Fixed bed phenol hydrogenation catalyst evaluation device

Abstract

The utility model relates to a fixed bed phenol hydrogenation catalyst evaluation device which comprises a reactor, the upper part of the reactor is provided with a feed port, the lower part of the reactor is provided with a discharge port, the discharge port is connected to a condenser through a pipeline, the lower part of the condenser is provided with a gas-liquid two-phase outlet, the gas-liquid two-phase outlet is connected to a gas-liquid separator through a pipeline, and the gas-phase outlet is arranged above the gas-liquid separator. The outlet of the circulating fan is connected to a phenol evaporator through a pipeline, the upper part of the phenol evaporator is provided with a gas phase outlet, the gas phase outlet is connected to a heater through a pipeline, the upper part of the heater is provided with a material outlet, and the material outlet is connected to a material inlet at the upper part of the reactor through a pipeline. The device can accurately adjust the temperature of a reaction hot spot, is suitable for comparison tests of multiple parameters such as system pressure, reaction temperature, hydrogen / phenol feed ratio, air speed and catalyst service life, almost completely fits an industrial device, and greatly improves the accuracy of a catalyst evaluation result.

Description

TECHNICAL FIELD

[0001] The utility model relates to catalyst evaluation device technical field, especially a fixed bed phenol hydrogenation catalyst evaluation device. BACKGROUND

[0002] At present, the process of producing cyclohexanone in industry mainly has three kinds: phenol hydrogenation, cyclohexane oxidation and cyclohexene hydration. Among them, phenol hydrogenation is the earliest industrialized cyclohexanone preparation process, compared with the other two processes, phenol hydrogenation has the advantages of mild operating conditions, simple process, low investment cost and less three wastes emission. But because the domestic phenol market is small in the early stage, the price is high, which leads to less application of the process in China.

[0003] With the development of domestic acetone industry, the market of phenol as its by-product is gradually opened. Since early 2024, the price of phenol and pure benzene has appeared to be inverted, and the advantage of phenol hydrogenation process to prepare cyclohexanone is gradually obvious.

[0004] In order to develop a suitable phenol hydrogenation catalyst, it is inevitable to carry out catalyst evaluation test to comprehensively investigate the performance of the catalyst. At present, the general fixed bed catalyst evaluation device is quite different from the hydrogenation industrial device, especially the phenol hydrogenation belongs to strong exothermic reaction, during the catalyst evaluation period, the hot spot temperature of the reactor is seriously over standard, which leads to large deviation between the evaluation result and the actual situation. For example, the published patent CN 110907559 B a universal fixed bed catalyst evaluation device; CN 216987592 U a hydrogenation catalyst performance evaluation device with gas circulation system. Such devices often have poor pertinence, low accuracy of evaluation results, and cannot objectively evaluate the catalyst.

[0005] Therefore, we need an evaluation device with high compatibility with phenol hydrogenation industrial device, accurate evaluation results, and objective reaction of catalyst performance, which can also meet the comparison test of multiple parameters such as system pressure, hot spot temperature, hydrogen / phenol feed ratio, space velocity and catalyst service life. SUMMARY

[0006] The technical problem to be solved by the utility model is to provide a fixed bed phenol hydrogenation catalyst evaluation device, which can efficiently and accurately evaluate phenol hydrogenation catalyst and quickly find out the catalyst suitable for industrial device.

[0007] To solve the above technical problems, the technical scheme adopted by the utility model is:

[0008] A fixed bed phenol hydrogenation catalyst evaluation device, including reactor, the upper portion of reactor is equipped with feed inlet, the lower portion is equipped with discharge port, the discharge port is connected to condenser through pipeline, the lower portion of condenser is equipped with gas-liquid two-phase outlet, the gas-liquid two-phase outlet is connected to gas-liquid separator through pipeline, the upper portion of gas-liquid separator is equipped with gas phase outlet, the lower portion is equipped with liquid phase outlet, the gas phase outlet of gas-liquid separator is connected to circulating fan through pipeline, the outlet of circulating fan is connected to phenol evaporator through pipeline, the upper portion of phenol evaporator is equipped with gas phase outlet, the gas phase outlet of phenol evaporator is connected to heater through pipeline, the upper portion of heater is equipped with discharge port, the discharge port of heater is connected to the upper portion feed inlet of reactor through pipeline.

[0009] Preferably, the middle portion of the reactor is equipped with a cooling jacket, and compressed air enters from the bottom of the jacket and is discharged from the top of the jacket.

[0010] Preferably, a temperature regulating valve is arranged on the discharge pipeline at the top of the jacket.

[0011] Preferably, a venting pipeline is arranged at the inlet of the circulating fan.

[0012] Further preferably, a pressure regulating valve is arranged on the venting pipeline.

[0013] Further preferably, a thermometer T1 is arranged at the outlet of the phenol evaporator, a thermometer T2 is arranged at the outlet of the heater, a thermometer T3 is arranged at the upper portion of the reactor, and a thermometer T5 is arranged at the outlet of the condenser.

[0014] Preferably, a temperature sleeve and a movable thermometer T4 are arranged inside the reactor.

[0015] Preferably, an online hydrogen analyzer A and an online pressure gauge P1 are arranged at the inlet of the circulating fan, and an online pressure gauge P2 is arranged at the outlet of the circulating fan.

[0016] Preferably, a fresh hydrogen pipeline and a flow meter F1 are arranged at the outlet of the circulating fan, a phenol pipeline and a flow meter F2 are arranged at the outlet of the circulating fan, and a flow meter F3 is arranged at the inlet of the circulating fan.

[0017] The utility model has the advantages that:

[0018] 1. The utility model can accurately adjust the reaction hot spot temperature, is suitable for the comparative test of multiple parameters such as system pressure, reaction temperature, hydrogen / phenol feed ratio, space velocity and catalyst service life, and the process flow of the evaluation device is almost 100% consistent with the hydrogenation industrial device, so as to ensure the follow-up of the evaluation result in the industrial device.

[0019] 2. The reaction hot spot temperature can be accurately adjusted through the reactor cooling jacket, and the accuracy of the evaluation result is greatly improved. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 The utility model discloses a fixed bed phenol hydrogenation catalyst evaluation device's flow diagram.

[0021] Wherein: reactor 1, condenser 2, gas-liquid separator 3, circulating fan 4, phenol evaporator 5, heater 6, temperature regulating valve 7, pressure regulating valve 8, hydrogen pipeline 9, phenol pipeline 10. DETAILED DESCRIPTION

[0022] As Figure 1 The utility model discloses a fixed bed phenol hydrogenation catalyst evaluation device, including reactor 1, the upper portion of reactor 1 is equipped with feed inlet, and the lower portion is equipped with discharge port, and the discharge port is connected to condenser 2 through pipeline, and the lower portion of condenser 2 is equipped with gas-liquid two-phase outlet, and the gas-liquid two-phase outlet is connected to gas-liquid separator 3 through pipeline, and the upper portion of gas-liquid separator 3 is equipped with gas phase outlet, and the lower portion is equipped with liquid phase outlet, and the gas phase outlet of gas-liquid separator 3 is connected to circulating fan 4 through pipeline, and the outlet of circulating fan 4 is connected to phenol evaporator 5 through pipeline, and the upper portion of phenol evaporator 5 is equipped with gas phase outlet, and the gas phase outlet of phenol evaporator 5 is connected to heater 6 through pipeline, and the upper portion of heater 6 is equipped with discharge port, and the discharge port of heater 6 is connected to the upper portion feed inlet of reactor 1 through pipeline.

[0023] Preferably, the middle part of reactor 1 is equipped with cooling jacket, and compressed air enters from the bottom of the jacket and is discharged from the top of the jacket.

[0024] Preferably, the top of the jacket of the reactor 1 is equipped with temperature regulating valve 7 on the discharge pipeline.

[0025] Preferably, the inlet of the circulating fan 4 is equipped with a vent line.

[0026] Further preferably, the vent line is equipped with pressure regulating valve 8.

[0027] Further preferably, the outlet of the phenol evaporator 5 is equipped with thermometer T1, the outlet of the heater 6 is equipped with thermometer T2, the upper portion of the reactor 1 is equipped with thermometer T3, and the outlet of the condenser 2 is equipped with thermometer T5.

[0028] Preferably, the inside of the reactor 1 is equipped with temperature sleeve and movable thermometer T4.

[0029] Preferably, the inlet of the circulating fan 4 is equipped with online hydrogen analyzer A and online pressure gauge P1, and the outlet of the circulating fan 4 is equipped with online pressure gauge P2.

[0030] Preferably, the outlet of the circulating fan 4 is equipped with fresh hydrogen pipeline 9 and flowmeter F1, the outlet of the circulating fan 4 is equipped with phenol pipeline 10 and flowmeter F2, and the inlet of the circulating fan 4 is equipped with flowmeter F3.

[0031] In a specific example, the catalyst loading height in the reactor is 8 cm, the reactor jacket length is 12 cm, and the distance between the inner wall of the annular jacket and the outer wall of the reactor is 5 mm.

[0032] Specifically, the catalyst loading is 35 g, the phenol amount is 0.55 ml / min, and the fresh hydrogen amount is 275 ml / min at standard conditions.

[0033] Further specifically, the circulating fan inlet pressure is 0.15 MPaG, the circulating fan inlet flow is 400 ml / min at standard conditions, and the hydrogen content in the circulating gas is 99%V.

[0034] The phenol evaporator outlet temperature is 160℃, the heater outlet temperature is 180℃, the reactor hot spot temperature is 180℃, and the condenser outlet temperature is 40℃.

[0035] The main process and principle of the present example are as follows: the circulating hydrogen gas at the outlet of the circulating fan 4 is fully mixed with fresh hydrogen gas, and then the mixed hydrogen gas disperses the liquid phenol to form a gas-liquid two-phase flow. In the phenol evaporator 5, the phenol in the form of droplets is all vaporized, and then heated to 180℃ by the heater 6, and then enters the reactor 1 for reaction. The heat released by the reaction is carried away by the compressed air in the reactor jacket, and the flow of the compressed air is controlled by the temperature regulating valve 7, so that the reaction hot spot temperature can be accurately adjusted. The product after reaction is cooled to 40℃ by the condenser 2, and then enters the gas-liquid separator 3, and the separated liquid phase is recovered from the bottom, and the incondensable gas is discharged from the top and recycled by the circulating fan 4 after being pressurized. In order to ensure the stability of the system pressure and the concentration of hydrogen in the circulating gas, the inert gas in the system can be discharged in time by the pressure regulating valve 8.

[0036] The above-mentioned embodiments are only preferred technical solutions of the present application, and should not be regarded as limiting the present application. The protection scope of the present application should be based on the technical solutions claimed in the claims, including equivalent replacement schemes of the technical features in the technical solutions claimed in the claims. That is, equivalent replacement improvements within this scope are also within the protection scope of the present application.

Claims

1. A fixed bed phenol hydrogenation catalyst evaluation apparatus comprising a reactor (1), characterized in that: The reactor (1) is provided with a feed inlet at the upper part and a discharge outlet at the lower part, the discharge outlet is connected to a condenser (2) through a pipeline, the lower part of the condenser (2) is provided with a gas-liquid two-phase outlet, the gas-liquid two-phase outlet is connected to a gas-liquid separator (3) through a pipeline, the upper part of the gas-liquid separator (3) is provided with a gas phase outlet, and the lower part is provided with a liquid phase outlet, the gas phase outlet of the gas-liquid separator (3) is connected to a circulating fan (4) through a pipeline, the outlet of the circulating fan (4) is connected to a phenol evaporator (5) through a pipeline, the upper part of the phenol evaporator (5) is provided with a gas phase outlet, the gas phase outlet of the phenol evaporator (5) is connected to a heater (6) through a pipeline, the upper part of the heater (6) is provided with a discharge outlet, and the discharge outlet of the heater (6) is connected to the feed inlet of the reactor (1) through a pipeline.

2. The fixed bed phenol hydrogenation catalyst evaluation apparatus according to claim 1, characterized by: The reactor (1) is provided with a cooling jacket in the middle part, and compressed air enters from the bottom of the jacket and is discharged from the top of the jacket.

3. The fixed bed phenol hydrogenation catalyst evaluation apparatus according to claim 1, characterized by: A temperature regulating valve (7) is arranged on the discharge pipeline at the top of the jacket of the reactor (1).

4. The fixed bed phenol hydrogenation catalyst evaluation apparatus according to claim 1, characterized by: An exhaust pipeline is arranged at the inlet of the circulating fan (4).

5. The fixed bed phenol hydrogenation catalyst evaluation apparatus according to claim 4, characterized by: A pressure regulating valve (8) is arranged on the exhaust pipeline.

6. The fixed bed phenol hydrogenation catalyst evaluation apparatus according to claim 1, characterized by: A thermometer T1 is arranged at the outlet of the phenol evaporator (5), a thermometer T2 is arranged at the outlet of the heater (6), a thermometer T3 is arranged at the upper part of the reactor (1), and a thermometer T5 is arranged at the outlet of the condenser (2).

7. The fixed bed phenol hydrogenation catalyst evaluation apparatus according to claim 1, characterized by: A temperature sleeve and a movable thermometer T4 are arranged inside the reactor (1).

8. The fixed bed phenol hydrogenation catalyst evaluation apparatus according to claim 1, characterized by: An online hydrogen analyzer A and an online pressure gauge P1 are arranged at the inlet of the circulating fan (4), and an online pressure gauge P2 is arranged at the outlet of the circulating fan (4).

9. The fixed bed phenol hydrogenation catalyst evaluation apparatus according to claim 1, characterized by: A fresh hydrogen pipeline (9) and a flowmeter F1 are arranged at the outlet of the circulating fan (4), a phenol pipeline (10) and a flowmeter F2 are arranged at the outlet of the circulating fan (4), and a flowmeter F3 is arranged at the inlet of the circulating fan (4).

Images