A device, method and application for preparing hydrogenated bisphenol A by hydrogenating bisphenol A

Abstract

The present invention provides an apparatus, method, and application for hydrogenating bisphenol A to produce hydrogenated bisphenol A. The apparatus comprises a hydrogen supply end, a bisphenol A supply end, and a bubble-cap tray tower. The bubble-cap tray tower comprises a liquid feed inlet, a gas feed inlet, a liquid discharge, and a gas discharge. The hydrogen supply end is connected to the gas feed inlet of the bubble-cap tray tower. The bisphenol A supply end is connected to the liquid feed inlet of the bubble-cap tray tower. The bubble-cap trays are used for the reaction of hydrogenating bisphenol A to produce hydrogenated bisphenol A. The present invention utilizes a bubble-cap tray tower to hydrogenate bisphenol A to produce hydrogenated bisphenol A. In the presence of a catalyst, a bisphenol A solution enters the tower from the middle, flows horizontally through the bubble-cap trays, and overflows downward, fully contacting hydrogen entering from the lower portion of the tower. This results in high reactant conversion rates and product yields.

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 a product generated by the catalytic hydrogenation reaction of bisphenol A. Since there are no unsaturated structures such as aromatic rings in the molecule, its 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, heat stability and weather resistance of the products, improve product quality, expand the application field, and make the products generate greater added value.

[0003] The bisphenol A hydrogenation reaction requires dissolving the bisphenol A (BPA) raw material in an organic solvent. The resulting solution is then mixed with hydrogen gas for hydrogenation. The hydrogen gas and the bisphenol A molecules in the raw material solution fully contact the catalyst surface, causing a hydrogenation reaction to produce hydrogenated bisphenol A. Bisphenol A hydrogenation generally utilizes a kettle or fixed-bed hydrogenation process. Typical reaction conditions include a temperature of 50-250°C and a hydrogen pressure of 1-30 MPa. A solvent is used during the reaction, and the reaction products are separated and purified using vacuum distillation or recrystallization.

[0004] Bisphenol A kettle hydrogenation process is generally batch type, can also be continuous type, technical process is for being dissolved in solvent by a certain ratio by Bisphenol A, add in the reactor with agitator together with the solid powder catalyst with carrier, carry out hydrogenation reaction under certain temperature, pressure, hydrogenation material removes catalyst (catalyst can be reused) after filtration, finally obtains hydrogenated bisphenol A product through removing solvent, the solvent removed can be recycled. Kettle hydrogenation reaction is more applicable for smaller production scale, and investment is also lower.But this operation has shortcomings such as complicated operation, catalyst loss is large.

[0005] The fixed-bed hydrogenation process for bisphenol A is a continuous hydrogenation process. A bisphenol A solution of a certain concentration is prepared in a solvent. After heating, the solution is mixed with hydrogen and fed into a hydrogenation reactor. The hydrogenation reaction proceeds under specific conditions, including pressure, temperature, space velocity, and hydrogen-to-oil ratio. The hydrogenated material undergoes cold gas-liquid separation to remove the solvent and byproducts. The hydrogenated bisphenol A product is then pelletized. Compared to kettle hydrogenation processes, fixed-bed hydrogenation requires higher equipment investment and places higher demands 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 an apparatus for hydrogenating bisphenol A to prepare hydrogenated 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 port, a gas feed port, 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 a vertical direction, the liquid feed port is located higher than the gas feed port, and the interior of the bubble cap plate tower is provided with several layers of tower plates a, the height of the tower plates a is located between the liquid inlet and the gas inlet, and the tower plates a are bubble cap plates for loading hydrogenation catalysts; the interior of the bubble cap plate tower is provided with several layers of tower plates b, which are in the form of sieve plates and are located higher than the liquid inlet for solvent removal.

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

[0014] Preferably, the bubble cap plate tower comprises 2-3 layers of plate 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 tray a includes a bubble cap, and the diameter of the tray a is 3 to 20 times the diameter of the bubble cap.

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

[0018] As a specific embodiment of the present invention, a filter screen is installed on tray a. The height of the filter screen is higher than the top of the bubble cap. The filter screen is fixedly connected to the bubble cap tray. The filter screen can prevent the loss of powdered catalyst during gas-liquid flow, ensuring that the amount of catalyst on the tray does not change and does not clog the tray nozzle.

[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 includes a return port, and the height of the return 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 reservoir, a hydrogen flowmeter, and a hydrogen heater. The hydrogen reservoir is used to store hydrogen before the reaction, the hydrogen flowmeter 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 reservoir, a bisphenol A flowmeter, and a bisphenol A heater. The bisphenol A reservoir 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 apparatus 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 tray tower. The condenser is used to condense hydrogen and solvent discharged from the top of the bubble-cap tray tower.

[0026] As a specific embodiment of the present invention, the device for preparing hydrogenated bisphenol A by hydrogenating bisphenol A further 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, which is used to reflux part of the solvent in the separator into 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 output port 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 into the bubble plate tower, and extracts the remaining solvent.

[0032] The solvent refluxed into the bubble cap plate tower undergoes a gas-liquid heat exchange with the gas generated within the bubble cap plate tower. Some by-products in the gas condense upon encountering the reflux solvent, and the non-condensable gas phase is discharged from the top of the tower. After condensation in the cooler, it enters the separation tank. After gas-liquid separation, it is extracted from the separation tank, achieving the removal of the solvent 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 apparatus provided by the first invention of the present invention, comprising the following steps: hydrogen enters a bubble-cap 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 bisphenol A solution, and the bisphenol A solution enters the bubble cap 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 liquefied solvent enter the 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 includes 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 utilizes a bubble-cap tray tower to hydrogenate bisphenol A to produce hydrogenated bisphenol A. In the presence of a catalyst, a bisphenol A solution enters the tower from the middle, flows horizontally through the bubble-cap tray, and overflows downward, fully contacting hydrogen entering from the lower portion of the tower. This results in high reactant conversion and product yields. The process is simple to operate and requires minimal investment. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1 Schematic diagram of the bisphenol A hydrogenation process 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 riser pipes on 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- tray a, 36- tray 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 with reference to specific examples, 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 includes 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 a vertical direction, the position of the liquid feed port 31 is higher than the gas feed port 32, and the interior of the bubble cap plate tower 3 is provided with several layers of tower plates a35, the height of the tower plate a35 is located between the liquid inlet 31 and the gas inlet 32, the tower plate a35 is a bubble cap tower plate, which is used to load the hydrogenation catalyst; the interior of the bubble cap plate tower 3 is provided with several layers of tower plates b36, the position of the tower plate b36 is higher than the liquid inlet, and the tower plate b36 is used to remove the solvent.

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

[0065] Specifically, the bubble cap plate tower includes 2 to 5 layers of tower 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, risers 352 are distributed on tray a35 and arranged in an equilateral triangle. Rising gas enters the upper layer from the lower layer through the risers 352. Round bubbles 351 are fixedly mounted on the top of the risers 352. Each bubble 351 has a triangular or quadrilateral slit at the bottom.

[0069] Specifically, each bubble cap tray is equipped with an overflow weir 353 , and the overflow weir 353 is higher than the top of the bubble cap 351 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. The filter screen 354 is fixedly connected to the bubble cap tower plate and 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 includes a condenser 4 , the inlet of the condenser 4 is connected to the gas discharge port 34 of the bubble-cap plate tower 3 .

[0075] As a specific embodiment of the present invention, the device for hydrogenating bisphenol A to prepare hydrogenated bisphenol A further 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 tray tower 3, the liquid output port d53 of the separator is connected to the outside world, and the gas output port 54 of the separator 5 is connected to the outside world. The separator 5 also includes a back pressure valve 55 connected to the gas output port 54. The back pressure valve 55 controls the pressure within the separator 5, refluxes part of the solvent in the separator 5 back to the bubble-cap tray tower 3, and extracts the remaining solvent.

[0076] Example 2

[0077] The bubble cap plate tower is used for the hydrogenation reaction of bisphenol A. The tower has 5 layers of trays b above the inlet of bisphenol A solution and 2 layers of bubble cap trays below. The diameter of the bubble cap tray is 50CM, and the ascending air pipe of the tray is Figure 3A circular bubble cap is fixedly installed on the top of the riser. The bubble cap has a diameter of 10 cm and a triangular slit at the bottom. The overflow weir of the bubble cap tray is higher than the top of the bubble cap. The tray is loaded with a powdered catalyst. The active component of the catalyst is Pd, and 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 tray. The liquid feed port of the tower is connected to a bisphenol A heater, the gas feed port is connected to a hydrogen heater, the gas discharge port of the bubble cap tray is connected to a 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 tray, which is used to reflux part of the solvent in the separator back into the bubble cap tray. 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, and the gas outlet of the separator is communicated with the outside for discharging the gas.

[0079] Bisphenol A was dissolved in isopropyl alcohol to a 15% mass concentration. The solution was then metered to a pressure of 4 MPa, preheated to 120°C, and introduced through the liquid feed port at a rate of 80 liters / hour. Hydrogen was then metered to a pressure of 4 MPa, heated to 120°C in a hydrogen heater, and introduced through the gas feed port at a rate of 400 liters / minute. The bubble-cap tray tower was insulated and heated on the outer layer. The bubble-cap tray temperature was 120-125°C and the pressure was 3.8-4 MPa. A differential pressure level gauge was installed at the bottom of the tower to discharge the partially desolvated hydrogenated bisphenol A solution. This gauge also controlled the bottom discharge volume and maintained the bottom liquid level. The bottom discharge composition was 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 trays b above the inlet of bisphenol A solution and 2 layers of bubble cap trays below. The tray diameter is 50CM and the tray ascending air pipe is Figure 3 A circular bubble cap is fixedly installed on the top of the riser. The bubble cap has a diameter of 10 cm and a triangular slit at the bottom. The overflow weir of the bubble cap tray is higher than the top of the bubble cap. The tray is loaded with a powdered catalyst. The active component of the catalyst is Ru, and 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 tray. The liquid feed inlet of the tower is connected to a bisphenol A heater, the gas feed inlet is connected to a hydrogen heater, the gas discharge port of the tower is connected to a condenser, and the material outlet of the condenser is connected to the liquid input port of the separator. The liquid output port c of the separator is connected to the return port of the bubble cap tray tower, which is used to reflux part of the solvent in the separator back into the bubble cap tray tower. The mass of the refluxed solvent is 40% of the total mass of the solvent in the separator.

[0082] Bisphenol A was dissolved in isopropyl alcohol to a 20% mass concentration. The solution was then metered to a pressure of 9 MPa, preheated to 140°C, and introduced through the tower's liquid feed port at a rate of 60 liters / hour. Hydrogen was then metered to a pressure of 9 MPa, heated to 140°C in a hydrogen heater, and introduced through the tower's gas feed port at a rate of 400 liters / minute. The tower's outer layer was insulated and heated to a bubble-cap tray temperature of 140-145°C at a pressure of 8.8-9 MPa. A differential pressure level gauge was installed at the bottom of the tower to discharge the partially desolvated hydrogenated bisphenol A solution. This gauge also controlled the amount of liquid discharged from the bottom of the tower to maintain the bottom liquid level. The composition of the bottom discharge was 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 trays b above the inlet of bisphenol A solution and 2 layers of bubble cap trays below. The tray diameter is 50CM and the tray ascending air pipe is Figure 3 A circular bubble cap is fixed on top of the riser. The bubble cap has a diameter of 10 cm and a triangular slit at its bottom. The overflow weir of the bubble cap tray is higher than the top of the bubble cap. The tray is loaded with a powdered catalyst. The active component of the catalyst is Pd, and 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 tray. 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, and the condenser material outlet is connected to the separation liquid input port. The liquid output port c of the separator is connected to the return port of the bubble cap tray column, used to reflux part of the solvent in the separator back into the bubble cap tray column. The mass of the refluxed solvent is 60% of the total mass of the solvent in the separator.

[0085] Bisphenol A was dissolved in isopropyl alcohol to a 10% concentration by mass. The solution was then metered to a pressure of 3 MPa, preheated to 180°C, and introduced through the tower's liquid feed port at a rate of 50 liters / hour. Hydrogen was then metered to a pressure of 3 MPa, heated to 180°C by a hydrogen heater, and introduced through the tower's gas feed port at a rate of 500 liters / minute. The tower's outer layer was insulated and heated to a bubble-cap tray temperature of 180-185°C at a pressure of 2.8-3 MPa. A differential pressure level gauge was installed at the bottom of the tower to discharge the partially desolvated hydrogenated bisphenol A solution. This gauge also controlled the amount of liquid discharged from the bottom of the tower to maintain the bottom liquid level. The composition of the bottom discharge was 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 trays b above the inlet of bisphenol A solution and 2 layers of bubble cap trays below. The tray diameter is 50CM and the tray ascending air pipe is Figure 3A circular bubble cap is fixedly installed on the top of the riser. The bubble cap has a diameter of 10 cm and a triangular slit at the bottom. The overflow weir of the bubble cap tray is higher than the top of the bubble cap. The tray is loaded with a powdered catalyst. The active component of the catalyst is Rh, and 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 tray. 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, and the condenser material outlet is connected to the liquid input port of the separator. The liquid output port c of the separator is connected to the return port of the bubble cap tray tower, which is used to reflux part of the solvent in the separator back into the bubble cap tray tower. The mass of the refluxed solvent is 20% of the total mass of the solvent in the separator.

[0088] Bisphenol A was dissolved in isopropyl alcohol to prepare a 15% bisphenol A solution. The solution was then metered to a pressure of 6 MPa and preheated to 100°C. The solution was introduced into the tower's liquid feed port at a rate of 80 liters / hour. Hydrogen was then metered to a pressure of 6 MPa and heated to 100°C in a hydrogen heater. The hydrogen was then introduced into the tower's gas feed port at a rate of 330 liters / minute. The tower's outer layer was insulated and heated to a bubble cap tray temperature of 110-115°C at a pressure of 5.8-6 MPa. A differential pressure level gauge was installed at the bottom of the tower to discharge the partially desolvated hydrogenated bisphenol A solution. This gauge also controlled the amount of liquid discharged from the bottom of the tower to maintain the bottom liquid level. The composition of the bottom discharge was analyzed, and the experimental results are shown in Table 1.

[0089] Example 6

[0090] A bubble-cap tray tower is used for the hydrogenation of bisphenol A. The tower has three trays (B) above the bisphenol A solution inlet and three bubble-cap trays (50 cm in diameter) below. A circular bubble cap (4 cm in diameter) is fixed to the top of the riser, with square slits cut into the bottom. The overflow weir of the bubble cap tray is higher than the top of the bubble cap. The trays are loaded with a powdered catalyst containing nickel as the active component and activated alumina as the carrier. The active component loading is 2% of the total catalyst weight, and the catalyst weight is 6 kg. A filter is installed after catalyst loading. The tower's liquid feed is connected to a bisphenol A heater, the gas feed is connected to a hydrogen heater, the gas discharge is connected to a condenser, the condenser outlet is connected to the liquid inlet of a separator, and the liquid discharge port (C) of the separator is connected to the return port of the bubble-cap tray tower, allowing some of the solvent in the separator to reflux back into the bubble-cap tray tower. The refluxed solvent weight accounts for 50% of the total solvent weight in the separator.

[0091] Bisphenol A was dissolved in isopropyl alcohol to a 15% mass concentration. The solution was then metered to a pressure of 6 MPa, preheated to 120°C, and introduced through the tower's liquid feed port at a rate of 80 liters / hour. Hydrogen was then metered to a pressure of 6 MPa, heated to 120°C by a hydrogen heater, and introduced through the tower's gas feed port at a rate of 400 liters / minute. The tower's outer layer was insulated and heated to a bubble-cap tray temperature of 120-125°C at a pressure of 5.8-6 MPa. A differential pressure level gauge was installed at the bottom of the tower to discharge the partially desolvated hydrogenated bisphenol A solution. This gauge also controlled the amount of liquid discharged from the bottom of the tower to maintain the bottom liquid level. The composition of the bottom discharge was analyzed, and the experimental results are shown in Table 1.

[0092] Example 7

[0093] A bubble-cap tray tower is used for the hydrogenation of bisphenol A. The tower has two trays (B) above the bisphenol A solution inlet and three bubble-cap trays (50 cm in diameter) below. A circular bubble cap (5 cm in diameter) is fixed to the top of the riser. The lower portion of the bubble cap has trapezoidal serrations. The overflow weir of the bubble cap tray is higher than the top of the bubble cap. The trays are loaded with a powdered catalyst containing nickel as the active component and activated carbon as the carrier. The active component loading is 2% of the total catalyst weight, totaling 5.5 kg. A filter is installed after catalyst loading. The tower's liquid feed is connected to a bisphenol A heater, the gas feed is connected to a hydrogen heater, the gas discharge is connected to a condenser, the condenser outlet is connected to the liquid inlet of a separator, and the liquid discharge port (C) of the separator is connected to the return port of the bubble-cap tray tower, allowing some of the solvent in the separator to reflux back into the bubble-cap tray tower. The refluxed solvent mass accounts for 30% of the total solvent mass in the separator.

[0094] Bisphenol A was dissolved in isopropyl alcohol to a 12% mass concentration. The solution was then metered to a pressure of 6 MPa, preheated to 120°C, and introduced through the tower's liquid feed port at a rate of 60 liters / hour. Hydrogen was then metered to a pressure of 6 MPa, heated to 120°C in a hydrogen heater, and introduced through the tower's gas feed port at a rate of 400 liters / minute. The tower's outer layer was insulated and heated to a bubble-cap tray temperature of 120-125°C at a pressure of 5.8-6 MPa. A differential pressure level gauge was installed at the bottom of the tower to discharge the partially desolvated hydrogenated bisphenol A solution. This gauge also controlled the amount of liquid discharged from the bottom of the tower to maintain the bottom liquid level. The composition of the bottom discharge was analyzed, and the experimental results are shown in Table 1.

[0095] Example 8

[0096] A bubble-cap tray tower was used for the hydrogenation of bisphenol A. The tower had five trays (B) above the bisphenol A solution inlet and two bubble-cap trays (50 cm in diameter) below. A circular bubble cap (15 cm in diameter) was fixed to the top of the riser. The lower portion of the bubble cap had trapezoidal serrations. The overflow weir of the bubble cap tray was higher than the top of the bubble cap. The trays were loaded with a powdered catalyst containing Pt as the active component on an activated alumina carrier at an active component loading of 1.2% of the total catalyst weight (3.5 kg). A filter screen was installed after catalyst loading. The tower's liquid feed was connected to a bisphenol A heater, the gas feed to a hydrogen heater, the gas discharge to a condenser, the condenser outlet to a separator liquid inlet, and the separator liquid outlet (C) to the bubble-cap tray return port, allowing some of the solvent in the separator to reflux back into the tower. The refluxed solvent amount accounted for 20% of the total solvent weight in the separator.

[0097] Bisphenol A was dissolved in isopropyl alcohol to a 20% mass concentration. The solution was then metered to a pressure of 8 MPa, preheated to 150°C, and introduced through the tower liquid feed at a rate of 60 liters / hour. Hydrogen was then metered to a pressure of 8 MPa, heated to 150°C by a hydrogen heater, and introduced through the tower gas feed at a rate of 400 liters / minute. The tower's outer layer was insulated and heated to a bubble cap tray temperature of 150-155°C at a pressure of 7.8-8 MPa. A differential pressure level gauge was installed at the bottom of the tower to discharge the partially desolvated hydrogenated bisphenol A solution. This gauge also controlled the bottom discharge volume and maintained the bottom liquid level. The bottom discharge composition was analyzed, and the experimental results are shown in Table 1.

[0098] Table 1 Analysis results of 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 produced by reaction ÷ mass of bisphenol A reacted) × 100%

[0103] Yield of hydrogenated bisphenol A = (mass of hydrogenated bisphenol A produced 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 of 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 function.

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 port, a gas feed port, 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 plate tower is used for carrying out a reaction of hydrogenating bisphenol A to prepare hydrogenated bisphenol A; The bubble cap plate tower is placed in a vertical direction, the position of the liquid feed port is higher than the gas feed port, the interior of the bubble cap plate tower is provided with a plurality of layers of trays a, the height of the trays a is located between the liquid inlet and the gas inlet, the trays a are bubble cap trays, and are used to load hydrogenation catalysts; the interior of the bubble cap plate tower is provided with a plurality of layers of trays b, the position of the trays b is higher than the liquid inlet, and the trays b are used to remove the solvent; The surface of the bubble cap tray is evenly distributed with riser pipes, a bubble cap is installed on the top of the riser pipe, and a slit is opened at the bottom of the bubble cap. An overflow weir is set on the bubble cap tray, and the height of the overflow weir is higher than the top of the bubble cap. A filter is installed on tray a; the height of the filter is higher than the top of the bubble cap, and the filter is fixedly connected to the bubble cap tray. The filter prevents the loss of powdered catalyst when the gas and liquid flow state.

2. The device according to claim 1, characterized in that The bubble-cap plate tower comprises 2 to 3 layers of tower plates a; and / or the bubble-cap plate tower comprises 2 to 5 layers of tower plates b.

3. The device according to claim 2, characterized in that The tray a comprises a bubble cap, and the diameter of the tray a is 3 to 20 times the diameter of the bubble cap.

4. The device according to claim 3, characterized in that The diameter of the tray a is 4 to 8 times the diameter of the bubble cap.

5. The device according to any one of claims 1 to 4, characterized in that: The bubble cap plate tower further comprises a return material port, the height of which is higher than the tower plate b.

6. The device according to claim 5, characterized in that The hydrogen 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.

7. The device according to claim 6, characterized in that The device for preparing hydrogenated bisphenol A by hydrogenating bisphenol A further comprises a condenser, the inlet of which is communicated with the gas discharge port of the bubble-cap plate tower.

8. The device according to claim 7, characterized in that The device for hydrogenating bisphenol A to prepare hydrogenated 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. 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-cap plate tower.

9. A method for preparing hydrogenated bisphenol A by hydrogenating bisphenol A using the apparatus according to any one of claims 1 to 8, 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 and bisphenol A contact the hydrogenation catalyst to undergo a hydrogenation reaction to obtain a product containing hydrogenated bisphenol A, and the gas is discharged.

10. The method for preparing hydrogenated bisphenol A by hydrogenating bisphenol A according to claim 9, characterized in that: The exhaust gas includes unreacted hydrogen and vaporized solvent.

11. The method for preparing hydrogenated bisphenol A by hydrogenating bisphenol A according to claim 10, 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 liquefied solvent enter a separator, the hydrogen is discharged from the gas outlet of the separator, a portion 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-cap plate tower is 2.8 to 9 MPa; and / or, the molar ratio of the hydrogen to bisphenol A feed is 20 to 80; and / or, the feed temperature of bisphenol A is 100 to 180° C.; and / or, the feed temperature of hydrogen is 100 to 180° C.; and / or, the hydrogenation catalyst includes a carrier and an active component, the carrier is selected from activated carbon, alumina or molecular sieve, and the active component is selected from ruthenium, rhodium, palladium, platinum or nickel.

12. Use of the device according to any one of claims 1 to 8 or the method according to any one of claims 9 to 11 in hydrogenating bisphenol A to produce hydrogenated bisphenol A.

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