CN202621125U - High-pressure reaction unit - Google Patents

High-pressure reaction unit Download PDF

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Publication number
CN202621125U
CN202621125U CN 201220177227 CN201220177227U CN202621125U CN 202621125 U CN202621125 U CN 202621125U CN 201220177227 CN201220177227 CN 201220177227 CN 201220177227 U CN201220177227 U CN 201220177227U CN 202621125 U CN202621125 U CN 202621125U
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reaction
gas
condenser
pressure
reactor
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汪权
王坤
吴爱峰
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Changshu Institute of Technology
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Abstract

本实用新型涉及一种高压反应装置,尤其是一种有液体参与化学反应的高压反应釜装置。它解决了现有高压反应釜一般只能在封闭体系中进行反应,难以满足某些需要不断通入气体,同时需要不断排放出尾气,尤其是有液体参与化学反应的高温高压反应体系的技术问题。其技术方案包括在高压反应釜外体上部安装冷却回流管路,使得反应过程中所产生的大量气体冷凝形成回流,重新进入反应釜继续进行反应。在冷却回流管路中,气体下行管路(10)、冷凝器(14)和进料/回流三通管(18)顺序连接,气体的流动方向和冷凝液体的流动方向都是竖直向下,使得冷凝液体更容易回流入反应釜继续进行反应。采用这种结构的冷却回流管路,冷却效果更好,提高了反应的转化率,节约了成本。

Figure 201220177227

The utility model relates to a high-pressure reaction device, in particular to a high-pressure reaction kettle device in which liquid participates in chemical reactions. It solves the technical problems that the existing high-pressure reactors can only react in a closed system, and it is difficult to meet certain needs of continuously feeding gas and continuously discharging tail gas, especially in high-temperature and high-pressure reaction systems where liquids participate in chemical reactions. . The technical solution includes installing a cooling return pipeline on the upper part of the outer body of the high-pressure reactor, so that a large amount of gas generated during the reaction is condensed to form a return flow, and then re-enters the reactor to continue the reaction. In the cooling return pipeline, the gas descending pipeline (10), the condenser (14) and the feed/return tee (18) are connected in sequence, and the flow direction of the gas and the flow direction of the condensed liquid are both vertically downward , making it easier for the condensed liquid to flow back into the reactor to continue the reaction. The cooling return pipeline with this structure has a better cooling effect, improves the conversion rate of the reaction, and saves the cost.

Figure 201220177227

Description

一种高压反应装置A high pressure reaction device

技术领域 technical field

本实用新型涉及一种高压反应装置,尤其是一种有液体参与化学反应的高压反应釜装置。The utility model relates to a high-pressure reaction device, in particular to a high-pressure reaction kettle device in which liquid participates in chemical reactions.

背景技术 Background technique

现有的高压反应釜在反应釜的上部或底部仅安装多个阀门,用于进料或出料。反应时所有阀门关闭,反应物在釜体内封闭环境下进行反应。这种结构的反应釜很难满足需要连续通入气体,并且需要不断排放出尾气的高温高压反应体系的要求。例如利用空气氧化环己烷制备环己醇和环己酮的反应,因为反应釜内空气成分中氧气的含量不断下降,需要不断地补充新鲜的空气,同时需要不断地排放出贫氧的空气尾气。另外,因为环己烷氧化反应是在加热加压的情况下进行的,通常反应温度在120℃以上,而环己烷的沸点为80.7℃,有大量的环己烷来不及反应就被空气尾气带出反应釜。在生产过程中,经检测,也有一部分的环己醇和环己酮被空气尾气带出,造成很大的浪费。Existing high-pressure reactors only have a plurality of valves installed on the top or bottom of the reactor for feeding or discharging. During the reaction, all valves are closed, and the reactants are reacted in a closed environment in the kettle body. Reactors with this structure are difficult to meet the requirements of a high-temperature and high-pressure reaction system that needs to continuously feed gas and continuously discharge tail gas. For example, the use of air to oxidize cyclohexane to prepare cyclohexanol and cyclohexanone, because the oxygen content in the air component in the reactor is continuously decreasing, fresh air needs to be continuously replenished, and oxygen-poor air tail gas needs to be continuously discharged at the same time. In addition, because the cyclohexane oxidation reaction is carried out under heat and pressure, usually the reaction temperature is above 120°C, and the boiling point of cyclohexane is 80.7°C, a large amount of cyclohexane will be carried by the air tail gas before it can react in time. out of the reactor. During the production process, it was detected that some cyclohexanol and cyclohexanone were taken out by the air exhaust, causing a lot of waste.

实用新型内容 Utility model content

本实用新型为了解决现有高压反应釜一般只能在封闭体系中进行反应,难以满足某些需要不断通入气体,同时需要不断排放出尾气,尤其是有液体参与化学反应的高温高压反应体系的问题,提供一种新型的高压反应釜装置。The utility model solves the problem that the existing high-pressure reactors generally can only react in a closed system, and it is difficult to meet certain requirements for continuously feeding gas and continuously discharging tail gas, especially for high-temperature and high-pressure reaction systems where liquids participate in chemical reactions. To solve the problem, a novel high-pressure reactor device is provided.

本实用新型提供以下技术解决方案:在高压反应釜外体上部安装冷却回流管路。所安装的冷却回流管路主要包括:与反应釜2相连的气体上行管路9;气体下行管路10;冷凝器14;通过进料阀17和进料管16连接的进料/回流三通管18。The utility model provides the following technical solutions: a cooling return pipeline is installed on the upper part of the outer body of the high-pressure reactor. The installed cooling return pipeline mainly includes: the gas uplink pipeline 9 connected with the reactor 2; the gas downlink pipeline 10; the condenser 14; the feed/reflux tee connected by the feed valve 17 and the feed pipe 16 Tube 18.

作为对上述技术方案的进一步改进,气体下行管路10、冷凝器14和进料/回流三通管18顺序连接。这样一来,气体的流动方向和冷凝液体的流动方向都是竖直向下,使得冷凝液体更容易回流入反应釜继续进行反应。As a further improvement to the above technical solution, the gas downlink pipeline 10, the condenser 14 and the feed/reflux tee pipe 18 are sequentially connected. In this way, the flow direction of the gas and the flow direction of the condensed liquid are both vertically downward, making it easier for the condensed liquid to flow back into the reactor to continue the reaction.

作为对上述技术方案更进一步的改进,在冷凝器14外体上部安装有放空管12,放空管12一端伸出冷凝器14外部,另一端伸进冷凝器14内部向下一直延伸到接近冷凝器14底部。这种结构的冷凝器,使得热气体在作为尾气被排出前,在冷凝管13中经历的路程更长,冷却效果更好。As a further improvement to the above technical solution, a vent pipe 12 is installed on the upper part of the outer body of the condenser 14. One end of the vent pipe 12 extends out of the condenser 14, and the other end extends into the interior of the condenser 14 and extends downward until close to The bottom of the condenser 14. The condenser with this structure makes the hot gas travel longer in the condensation pipe 13 before being discharged as exhaust gas, and the cooling effect is better.

本实用新型与现有技术相比有如下优点:由于冷却回流管路的安装,使得反应过程中所产生的大量气体冷凝形成回流,重新进入反应釜继续进行反应,提高了反应的转化率,节约了成本。现有技术中实验室常压反应装置的冷凝器通常安装在出料口和气体上行管路之间,冷凝液体可以回流入反应釜;但是对于高压反应装置来说,高压气体的流动方向和冷凝液体的流动方向相反,由于高压气体向上的推动作用,使得冷凝液体很难回流入反应釜继续反应,而本实用新型反应装置中冷凝器12所采用的安装方式使得气体的流动方向和冷凝液体的流动方向都是竖直向下,冷凝液体更容易回流入反应釜;此外,本实用新型反应装置中,冷凝器14的内部结构设计,使得热气体被冷凝管13冷却的距离增长,冷却效果更好。Compared with the prior art, the utility model has the following advantages: due to the installation of the cooling reflux pipeline, a large amount of gas generated in the reaction process is condensed to form a reflux, which re-enters the reactor to continue the reaction, improves the conversion rate of the reaction, saves costs. In the prior art, the condenser of the laboratory normal pressure reaction device is usually installed between the discharge port and the gas upstream pipeline, and the condensed liquid can flow back into the reactor; but for the high pressure reaction device, the flow direction of the high pressure gas and the condensation The flow direction of the liquid is opposite. Due to the upward push of the high-pressure gas, it is difficult for the condensed liquid to flow back into the reactor to continue the reaction. However, the installation method adopted by the condenser 12 in the reaction device of the present invention makes the flow direction of the gas consistent with the direction of the condensed liquid. The flow direction is all vertically downward, and it is easier for the condensed liquid to flow back into the reactor; in addition, in the reaction device of the present utility model, the internal structure design of the condenser 14 makes the distance that the hot gas is cooled by the condensing pipe 13 increase, and the cooling effect is better. good.

附图说明 Description of drawings

图1为本实用新型高压反应装置的结构示意图。Fig. 1 is the structural representation of the utility model high-pressure reaction device.

图1中,1.加热夹套;2.高压釜;3.搅拌器;4.温度计套管和热电偶温度计;5.出料口;6.压力表;7.搅拌电机;8.1#回流阀;9.气体上行管路;10.气体下行管路;11.放空阀;12.放空管;13.冷凝管;14.冷凝器;15.2#回流阀;16.进料管;17.进料阀;18.进料/回流三通管;19.高压釜进料阀;20.高压釜进料管。In Fig. 1, 1. Heating jacket; 2. Autoclave; 3. Stirrer; 4. Thermometer casing and thermocouple thermometer; 5. Discharge port; 6. Pressure gauge; 7. Stirring motor; 8.1# return valve ;9. Gas upstream pipeline; 10. Gas downstream pipeline; 11. Vent valve; 12. Vent pipe; 13. Condenser pipe; 14. Condenser; Material valve; 18. Feed/return tee pipe; 19. Autoclave feed valve; 20. Autoclave feed pipe.

具体实施方式 Detailed ways

下面结合附图和具体实施方式对本实用新型作进一步的描述。Below in conjunction with accompanying drawing and specific embodiment, the utility model is further described.

本实用新型高压反应装置的主体是一个高压反应釜,在其外体上部安装冷却回流管路,其结构主要包括进料管16、高压釜2、气体上行管路9、气体下行管路10、冷凝器14、进料/回流三通管18、放空管12以及若个阀门。The main body of the high-pressure reaction device of the present utility model is a high-pressure reaction kettle, and a cooling return pipeline is installed on the upper part of its outer body. Condenser 14, feed/reflux tee pipe 18, vent pipe 12 and several valves.

具体来说,高压釜2外部安装有加热套管1,高压釜2内部安装有搅拌器3、温度计套管和热电偶温度计4和高压釜进料管20。高压釜2的外体上部安装有压力表6和搅拌电机7。高压釜2的上部开有出料口5,按顺序依次连接1#回流阀8、气体上行管路9、气体下行管路10、冷凝器14、2#回流阀15、进料/回流三通管18和高压釜进料阀19。进料管16通过进料阀17和进料/回流三通管18连接。Specifically, a heating jacket 1 is installed outside the autoclave 2 , and an agitator 3 , a thermometer sleeve, a thermocouple thermometer 4 and an autoclave feed pipe 20 are installed inside the autoclave 2 . A pressure gauge 6 and a stirring motor 7 are installed on the upper part of the outer body of the autoclave 2 . The upper part of the autoclave 2 has a discharge port 5, which is connected in sequence with the 1# return valve 8, the gas upstream pipeline 9, the gas downstream pipeline 10, the condenser 14, the 2# return valve 15, and the feed/reflux tee Tube 18 and autoclave feed valve 19. The feed pipe 16 is connected with a feed/return tee pipe 18 through a feed valve 17 .

冷凝器14的空腔内部安装有弯曲的冷凝管13。在冷凝器14外体上部安装有放空管12,放空管12一端伸出冷凝器14外部,另一端伸进冷凝器14内部向下一直延伸到接近冷凝器14底部。A curved condenser pipe 13 is installed inside the cavity of the condenser 14 . An emptying pipe 12 is installed on the top of the outer body of the condenser 14 . One end of the emptying pipe 12 stretches out of the condenser 14 , and the other end extends into the inside of the condenser 14 and extends downward until close to the bottom of the condenser 14 .

图1中的各种箭头标出了该系统的工作原理。下面以利用空气氧化环己烷的反应为例,对本实用新型的技术方案所具备的功能及实现方式作进一步的描述。The various arrows in Figure 1 indicate how the system works. Taking the reaction of using air to oxidize cyclohexane as an example, the functions and implementation methods of the technical solution of the present invention will be further described.

(1)实线箭头标出了反应时,空气从进料管16进入,依次经过进料阀17,进料/回流三通管18,高压釜进料阀19,高压釜进料管20进入反应釜,在设定温度和压力下与环己烷和催化剂的混合物反应,部分未反应完全的环己烷、少量环己醇和环己酮受热变为蒸汽,随着空气尾气依次进入气体上行管路9、气体下行管路10和冷凝器14,在冷凝器14中,大部分环己烷、环己醇和环己酮被冷却变为液体,依次经过2#回流阀15、进料/回流三通管18和高压釜进料阀19重新回流入高压釜2继续参与反应,提高了反应的转化率,节约了成本;主要成分为氮气的空气尾气经由放空阀11从放空管12排出,通过调节放空阀11可以调节排放出的尾气流量的大小,并调节反应体系内部的压力。(1) When the solid line arrow marks the reaction, the air enters from the feed pipe 16, passes through the feed valve 17 successively, the feed/reflux tee pipe 18, the autoclave feed valve 19, and the autoclave feed pipe 20 enters The reaction kettle reacts with the mixture of cyclohexane and catalyst at the set temperature and pressure. Part of the unreacted cyclohexane, a small amount of cyclohexanol and cyclohexanone are heated and turned into steam, and enter the gas up pipe in sequence with the air tail gas Road 9, gas downlink pipeline 10 and condenser 14, in condenser 14, most of cyclohexane, cyclohexanol and cyclohexanone are cooled to become liquid, pass through 2# reflux valve 15, feed/reflux three The through pipe 18 and the autoclave feed valve 19 flow back into the autoclave 2 to continue to participate in the reaction, which improves the conversion rate of the reaction and saves costs; the air tail gas whose main component is nitrogen is discharged from the vent pipe 12 through the vent valve 11, and passes through Adjusting the vent valve 11 can adjust the flow rate of the discharged tail gas and adjust the pressure inside the reaction system.

(2)虚线箭头标出了反应时,冷凝管13中冷却介质的流动方向,冷却介质可以为盐水或循环自来水,采取从冷凝管13的下部进入口进入,从其上部排出口排出的方式。(2) dotted line arrow has marked reaction, and the flow direction of cooling medium in condensation tube 13, cooling medium can be salt water or circulating tap water, takes to enter from the bottom inlet of condensation tube 13, discharges from its top outlet.

当然,本实用新型的技术方案中的冷凝器14的结构不局限于上述形式,若有其它形式可使得气体的流动方向和冷凝液体的流动方向都是竖直向下,冷凝液体更容易回流入反应釜,也属于本实用新型的保护范围。Of course, the structure of the condenser 14 in the technical solution of the utility model is not limited to the above-mentioned form, if there are other forms, the flow direction of the gas and the flow direction of the condensed liquid are all vertically downward, and the condensed liquid is more likely to flow back Reactor also belongs to the protection scope of the present utility model.

Claims (3)

1.一种高压反应装置,其特征在于:在高压反应釜外体上部安装冷却回流管路,所安装的冷却回流管路主要包括与反应釜(2)相连的气体上行管路(9)、气体下行管路(10)、冷凝器(14)、通过进料阀(17)和进料管(16)连接的进料/回流三通管(18)。 1. A high-pressure reaction device, characterized in that: a cooling reflux pipeline is installed on the upper part of the high-pressure reactor outer body, and the installed cooling reflux pipeline mainly includes a gas uplink pipeline (9) connected to the reactor (2), Gas down line (10), condenser (14), feed/reflux tee (18) connected through feed valve (17) and feed pipe (16). 2.按照权利要求1所述的高压反应装置,其特征在于:气体下行管路(10)、冷凝器(14)和进料/回流三通管(18)顺序连接。 2. The high-pressure reaction device according to claim 1, characterized in that: the gas downlink pipeline (10), the condenser (14) and the feed/return three-way pipe (18) are sequentially connected. 3.按照权利要求1或2所述的高压反应装置,其特征在于:在冷凝器(14)外体上部安装有放空管(12),放空管(12)一端伸出冷凝器(14)外部,另一端伸进冷凝器(14)内部向下一直延伸到接近冷凝器(14)底部。  3. according to the described high-pressure reactor of claim 1 or 2, it is characterized in that: a vent pipe (12) is installed on the outer body top of the condenser (14), and one end of the vent pipe (12) stretches out of the condenser (14 ) outside, and the other end stretches into the condenser (14) and extends down to the bottom of the condenser (14). the
CN 201220177227 2012-04-25 2012-04-25 High-pressure reaction unit Expired - Fee Related CN202621125U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107175047A (en) * 2017-07-11 2017-09-19 南通协鑫热熔胶有限公司 A kind of autoclave steam retracting device
CN110433734A (en) * 2019-08-14 2019-11-12 南通鸿富达利化工有限公司 A kind of pinacoline condensation reaction exhaust apparatus
CN112954831A (en) * 2021-01-27 2021-06-11 浙江万森电热设备股份有限公司 Control device of explosion-proof electric heating equipment

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107175047A (en) * 2017-07-11 2017-09-19 南通协鑫热熔胶有限公司 A kind of autoclave steam retracting device
CN110433734A (en) * 2019-08-14 2019-11-12 南通鸿富达利化工有限公司 A kind of pinacoline condensation reaction exhaust apparatus
CN112954831A (en) * 2021-01-27 2021-06-11 浙江万森电热设备股份有限公司 Control device of explosion-proof electric heating equipment

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