Device and method for preparing hydrogenated bisphenol A through bisphenol A hydrogenation and application

Abstract

The invention provides a device and method for preparing hydrogenated bisphenol A through bisphenol A hydrogenation and application. The invention discloses a device for preparing hydrogenated bisphenol A by bisphenol A hydrogenation. The device comprises a hydrogen supply end, a bisphenol A supply end and a bubble cap plate tower, the bubble cap plate type tower comprises a liquid feeding hole, a gas feeding hole, a liquid discharging hole and a gas discharging hole; the hydrogen supply end is connected with a gas inlet of the bubble cap plate type tower; the bisphenol A supply end is connected with a liquid feeding hole of the bubble cap plate type tower; and the bubble cap tower plate is used for carrying out a reaction for preparing hydrogenated bisphenol A through bisphenol A hydrogenation. According to the invention, a bubble cap plate type tower is adopted to carry out a reaction for preparing hydrogenated bisphenol A through bisphenol A hydrogenation, and in the presence of a catalyst, a bisphenol A solution enters from the middle part of the tower, transversely flows through a bubble cap tower plate, overflows downwards and is in full contact with hydrogen entering from the lower part of the tower. And the conversion rate of reactants and the yield of products are high.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical synthesis, and in particular to a device, method and application of preparing hydrogenated bisphenol A by hydrogenating bisphenol A. Background Art

[0002] Hydrogenated bisphenol A is the product of the catalytic hydrogenation reaction of bisphenol A. Since there are no unsaturated structures such as aromatic rings in the molecule, the molecular structure is stable. Using hydrogenated bisphenol A instead of bisphenol A to produce epoxy resin, polycarbonate and other polymer materials can improve the light, thermal stability and weather resistance of the product, improve product quality, expand the application field, and make the product generate greater added value.

[0003] The hydrogenation reaction of bisphenol A requires dissolving the bisphenol A (BPA) raw material in an organic solvent, mixing it with hydrogen in the form of a solution, and then conducting a hydrogenation reaction. The hydrogen and the bisphenol A molecules in the raw material solution are fully in contact on the catalyst surface, and a hydrogenation reaction occurs to generate hydrogenated bisphenol A. Bisphenol A hydrogenation generally adopts a kettle or fixed bed hydrogenation process. The general reaction conditions are a temperature of 50 to 250°C and a hydrogen pressure of 1 to 30 MPa. Solvents are used in the reaction process, and the reaction products are separated and purified by vacuum distillation or recrystallization.

[0004] Bisphenol A kettle hydrogenation process is generally intermittent, and can also be continuous. The process is to dissolve Bisphenol A in a solvent at a certain ratio, add it into a reactor with a stirrer together with a solid powder catalyst with a carrier, and carry out hydrogenation reaction at a certain temperature and pressure. The hydrogenation material is filtered to remove the catalyst (the catalyst can be reused), and finally the hydrogenated Bisphenol A product is obtained by removing the solvent, and the removed solvent can be recycled. The kettle hydrogenation reaction is more suitable for smaller production scales, and the investment is also lower. However, this process has the disadvantages of complicated operation and large catalyst loss.

[0005] The fixed bed hydrogenation process of bisphenol A is a continuous hydrogenation process. Bisphenol A solvent is prepared into a bisphenol A solution of a certain concentration in a solvent. After heating, the bisphenol A solution is mixed with hydrogen and enters the hydrogenation reactor to carry out hydrogenation reaction under certain pressure, temperature, space velocity, hydrogen-to-oil ratio and other conditions. After hydrogenation, the material is separated by cold air and liquid, and the solvent and by-products are removed. After granulation, the hydrogenated bisphenol A product is obtained. Compared with the kettle hydrogenation process, the fixed bed hydrogenation process has a larger equipment investment and high requirements on the performance of the hydrogenation catalyst. Summary of the invention

[0006] In order to solve the above problems in the prior art, the present invention proposes a device, method and application for preparing hydrogenated bisphenol A by hydrogenating bisphenol A.

[0007] In a first aspect, the present invention provides a device for preparing hydrogenated bisphenol A by hydrogenating bisphenol A, comprising a hydrogen supply end, a bisphenol A supply end and a bubble cap plate tower;

[0008] The bubble cap plate tower includes a liquid feed inlet, a gas feed inlet, a liquid discharge port, and a gas discharge port;

[0009] The hydrogen supply end is connected to the gas feed port of the bubble cap plate tower;

[0010] The bisphenol A supply end is connected to the liquid feed port of the bubble cap plate tower;

[0011] The bubble cap tray is used for the reaction of hydrogenating bisphenol A to prepare hydrogenated bisphenol A.

[0012] As a specific embodiment of the present invention, the bubble cap plate tower is placed in the vertical direction, the position of the liquid feed port is higher than the gas feed port, and a plurality of layers of tower plates a are arranged inside the bubble cap plate tower. The height of the tower plate a is between the liquid inlet and the gas inlet. The tower plate a is a bubble cap plate for loading a hydrogenation catalyst. The interior of the bubble cap plate tower is provided with a plurality of layers of tower plates b. The tower plate b is in the form of a sieve plate. The position of the tower plate b is higher than the liquid inlet for solvent removal.

[0013] The surface of the bubble cap plate is evenly distributed with risers, bubbles are installed on the top of the risers, and slits are provided at the bottom of the bubbles. The bubble cap plate is provided with an overflow weir, and the height of the overflow weir is higher than the top of the bubble cap. Gas-liquid reaction can be carried out in the bubble cap plate, and the liquid flows down from the overflow weir and flows horizontally through the bubble cap plate. Since the overflow weir maintains a certain height, a liquid seal of a certain height can be formed on the bubble cap plate. The gas rising in the riser enters the liquid layer through the slits, disperses into many tiny bubbles to form a bubbling layer, realizes full contact between gas and liquid, generates a large number of interfaces between gas and liquid phases, and improves mass transfer and heat transfer effects. The bubble cap plate in the present invention can use the bubble cap plate in the existing bubble cap tower.

[0014] Preferably, the bubble cap plate tower comprises 2-3 layers of plates a;

[0015] Preferably, the bubble-cap plate tower comprises 2-5 layers of plates b.

[0016] As a specific embodiment of the present invention, the tower plate a includes a bubble cap, and the diameter of the tower plate a is 3 to 20 times the diameter of the bubble cap.

[0017] Preferably, the plate diameter in the plate a is 4 to 8 times the bubble cap diameter.

[0018] As a specific embodiment of the present invention, a filter screen is installed on the tray a. The height of the filter screen is higher than the top of the bubble cap, and the filter screen is fixedly connected to the bubble cap tray. The filter screen can prevent the powdered catalyst from being lost under the gas-liquid flow state, ensuring that the amount of catalyst on the tray will not change and block the tray pipe opening.

[0019] Specifically, the catalyst used in the bisphenol A hydrogenation process of the present invention is a powdered catalyst, including a carrier and an active component;

[0020] The carrier is selected from activated carbon, alumina, and molecular sieve;

[0021] The active component is selected from ruthenium, rhodium, palladium, platinum and nickel.

[0022] As a specific embodiment of the present invention, the bubble cap plate tower further comprises a return material port, and the height of the return material port is higher than the tower plate b.

[0023] As a specific embodiment of the present invention, the hydrogen raw material supply end includes a hydrogen storage device, a hydrogen flow meter and a hydrogen heater. The hydrogen storage device is used to store hydrogen before the reaction, the hydrogen flow meter is used to increase the pressure of the hydrogen, and the hydrogen heater is used to preheat the hydrogen before the reaction.

[0024] As a specific embodiment of the present invention, the bisphenol A supply end includes a bisphenol A storage, a bisphenol A flowmeter and a bisphenol A heater. The bisphenol A storage is used to store bisphenol A before reaction, the bisphenol A flowmeter is used to increase the pressure of bisphenol A, and the bisphenol A heater is used to preheat the bisphenol A before reaction.

[0025] As a specific embodiment of the present invention, the device for preparing hydrogenated bisphenol A by hydrogenating bisphenol A further comprises a condenser, the inlet of the condenser is connected to the gas outlet of the bubble cap plate tower, and the condenser is used to condense the hydrogen and solvent discharged from the top of the bubble cap plate tower.

[0026] As a specific embodiment of the present invention, the device for preparing hydrogenated bisphenol A by hydrogenating bisphenol A also includes a separator, which is a sealed container having a liquid input port, a liquid output port c, a liquid output port d and a gas output port.

[0027] The liquid input port of the separator is communicated with the outlet of the condenser and is used for receiving the liquid condensed by the condenser.

[0028] The liquid outlet c of the separator is connected to the return port of the bubble cap plate tower, and is used to reflux part of the solvent in the separator to the bubble cap plate tower. The mass of the refluxed solvent is 20-60% of the total mass of the solvent in the separator.

[0029] The liquid outlet d of the separator is connected to the outside for discharging the remaining solvent.

[0030] The gas outlet of the separator is communicated with the outside for discharging gas.

[0031] The separator also includes a back pressure valve connected to the gas output port. The back pressure valve controls the pressure in the separator, refluxes part of the solvent in the separator to the bubble plate tower, and extracts the remaining solvent.

[0032] The solvent refluxed into the bubble cap plate tower exchanges gas-liquid heat with the gas generated in the bubble cap plate tower. Some by-products in the gas condense after encountering the reflux solvent, and the non-condensable gas phase is discharged from the top of the tower, condensed by the cooler and enters the separation tank. After gas-liquid separation, it is extracted from the separation tank to achieve the removal of the solvent part and by-products. The extracted solvent can be recycled after treatment.

[0033] In a second aspect, the present invention provides a method for preparing hydrogenated bisphenol A by hydrogenating bisphenol A using the device provided by the first invention of the present invention, comprising the following steps: hydrogen enters a bubble plate tower through a gas feed port, and bisphenol A enters a liquid feed port, the hydrogen reacts with bisphenol A to obtain a product containing hydrogenated bisphenol A, and the gas is discharged.

[0034] Preferably, hydrogen gas contacts bisphenol A with a hydrogenation catalyst to cause a hydrogenation reaction.

[0035] Preferably, the exhaust gas comprises hydrogen and vaporized solvent.

[0036] As a specific embodiment of the present invention, before the reaction, bisphenol A and a solvent are prepared into a solution containing bisphenol A, and the solution containing bisphenol A enters the bubble plate tower through a liquid feed port for reaction.

[0037] As a specific embodiment of the present invention, the product containing hydrogenated bisphenol A is discharged from the liquid discharge port of the bubble cap plate tower;

[0038] As a specific embodiment of the present invention, the vaporized solvent and unreacted hydrogen are discharged from the gas outlet of the bubble cap plate tower, the vaporized solvent and unreacted hydrogen discharged from the gas outlet are condensed in a condenser to obtain hydrogen and liquefied solvent, the hydrogen and the liquefied solvent enter a separator, the hydrogen is discharged from the gas outlet of the separator, the partially liquefied solvent is refluxed to the bubble cap plate tower through the liquid outlet c, and the remaining liquefied solvent is discharged from the liquid outlet d.

[0039] As a specific embodiment of the present invention, the operating pressure of the bubble cap plate tower is 2.8 to 9 MPa;

[0040] As a specific embodiment of the present invention, the molar ratio of hydrogen to bisphenol A feed is 20-80.

[0041] As a specific embodiment of the present invention, the feed temperature of bisphenol A is 100-180°C.

[0042] As a specific embodiment of the present invention, the feed temperature of hydrogen is 100-180°C.

[0043] As a specific embodiment of the present invention, the hydrogenation catalyst comprises a carrier and an active component, the carrier is selected from activated carbon, alumina, and molecular sieves, and the active component is selected from ruthenium, rhodium, palladium, platinum, and nickel.

[0044] In a third aspect, the present invention provides an application of the device provided by the first aspect of the present invention or the method provided by the second aspect of the present invention in the hydrogenation of bisphenol A to produce hydrogenated bisphenol A.

[0045] Compared with the prior art, the present invention has the following beneficial effects.

[0046] The present invention adopts a bubble cap plate tower to carry out the reaction of hydrogenating bisphenol A to prepare hydrogenated bisphenol A. In the presence of a catalyst, a bisphenol A solution enters the tower from the middle part, flows horizontally through the bubble cap plate, overflows downward, and fully contacts with hydrogen entering from the bottom part of the tower. The conversion rate of the reactant and the yield of the product are high. The operation is simple and the investment is small. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1 Schematic diagram of the hydrogenation process of bisphenol A in Example 1 of the present invention;

[0048] Figure 2 A schematic plan view of a bubble cap tray in Example 1 of the present invention;

[0049] Figure 3 Schematic diagram of the distribution of the riser pipes of the bubble cap tray in Example 1 of the present invention;

[0050] Among them, 1-hydrogen supply end, 11-hydrogen storage, 12-hydrogen dosimeter, 13-hydrogen heater;

[0051] 2-bisphenol A supply end, 21-bisphenol storage, 22-bisphenol A dosimeter, 23-bisphenol A heater;

[0052] 3- bubble cap plate tower, 31- liquid feed port, 32- gas feed port, 33- liquid discharge port, 34- gas discharge port, 35- tower plate a, 36- tower plate b, 37- return port.

[0053] 351- bubble cap, 352- riser pipe, 353- overflow weir, 354- filter screen,

[0054] 4- Condenser,

[0055] 5-separator, 51-liquid input port, 52-liquid output port c, 53-liquid output port d, 54-gas output port, 55-back pressure valve. DETAILED DESCRIPTION

[0056] The present invention will be further described below in conjunction with specific embodiments, but they do not constitute any limitation to the present invention.

[0057] Example 1

[0058] A device for preparing hydrogenated bisphenol A by hydrogenating bisphenol A, comprising a hydrogen supply end 1, a bisphenol A supply end 2 and a bubble cap plate tower 3;

[0059] The bubble cap plate tower 3 comprises a liquid feed port 31, a gas feed port 32, a liquid discharge port 33, and a gas discharge port 34;

[0060] The hydrogen supply end is connected to the gas feed port 34 of the bubble cap plate tower 3;

[0061] The bisphenol A supply end is connected to the liquid feed port 31 of the bubble cap plate tower 3;

[0062] The bubble cap tray is used for the reaction of hydrogenating bisphenol A to prepare hydrogenated bisphenol A.

[0063] As a specific embodiment of the present invention, the bubble cap plate tower 3 is placed in the vertical direction, the position of the liquid feed port 31 is higher than the gas feed port 32, and a plurality of layers of tower plates a35 are arranged inside the bubble cap plate tower 3. The height of the tower plate a35 is between the liquid inlet 31 and the gas inlet 32. The tower plate a35 is a bubble cap plate for loading a hydrogenation catalyst. The bubble cap plate tower 3 is provided with a plurality of layers of tower plates b36. The position of the tower plate b36 is higher than the liquid inlet. The tower plate b36 is used for removing the solvent.

[0064] Specifically, the bubble cap plate tower 3 includes 2-3 layers of plates a35;

[0065] Specifically, the bubble cap plate tower includes 2-5 layers of plates b36.

[0066] As a specific embodiment of the present invention, the tower plate a35 includes a bubble cap 351, a riser 352, an overflow weir 353 and a filter screen 354.

[0067] Specifically, the plate diameter of the plate a35 is 3 to 20 times, specifically 4 to 8 times, the diameter of the bubble cap 351;

[0068] Specifically, the tower plate a35 is provided with riser pipes 352, which are arranged in an equilateral triangle. The rising gas enters the upper layer from the lower layer through the riser pipes 352, and a circular bubble cap 351 is fixedly installed on the top of the riser pipe 352. The lower part of each bubble cap 351 has a tooth gap, which is a triangle or a quadrilateral.

[0069] Specifically, each bubble cap tray is provided with an overflow weir 353 , and the overflow weir 353 is higher than the top of the bubble cap 351 , so as to ensure that a liquid seal is formed after the liquid flows through.

[0070] Specifically, the tower plate a is installed with a filter screen 354, which is made of stainless steel 304 or 316. The height of the filter screen 354 is higher than the top of the bubble cap 351, and the filter screen 354 is fixedly connected to the bubble cap tower plate. The filter screen 354 is used to prevent the catalyst from being lost.

[0071] As a specific embodiment of the present invention, the bubble cap plate tower 3 further includes a return port 37, and the height of the return port 37 is higher than the tower plate b36.

[0072] As a specific embodiment of the present invention, the hydrogen raw material supply end 1 includes a hydrogen storage 11, a hydrogen flow meter 12 and a hydrogen heater 13;

[0073] As a specific embodiment of the present invention, the bisphenol A supply end 2 includes a bisphenol A storage 21 , a bisphenol A flow meter 22 and a bisphenol A heater 23 .

[0074] As a specific embodiment of the present invention, the device for preparing hydrogenated bisphenol A by hydrogenating bisphenol A further comprises a condenser 4 , and an inlet of the condenser 4 is connected to a gas outlet 34 of the bubble-cap plate tower 3 .

[0075] As a specific embodiment of the present invention, the device for preparing hydrogenated bisphenol A by hydrogenation of bisphenol A also includes a separator 5, which is a sealed container having a liquid input port 51, a liquid output port c52, a liquid output port d53 and a gas output port 54. The liquid input port 51 of the separator 5 is connected to the outlet of the condenser 4, the liquid output port c52 of the separator is connected to the return port 37 of the bubble cap plate tower 3, the liquid output port d53 of the separator is connected to the outside, and the gas output port 54 of the separator 5 is connected to the outside. The separator 5 also includes a back pressure valve 55 connected to the gas output port 54, and the back pressure valve 55 controls the pressure in the separator 5, and refluxes part of the solvent in the separator 5 to the bubble cap plate tower 3, and the remaining solvent is extracted.

[0076] Example 2

[0077] The bubble cap plate tower is used for the hydrogenation reaction of bisphenol A. The tower has 5 layers of plates b above the inlet of bisphenol A solution and 2 layers of bubble cap plates below. The diameter of the bubble cap plate is 50CM, and the ascending gas pipe of the plate is Figure 3A circular bubble cap is fixed on the top of the riser, with a diameter of 10CM. A triangular tooth gap is opened at the bottom of the bubble cap. The overflow weir of the bubble cap plate is higher than the top of the bubble cap. The plate is loaded with a powdered catalyst, the active component of the catalyst is Pd, the carrier is activated carbon, the active component loading is 1% of the catalyst dosage, and the catalyst dosage is 3 kg. After loading the catalyst, a filter is installed on the plate. The liquid feed port of the tower is connected to the bisphenol A heater, the gas feed port is connected to the hydrogen heater, the gas discharge port of the bubble cap plate tower is connected to the condenser, the material outlet of the condenser is connected to the liquid input port of the separator, and the liquid output port c of the separator is connected to the return port of the bubble cap plate tower, which is used to reflux part of the solvent in the separator to the bubble cap plate tower. The mass of the refluxed solvent is 40% of the total mass of the solvent in the separator.

[0078] The liquid outlet d of the separator is communicated with the outside for discharging the remaining solvent. The gas outlet of the separator is communicated with the outside for discharging the gas.

[0079] Bisphenol A is dissolved in isopropanol and prepared into a solution with a mass concentration of 15%. The solution is pressurized to 4MPa by metering, preheated to 120°C, and enters from the liquid feed port at a flow rate of 80 liters / hour. Hydrogen is pressurized to 4MPa and metered before entering the hydrogen heater to be heated to 120°C. It enters from the gas feed port of the tower at a flow rate of 400 liters / minute. The outer layer of the bubble plate tower is insulated and heated. The bubble plate temperature is 120-125°C and the pressure is 3.8-4MPa. A differential pressure level gauge is set at the bottom of the tower, and the hydrogenated bisphenol A solution with some solvent removed is discharged from the bottom of the tower. A differential pressure level gauge is set at the bottom of the tower to control the amount of liquid discharged from the bottom of the tower and maintain the liquid level of the bottom of the tower. The composition of the discharged material at the bottom of the tower is analyzed, and the experimental results are shown in Table 1.

[0080] Example 3

[0081] A bubble cap plate tower is used for the hydrogenation reaction of bisphenol A. The tower has 5 layers of plates b above the inlet of bisphenol A solution and 2 layers of bubble cap plates below. The diameter of the plate is 50CM. The ascending gas pipe of the plate is Figure 3 A circular bubble cap is fixed on the top of the riser, with a diameter of 10 cm. A triangular tooth gap is opened at the bottom of the bubble cap. The overflow weir of the bubble cap plate is higher than the top of the bubble cap. The plate is loaded with a powdered catalyst, the active component of the catalyst is Ru, the carrier is activated alumina, the active component loading is 1.5% of the catalyst dosage, and the catalyst dosage is 4.5 kg. After loading the catalyst, a filter is installed on the plate. The tower liquid feed port is connected to the bisphenol A heater, the gas feed port is connected to the hydrogen heater, the tower gas discharge port is connected to the condenser, the condenser material outlet is connected to the separator liquid input port, and the liquid output port c of the separator is connected to the return port of the bubble cap plate tower, which is used to reflux part of the solvent in the separator to the bubble cap plate tower. The mass of the refluxed solvent is 40% of the total mass of the solvent in the separator.

[0082] Bisphenol A is dissolved in isopropanol and prepared into a solution with a mass concentration of 20%. The solution is pressurized to 9MPa by metering, preheated to 140°C, and enters the tower liquid feed port at a flow rate of 60 liters / hour. Hydrogen is pressurized to 9MPa and metered before entering the hydrogen heater to be heated to 140°C. It enters the tower gas feed port at a flow rate of 400 liters / minute. The outer layer of the tower is insulated and heated, the bubble plate temperature is 140-145°C, and the pressure is 8.8-9MPa. A differential pressure level gauge is set at the bottom of the tower, and the hydrogenated bisphenol A solution with some solvent removed is discharged from the bottom of the tower. A differential pressure level gauge is set at the bottom of the tower to control the amount of liquid discharged from the bottom of the tower and maintain the liquid level of the bottom of the tower. The composition of the discharged material at the bottom of the tower is analyzed, and the experimental results are shown in Table 1.

[0083] Example 4

[0084] A bubble cap plate tower is used for the hydrogenation reaction of bisphenol A. The tower has 5 layers of plates b above the inlet of bisphenol A solution and 2 layers of bubble cap plates below. The diameter of the plate is 50CM. The ascending gas pipe of the plate is Figure 3 A circular bubble cap is fixed on the top of the riser, with a diameter of 10CM. A triangular tooth gap is opened at the bottom of the bubble cap. The overflow weir of the bubble cap plate is higher than the top of the bubble cap. The plate is loaded with a powdered catalyst, the active component of the catalyst is Pd, the carrier is activated alumina, the active component loading is 1.5% of the catalyst dosage, and the catalyst dosage is 5 kg. After loading the catalyst, a filter is installed on the plate. The tower liquid feed port is connected to the bisphenol A heater, the gas feed port is connected to the hydrogen heater, the tower gas outlet is connected to the condenser, the condenser material outlet is connected to the separation liquid input port, and the liquid output port c of the separator is connected to the return port of the bubble cap plate tower, which is used to reflux part of the solvent in the separator to the bubble cap plate tower. The mass of the refluxed solvent is 60% of the total mass of the solvent in the separator.

[0085] Bisphenol A is dissolved in isopropanol and prepared into a solution with a mass concentration of 10%. The solution is pressurized to 3MPa by metering, preheated to 180°C, and enters the tower liquid feed port at a flow rate of 50 liters / hour. Hydrogen is pressurized to 3MPa and metered before entering the hydrogen heater to be heated to 180°C. It enters the tower gas feed port at a flow rate of 500 liters / minute. The outer layer of the tower is insulated and heated, the bubble plate temperature is 180-185°C, and the pressure is 2.8-3MPa. A differential pressure level gauge is set at the bottom of the tower, and the hydrogenated bisphenol A solution with some solvent removed is discharged from the bottom of the tower. A differential pressure level gauge is set at the bottom of the tower to control the amount of liquid discharged from the bottom of the tower and maintain the liquid level of the bottom of the tower. The composition of the discharged material at the bottom of the tower is analyzed, and the experimental results are shown in Table 1.

[0086] Example 5

[0087] A bubble cap plate tower is used for the hydrogenation reaction of bisphenol A. The tower has 5 layers of plates b above the inlet of bisphenol A solution and 2 layers of bubble cap plates below. The diameter of the plate is 50CM. The ascending gas pipe of the plate is Figure 3A circular bubble cap is fixed on the top of the riser, with a diameter of 10 cm. A triangular tooth gap is opened at the bottom of the bubble cap. The overflow weir height of the bubble cap plate is higher than the top of the bubble cap. The plate is loaded with a powdered catalyst, the active component of the catalyst is Rh, the carrier is activated carbon, the active component loading is 0.8% of the catalyst dosage, and the catalyst dosage is 2.7 kg. After loading the catalyst, a filter is installed on the plate. The tower liquid feed port is connected to the bisphenol A heater, the gas feed port is connected to the hydrogen heater, the tower gas discharge port is connected to the condenser, the condenser material outlet is connected to the separator liquid input port, and the liquid output port c of the separator is connected to the return port of the bubble cap plate tower, which is used to reflux part of the solvent in the separator to the bubble cap plate tower. The mass of the refluxed solvent is 20% of the total mass of the solvent in the separator.

[0088] Bisphenol A is dissolved in isopropanol and prepared into a bisphenol A solution with a mass concentration of 15%. The pressure is increased by 6MPa after metering, and it is preheated to 100°C. The bisphenol A solution enters the tower liquid feed port at a flow rate of 80 liters / hour. Hydrogen is pressurized by 6MPa and metered into the hydrogen heater to be heated to 100°C, and enters the tower gas feed port at a flow rate of 330 liters / minute. The outer layer of the tower is insulated and heated, the bubble plate temperature is 110-115°C, and the pressure is 5.8-6MPa. A differential pressure level gauge is set at the bottom of the tower, and the hydrogenated bisphenol A solution with some solvent removed is discharged from the bottom of the tower. A differential pressure level gauge is set at the bottom of the tower to control the amount of liquid discharged from the bottom of the tower and maintain the liquid level of the tower bottom. The composition of the material discharged from the bottom of the tower is analyzed, and the experimental results are shown in Table 1.

[0089] Example 6

[0090] A bubble cap plate tower is used for bisphenol A hydrogenation reaction. The tower has 3 layers of plates b above the inlet of bisphenol A solution, 3 layers of bubble cap plates are installed below, the plate diameter is 50CM, a circular bubble cap is fixedly installed on the top of the riser, the bubble cap diameter is 4CM, a square tooth gap is opened at the bottom of the bubble cap, the overflow weir height of the bubble cap plate is higher than the top of the bubble cap, the plate is filled with powdered catalyst, the catalyst active component is Ni, the carrier is activated alumina, the active component loading is 2% of the catalyst dosage, the catalyst dosage is 6 kg, and a filter is installed on the plate after the catalyst is filled. The tower liquid feed port is connected to a bisphenol A heater, the gas feed port is connected to a hydrogen heater, the tower gas discharge port is connected to a condenser, the condenser material outlet is connected to a separator liquid input port, and the separator liquid output port c is connected to the return port of the bubble cap plate tower, which is used to reflux part of the solvent in the separator to the bubble cap plate tower, and the reflux solvent mass is 50% of the total mass of the solvent in the separator.

[0091] Bisphenol A is dissolved in isopropanol and prepared into a solution with a mass concentration of 15%. The solution is pressurized to 6MPa by metering, preheated to 120°C, and enters the tower liquid feed port at a flow rate of 80 liters / hour. Hydrogen is pressurized to 6MPa and metered before entering the hydrogen heater to be heated to 120°C. It enters the tower gas feed port at a flow rate of 400 liters / minute. The outer layer of the tower is insulated and heated, the bubble plate temperature is 120-125°C, and the pressure is 5.8-6MPa. A differential pressure level gauge is set at the bottom of the tower, and the hydrogenated bisphenol A solution with some solvent removed is discharged from the bottom of the tower. A differential pressure level gauge is set at the bottom of the tower to control the amount of liquid discharged from the bottom of the tower and maintain the liquid level of the bottom of the tower. The composition of the discharged material at the bottom of the tower is analyzed, and the experimental results are shown in Table 1.

[0092] Example 7

[0093] A bubble cap plate tower is used for bisphenol A hydrogenation reaction. The tower has two layers of plates b above the inlet of bisphenol A solution, and three layers of bubble cap plates are installed below. The diameter of the plates is 50 cm. A circular bubble cap is fixedly installed on the top of the riser, and the diameter of the bubble cap is 5 cm. The lower part of the bubble cap has a trapezoidal tooth gap. The overflow weir of the bubble cap plate is higher than the top of the bubble cap. The plate is loaded with a powdered catalyst. The active component of the catalyst is Ni, and the carrier is activated carbon. The active component loading is 2% of the catalyst dosage. The catalyst dosage is 5.5 kg. After the catalyst is loaded, a filter is installed on the plate. The tower liquid feed port is connected to a bisphenol A heater, the gas feed port is connected to a hydrogen heater, the tower gas discharge port is connected to a condenser, the condenser material outlet is connected to a separator liquid input port, and the liquid output port c of the separator is connected to the return port of the bubble cap plate tower, which is used to reflux part of the solvent in the separator to the bubble cap plate tower. The mass of the refluxed solvent is 30% of the total mass of the solvent in the separator.

[0094] Bisphenol A is dissolved in isopropanol and prepared into a solution with a mass concentration of 12%. The solution is pressurized to 6MPa by metering, preheated to 120°C, and enters the tower liquid feed port at a flow rate of 60 liters / hour. Hydrogen is pressurized to 6MPa and metered before entering the hydrogen heater to be heated to 120°C. It enters the tower gas feed port at a flow rate of 400 liters / minute. The outer layer of the tower is insulated and heated, the bubble plate temperature is 120-125°C, and the pressure is 5.8-6MPa. A differential pressure level gauge is set at the bottom of the tower, and the hydrogenated bisphenol A solution with some solvent removed is discharged from the bottom of the tower. A differential pressure level gauge is set at the bottom of the tower to control the amount of liquid discharged from the bottom of the tower and maintain the liquid level of the bottom of the tower. The composition of the discharged material at the bottom of the tower is analyzed, and the experimental results are shown in Table 1.

[0095] Example 8

[0096] A bubble cap plate tower is used for bisphenol A hydrogenation reaction. The tower has 5 layers of plates b above the inlet of bisphenol A solution, 2 layers of bubble cap plates are installed below, the plate diameter is 50CM, a circular bubble cap is fixedly installed on the top of the riser, the bubble cap diameter is 15CM, the lower part of the bubble cap is provided with a trapezoidal tooth gap, the overflow weir height of the bubble cap plate is higher than the top of the bubble cap, the plate is filled with powdered catalyst, the catalyst active component is Pt, the carrier is activated alumina, the active component loading is 1.2% of the catalyst dosage, the catalyst dosage is 3.5 kg, and a filter is installed on the plate after the catalyst is filled. The tower liquid feed port is connected to a bisphenol A heater, the gas feed port is connected to a hydrogen heater, the tower gas discharge port is connected to a condenser, the condenser material outlet is connected to a separator liquid input port, and the liquid output port c of the separator is connected to the return port of the bubble cap plate tower, which is used to reflux part of the solvent in the separator to the bubble cap plate tower, and the refluxed solvent mass is 20% of the total mass of the solvent in the separator.

[0097] Bisphenol A is dissolved in isopropanol and prepared into a solution with a mass concentration of 20%. The solution is pressurized to 8MPa by metering, preheated to 150°C, and fed into the tower liquid feed at a flow rate of 60 liters / hour. Hydrogen is pressurized to 8MPa and metered before entering the hydrogen heater to be heated to 150°C. It enters the tower gas feed port at a flow rate of 400 liters / minute. The outer layer of the tower is insulated and heated, the bubble plate temperature is 150-155°C, and the pressure is 7.8-8MPa. A differential pressure level gauge is set at the bottom of the tower, and the hydrogenated bisphenol A solution with some solvent removed is discharged from the bottom of the tower. A differential pressure level gauge is set at the bottom of the tower to control the amount of liquid discharged from the bottom of the tower and maintain the liquid level of the bottom of the tower. The composition of the discharged material at the bottom of the tower is analyzed, and the experimental results are shown in Table 1.

[0098] Table 1 Analysis results of the bottom discharge

[0099]

[0100] The samples in Table 1 were analyzed by gas chromatography. The analysis results of product purity, by-products and unsaturated products in Table 1 were directly obtained by gas chromatography, and the solvent in the sample was not integrated during the analysis.

[0101] Bisphenol A conversion rate = (mass of bisphenol A reacted / mass of bisphenol A raw material) × 100%

[0102] Selectivity of hydrogenated bisphenol A = (mass of hydrogenated bisphenol A generated by reaction / mass of bisphenol A reacted) × 100%

[0103] Hydrogenated bisphenol A yield = (mass of hydrogenated bisphenol A generated by reaction / mass of bisphenol A raw material) × 100%

[0104] Solvent removal rate = (mass of solvent separated by the separator ÷ mass of solvent in the bisphenol A solution entering the tower) × 100%

[0105] It should be noted that the embodiments described above are only used to explain the present invention and do not constitute any limitation to the present invention. The present invention has been described with reference to typical embodiments, but it should be understood that the words used therein are descriptive and explanatory words, rather than restrictive words. The present invention may be modified as specified within the scope of the claims of the present invention, and the present invention may be revised without departing from the scope and spirit of the present invention. Although the present invention described therein relates to specific methods, materials and embodiments, it does not mean that the present invention is limited to the specific examples disclosed therein, on the contrary, the present invention can be extended to all other methods and applications with the same functions.

Claims

1. A device for preparing hydrogenated bisphenol A by hydrogenating bisphenol A, characterized in that: It includes a hydrogen supply end, a bisphenol A supply end and a bubble cap plate tower; The bubble cap plate tower comprises a liquid feed inlet, a gas feed inlet, a liquid discharge port, and a gas discharge port; The hydrogen supply end is connected to the gas feed port of the bubble cap plate tower; The bisphenol A supply end is connected to the liquid feed port of the bubble cap plate tower; The bubble cap tray is used for the reaction of hydrogenating bisphenol A to prepare hydrogenated bisphenol A.

2. The device according to claim 1, characterized in that The bubble cap plate tower is placed in the vertical direction, the position of the liquid feed port is higher than the gas feed port, a plurality of layers of plates a are arranged inside the bubble cap plate tower, the height of the plates a is between the liquid inlet and the gas inlet, the plates a are bubble cap plates, and are used to load hydrogenation catalysts; a plurality of layers of plates b are arranged inside the bubble cap plate tower, the positions of the plates b are higher than the liquid inlet, and the plates b36 are used to remove solvents; preferably, the bubble cap plate tower includes 2 to 3 layers of plates a; and / or the bubble cap plate tower includes 2 to 5 layers of plates b.

3. The device according to claim 2, characterized in that The tower plate a comprises a bubble cap, and the diameter of the tower plate a is 3 to 20 times, preferably 4 to 8 times, the diameter of the bubble cap; and / or, the tower plate a is equipped with a filter screen, and the filter screen is used to prevent the loss of the catalyst.

4. The device according to any one of claims 1 to 3, characterized in that: The bubble cap plate tower also includes a return port, and the height of the return port is higher than the tower plate b.

5. The device according to claim 4, characterized in that The hydrogen raw material supply end includes a hydrogen storage device, a hydrogen flow meter and a hydrogen heater; and / or, the bisphenol A supply end includes a bisphenol A storage device, a bisphenol A flow meter and a bisphenol A heater.

6. The device according to claim 5, characterized in that The device for preparing hydrogenated bisphenol A by hydrogenating bisphenol A further comprises a condenser, the inlet of which is connected to the gas outlet of the bubble cap plate tower.

7. The device according to claim 5 or 6, characterized in that The device for preparing hydrogenated bisphenol A by hydrogenating bisphenol A also includes a separator, which is a sealed container with a liquid input port, a liquid output port c, a liquid output port d and a gas output port. The liquid input port of the separator is connected to the outlet of the condenser, and the liquid output port c of the separator is connected to the return port of the bubble plate tower.

8. A method for preparing hydrogenated bisphenol A by hydrogenating bisphenol A using the device according to any one of claims 1 to 7, characterized in that: The steps include: Hydrogen enters the bubble-cap plate tower through the gas feed port, and bisphenol A enters the bubble-cap plate tower through the liquid feed port. The hydrogen reacts with bisphenol A to obtain a product containing hydrogenated bisphenol A, and the gas is discharged. Preferably, the hydrogen and bisphenol A contact the hydrogenation catalyst to undergo a hydrogenation reaction. Preferably, the discharged gas includes unreacted hydrogen and vaporized solvent.

9. The method for preparing hydrogenated bisphenol A by hydrogenating bisphenol A according to claim 8, characterized in that: The product containing hydrogenated bisphenol A is discharged from the liquid discharge port of the bubble cap plate tower; And / or, the vaporized solvent and unreacted hydrogen are discharged from the gas outlet of the bubble cap plate tower, the vaporized solvent and unreacted hydrogen discharged from the gas outlet are condensed in a condenser to obtain hydrogen and liquefied solvent, the hydrogen and the liquefied solvent enter a separator, the hydrogen is discharged from the gas outlet of the separator, a part of the liquefied solvent is refluxed to the bubble cap plate tower through the liquid outlet c, and the remaining liquefied solvent is discharged from the liquid outlet d; And / or, the operating pressure of the bubble plate tower is 2.8-9 MPa; and / or, the molar ratio of hydrogen to bisphenol A feed is 20-80; and / or, the feed temperature of bisphenol A is 100-180°C; and / or, the feed temperature of hydrogen is 100-180°C; and / or, the hydrogenation catalyst comprises a carrier and an active component, the carrier is selected from activated carbon, alumina, molecular sieve, and the active component is selected from ruthenium, rhodium, palladium, platinum, and nickel.

10. Use of the device according to any one of claims 1 to 7 or the method according to claim 8 or 9 in the hydrogenation of bisphenol A to produce hydrogenated bisphenol A.

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