claim 1, wherein: the gas distributor (8) is a metal coil pipe with micropores, and the pore size of the micropores is 0.5-10 mu m.
4. A photochemical reactor as claimed in claim 1, wherein: the ultraviolet light generator (1) is provided with a detachable glass sealing tube (11), and an ultraviolet light irradiation light source is sleeved in the glass sealing tube (11).
5. A photochemical reactor as claimed in claim 1, wherein: the photochemical reaction kettle (3) is provided with a jacket, and the jacket is provided with a refrigerant inlet (9) and a refrigerant outlet (10).
CN202022959635.8U 2020-12-11 2020-12-11 Photochemical reaction kettle Active CN214183030U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202022959635.8U CN214183030U (en) 2020-12-11 2020-12-11 Photochemical reaction kettle

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114505029A (en) * 2022-02-24 2022-05-17 郑州长城科工贸有限公司 Top-side illumination type photochemical reactor and using method thereof
CN114950294A (en) * 2021-12-10 2022-08-30 西安交通大学 Device for preparing polythioether rubber by continuous photosynthesis

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114950294A (en) * 2021-12-10 2022-08-30 西安交通大学 Device for preparing polythioether rubber by continuous photosynthesis
CN114505029A (en) * 2022-02-24 2022-05-17 郑州长城科工贸有限公司 Top-side illumination type photochemical reactor and using method thereof

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CP01 Change in the name or title of a patent holder

Address after: No.168, Tengfei 6th Road, Southwest Airport Economic Development Zone, Shuangliu District, Chengdu, Sichuan 610200 China (Sichuan) pilot Free Trade Zone, Chengdu

Patentee after: Chengdu Chenguang Boda New Material Co.,Ltd.

Address before: No.168, Tengfei 6th Road, Southwest Airport Economic Development Zone, Shuangliu District, Chengdu, Sichuan 610200 China (Sichuan) pilot Free Trade Zone, Chengdu

Patentee before: CHENGUANG FLUORO & SILICONE ELASTOMERS CO.,LTD.

CP01 Change in the name or title of a patent holder
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of utility model: A photochemical reaction kettle

Effective date of registration: 20220712

Granted publication date: 20210914

Pledgee: China Minsheng Banking Corp Chengdu branch

Pledgor: Chengdu Chenguang Boda New Material Co.,Ltd.

Registration number: Y2022510000201

PE01 Entry into force of the registration of the contract for pledge of patent right