Oxidation reaction device

Abstract

The utility model provides an oxidation reaction device which comprises a main body reactor used for providing an oxidation reaction place; the liquid injection mechanism is arranged on the main body reactor, is connected with the top of the main body reactor and is used for mixing an oxygen-containing raw material and a reaction liquid; the oxidation raw material gas inlet mechanism is connected with the liquid injection mechanism and is used for providing an oxygen-containing raw material for the liquid injection mechanism; the liquid circulating pump is connected with the bottom of the main body reactor and is used for realizing liquid circulation of the reaction liquid; and the heat exchange mechanism is connected with the main body reactor, the oxidation raw material gas inlet mechanism, the liquid injection mechanism and the liquid circulating pump, and is used for cooling the oxygen-containing material and the reaction liquid after the reaction. An oxidation raw material gas inlet mechanism is arranged, and oxygen-containing gas enters a condensed gas phase, so that the explosion risk is reduced, and the reaction safety is greatly improved; and the oxygen-containing raw material and the cooled reaction liquid are mixed in the liquid injection mechanism, so that the gas-liquid contact probability is greatly increased.

Description

Technical Field

[0001] The utility model relates to the technical field of fine chemical industry, in particular to an oxidation reaction device. Background Art

[0002] Aldehydes such as heliotropin are precious spices that can be used in flavors and fragrances, foods, daily chemical additives, and pharmaceutical intermediates. Generally, aldehyde products are obtained from alcohols through oxidation reactions. In the oxidation reaction, the most important device is the oxidation reaction device. Oxidation reactions usually require the participation of oxygen-containing raw materials, which include oxygen-containing gases or ozone. Oxidation involving oxygen-containing raw materials will be the direction of future technological improvements because it is cleaner and has lower costs. In industrial production, the application scope of oxygen will become wider and wider.

[0003] The devices involved in introducing oxygen-containing raw gas into the reactor all ventilate directly into the reactor. The main problems with this type of equipment are: ① The reaction is a gas-liquid two-phase reaction, and the mass transfer effect of the existing devices is poor, resulting in low reaction efficiency; ② Since there is a large amount of flammable gas in the reactor, the limiting oxygen concentration (LOC) of most flammable gases is less than 10%. If oxygen is directly introduced into the reactor, there is an extremely high risk of combustion and explosion, and the existing devices cannot solve the combustion and explosion risks of the reaction.

[0004] In patent CN202021760690.8, ozone is directly introduced from the gas phase space above the kettle, the gas diffusion is slow, and the local oxygen concentration is too high, posing a greater safety risk; in patent CN200920169123.2, ozone is introduced into the reactor from the bottom distributor. This design can solve the problem of poor mass transfer and improve the reaction efficiency to a certain extent. However, after the unconsumed ozone enters the gas phase space from the reaction liquid surface, there is still a greater risk of combustion and explosion, and the reaction liquid of this equipment will flow back into the bottom distributor, which has a greater risk of combustion and explosion in an ozone environment; in patent CN202222720932.6, HCl gas is introduced from the gas phase space, which is conducive to gas-liquid mass transfer, but the risk of combustion and explosion is higher when oxygen is introduced from the gas phase space.

[0005] Therefore, it is necessary to provide an oxidation reaction device to solve the problems of low gas-liquid mass transfer efficiency and low reaction safety. Utility Model Content

[0006] The utility model provides an oxidation reaction device to solve the defects in the prior art.

[0007] The utility model provides an oxidation reaction device, comprising:

[0008] The main reactor is used to provide an oxidation reaction site;

[0009] A liquid injection mechanism is disposed on the main reactor and connected to the top of the main reactor, and is used to mix the oxygen-containing raw material and the reaction liquid;

[0010] An oxidizing raw material intake mechanism, connected to the liquid injection mechanism, for providing oxygen-containing raw materials to the liquid injection mechanism;

[0011] A liquid circulation pump, connected to the bottom of the main reactor, for realizing liquid circulation of the reaction liquid;

[0012] The heat exchange mechanism includes two heat exchangers, one of which is connected to the main reactor and the oxidation raw material intake mechanism, and the other is connected to the liquid injection mechanism and the liquid circulation pump, and is used to cool the oxygen-containing material and reaction liquid after the reaction.

[0013] According to an oxidation reaction device provided by the utility model, a coil is arranged on the main reactor, and a liquid inlet and a liquid outlet are arranged on the coil for introducing liquids of different temperatures to adjust the temperature of the main reactor.

[0014] According to an oxidation reaction device provided by the utility model, the liquid injection mechanism includes:

[0015] A mixing reactor, used for mixing the oxygen-containing material and the reaction liquid;

[0016] An air inlet pipe, connected to the mixing reactor, for introducing oxygen-containing materials;

[0017] A liquid inlet pipe, disposed on the mixing reactor, connected to the mixing reactor, and used for introducing the reaction liquid;

[0018] The material discharge pipe is arranged at the bottom of the mixing reactor and connected to the bottom of the mixing reactor, and is used for introducing oxygen-containing material and reaction liquid into the main reactor.

[0019] According to an oxidation reaction device provided by the utility model, the outlet of the material discharge pipe extends below the internal liquid level of the main reactor.

[0020] According to an oxidation reaction device provided by the utility model, the air inlet pipe connects the mixing reactor with the oxidation raw material air inlet mechanism, and the liquid inlet pipe connects the mixing reactor with the heat exchange mechanism.

[0021] According to an oxidation reaction device provided by the utility model, the oxidation raw material intake mechanism comprises:

[0022] A gas distribution tank, on which an inert gas inlet, an oxygen-containing gas inlet and an oxygen-containing raw material inlet are arranged, and the gas distribution tank is connected to the inlet pipe through a delivery pipe;

[0023] An oxygen analyzer 1 is arranged in the gas distribution tank and is used to detect the oxygen content.

[0024] According to an oxidation reaction device provided by the utility model, the heat exchange mechanism includes:

[0025] Heat exchanger 1 is arranged above the main reactor, with its input end connected to the gas phase space at the upper part of the main reactor, and its output end connected to the oxygen-containing raw material inlet of the gas distribution tank, for cooling the residual oxygen-containing raw material after the reaction;

[0026] The second heat exchanger is arranged between the liquid circulation pump and the liquid injection mechanism, with its input end connected to the liquid circulation pump and its output end connected to the liquid injection mechanism, and is used for cooling the reaction liquid after the reaction.

[0027] According to an oxidation reaction device provided by the utility model, an oxygen analyzer 2 is arranged in the gas phase space at the upper part of the main reactor, which is used to detect the oxygen content in the main reactor.

[0028] According to an oxidation reaction device provided by the utility model, the oxidation reaction device is applied to the oxidation reaction of alcohol to aldehyde with the participation of oxygen-containing gas or ozone.

[0029] The utility model provides an oxidation reaction device, which mixes the cooled oxygen-containing raw material with the oxygen-containing gas and the inert gas by arranging an oxidation raw material air intake mechanism and a heat exchanger, and the oxygen-containing gas enters the condensed gas phase, which can reduce the amount of combustible gas and reduce the risk of combustion and explosion. The oxygen-containing gas is fully mixed and diluted in the gas distribution tank, and the oxygen content is detected by an oxygen analyzer, which greatly improves the reaction safety. By arranging a liquid injection mechanism and a heat exchanger, the oxygen-containing raw material and the cooled reaction liquid are mixed in the liquid injection mechanism, which greatly improves the gas-liquid contact probability, strengthens the mass transfer, and improves the reaction efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the technical solutions in the present invention or the prior art, a brief introduction will be given below to the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0031] Figure 1 It is a structural schematic diagram of an oxidation reaction device provided in an embodiment of the utility model;

[0032] Figure 2 It is a schematic diagram of the cross-sectional structure of an oxidation reaction device provided in an embodiment of the utility model.

[0033] Among them, 1-main reactor, 2-liquid injection mechanism, 3-oxidation raw material intake mechanism, 4-liquid circulation pump, 5-heat exchange mechanism, 6-coil;

[0034] 21-mixing reactor, 22-air inlet pipe, 23-liquid inlet pipe, 24-material discharge pipe;

[0035] 31-gas distribution tank, 32-oxygen analyzer 1;

[0036] 51-heat exchanger one, 52-heat exchanger two. DETAILED DESCRIPTION

[0037] In order to make the purpose, technical solution and advantages of the utility model clearer, the technical solution of the utility model will be clearly and completely described below in conjunction with the drawings in the utility model. Obviously, the described embodiments are part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0038] An oxidation reaction device in an embodiment of the present application includes:

[0039] The main reactor 1 is used to provide an oxidation reaction site;

[0040] A liquid injection mechanism 2 is disposed on the main reactor 1 and connected to the top of the main reactor 1, and is used to mix the oxygen-containing raw material and the reaction liquid;

[0041] An oxidizing raw material intake mechanism 3, connected to the liquid injection mechanism 2, for providing oxygen-containing raw materials to the liquid injection mechanism 2;

[0042] A liquid circulation pump 4 is connected to the bottom of the main reactor 1 and is used to realize liquid circulation of the reaction liquid;

[0043] The heat exchange mechanism 5 includes two heat exchangers, one of which is connected to the main reactor 1 and the oxidation raw material intake mechanism 3, and the other is connected to the liquid injection mechanism 2 and the liquid circulation pump 4, for cooling the oxygen-containing material and reaction liquid after the reaction.

[0044] According to an oxidation reaction device provided by the utility model, the main reactor 1 is provided with a coil 6 , and the coil 6 is provided with a liquid inlet and a liquid outlet for introducing liquids of different temperatures to adjust the temperature of the main reactor 1 .

[0045] To further optimize the above technical solution, the liquid injection mechanism 2 includes:

[0046] A mixing reactor 21, used for mixing the oxygen-containing material and the reaction liquid;

[0047] An air inlet pipe 22, connected to the mixing reactor 21, for introducing oxygen-containing materials;

[0048] A liquid inlet pipe 23, disposed on the mixing reactor 21, connected to the mixing reactor 21, and used for introducing the reaction liquid;

[0049] The material discharge pipe 24 is disposed at the bottom of the mixing reactor 21 and connected to the bottom of the mixing reactor 21 , and is used to introduce oxygen-containing materials and reaction liquid into the main reactor 1 .

[0050] The outlet of the material discharge pipe 24 extends below the internal liquid level of the main reactor 1 .

[0051] The air inlet pipe 22 connects the mixing reactor 21 with the oxidation raw material air inlet mechanism 3 , and the liquid inlet pipe 23 connects the mixing reactor 21 with the heat exchange mechanism 5 .

[0052] Specifically, the liquid injection mechanism 2 can serve as the inlet of the main reactor 1. The oxygen-containing raw material and the cooled reaction liquid are mixed in the liquid injection mechanism 2, and are evenly mixed through the liquid injection mechanism 2 and enter the reaction chamber, which greatly increases the probability of gas-liquid contact and improves the reaction efficiency. The liquid injection mechanism 2 can use a loop reactor or a Venturi reactor.

[0053] In order to further optimize the above technical solution, the oxidation raw material intake mechanism 3 includes:

[0054] A gas distribution tank 31, on which an inert gas inlet, an oxygen-containing gas inlet and an oxygen-containing raw material inlet are provided, and the gas distribution tank 31 is connected to the inlet pipe 22 through a delivery pipe;

[0055] An oxygen analyzer 32 is disposed in the gas distribution tank 31 and is used to detect the oxygen content.

[0056] Specifically, the oxidation raw material intake mechanism 3 includes an inert gas and an oxygen-containing gas inlet. The inert gas nitrogen is first filled into the gas distribution tank 31. The heat exchange mechanism 5 cools most of the combustible gas in the circulation process and then passes it into the gas distribution tank 31. The cooled gas phase is equivalent to an inert gas environment. Oxygen enters the condensed gas phase to eliminate the risk of combustion and explosion of combustible gas. The oxygen is fully mixed and diluted to below LOC in the gas distribution tank 31 before entering the reaction chamber. The gas distribution tank 31 is provided with an oxygen analyzer 32, preferably an online oxygen analyzer, to facilitate the control of oxygen content and improve reaction safety.

[0057] To further optimize the above technical solution, the heat exchange mechanism 5 includes:

[0058] The heat exchanger 51 is arranged above the main reactor 1, with its input end connected to the gas phase space at the upper part of the main reactor 1, and its output end connected to the oxygen-containing raw material inlet of the gas distribution tank 31, for cooling the residual oxygen-containing raw material after the reaction;

[0059] The second heat exchanger 52 is disposed between the liquid circulation pump 4 and the liquid injection mechanism 2, with its input end connected to the liquid circulation pump 4 and its output end connected to the liquid injection mechanism 2, for cooling the reaction liquid after the reaction.

[0060] Specifically, the liquid circulation drives the gas phase circulation. The heat exchanger 51 is located above the main reactor 1, and fully condenses the combustible gas in the gas phase space, which is used to cool the combustible gas above the main reactor 1, that is, the oxygen-containing raw gas that has not reacted completely. After being adjusted to the target oxygen content by nitrogen and other gases in the gas distribution tank 31, it is re-introduced into the liquid injection mechanism 2 to enter the main reactor 1 to participate in the reaction;

[0061] The heat exchanger 2 52 located between the liquid circulation pump 4 and the liquid injection mechanism 2 can re-enter the main reactor 1 through the liquid injection mechanism 2 after heat exchange with the reaction liquid in the main reactor 1. The reaction liquid is continuously transported from the bottom of the main reactor 1 to the inlet of the main reactor 1 through the circulation pump 4, and the reaction heat is efficiently removed by the external heat exchanger 2 52. The cooled reaction liquid can reduce the gas phase space above the main reactor 1, and the volume of the oxygen-containing raw gas decreases as the temperature decreases, which can reduce the risk of fire explosion.

[0062] To further optimize the above technical solution, an oxygen analyzer 11 is provided in the gas phase space at the upper part of the main reactor 1 to detect the oxygen content in the main reactor 1. An online oxygen analyzer is preferred to facilitate the control of the oxygen content in the reaction system and improve the safety of the reaction.

[0063] To further optimize the above technical solution, the oxidation reaction device is applied to the oxidation reaction of alcohol to aldehyde with the participation of oxygen-containing gas or ozone. The oxidation reaction device is applied to the oxidation reaction of alcohol to aldehyde with the participation of oxygen-containing gas or ozone, including heliotropin.

[0064] Working principle: the oxidation raw material air intake mechanism introduces inert gas into the gas distribution tank 31, and mixes the oxygen-containing raw material cooled by the heat exchanger 51 with the oxygen-containing gas. The oxygen-containing gas enters the condensed gas phase, which can reduce the amount of combustible gas and reduce the risk of explosion. The oxygen-containing gas is fully mixed and diluted in the gas distribution tank 31, and the oxygen content is detected by the oxygen analyzer 32, and the prepared oxygen-containing raw material is introduced into the liquid injection mechanism 2; the liquid injection mechanism 2 serves as the inlet of the main reactor 1, and can be introduced with the reaction liquid. The oxygen-containing raw material and the reaction liquid cooled by the heat exchanger 52 are mixed in the liquid injection mechanism 2, which greatly improves the gas-liquid contact probability. There will be combustible gas of the oxygen-containing raw material gas that has not reacted completely in the main reactor 1, which can be mixed with the oxygen-containing gas after being cooled by the heat exchanger 51. The liquid circulation pump 4 realizes liquid circulation, and the reaction liquid in the main reactor 1 is introduced into the heat exchanger 52, and re-enters the liquid injection mechanism 2 after heat exchange and cooling.

[0065] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the utility model, rather than to limit it. Although the utility model has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the various embodiments of the utility model.

Claims

1. An oxidation reaction device, characterized in that: include: The main reactor is used to provide an oxidation reaction site; A liquid injection mechanism is disposed on the main reactor and connected to the top of the main reactor, and is used to mix the oxygen-containing raw material and the reaction liquid; An oxidizing raw material intake mechanism, connected to the liquid injection mechanism, for providing oxygen-containing raw materials to the liquid injection mechanism; A liquid circulation pump, connected to the bottom of the main reactor, for realizing liquid circulation of the reaction liquid; The heat exchange mechanism includes two heat exchangers, one of which is connected to the main reactor and the oxidation raw material intake mechanism, and the other is connected to the liquid injection mechanism and the liquid circulation pump, and is used to cool the oxygen-containing material and reaction liquid after the reaction.

2. An oxidation reaction device according to claim 1, characterized in that: The main reactor is provided with a coil for introducing liquids of different temperatures to adjust the temperature of the main reactor.

3. An oxidation reaction device according to claim 2, characterized in that: The coil is provided with a liquid inlet and a liquid outlet for introducing and discharging liquids of different temperatures.

4. An oxidation reaction device according to claim 1, characterized in that: The liquid injection mechanism comprises: A mixing reactor, used for mixing the oxygen-containing material and the reaction liquid; An air inlet pipe, connected to the mixing reactor, for introducing oxygen-containing materials; A liquid inlet pipe, disposed on the mixing reactor, connected to the mixing reactor, and used for introducing the reaction liquid; The material discharge pipe is arranged at the bottom of the mixing reactor and connected to the bottom of the mixing reactor, and is used for introducing oxygen-containing material and reaction liquid into the main reactor.

5. An oxidation reaction device according to claim 4, characterized in that: The outlet of the material discharge pipe extends below the internal liquid level of the main reactor.

6. An oxidation reaction device according to claim 4, characterized in that: The air inlet pipe connects the mixing reactor with the oxidation raw material air inlet mechanism, and the liquid inlet pipe connects the mixing reactor with the heat exchange mechanism.

7. An oxidation reaction device according to claim 4, characterized in that: The oxidation raw material intake mechanism comprises: A gas distribution tank, on which an inert gas inlet, an oxygen-containing gas inlet and an oxygen-containing raw material inlet are arranged, and the gas distribution tank is connected to the inlet pipe through a delivery pipe; The oxygen analyzer 1 is arranged in the gas distribution tank and is used to detect the oxygen content in the gas distribution tank.

8. An oxidation reaction device according to claim 7, characterized in that: The heat exchange mechanism comprises: Heat exchanger 1 is arranged above the main reactor, with its input end connected to the gas phase space at the upper part of the main reactor, and its output end connected to the oxygen-containing raw material inlet of the gas distribution tank, for cooling the residual oxygen-containing raw material after the reaction; The second heat exchanger is arranged between the liquid circulation pump and the liquid injection mechanism, with its input end connected to the liquid circulation pump and its output end connected to the liquid injection mechanism, and is used for cooling the reaction liquid after the reaction.

9. An oxidation reaction device according to claim 1, characterized in that: An oxygen analyzer 2 is arranged in the gas phase space at the upper part of the main reactor to detect the oxygen content in the main reactor.

10. An oxidation reaction device according to any one of claims 1 to 9, characterized in that: The oxidation reaction device is used for the oxidation reaction of alcohol to aldehyde with the participation of oxygen-containing gas or ozone.

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