An apparatus and method for the one-step oxidation of cyclohexane to produce alcohol-ketone dicarboxylate

Abstract

An apparatus for one-step oxidation of cyclohexane to generate alcohol-ketone dicarboxylate esters, comprising at least one reactor, a first washing tower and a second washing tower. A washing chamber is provided at the top of the reactor, and an oxygen source distributor is provided at the bottom. A first feed inlet is provided at the bottom of the reactor, and an overflow port is provided on the side wall. A second feed inlet is provided in the washing chamber, and an exhaust port is provided at the top. A first air inlet is provided at the lower part of the side wall of the first washing tower, and a first washing liquid inlet is provided at the upper part of the side wall. A second air inlet is provided at the lower part of the side wall of the second washing tower, and a second washing liquid inlet is provided at the upper part of the side wall. The first feed inlet and the second feed inlet of the reaction tower are both connected to a cyclohexane source, the exhaust port is connected to the first air inlet, the first washing liquid inlet is connected to a desalinated water source and a liquid caustic source, the second air inlet is connected to the top of the first washing tower through a pipeline, and the second washing liquid inlet is connected to an alcohol-ketone source. The structure of the present invention is simple and convenient for maintenance, and on the basis of ensuring long-term normal and stable operation, environmental pollution can be effectively avoided.

Description

Technical Field

[0001] The present invention relates to the chemical industry field, and particularly relates to an apparatus and a method for directly oxidizing cyclohexane to generate alcohol-ketone dicarboxylate. Background Art

[0002] Cyclohexane is an important chemical intermediate. When cyclohexane is oxidized to generate alcohol-ketone dicarboxylate, cyclohexanol, cyclohexanone and dicarboxylate therein are all important chemical raw materials and can be used in the production of caprolactam and nylon-66. At present, catalytic oxidation of cyclohexane has replaced non-catalytic oxidation of cyclohexane. Compared with non-catalytic oxidation, catalytic oxidation of cyclohexane has the following advantages:

[0003] 1. The required amount of catalyst is small, the process flow is short, the number of equipment units is significantly reduced, and the total investment of the device is small;

[0004] 2. The operating temperature in the process of catalytic oxidation of cyclohexane is low, and the process is simple and reliable;

[0005] 3. The process flows of the supporting decomposition system and separation system are short, and energy is saved and consumption is reduced.

[0006] However, for the production equipment currently in use, since compressed air is used as the oxygen source, excessive air carries cyclohexane and alcohol-ketone dicarboxylate products and enters the scrubbing tower through the tail gas pipeline. The carried dicarboxylate crystallizes in the tail gas pipeline, resulting in blockage of the tail gas pipeline. In addition, the supporting scrubbing tower cannot effectively remove the organic substances mixed in the tail gas, which also causes environmental pollution.

[0007] Therefore, how to ensure the long-term normal operation of the production equipment is an urgent problem to be solved by those skilled in the art. Summary of the Invention

[0008] One of the purposes of the present invention is to provide, in view of the deficiencies of the prior art, an apparatus for directly oxidizing cyclohexane to generate alcohol-ketone dicarboxylate, which has a simple structure and is convenient for maintenance, and can effectively avoid environmental pollution on the basis of ensuring long-term normal and stable operation.

[0009] Another purpose of the present invention is to provide a method for synthesizing alcohol-ketone dicarboxylate by using the above apparatus, which has a simple and reliable process and can effectively meet the actual needs of enterprises.

[0010] One of the technical solutions to achieve the purpose of the present invention is: a device for the one-step oxidation of cyclohexane to produce alcohol-ketone dicarboxylate esters, which includes a reaction system and a tail gas treatment system. The reaction system includes at least one reactor. A washing chamber is provided at the top of the reactor, and an oxygen source distributor is provided at the bottom. A first feed port is provided at the bottom of the reactor, and an overflow port is provided on the side wall. A second feed port is provided in the washing chamber, and a first exhaust port is provided at the top. The tail gas treatment system includes a first washing tower and a second washing tower. A washing liquid circulation pipeline is provided at the bottom of each washing tower. A first air inlet is provided at the lower part of the side wall of the first washing tower, and a first washing liquid inlet is provided at the upper part of the side wall. A second air inlet is provided at the lower part of the side wall of the second washing tower, and a second washing liquid inlet is provided at the upper part of the side wall. The first feed port and the second feed port of the reaction system are both connected to a cyclohexane source. The first exhaust port is connected to the first air inlet of the tail gas treatment system. The first washing liquid inlet of the tail gas treatment system is connected to a desalinated water source and a liquid alkali source. The second air inlet is connected to the top of the first washing tower through a pipeline. The second washing liquid inlet is connected to an alcohol-ketone source.

[0011] Further, it further includes a third washing tower. An outlet is provided at the bottom of the third washing tower, a third air inlet is provided at the lower part of the side wall, and a third washing liquid inlet is provided at the upper part of the side wall. The outlet is connected to the first feed port and the second feed port of the reaction system. The third air inlet is connected to the first exhaust port of the reactor. The first air inlet of the first washing tower is connected to the top of the third washing tower through a pipeline. The third washing liquid inlet is connected to a cyclohexane source.

[0012] Preferably, the number of the third washing towers is two, which are connected in series as a whole. The oxygen source distributor is connected to a compressed air source and / or a compressed oxygen source.

[0013] Preferably, the first washing tower, the second washing tower, and the third washing tower are all packed towers. Each air inlet is located below the packing of the corresponding washing tower, and each washing liquid inlet is located above the packing of the corresponding washing tower.

[0014] Further, a second exhaust port is provided at the top of the reactor. A valve is provided at the second exhaust port, which is connected to the air inlet of the washing tower in parallel after being connected in parallel with the first exhaust port.

[0015] Preferably, the number of the reactors is multiple, which are connected in series as a whole. The overflow port of the upstream reactor is connected to the first feed port of the downstream reactor, and the second feed ports of each reactor are connected in parallel.

[0016] Further, it further includes a distillation system. The liquid inlet end of the distillation system is connected to the overflow port of the reactor through a buffer tank. The distillation system is provided with a desalinated water pipe.

[0017] The technical solution for achieving the second object of the present invention is: A method for synthesizing alkyd diester using any of the above-mentioned devices, comprising the following steps:

[0018] 1) Add lye and demineralized water through the first washing liquid inlet and circulate in the first washing tower. Add alkyd through the second washing liquid inlet and circulate in the second washing tower. Add cyclohexane through the third washing liquid inlet. The cyclohexane converges at the bottom of the first washing tower, mixes with the catalyst, and then enters the reactor through the first feed port and the second feed port. The catalyst is a transition metal porphyrin compound, and the addition amount is 1-5 ppm;

[0019] 2) Excess air enters the reactor through the oxygen source distributor, and an oxidation reaction is carried out while controlling the temperature at 140-150 °C and the pressure at 0.9-1.1 Mpa;

[0020] 3) The reaction liquid containing alkyd diester is discharged from the overflow port of the reactor and subjected to rectification to obtain an alkyd diester product;

[0021] 4) Excess air or oxygen is washed in the washing chamber and then sent to the tail gas treatment system. After being washed with cyclohexane, lye, and alkyd in sequence, it is discharged for incineration.

[0022] Preferably, in step 1), the flow rate ratio of the first feed port to the second feed port is 25:1. The catalyst is any one or several of cobalt tetraphenylporphyrin, porphyrin iron, porphyrin manganese, and porphyrin copper. In step 2), the temperature is 142-146 °C, the pressure is 0.95-1.05 Mpa, and the volume ratio of the flow rate of air to cyclohexane is 40-80:1

[0023] Further, in step 3), the rectification is to evaporate and concentrate by controlling the temperature at 75-90 °C in the distillation system. Demineralized water is added to the bottom liquid of the tower, and the product containing alkyd diester is discharged.

[0024] Adopting the above technical solution has the following beneficial effects:

[0025] 1. The device for the one-step oxidation of cyclohexane to generate alcohol-ketone dicarboxylate ester of the present invention includes a reaction system and a tail gas treatment system. Among them, the reaction system is used for the one-step oxidation to generate alcohol-ketone and by-product dicarboxylate ester, and the tail gas treatment system is used for washing the reaction tail gas. The reaction system includes at least one reactor. A washing chamber is arranged at the top of the reactor, and an oxygen source distributor is arranged at the bottom. A first feed port is arranged at the bottom of the reactor, and an overflow port is arranged on the side wall. A second feed port is arranged in the washing chamber, and a first exhaust port is arranged at the top. Air or oxygen is evenly distributed at the bottom of the reactor through the oxygen source distributor, and the excessive air or oxygen is discharged out of the reactor through the washing chamber and the first exhaust port of the reactor. Both the first feed port and the second feed port are used to add cyclohexane into the reactor, and the cyclohexane added through the second feed port is used to wash the tail gas discharged through the washing chamber, reducing the content of organic substances carried by the discharged tail gas. In addition, by flushing the washing chamber with cyclohexane, the blockage of the pipeline caused by the crystallization of the carried organic substances (mainly dicarboxylic acid) in the tail gas pipeline can be avoided, ensuring the long-term normal operation of the reactor. The tail gas treatment system includes a first washing tower and a second washing tower. A washing liquid circulation pipeline is arranged at the bottom of each washing tower to make full use of the washing liquid. A first air inlet is arranged at the lower part of the side wall of the first washing tower, and a first washing liquid inlet is arranged at the upper part of the side wall. A second air inlet is arranged at the lower part of the side wall of the second washing tower, and a second washing liquid inlet is arranged at the upper part of the side wall. The first feed port and the second feed port of the reaction system are both connected to the cyclohexane source for adding cyclohexane. The first exhaust port is connected to the first air inlet of the tail gas treatment system. The first washing liquid inlet of the tail gas treatment system is connected to the desalted water source and the liquid alkali source. The second air inlet is connected to the top of the first washing tower through a pipeline. The second washing liquid inlet is connected to the alcohol-ketone source. The tail gas after preliminary treatment enters the first washing tower through the first air inlet. Using alkali liquor and desalted water as washing liquids, after eluting most of the dicarboxylic acid (reacting with the alkali liquor and being easily soluble in desalted water) in it, the tail gas carrying alcohol-ketone (cyclohexanol, cyclohexanone) enters the second washing tower through the second air inlet. Using alcohol-ketone as the washing liquid, after eluting most of the alcohol-ketone in it, the tail gas is discharged from the tail gas treatment system, and the content of organic substances in it can be reduced to less than 0.5%.

[0026] 2. It further includes a third washing tower. An outlet is provided at the bottom of the third washing tower, a third air inlet is provided at the lower part of the side wall, and a third washing liquid inlet is provided at the upper part of the side wall. The outlet is connected to the first feed port and the second feed port of the reaction system. The third air inlet is connected to the first exhaust port of the reactor. The first air inlet of the first washing tower is connected to the top of the third washing tower through a pipeline. The third washing liquid inlet is connected to a cyclohexane source. That is, cyclohexane as a raw material first serves as a washing liquid to pass through the third washing tower and enters the reactor through the first feed port and the second feed port. In the third washing tower, the tail gas that has undergone preliminary treatment is washed, so that the cyclohexane and part of the alcohol ketone carried in the tail gas flow back to the reactor. In addition, the tail gas is cooled, and the washing and absorption efficiency of the downstream washing tower is also improved.

[0027] 3. A second exhaust port is provided at the top of the reactor. A valve is provided at the second exhaust port. After being connected in parallel with the first exhaust port, it is connected to the air inlet of the washing tower. According to the actual situation, the tail gas can be discharged from the reactor through the second exhaust port to meet the actual needs of the enterprise.

[0028] 4. It further includes a distillation system. The liquid inlet end of the distillation system is connected to the overflow port of the reactor through a buffer tank. The distillation system is provided with a desalinated water pipe. The reaction liquid (oxidation liquid) containing alcohol ketone and dibasic acid ester overflows and enters the buffer tank, and then enters the distillation system in a steady flow. By controlling the distillation temperature of the distillation system, the small molecule raw materials and impurities are separated in the form of vapor phase, while the alcohol ketone and dibasic acid ester are retained in the tower bottom liquid, and the concentration is increased. Desalinated water is added through the desalinated water pipe to dissolve as much dibasic acid as possible, and finally a high-concentration alcohol ketone and dibasic acid ester solution is discharged.

[0029] 5. In the method for producing alcohol ketone dibasic acid of the present invention, cyclohexane containing a catalyst is added through the first feed port and the second feed port, and oxidation is carried out by adding through an oxygen source distributor provided at the bottom of the reactor, so that cyclohexane is oxidized to cyclohexanol and cyclohexanone under the action of the catalyst, and dibasic acid ester and other small amounts of impurities are by-produced. It has the advantages of high conversion rate (reaching 6-8%), high selectivity (above 85%), low unit consumption, and low cost (the unit consumption of cyclohexane is reduced from 1.02 to 0.9), and the process flow is short. The first feed port and the second feed port feed at the same time, which can effectively control the reaction temperature and improve the conversion rate and yield of the target product. By controlling the temperature in the reactor at 140-150°C and the pressure at 0.9-1.1 Mpa, the purpose is to reduce the by-production amount. If the temperature is too high, the alcohol ketone and dibasic acid ester generated are likely to undergo a condensation reaction at high temperature to generate other polymer impurities. If the temperature is too low, the reaction efficiency is too slow.

[0030] 6. The method for producing alkyd diester of the present invention involves washing the tail gas containing organic substances (alkyd and diester) in the reactor, effectively reducing the content of dibasic acid, especially adipic acid (produced by the decomposition of diester), in the tail gas pipeline, avoiding blockage of the tail gas pipeline. The preliminarily treated tail gas is cooled (with cyclohexane) and then washed with lye and alkyd, so that the content of organic substances in the exhausted tail gas is reduced to less than 0.5%. Then, it continues to be catalytically combusted to reduce the content of organic substances in the tail gas to ≤20 mg / m 3 and then sent to the power generation device for power generation, achieving the purpose of recycling the tail gas.

[0031] The following is a further description in conjunction with the drawings and specific embodiments. Description of the Drawings

[0032] Figure 1 It is a connection schematic diagram of the device of the present invention;

[0033] Figure 2 It is a connection schematic diagram of the reaction system of the device of the present invention;

[0034] Figure 3 It is a connection schematic diagram of the tail gas treatment system of the device of the present invention.

[0035] In the drawings, 1 is the reaction system, 11 is the reactor, 111 is the first feed port, 112 is the overflow port, 113 is the second exhaust port, 12 is the washing chamber, 121 is the second feed port, 122 is the first exhaust port, 13 is the oxygen source distributor, 2 is the tail gas treatment system, 21 is the first washing tower, 211 is the first intake port, 212 is the first washing liquid inlet, 22 is the second washing tower, 221 is the second intake port, 222 is the second washing liquid inlet, 23 is the third washing tower, 231 is the liquid outlet, 232 is the third intake port, 233 is the third washing liquid inlet, 3 is the distillation system, 31 is the desalination water pipe, and 4 is the buffer tank. Specific Embodiments

[0036] In the present invention, the raw material used is 99.8% cyclohexane.

[0037] Example 1

[0038] See Figures 1 to 3, The device for the one-step oxidation of cyclohexane to generate alcohol-ketone dicarboxylate ester comprises a reaction system 1 and a tail gas treatment system 2. The reaction system 1 includes six reactors 11. A washing chamber 12 is provided at the top of each reactor 11, and an oxygen source distributor 13 is provided at the bottom of each reactor 11. The oxygen source distributors are all connected to a compressed air source. A first feed inlet 111 is provided at the bottom of each reactor, an overflow port 112 is provided on the side wall, a second feed inlet 121 is provided in the washing chamber 12, and a first exhaust port 122 is provided at the top. Specifically, these six reactors are connected in series to form an integral body. The overflow port of the reactor located upstream is connected to the first feed inlet of the reactor located downstream. The second feed inlets of the six reactors are connected in parallel. Obviously, valves need to be provided at each first feed inlet and second feed inlet. In this embodiment, a second exhaust port 113 is further provided at the top of each reactor 11, and a valve is provided at the second exhaust port 113. In addition, a distillation system 3 is included. The distillation system usually adopts a multi-stage distillation column and is connected in series to form an integral body. The liquid inlet end of the distillation system 3 is connected to the overflow port 112 of the reactor at the downstream end through a buffer tank 4. A desalting water pipe 31 is provided in each distillation column of the distillation system. The tail gas treatment system 2 includes a first washing tower 21, a second washing tower 22, and a third washing tower 23. Each washing tower adopts a packed tower. The number of the first washing towers is one, the number of the second washing towers is one, and the number of the third washing towers is two. The two third washing towers are connected in series to form an integral body. A washing liquid circulation pipeline is provided at the bottom of the first washing tower and the second washing tower. Obviously, a circulation pump is provided on the washing liquid circulation pipeline. A first air inlet 211 is provided at the lower part of the side wall of the first washing tower 21, and a first washing liquid inlet 212 is provided at the upper part of the side wall. A second air inlet 221 is provided at the lower part of the side wall of the second washing tower 22, and a second washing liquid inlet 222 is provided at the upper part of the side wall. A liquid outlet 231 is provided at the bottom of the third washing tower 23, a third air inlet 232 is provided at the lower part of the side wall, and a third washing liquid inlet 233 is provided at the upper part of the side wall. Obviously, among them, the liquid outlet of the first third washing tower is connected to the third washing liquid inlet of the second third washing tower through a pipeline. The third washing liquid inlet of the first third washing tower is connected to the cyclohexane source. The liquid outlet of the second third washing tower is connected in parallel with the second feed inlets 121 of each reactor and is connected to the first feed inlet 111 of the reactor at the upstream end. The third air inlet 232 of the second third washing tower is connected in parallel with the first exhaust ports 122 and the second exhaust ports 113 of each reactor. The third air inlet of the first third washing tower is connected to the top of the second third washing tower through a pipeline.The first air inlet 211 of the first washing tower 21 is connected to the top of the first third washing tower 23 through a pipeline. The first washing liquid inlet 212 is connected to the desalted water source and the liquid caustic source. The second air inlet 221 of the second washing tower is connected to the top of the first washing tower 21 through a pipeline. The second washing liquid inlet 222 is connected to the alcohol-ketone source. Further, the first washing tower 21, the second washing tower 22, and the third washing tower 23 are all packed towers. Each air inlet is located below the packing of the corresponding washing tower, and each washing liquid inlet is located above the packing of the corresponding washing tower.

[0039] Example 2

[0040] The alcohol-ketone dibasic acid ester was synthesized using the apparatus of Example 1:

[0041] 300 m of cyclohexane 3 / h, 0.5 kg / h of cobalt porphyrin catalyst. First, it was added to the third washing tower, and then it entered the 1# oxidation kettle while maintaining the flow rate ratio of the two feed inlets at 25:1. Six oxidation kettles were connected in series and overflowed from the 1# to the 6# oxidation kettle in sequence. A certain amount of air was distributed to each oxidation reactor, and the total amount of air was 25000 Nm 3 / h, pressure 1.0 Mpa. The cyclohexane and air underwent a low-temperature oxidation reaction under the action of the catalyst. The reactor temperature was controlled at 140 - 146 °C. The oxidation liquid after the cyclohexane oxidation reaction was washed with water and then refined by alkane rectification to obtain the product alcohol-ketone dibasic acid ester.

[0042] After testing, in the obtained product, cyclohexane was 0.00075%, cyclohexanol was 27.52%, cyclohexanone was 19.35%, dibasic acid was 25.34%, ester was 9.58%, and water was 18.21%. This process does not require an alkali decomposition reaction, the conversion rate of the raw material cyclohexane is close to 100%, the acids and esters are effectively utilized, and the carbon utilization rate is greatly improved.

[0043] The gas phase port of each oxidation reactor is connected to the tail gas washing tower. Cyclohexane at 135 °C in the direct heat exchange tower is used to spray and wash the oxidation tail gas in the tail gas washing tower. The feed rate is 10 m 3 / h, the operating pressure of the tail gas washing tower is 3 - 10 bar. The raw material oxidation tail gas is spray-washed. Substances such as ketones, alcohols, acids, and esters that are prone to slag formation in the oxidation tail gas are washed down to the maximum extent and returned to the oxidation kettle, preventing substances such as ketones, alcohols, acids, and esters from forming slag in the oxidation tail gas pipeline, and enabling the smooth flow of the oxidation tail gas in the oxidation tail gas pipeline to achieve the purpose of washing and purifying the oxidation tail gas.

[0044] Verified by the applicant's tests, the annual operating cycle of the device of the present invention has increased from 6500 hours of the traditional oxidation device to 7220 hours.

Claims

1. A device for one-step oxidation of cyclohexane to produce alcohol ketone dibasic acid esters, characterized in that: It comprises a reaction system (1), an exhaust gas treatment system (2), The reaction system (1) comprises at least one reactor (11), wherein a washing chamber (12) is arranged at the top of the reactor (11), and an oxygen source distributor (13) is arranged at the bottom; a first feed port (111) is arranged at the bottom of the reactor, and an overflow port (112) is arranged at the side wall; a second feed port (121) is arranged at the washing chamber (12), and a first exhaust port (122) is arranged at the top; the first feed port and the second feed port are both used to add cyclohexane into the reactor, and the cyclohexane added at the second feed port is used to wash the tail gas discharged from the washing chamber. The tail gas treatment system (2) comprises a first washing tower (21) and a second washing tower (22), wherein a washing liquid circulation pipeline is arranged at the bottom of each washing tower, a first air inlet (211) is arranged at the lower part of the side wall of the first washing tower (21), and a first washing liquid inlet (212) is arranged at the upper part of the side wall, and a second air inlet (221) is arranged at the lower part of the side wall of the second washing tower (22), and a second washing liquid inlet (222) is arranged at the upper part of the side wall. The first feed port (111) and the second feed port (121) of the reaction system are both connected to a cyclohexane source, the first exhaust port (122) is connected to a first air inlet (211) of a tail gas treatment system, the first washing liquid inlet (212) of the tail gas treatment system is connected to a desalted water source and a liquid alkali source, the second air inlet (221) is connected to the top of a first washing tower (21) via a pipeline, and the second washing liquid inlet (222) is connected to an alcohol ketone source.

2. A device for one-step oxidation of cyclohexane to produce alcohol ketone dibasic acid esters, characterized in that: It comprises a reaction system (1), an exhaust gas treatment system (2), The reaction system (1) comprises at least one reactor (11), wherein a washing chamber (12) is arranged at the top of the reactor (11), and an oxygen source distributor (13) is arranged at the bottom; a first feed port (111) is arranged at the bottom of the reactor, and an overflow port (112) is arranged at the side wall; a second feed port (121) is arranged at the washing chamber (12), and a first exhaust port (122) is arranged at the top; the first feed port and the second feed port are both used to add cyclohexane into the reactor, and the cyclohexane added at the second feed port is used to wash the tail gas discharged from the washing chamber. The tail gas treatment system (2) comprises a first washing tower (21) and a second washing tower (22), wherein a washing liquid circulation pipeline is arranged at the bottom of each washing tower, a first air inlet (211) is arranged at the lower part of the side wall of the first washing tower (21), and a first washing liquid inlet (212) is arranged at the upper part of the side wall, and a second air inlet (221) is arranged at the lower part of the side wall of the second washing tower (22), and a second washing liquid inlet (222) is arranged at the upper part of the side wall. The third washing tower (23) further comprises a third washing tower (23), wherein a liquid outlet (231) is arranged at the bottom of the third washing tower (23), a third air inlet (232) is arranged at the lower part of the side wall, and a third washing liquid inlet (233) is arranged at the upper part of the side wall, the liquid outlet (231) is connected to the first feed inlet (111) and the second feed inlet (121) of the reaction system, the third air inlet (232) is connected to the first exhaust port (122) of the reactor, the first air inlet (211) of the first washing tower (21) is connected to the top of the third washing tower (23) via a pipeline, and the third washing liquid inlet (233) is connected to a cyclohexane source. The first feed port (111) and the second feed port (121) of the reaction system are both connected to a cyclohexane source, the first washing liquid inlet (212) of the tail gas treatment system is connected to a desalted water source and a liquid alkali source, the second air inlet (221) is connected to the top of the first washing tower (21) through a pipeline, and the second washing liquid inlet (222) is connected to an alcohol ketone source.

3. The device for producing alcohol ketone dibasic acid ester by one-step oxidation of cyclohexane according to claim 2, characterized in that: The number of the third washing towers (23) is two, which are connected in series to form a whole, and the oxygen source distributor (13) is connected to a compressed air source and / or a compressed oxygen source.

4. The device for producing alcohol ketone dibasic acid ester by one-step oxidation of cyclohexane according to claim 2 or 3, characterized in that: The first washing tower (21), the second washing tower (22), and the third washing tower (23) are all packed towers, each air inlet is located below the packing of the corresponding washing tower, and each washing liquid inlet is located above the packing of the corresponding washing tower.

5. The device for producing alcohol ketone dibasic acid ester by one-step oxidation of cyclohexane according to any one of claims 1 to 3, characterized in that: The top of the reactor (11) is provided with a second exhaust port (113), the second exhaust port (113) being provided with a valve and connected in parallel with the first exhaust port to the air inlet of the washing tower.

6. The device for producing alcohol ketone dibasic acid ester by one-step oxidation of cyclohexane according to any one of claims 1 to 3, characterized in that: The number of the reactors (11) is multiple and they are connected in series to form a whole, the overflow port of the upstream reactor is connected to the first feed port of the downstream reactor, and the second feed ports of the reactors are connected in parallel.

7. The device for producing alcohol ketone dibasic acid ester by one-step oxidation of cyclohexane according to any one of claims 1 to 3, characterized in that: It also includes a distillation system (3), wherein the liquid inlet end of the distillation system (3) is connected to the overflow port (112) of the reactor via a buffer tank (4), and the distillation system is provided with a desalted water pipe (31).

8. A method for synthesizing alcohol ketone dibasic esters using the device described in claim 2 or 3, characterized in that: The following steps are involved: 1) adding alkali solution and desalted water through the first washing liquid inlet and circulating them in the first washing tower, adding alcohol ketone through the second washing liquid inlet and circulating them in the second washing tower, adding cyclohexane through the third washing liquid inlet, collecting the cyclohexane at the bottom of the third washing tower, mixing with the catalyst and entering the reactor through the first feed inlet and the second feed inlet, wherein the catalyst is a transition metal porphyrin compound and the addition amount is 1-5ppm; 2) Excess air or oxygen enters the reactor through the oxygen source distributor, and the temperature is controlled at 140-150°C and the pressure is 0.9-1.1Mpa for oxidation reaction; 3) The reaction liquid containing alcohol ketone dibasic acid ester is discharged from the overflow port of the reactor and distilled to obtain the alcohol ketone dibasic acid ester product; 4) After being washed in the washing chamber, the excess air or oxygen is sent to the exhaust gas treatment system, and is washed with cyclohexane, alkali solution, and alcohol ketone in sequence before being discharged for incineration.

9. The method according to claim 8, characterized in that Step 1) the flow ratio of the first feed port and the second feed port is 25:1, the catalyst is any one or more of tetraphenylporphyrin cobalt, porphyrin iron, porphyrin manganese, and porphyrin copper, step 2) the temperature is 142-146°C, the pressure is 0.95-1.05Mpa, and the flow volume ratio of air to cyclohexane is 40-80:

1.

10. The method according to claim 8, characterized in that Step 3) The rectification is to control the temperature in the distillation system to 75-90°C for evaporation and concentration, add desalted water to the obtained bottom liquid, and discharge it to obtain a product containing alcohol ketone dibasic acid ester.

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