Continuous stirring tank type reaction device and method for increasing cyclohexane non-catalytic oxidation conversion rate

Abstract

The invention provides a continuous stirred tank type reaction device and a method for increasing the non-catalytic oxidation conversion rate of cyclohexane. The reaction kettle is provided with a stirring paddle and a baffle plate, different combination types of the stirring paddle and the baffle plate can generate different fluid flow patterns, and the different fluid flow patterns are matched with different reaction temperatures, pressures and stirring rotating speeds, so that the non-catalytic oxidation conversion rate of cyclohexane can be improved; meanwhile, high selectivity of three target products including cyclohexanol, cyclohexanone and cyclohexyl hydroperoxide is kept. Under an orthogonal test condition, the optimized cyclohexane conversion rate is 8.1%-9.6%, and the selectivity is 87.2%-90.5%. Under similar conditions of a simulated industrial device, the optimized cyclohexane conversion rate is 8.2%, and the selectivity is 89.8%. Compared with a non-catalytic oxidation reaction of cyclohexane in a conventional continuous stirred tank reactor, the method has the advantages that the conversion rate of cyclohexane is increased by 60%-100%, and meanwhile, the selectivity of a target product is still kept at an ideal high level (87%-90%).

Description

Technical Field

[0001] The present invention relates to a hydrocarbon oxidation reaction, and more specifically to a continuous stirred tank reactor, a hardware setting combination of the reactor (stirring paddles with different properties + baffles), and the use of the continuous stirred tank reactor to perform a cyclohexane liquid phase non-catalyzed oxidation reaction through empirical optimization / orthogonal test optimization / simulated industrial condition optimization of reaction operating conditions, thereby achieving improved optimization of cyclohexane conversion rate. Background Art

[0002] The activation and functionalization of alkanes have very important scientific significance and great application value. Cyclohexane (CHX) oxidation is one of the most representative alkane oxidation reactions and is also a very important chemical production process. It is mainly used to prepare cyclohexanone and cyclohexanol (commonly known as KA oil), both of which are important raw materials for the production of caprolactam.

[0003] At present, most cyclohexanol and cyclohexanone are produced by cyclohexane liquid phase oxidation. Cyclohexane oxidation to prepare KA oil can be divided into non-catalytic oxidation and catalytic oxidation. In the oxidation reaction, according to the type of oxidant used, it can be divided into oxygen method and other oxidant methods, including H2O2, (CH3)3COOH (TBHP), NaClO, etc. Cyclohexane liquid phase air oxidation belongs to the free radical self-oxidation mechanism, involving the formation of cyclohexyl hydroperoxide (CHHP), and then the peroxide decomposes into cyclohexanol and cyclohexanone.

[0004] At present, the industrial processes for preparing cyclohexanol and cyclohexanone by oxidizing cyclohexane with oxygen mainly include boric acid catalytic oxidation, cobalt salt catalytic oxidation and peroxide oxidation. The domestic cyclohexane oxidation process mainly adopts the Dutch DSM process of non-catalytic oxidation. In industry, whether using water-soluble cobalt salt catalysis or non-catalytic oxidation of cyclohexane, in order to maintain a high selectivity of KA oil, the conversion rate is only 3%-5%. Therefore, the non-catalytic oxidation process for preparing cyclohexanol and cyclohexanone by oxidizing cyclohexane with oxygen is still under continuous improvement research, with the goal of maintaining the selectivity of cyclohexanone / cyclohexanol as much as possible while improving the conversion rate of cyclohexane.

[0005] The present invention aims to design a novel continuous stirred tank reactor to produce a liquid flow pattern that is beneficial to improving the conversion rate of cyclohexane without catalytic oxidation while maintaining high selectivity of the target product. The device can significantly improve the problems of low cyclohexane conversion rate and high energy consumption in the production of cyclohexanone in existing devices. Summary of the invention

[0006] The object of the present invention is to provide a continuous stirred tank reactor for improving the conversion rate of cyclohexane without catalytic oxidation. By setting different stirring paddle + baffle combinations, the reaction temperature, pressure and oxygen-nitrogen ratio are controlled and optimized, which can effectively solve the long-standing problem of low cyclohexane conversion rate in the prior art.

[0007] The main technical solution of the present invention is a continuous stirred tank reactor, characterized in that a freely replaceable stirring paddle and / or a plurality of baffles are arranged in the reactor of the reactor, and the stirring paddle and / or Different combinations of baffles can produce different fluid flow patterns.

[0008] According to one embodiment of the present application, the agitator is selected from a disc turbine type pitched blade, an open turbine type pitched blade or an open turbine type straight blade agitator, wherein the disc turbine type pitched blade agitator generates both radial flow and axial flow; the open turbine type pitched blade agitator generates a flow close to the axial flow; and the open turbine type straight blade agitator mainly generates a radial flow.

[0009] Preferably, the reaction of the present invention is carried out in a 1 L continuous stirred tank reactor. The typical values ​​of the stirring paddle parameters are: for the open turbine straight blade paddle / pitch blade paddle, the diameter is 30 mm, the blade width is 7 mm, the blade thickness is 1.5-2.0 mm, and the pitch angle is 45 degrees for the pitch blade paddle, and the number of blades is 6. For the disc turbine pitch blade paddle, the diameter is 30 mm, the center disc diameter is 20 mm, the blade width is 7 mm, the blade thickness is 1.5-2.0 mm, the pitch angle is 45 degrees, and the number of blades is 6.

[0010] According to one embodiment of the present application, the baffle is a long vertical baffle, the number of baffles is 2 to 4, and the width of the baffle is 1 / 12 to 1 / 10 of the diameter of the reactor inside the reactor.

[0011] Preferably, the reaction of the present invention is carried out in a 1 L continuous stirred tank reactor. Typical values ​​of the baffle parameters are: baffle width 9 mm, baffle length 130 mm, baffle thickness 2 mm, and baffle number 4. Baffle position: the upper end is slightly higher than the highest liquid level in the tank, and the lower end is close to the paddle.

[0012] According to one embodiment of the present application, the combination of the agitator paddle and / or baffle is: "disc turbine type pitched blade agitator paddle + no baffle", "open turbine type pitched blade agitator paddle + baffle" or "open turbine type straight blade agitator paddle + baffle". The combination of radial flow type agitator paddle + baffle can enhance the axial flow. The radial flow liquid discharged from the end of the radial flow blade carries the surrounding static and flowing liquids to the baffle to form an up and down circulation flow. The stirred liquid has both strong convection circulation and strong flow diffusion, presenting the best flow pattern for stirring, eliminating the stirring dead zone, and enhancing the gas-liquid interface mass transfer.

[0013] The present invention also provides a method for improving the conversion rate of cyclohexane non-catalytic oxidation, which is characterized by using the above-mentioned continuous stirred tank reaction device to carry out liquid-phase non-catalytic oxidation reaction of cyclohexane.

[0014] According to one embodiment of the present application, the reaction temperature is 150-170° C., the reaction time is 1-3 h, and the reaction pressure is 1.5-1.7 MPa.

[0015] According to one embodiment of the present application, the stirring speed is 400-550 rpm.

[0016] According to one embodiment of the present application, the volume ratio of oxygen to nitrogen is 0.21:1~0.5:1.

[0017] According to one embodiment of the present application, the total flow rate of the oxygen-nitrogen mixed gas is 200-523 mL / min.

[0018] According to one embodiment of the present application, the reaction temperature, pressure and stirring speed can be accurately adjusted and controlled online in real time by a computer.

[0019] The advantages of the present invention are as follows: by turning on the turbine straight-blade stirring paddle and setting the baffle at the same time, under the orthogonal test conditions, the cyclohexane conversion rate is 8.1%-9.6%, and the selectivity is 87%-90%. Under similar conditions of large-scale plant equipment in factories, the cyclohexane conversion rate is 8.2%, and the selectivity is 89.8%. Through simple technical transformation, the cyclohexane conversion rate level can be increased by 3-5 percentage points, while maintaining the target product selectivity of 85%-90%. In other words, while basically maintaining the existing main process operating conditions, the production efficiency of cyclohexane non-catalytic oxidation can be increased by 60% or more. Without increasing the number of reactors and the size of the reactor, the production capacity can be increased to 1.6 times or more of the original. The present invention can significantly reduce the production cost of unit mass products and effectively improve the comprehensive competitiveness of the production process. DETAILED DESCRIPTION

[0020] The present invention is described in detail below with reference to the embodiments.

[0021] In the specific implementation section below, the continuous stirred tank reactor of the present application, the hardware configuration combination of the device (stirring paddles + baffles with different properties) and the process for carrying out liquid-phase non-catalytic oxidation of cyclohexane are further introduced.

[0022] "Range" disclosed in the present invention is in the form of lower limit and upper limit. It can be one or more lower limits, and one or more upper limits respectively. A given range is defined by selecting a lower limit and an upper limit. The selected lower limit and upper limit define the boundaries of a particular range. All ranges that can be defined in this way are inclusive and combinable, i.e. any lower limit can be combined with any upper limit to form a range. For example, for a particular parameter, a range of 60-120 and 80-110 is listed, and it is understood that a range of 60-110 and 80-120 is also expected. In addition, if the minimum range values ​​1 and 2 are listed, and if the maximum range values ​​3, 4 and 5 are listed, the following ranges can all be expected: 1-3, 1-4, 1-5, 2-3, 2-4 and 2-5.

[0023] In the present invention, unless otherwise specified, the numerical range "ab" represents an abbreviation of any real number combination between a and b, where a and b are real numbers. For example, the numerical range "0-5" means that all real numbers between "0-5" have been listed in this document, and "0-5" is just an abbreviation of these numerical combinations.

[0024] In the present invention, unless otherwise specified, all embodiments and preferred embodiments mentioned herein can be combined with each other to form a new technical solution.

[0025] In the present invention, unless otherwise specified, all technical features and preferred features mentioned herein can be combined with each other to form a new technical solution.

[0026] In the present invention, if there is no special explanation, the "including" mentioned herein means open or closed. For example, the "including" may mean that other components not listed may also be included, or only the listed components may be included.

[0027] The invention develops an innovative continuous stirred tank reaction device, which includes any one of a disc turbine type inclined blade, an open turbine type inclined blade, and an open turbine type straight blade stirring paddle.

[0028] According to one embodiment of the present invention, the continuous stirred tank reactor may be equipped with long vertical baffles, and the number of baffles may be 2, 3, or 4.

[0029] According to one embodiment of the present invention, the continuous stirred tank reactor may be configured with a long vertical baffle, and the width of the baffle may be 1 / 12 of the inner kettle diameter, or 1 / 11 of the inner kettle diameter, or 1 / 10 of the inner kettle diameter, or within the numerical range obtained by combining any two of the above endpoints.

[0030] According to one embodiment of the present invention, the combination of the stirring paddle and the baffle of the continuous stirred tank reactor can be "pitch-blade disc turbine stirring paddle + no baffle", or "open turbine pitch-blade stirring paddle + baffle", or "open turbine straight-blade stirring paddle + baffle".

[0031] According to one embodiment of the present invention, the reaction is carried out at a temperature of 150-170°C for 1.0 to 3 hours, for example, the catalytic temperature can be 150-160°C, or 160-170°C, and the continuous reaction time can be 1-1.5 hours, or 1.5-2 hours, or 2-3 hours, or within the numerical range obtained by combining any two of the above endpoints.

[0032] According to one embodiment of the present invention, the reaction is carried out at a pressure of 1.5-1.7 MPa, for example, the reaction pressure may be 1.50-1.55 MPa, or 1.55-1.60 MPa, or 1.60-1.70 MPa, or within the numerical range obtained by combining any two of the above endpoints.

[0033] According to one embodiment of the present invention, the reaction is carried out at a stirring speed of 400-550 rpm, for example, the stirring speed may be 400-450 rpm, or 450-500 rpm, or 500-550 rpm, or within a numerical range obtained by combining any two of the above endpoints.

[0034] According to one embodiment of the present invention, the reaction is carried out at an oxygen-nitrogen volume ratio of 0.21 to 0.5, for example, the oxygen-nitrogen volume ratio can be 0.21-0.3, or 0.30-0.40, or 0.40-0.50, or within the numerical range obtained by combining any two of the above endpoints.

[0035] According to one embodiment of the present invention, the reaction is carried out at a total flow rate of the oxygen-nitrogen mixture of 200-523 mL / min, for example, the total flow rate of the oxygen-nitrogen mixture may be 200-300 mL / min, or 300-400 mL / min, or 400-450 mL / min, or 450-523 mL / min, or within a numerical range obtained by combining any two of the above endpoints.

[0036] The present application is described below in the form of specific examples, and its purpose is to better understand the content of the present application. It should be understood that these examples are merely illustrative and non-restrictive. The reagents used in the examples are conventionally purchased from the market unless otherwise stated. The methods and conditions used in the examples are conventional methods and conditions unless otherwise specified. All raw materials used in the following examples are analytically pure and are used directly without further purification. Example 1

[0037] This embodiment uses a disc turbine type oblique blade stirring paddle + baffleless combination. Add 500 mL of cyclohexane to the inner kettle of the continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in the closed state. Set the reaction pressure to 1.6 Mpa on the computer screen. Set the nitrogen flow rate to 160 mL / min on the computer screen. Set the reaction temperature to 150C on the computer screen, and press the power key to turn on the power heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 40 mL / min on the computer. Start the reaction with timing. At a specific stage in the reaction process, the liquid sample is sampled according to the following steps: first open the switch valve on the sampling tube, then open the needle valve very carefully and slowly to drive away the dead volume, and then collect the liquid sample in a sample bottle. When collecting the liquid sample next time, in order to prevent the collection of the condensed sample from the previous sampling in the tube, the first part of the liquid sample should be collected in another sample bottle (discarded), and the latter part of the liquid sample is collected and derivatized and chromatographically analyzed. After 3 hours of reaction, the sample was analyzed and the conversion rate of cyclohexane was measured to be 4.7%, and the selectivity of the target product cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 36.5%, 29.4%, and 15.8%, respectively, and the total selectivity of the target product was 81.7%. Example 2

[0038] This embodiment uses a disc turbine type inclined blade stirring paddle + baffleless combination. Add 500 mL of cyclohexane to the inner kettle of the continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in the closed state. Set the reaction pressure to 1.5 Mpa on the computer screen. Set the nitrogen flow rate to 160 mL / min on the computer screen. Set the reaction temperature to 160C on the computer screen, and press the power key to turn on the power heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 40 mL / min on the computer. Start the reaction. After 3 hours of reaction, sample analysis was performed and the conversion rate of cyclohexane was measured to be 5.3%. The selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 44.1%, 20.7%, and 10.4%, respectively, and the total selectivity of the target products was 76.3%. Example 3

[0039] This embodiment uses a disc turbine type oblique blade stirring paddle + baffleless combination. Add 500 mL of cyclohexane to the inner kettle of the continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in the closed state. Set the reaction pressure to 1.6 Mpa on the computer screen. Set the nitrogen flow rate to 160 mL / min on the computer screen. Set the reaction temperature to 170C on the computer screen, and press the power key to turn on the power heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 40 mL / min on the computer. Start the reaction. After 2 hours of reaction, sample analysis was performed and the conversion rate of cyclohexane was measured to be 3.5%. The selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 46.2%, 17.5%, and 10.8%, respectively, and the total selectivity of the target products was 74.5%. Example 4

[0040] This embodiment uses a disc turbine type oblique blade stirring paddle + baffleless combination. Add 500 mL of cyclohexane to the inner kettle of the continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in the closed state. Set the reaction pressure to 1.7 Mpa on the computer screen. Set the nitrogen flow rate to 160 mL / min on the computer screen. Set the reaction temperature to 160C on the computer screen, and press the power key to turn on the power heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 40 mL / min on the computer. Start the reaction. After 2 hours of reaction, take a sample for analysis, and the conversion rate of cyclohexane is 1.9%, the selectivity of the target product cyclohexanol, cyclohexanone, and cyclohexyl peroxide is 5.5%, 26.2%, and 40.6%, respectively, and the total selectivity of the target product is 72.3%. Example 5

[0041] This embodiment adopts a combination of an open turbine-type inclined blade stirring paddle + a baffle. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring connection. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in the closed state. Set the reaction pressure to 1.6 Mpa on the computer screen. Set the nitrogen flow rate to 160 mL / min on the computer screen. Set the reaction temperature to 160C on the computer screen, and press the power key to turn on the power heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, sample analysis was performed and the conversion rate of cyclohexane was found to be 10.1%. The selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 50.1%, 26.3%, and 7.9%, respectively, and the total selectivity of the target products was 84.3%. Example 6

[0042] This embodiment adopts a combination of an open turbine-type inclined blade stirring paddle + a baffle. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring connection. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in the closed state. Set the reaction pressure to 1.5 Mpa on the computer screen. Set the nitrogen flow rate to 240 mL / min on the computer screen. Set the reaction temperature to 160C on the computer screen, and press the power key to turn on the power heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, take a sample for analysis, and the conversion rate of cyclohexane is 9.3%, the selectivity of the target product cyclohexanol, cyclohexanone, and cyclohexyl peroxide is 45.0%, 29.0%, and 2.9%, respectively, and the total selectivity of the target product is 76.9%. Example 7

[0043] This embodiment adopts a combination of an open turbine-type inclined blade stirring paddle + a baffle. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring connection. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in a closed state. Set the reaction pressure to 1.5 Mpa on the computer screen. Set the nitrogen flow rate to 160 mL / min on the computer screen. Set the reaction temperature to 165C on the computer screen, and press the power key to power on the heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, sample analysis was performed and the conversion rate of cyclohexane was measured to be 8.0%, and the selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 49.0%, 22.9%, and 6.3%, respectively, and the total selectivity of the target products was 78.2%. Example 8

[0044] This embodiment adopts a combination of an open turbine straight-blade stirring paddle + a baffle. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring connection. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in the closed state. Set the reaction pressure to 1.6 Mpa on the computer screen. Set the nitrogen flow rate to 160 mL / min on the computer screen. Set the reaction temperature to 160C on the computer screen, and press the power key to turn on the power heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, take a sample for analysis, and the conversion rate of cyclohexane is 10.3%, the selectivity of the target product cyclohexanol, cyclohexanone, and cyclohexyl peroxide is 49.5%, 24.6%, and 11.5%, respectively, and the total selectivity of the target product is 85.6%. Example 9

[0045] This embodiment adopts a combination of open turbine straight blade stirring paddle + baffle. Add 500 mL of cyclohexane to the inner kettle of the continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in the closed state. Set the reaction pressure to 1.5 Mpa on the computer screen. Set the nitrogen flow rate to 160 mL / min on the computer screen. Set the reaction temperature to 165C on the computer screen, and press the power key to turn on the power heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, take a sample for analysis, and the conversion rate of cyclohexane is 10.2%, the selectivity of the target product cyclohexanol, cyclohexanone, and cyclohexyl peroxide is 51.7%, 23.8%, and 6.2%, respectively, and the total selectivity of the target product is 81.7%. Example 10

[0046] This embodiment adopts a combination of open turbine straight blade stirring paddle + baffle. Add 500 mL of cyclohexane to the inner kettle of the continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in the closed state. Set the reaction pressure to 1.5 Mpa on the computer screen. Set the nitrogen flow rate to 240 mL / min on the computer screen. Set the reaction temperature to 160C on the computer screen, and press the power key to turn on the power heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, sample analysis was performed and the conversion rate of cyclohexane was measured to be 9.0%, and the selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 48.8%, 22.2%, and 14.8%, respectively, and the total selectivity of the target products was 85.8%. Embodiment 11

[0047] This embodiment uses a combination of a turbine straight-blade stirring paddle and a baffle to optimize the conditions of an orthogonal experiment. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring connection. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 550 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in a closed state. Set the reaction pressure to 1.55 Mpa on the computer screen. Set the nitrogen flow rate to 240 mL / min on the computer screen. Set the reaction temperature to 160C on the computer screen, and press the power key to power on the heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, take a sample for analysis, and the conversion rate of cyclohexane is 9.6%, the selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide are 47.7%, 30.9%, and 8.6%, respectively, and the total selectivity of the target products is 87.2%. Example 12

[0048] This embodiment uses a combination of a turbine straight-blade stirring paddle and a baffle to optimize the conditions of an orthogonal experiment. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring connection. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 450 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in a closed state. Set the reaction pressure to 1.60 Mpa on the computer screen. Set the nitrogen flow rate to 280 mL / min on the computer screen. Set the reaction temperature to 165C on the computer screen, and press the power key to power on the heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, sample analysis was performed and the conversion rate of cyclohexane was measured to be 9.8%, and the selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 54.2%, 23.4%, and 7.3%, respectively, and the total selectivity of the target products was 84.9%. Embodiment 13

[0049] This embodiment uses a combination of a turbine straight-blade stirring paddle and a baffle to optimize the conditions of an orthogonal experiment. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring connection. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in a closed state. Set the reaction pressure to 1.55 Mpa on the computer screen. Set the nitrogen flow rate to 160 mL / min on the computer screen. Set the reaction temperature to 165C on the computer screen, and press the power key to power on the heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, take a sample for analysis, and the conversion rate of cyclohexane is 10.3%, the selectivity of the target product cyclohexanol, cyclohexanone, and cyclohexyl peroxide is 53.9%, 24.1%, and 7.2%, respectively, and the total selectivity of the target product is 85.2%. Embodiment 14

[0050] This embodiment uses a combination of a turbine straight-blade stirring paddle and a baffle to optimize the conditions of an orthogonal experiment. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring connection. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 550 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in a closed state. Set the reaction pressure to 1.65 Mpa on the computer screen. Set the nitrogen flow rate to 280 mL / min on the computer screen. Set the reaction temperature to 150C on the computer screen, and press the power key to power on the heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, sample analysis was performed and the conversion rate of cyclohexane was measured to be 7.3%, and the selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 38.5%, 21.3%, and 34.9%, respectively, and the total selectivity of the target product was 94.7%. Embodiment 15

[0051] This embodiment uses a combination of a turbine straight-blade stirring paddle and a baffle to optimize the conditions of an orthogonal experiment. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring connection. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in a closed state. Set the reaction pressure to 1.60 Mpa on the computer screen. Set the nitrogen flow rate to 240 mL / min on the computer screen. Set the reaction temperature to 150C on the computer screen, and press the power key to power on the heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, take a sample for analysis, and the conversion rate of cyclohexane is 6.8%, the selectivity of the target product cyclohexanol, cyclohexanone, and cyclohexyl peroxide is 35.8%, 19.6%, and 38.3%, respectively, and the total selectivity of the target product is 93.7%. Example 16

[0052] This embodiment uses a combination of a turbine straight-blade stirring paddle and a baffle to optimize the conditions of an orthogonal experiment. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the reactor stirring and connecting cooling jacket. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 450 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in a closed state. Set the reaction pressure to 1.65 Mpa on the computer screen. Set the nitrogen flow rate to 160 mL / min on the computer screen. Set the reaction temperature to 160C on the computer screen, and press the power key to power on the heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, sample analysis was performed and the conversion rate of cyclohexane was measured to be 9.8%, and the selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 48.8%, 25.0%, and 9.9%, respectively, and the total selectivity of the target products was 83.7%. Embodiment 17

[0053] This embodiment uses a combination of a turbine straight-blade stirring paddle and a baffle to optimize the conditions of an orthogonal experiment. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the reactor stirring and connecting cooling jacket. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 450 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in a closed state. Set the reaction pressure to 1.50 Mpa on the computer screen. Set the nitrogen flow rate to 240 mL / min on the computer screen. Set the reaction temperature to 155C on the computer screen, and press the power key to power on the heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, sample analysis was performed and the conversion rate of cyclohexane was measured to be 8.1%. The selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 46.9%, 22.4%, and 21.2%, respectively, and the total selectivity of the target products was 90.5%. Embodiment 18

[0054] This embodiment uses a combination of a turbine straight-blade stirring paddle and a baffle to optimize the conditions of an orthogonal experiment. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the reactor stirring and connecting cooling jacket. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 550 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in a closed state. Set the reaction pressure to 1.50 Mpa on the computer screen. Set the nitrogen flow rate to 200 mL / min on the computer screen. Set the reaction temperature to 165C on the computer screen, and press the power key to power on the heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, take a sample for analysis, and the conversion rate of cyclohexane is 10.7%, the selectivity of the target product cyclohexanol, cyclohexanone, and cyclohexyl peroxide is 53.3%, 21.9%, and 8.4%, respectively, and the total selectivity of the target product is 85.6%. Embodiment 19

[0055] This embodiment uses a combination of a turbine straight-blade stirring paddle and a baffle to optimize the conditions of an orthogonal experiment. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the cooling jacket connected to the reactor stirring connection. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Turn on the stirring controller and set the stirring speed to 550 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time make sure that its bypass is in a closed state. Set the reaction pressure to 1.60 Mpa on the computer screen. Set the nitrogen flow rate to 160 mL / min on the computer screen. Set the reaction temperature to 155C on the computer screen, and press the power key to power on the heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC, and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 2 hours of reaction, sample analysis was performed and the conversion rate of cyclohexane was measured to be 7.1%, and the selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 35.2%, 18.4%, and 39.4%, respectively, and the total selectivity of the target product was 93.0%. Embodiment 20

[0056] This embodiment uses a combination of a turbine straight-blade stirring paddle + a baffle to simulate the cyclohexane non-catalytic oxidation experiment in industry for condition optimization. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the reactor stirring and connecting cooling jacket. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8Mpa. Turn on the stirring controller and set the stirring speed to 550 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time determine that its bypass is in a closed state. Set the reaction pressure to 1.10Mpa on the computer screen. Set the nitrogen flow rate to 376 mL / min on the computer screen. Set the reaction temperature to 170C on the computer screen and press the power button to turn on the heating. When the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC and set the oxygen flow rate to 100 mL / min on the computer. Start the reaction. After 1.5 hours of reaction, take a sample for analysis and the conversion rate of cyclohexane is 8.2%. The selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide are 57.3%, 21.1%, and 8.3%, respectively. The total selectivity of the target product is 86.7%. Embodiment 21

[0057] This embodiment uses a combination of a turbine straight-blade stirring paddle + a baffle to simulate the cyclohexane non-catalytic oxidation experiment in industry for condition optimization. Add 500 mL of cyclohexane to the inner kettle of a continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and pass tap water to the reactor stirring and connecting cooling jacket. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8Mpa. Turn on the stirring controller and set the stirring speed to 550 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time determine that its bypass is in a closed state. Set the reaction pressure to 1.10Mpa on the computer screen. Set the nitrogen flow rate to 300 mL / min on the computer screen. Set the reaction temperature to 165°C on the computer screen and press the power button to turn on the heating. When the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC and set the oxygen flow rate to 80 mL / min on the computer. Start the reaction. After 1.5 hours of reaction, take a sample for analysis and the conversion rate of cyclohexane is 7.3%. The selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide are 52.1%, 19.7%, and 18.7%, respectively. The total selectivity of the target product is 90.5%. Embodiment 22

[0058] This embodiment uses a turbine straight-blade stirring paddle + baffle combination to simulate the industrial cyclohexane non-catalytic oxidation experiment for condition optimization. Add 500 mL of cyclohexane to the inner kettle of the continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and the reactor stirring connection cooling jacket is passed through tap water. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time determine that its bypass is in a closed state. Set the reaction pressure to 1.10Mpa on the computer screen. Set the nitrogen flow rate to 413 mL / min on the computer screen. Set the reaction temperature to 170°C on the computer screen and press the power button to turn on the heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC and set the oxygen flow rate to 110 mL / min on the computer. Start the reaction. After 1.5 hours of reaction, sample analysis was performed and the conversion rate of cyclohexane was measured to be 8.2%. The selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 53.7%, 21.2%, and 15.0%, respectively, and the total selectivity of the target product was 89.9%. Embodiment 23

[0059] This embodiment uses a turbine straight-blade stirring paddle + baffle combination to simulate the industrial cyclohexane non-catalytic oxidation experiment for condition optimization. Add 500 mL of cyclohexane to the inner kettle of the continuous stirred tank reactor, carefully close the reactor cover and seal the reactor (closing the reactor should be done slowly). Open the low-temperature circulating water bath, pass the circulating cooling water, and the reactor stirring connection cooling jacket is passed through tap water. Turn on the computer and related control software. Add an ice-water mixture to the low-temperature cooling tank. Open the nitrogen cylinder and make the secondary gauge pressure 1.5~1.8 Mpa. Open the oxygen cylinder and make the secondary gauge pressure 1.5~1.8Mpa. Turn on the stirring controller and set the stirring speed to 500 rpm. Open the switch valves on both sides of the nitrogen MFC, and then open the switch valves on both sides of the pneumatic diaphragm valve, and at the same time determine that its bypass is in a closed state. Set the reaction pressure to 1.10Mpa on the computer screen. Set the nitrogen flow rate to 376 mL / min on the computer screen. Set the reaction temperature to 165°C on the computer screen and press the power button to turn on the heating. After the reactor temperature reaches the set temperature and stabilizes, open the switch valves on both sides of the oxygen MFC and set the oxygen flow rate to 100 mL / min on the computer. Start the reaction. After 1.5 hours of reaction, sample analysis was performed and the conversion rate of cyclohexane was measured to be 7.0%. The selectivity of the target products cyclohexanol, cyclohexanone, and cyclohexyl peroxide was 51.7%, 20.4%, and 16.6%, respectively, and the total selectivity of the target product was 88.7%.

[0060] The results of the embodiment show that the ideal results can be obtained by using the hardware setting of "open turbine straight blade stirring paddle + baffle". At a reaction temperature of more than 160°C, a reaction pressure of 1.5-1.6 MPa, an O2 / N2 mixed gas flow rate of 240-320 mL / min, an O2 / N2 volume ratio of 1:3~1:2, and a reaction time of 2 h, the cyclohexane conversion rate can reach 9-10%, and the selectivity can be maintained at about 85%. Orthogonal experiments show that the optimized reaction performance is a cyclohexane conversion rate of 8.1%-9.6% and a selectivity of 87.2%-90.5%. Simulating the conditions of the cyclohexane non-catalytic oxidation reaction of industrial equipment, the cyclohexane conversion rate on the device of the present invention is more than 8%, and the target product selectivity can reach 89%. Under the premise of maintaining the selectivity of the target product, the cyclohexane conversion rate is increased by 60-100%.

Claims

1. A continuous stirred tank reactor, characterized in that A freely replaceable stirring paddle and / or a plurality of baffles are arranged in the reactor of the reaction device. and / or Different combinations of baffles can produce different fluid flow patterns.

2. The continuous stirred tank reactor according to claim 1, characterized in that The agitator is selected from a disc turbine type pitched blade, an open turbine type pitched blade or an open turbine type straight blade agitator, wherein the disc turbine type pitched blade agitator generates both radial flow and axial flow; the open turbine type pitched blade agitator generates a nearly axial flow; and the open turbine type straight blade agitator mainly generates a radial flow.

3. The continuous stirred tank reactor according to claim 1, characterized in that The baffles are long vertical strips, the number of baffles is 2 to 4, and the width of the baffles is 1 / 12 to 1 / 10 of the diameter of the reactor.

4. The continuous stirred tank reactor according to any one of claims 1 to 3, characterized in that The combination of the stirring paddle and / or the baffle is: "disk turbine type pitched blade stirring paddle + no baffle", "open turbine type pitched blade stirring paddle + baffle" or "open turbine type straight blade stirring paddle + baffle".

5. A method for improving the conversion rate of cyclohexane without catalytic oxidation, characterized in that The continuous stirred tank reactor according to any one of claims 1 to 4 is used to carry out the liquid phase non-catalyzed oxidation reaction of cyclohexane.

6. The method according to claim 6, characterized in that Reaction temperature: 150-170°C, reaction time: 1-3h, reaction pressure: 1.5-1.7 MPa.

7. The method according to claim 6, characterized in that Stirring speed: 400-550 rpm.

8. The method according to claim 6, characterized in that The volume ratio of oxygen to nitrogen is 0.21:1~0.5:

1.

9. The method according to claim 6, characterized in that The total flow rate of oxygen and nitrogen mixture is 200-523 mL / min.

10. The method according to claim 1, characterized in that The reaction temperature, pressure and stirring speed are accurately adjusted and controlled online in real time by a computer.