Device and method for refining hydrogenated bisphenol A and application

By using a distillation tower and solid-liquid separator during the refining process of hydrogenated bisphenol A, combined with solvent replacement and condenser recovery technology, the problem of the boiling point of by-products and hydrogenated bisphenol A is solved, and high purity and high harvest are achieved Hydrogenated bisphenol A products are suitable for high-end materials.

CN119280852AActive Publication Date: 2025-01-10CHINA PETROLEUM & CHEMICAL CORP
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Patent Information

Application Number
CN202310840660.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-07-10
Publication Date
2025-01-10
Estimated Expiration
2043-07-10

AI Technical Summary

Technical Problem

During the refining process of existing hydrogenated bisphenol A, the boiling point and polarity of hydrogenated bisphenol A are similar, resulting in poor separation effect of distillation tower and evaporator, resulting in high-end fields for the purity and by-product content of hydrogenated bisphenol A. Difficult to satisfy.

Method used

Using a device including a distillation tower, cooling assembly and solid-liquid separator, the efficient hydrogenated bisphenol A purity is achieved through solvent replacement and condenser recovery. The boiling point of solvent b in the device is higher than solvent a, and a vacuum pump is established. Vacuum conditions to improve separation efficiency.

Benefits of technology

It has achieved high purity (greater than 98%) and high yield (93%) of hydrogenated bisphenol A, and is suitable for high-end fields such as 3D printing materials and electronic packaging materials.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention provides a device and method for refining hydrogenated bisphenol A and application. The device for refining hydrogenated bisphenol A comprises a to-be-refined hydrogenated bisphenol A supply end, a solvent b supply end, a rectifying tower, a cooling assembly, a solid-liquid separator and a pipeline, the rectifying tower is arranged in the vertical direction and comprises a feeding port a, a feeding port b, a discharging port c and a discharging port d, the feeding port a is higher than the feeding port b and the discharging port d, and the cooling assembly is arranged in the discharging port c. The supply end of hydrogenated bisphenol A to be refined is communicated with the feed port b, and the supply end of a solvent b is communicated with the feed port a; the rectifying tower, the cooling assembly and the solid-liquid separator are sequentially connected through pipelines, and the cooling assembly is communicated with a discharging port c of the rectifying tower. The hydrogenated bisphenol A product is refined by adopting the device and the method provided by the invention, and the obtained refined bisphenol A is high in purity and can be applied to the fields of 3D printing materials, electronic packaging materials and the like.
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Description

Technical Field

[0001] The invention relates to the field of hydrogenated bisphenol A preparation, and in particular to a device, method and application for refining hydrogenated bisphenol A. Background Art

[0002] Bisphenol A epoxy resin is a linear polymer formed by polycondensation of diphenol propane (bisphenol A) and epichlorohydrin in the presence of a catalyst. Bisphenol A epoxy resin is widely used in plastic packaging materials and has good mechanical and electrical insulation properties, chemical resistance and adhesion properties, stability, etc. Ordinary bisphenol A epoxy resin contains unsaturated benzene ring structure in the molecular chain, which is easy to age and discolor under long-term irradiation of ultraviolet light, and causes its transparency, insulation, strength and other properties to drop significantly. If the benzene ring on the molecular chain is replaced with a saturated cyclic hydrocarbon structure, the obtained hydrogenated bisphenol A epoxy resin can effectively overcome the above-mentioned shortcomings without reducing its mechanical properties and heat resistance. Hydrogenated bisphenol A (2,2-bis (4-hydroxycyclohexyl) propane) is an important monomer for manufacturing hydrogenated bisphenol A special epoxy resin. Hydrogenated bisphenol A has a stable molecular structure and can be used not only to manufacture hydrogenated bisphenol A special epoxy resin, but also to manufacture unsaturated polyester resin, polycarbonate, polyacrylic resin and other polymer synthetic materials. It can effectively improve the weather resistance, light and heat stability of synthetic resins, expand the application areas of resin products, and can be used in aerospace materials, electronic packaging materials, electronic and electrical materials, sealants, automotive coatings and other fields.

[0003] Hydrogenated bisphenol A is an alicyclic diol obtained by hydrogenating and saturating the two benzene rings in the bisphenol A (BPA) molecule using catalytic hydrogenation technology. The preparation of hydrogenated bisphenol A by hydrogenation of bisphenol A is based on bisphenol A (BPA) as a raw material, and is generated by a hydrogenation reaction under the action of a catalyst in a solution state. The process can adopt an intermittent or continuous hydrogenation reaction. Whether the intermittent or continuous hydrogenation reaction process, a solvent is used. The reaction requires that the bisphenol A (BPA) raw material be dissolved in an organic solvent to form a raw material solution of a certain concentration, and the hydrogenation reaction is carried out in the form of a solution. The solvent itself does not participate in the reaction. Its role is to facilitate the distribution of raw material molecules on the catalyst surface, adsorption, and desorption of reaction products from the catalyst surface and other mass transfer processes. At the same time, the solvent also has good solubility for bisphenol A at room temperature, which is conducive to fluid transportation.

[0004] In the prior art, the literature and patents on hydrogenated bisphenol A focus on hydrogenation processes, hydrogenation catalysts, and the application in the preparation of synthetic materials such as epoxy resins and polycarbonates, and there are few reports on the desolventization and refining processes of hydrogenated bisphenol A. The concentration of hydrogenated bisphenol A in commercially available hydrogenated bisphenol A reaching more than 96% can meet the needs of general hydrogenated bisphenol A epoxy resin production, but if it is applied in high-end fields, such as 3D printing materials, electronic packaging materials, etc., there are higher requirements for the purity of hydrogenated bisphenol A and the content of by-products.

[0005] Bisphenol A and hydrogenated bisphenol A have good solubility in solution. The selected solvent has a significant difference in boiling point with hydrogenated bisphenol A under normal pressure and vacuum conditions. Therefore, the distillation tower, evaporator and other equipment are used to remove solvents and by-products, which is the main refining method for hydrogenated bisphenol A. However, since the by-products produced by side reactions during the hydrogenation process have similar physical properties such as boiling point and polarity to hydrogenated bisphenol A, if it is necessary to remove by-products during the refining process to obtain a product with higher purity of hydrogenated bisphenol A, the distillation tower and evaporator must have a higher separation effect, and the equipment investment and energy consumption are relatively large. 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 refining hydrogenated bisphenol A.

[0007] In a first aspect, the present invention provides a device for refining hydrogenated bisphenol A.

[0008] It includes a supply end of hydrogenated bisphenol A to be refined, a supply end of solvent B, a distillation tower, a cooling component, a solid-liquid separator and a pipeline.

[0009] The distillation tower is placed in a vertical direction, and comprises a feed port a, a feed port b, a discharge port c and a discharge port d. The height of the feed port a is higher than the feed port b and the discharge port d. The supply end of the hydrogenated bisphenol A to be refined is connected to the feed port b, and the supply end of the solvent b is connected to the feed port a.

[0010] The distillation tower, the cooling component, and the solid-liquid separator are connected in sequence through pipelines, and the cooling component is connected to the discharge port c of the distillation tower;

[0011] The hydrogenated bisphenol A to be refined comprises hydrogenated bisphenol A and solvent a;

[0012] The distillation tower is used to replace the solvent a in the hydrogenated bisphenol A to be refined with the solvent b;

[0013] The cooling component is used to precipitate hydrogenated bisphenol A from solvent b;

[0014] The solid-liquid separator is used to separate the hydrogenated bisphenol A precipitated from the cooling component from the solvent B.

[0015] As a specific embodiment of the present invention, the solid-liquid separator is a centrifuge.

[0016] Preferably, the boiling point of the solvent b is higher than that of the solvent a, and the difference between the boiling points of the solvent a and the solvent b is less than or equal to 30° C. When the difference between the boiling points of the solvent a and the solvent b is greater than 30° C., a reactor with an external heating jacket or an internal heating coil can be used to replace the distillation tower.

[0017] As a specific embodiment of the present invention, the device for refining hydrogenated bisphenol A further comprises a solvent recovery tank, which is connected to the discharge port d of the distillation tower and is used to recover the solvent, specifically, to recover the solvent a.

[0018] As a specific embodiment of the present invention, the solvent recovery tank and the discharge port d are also provided with a condenser. The condenser is used to condense the gas phase solvent a discharged from the distillation tower.

[0019] As a specific embodiment of the present invention, the device for refining hydrogenated bisphenol A further comprises a vacuum pump, which is connected to the solvent recovery tank and is used to establish vacuum conditions in the device for refining hydrogenated bisphenol A.

[0020] As a specific embodiment of the present invention, the supply end of the hydrogenated bisphenol A to be refined includes a hydrogenated bisphenol A storage tank to be refined and a hydrogenated bisphenol A feed pump to be refined; the hydrogenated bisphenol A feed pump to be refined is used to control the feed rate of the hydrogenated bisphenol A to be refined.

[0021] As a specific embodiment of the present invention, the solvent b supply end further includes a solvent b storage and a solvent b feed pump; the solvent b feed pump is used to control the feed speed of the solvent b.

[0022] As a specific embodiment of the present invention, the device for refining hydrogenated bisphenol A further comprises a flow valve arranged on the feed pipeline of the distillation tower, and the flow valve is used to control the flow rate of the feed of the distillation tower. In the case of high vacuum, the feed pump of the hydrogenated bisphenol A to be refined and the feed pump of the solvent B may not be set up, but a flow control valve needs to be set on the pipeline of the distillation tower feed to achieve the hydrogenated bisphenol A to be refined and the solvent B to smoothly enter the distillation tower and achieve flow control.

[0023] As a specific embodiment of the present invention, the device for refining hydrogenated bisphenol A includes a discharge pump connected to a discharge port b, and the discharge pump is used to control the discharge of the discharge port d of the distillation tower.

[0024] As a specific embodiment of the present invention, the cooling component includes a reactor, a cooler and a temperature controller, the cooler is used to reduce the temperature inside the reactor, and the temperature controller is used to control the cooling rate of the cooler. Specifically, the cooler in the present invention is a heating jacket arranged outside the reactor or a heating coil arranged inside the reactor. Specifically, the temperature controller is a temperature control circulator.

[0025] As a specific embodiment of the present invention, the reactor comprises a feed port e and a discharge port f, the reactor is placed vertically, the feed port e is located at the top of the reactor, and the discharge port f is located at the bottom of the reactor. The feed port e is connected to the discharge port c of the distillation tower, and the discharge port f is connected to the solid-liquid separator.

[0026] As a specific embodiment of the present invention, the reactor is provided with a stirring device.

[0027] As a specific embodiment of the present invention, the device also includes a drying box, which is used to dry the hydrogenated bisphenol A obtained after separation by the solid-liquid separator.

[0028] In a second aspect, the present invention provides a method for refining hydrogenated bisphenol A to be refined using the device provided in the first aspect of the present invention, comprising the following steps:

[0029] Step S1: introducing the hydrogenated bisphenol A to be purified into a distillation tower, wherein the hydrogenated bisphenol A to be purified is separated into bisphenol A and solvent a in the distillation tower, and the solvent a is discharged from the distillation tower;

[0030] Step S2: introducing solvent b into the distillation tower, and mixing solvent b with hydrogenated bisphenol A;

[0031] Step S3: precipitating hydrogenated bisphenol A from solution b;

[0032] Step S4: Separating the hydrogenated bisphenol A precipitated in step S3 from the solvent b to obtain hydrogenated bisphenol A.

[0033] As a specific implementation mode of the present invention, step S4 further includes step S5, and step S5 is drying the hydrogenated bisphenol A obtained after the solid-liquid separation in step S4.

[0034] As a specific embodiment of the present invention, the solvent a includes at least one of ethanol, isopropanol, isobutanol and cyclohexanol.

[0035] As a specific embodiment of the present invention, solution b includes one or more of toluene, p-xylene, o-xylene, m-xylene, mixed xylenes, mesitylene, and durene.

[0036] As a specific embodiment of the present invention, the amount of solvent b added to the distillation tower is 20% to 300% of the mass of hydrogenated bisphenol A to be purified.

[0037] Preferably, the amount of solvent b added to the distillation tower is 40% to 100% of the mass of hydrogenated bisphenol A to be refined.

[0038] As a specific embodiment of the present invention, the amount of solvent b added to the distillation tower is 2 to 10 times the mass of hydrogenated bisphenol A in the hydrogenated bisphenol A to be refined.

[0039] Preferably, the amount of solvent b added to the distillation tower is 3 to 6 times the mass of hydrogenated bisphenol A in the hydrogenated bisphenol A to be refined.

[0040] And / or, as a specific embodiment of the present invention, solution b is introduced into the distillation tower when the mass of the residual solvent a in the distillation tower is 50% of the total mass of the solution in the distillation tower or the mass of the residual solvent a in the distillation tower is less than 50% of the total mass of the solution in the distillation tower.

[0041] As a specific embodiment of the present invention, the pressure in the distillation tower is atmospheric pressure or the pressure is controlled to be 0 to -0.09MPaG. During the solvent replacement process, when the boiling point of solvent a is less than 85°C, solvent replacement is carried out under atmospheric pressure, and the removal of solvent a and the replenishment of solvent b can be carried out simultaneously; when the boiling point of solvent a is greater than 85°C, solvent replacement is carried out under reduced pressure, and the higher the boiling point, the higher the vacuum required. When the boiling point of solvent b is higher than that of solvent a, and the difference between the two is greater than 20°C, the removal of solvent a and the replenishment of solvent b can be carried out simultaneously; when the difference between the two is less than or equal to 20°C, even when the boiling point of solvent b is lower than that of solvent a, solvent a is removed first, and after the solvent removal rate is reached, the temperature is controlled to slowly replenish solvent b.

[0042] And / or, as an embodiment of the present invention, step 3 is to place the mixture of hydrogenated bisphenol A and solution b in a reactor, and to precipitate hydrogenated bisphenol A from solution b by lowering the temperature of the reactor.

[0043] Preferably, when the temperature of the mixture is above 60° C., the cooling rate of the reactor is 5 to 15° C. / H1.

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

[0045] In a fourth aspect, the present invention provides a refined hydrogenated bisphenol A prepared by the apparatus provided by the first aspect of the present invention or the method provided by the second aspect of the present invention, wherein the mass content of hydrogenated bisphenol A in the refined hydrogenated bisphenol A is greater than 98%.

[0046] Compared with the prior art, the present invention has the following beneficial effects.

[0047] The device and method of the present invention are used to purify the hydrogenated bisphenol A product. The obtained purified bisphenol A has high purity and can be applied to the fields of 3D printing materials, electronic packaging materials, etc. The mass content of hydrogenated bisphenol A in the hydrogenated bisphenol A obtained after purification by the present invention can reach 98%. And the single-pass yield of hydrogenated bisphenol A can reach 93%. BRIEF DESCRIPTION OF THE DRAWINGS

[0048] Figure 1 This is a schematic diagram of the refining process of hydrogenated bisphenol A of the present invention;

[0049] 1-supply end of hydrogenated bisphenol A to be refined, 11-storage tank of hydrogenated bisphenol A to be refined, 12-feed pump of hydrogenated bisphenol A to be refined,

[0050] 2-solvent b supply end, 21-solvent b storage, 22-solvent b feed pump,

[0051] 3-distillation tower, 31-feed port a, 32-feed port b, 33-discharge port c, 34-discharge port d,

[0052] 4-cooling component, 41-reactor, 42-cooler, 43-temperature control circulator, 411-feeding port e, 412-discharging port f,

[0053] 5-solid-liquid separator, 6-solvent recovery tank, 7-condenser,

[0054] 8- vacuum pump, 9- discharge pump, 10- drying oven. DETAILED DESCRIPTION

[0055] The present invention will be further described below in conjunction with specific embodiments, but they do not constitute any limitation to the present invention.

[0056] Example 1

[0057] A device for refining hydrogenated bisphenol A, comprising a hydrogenated bisphenol A supply end 1 to be refined, a solvent B supply end 2, a distillation tower 3, a cooling component 4, a solid-liquid separator 5 and a pipeline;

[0058] The distillation tower 3 is placed in the vertical direction, and includes a feed port a31, a feed port b32, a discharge port c33 and a discharge port d34. The height of the feed port a is higher than that of the feed port b. The supply end of the hydrogenated bisphenol A to be refined is connected to the feed port b32, and the supply end of the solvent b is connected to the feed port 31.

[0059] The distillation tower 3 , the cooling component 4 , and the solid-liquid separator 5 are connected in sequence through pipelines, and the cooling component 4 is connected to the bottom of the distillation tower 3 .

[0060] Specifically, the hydrogenated bisphenol A to be refined includes hydrogenated bisphenol A and solvent a;

[0061] Specifically, the distillation tower 3 is used to replace the solvent a in the hydrogenated bisphenol A to be refined with the solvent b;

[0062] Specifically, the cooling component is used to precipitate hydrogenated bisphenol A from solvent b;

[0063] Specifically, the solid-liquid separator 5 is used to separate the hydrogenated bisphenol A precipitated in the cooling component 4 from the solvent b.

[0064] Furthermore, the device for refining bisphenol A further comprises a solvent recovery tank 6, which is connected to the top of the discharge port d34 of the distillation tower 3, and a condenser 7 is directly provided between the solvent recovery tank 6 and the discharge port d34. The condenser 7 is used to condense the gas phase solvent a discharged from the distillation tower 3.

[0065] Specifically, the device for refining hydrogenated bisphenol A further includes a vacuum pump 8, which is connected to a solvent recovery tank 6 to establish vacuum conditions in the device for refining hydrogenated bisphenol A.

[0066] Furthermore, the hydrogenated bisphenol A supply end 1 to be refined includes a hydrogenated bisphenol A storage tank 11 to be refined and a hydrogenated bisphenol A feed pump 12 to be refined; the hydrogenated bisphenol A feed pump 12 to be refined is used to control the feed rate of the hydrogenated bisphenol A to be refined.

[0067] Specifically, the solvent b supply end 2 further includes a solvent b storage 21 and a solvent b feed pump 22; the solvent b feed pump 22 is used to control the feed speed of the solvent b.

[0068] Specifically, the device for refining hydrogenated bisphenol A further comprises a flow valve disposed on the feed pipeline of the distillation tower, and the flow valve is used to control the flow rate of the feed to the distillation tower. In the case of high vacuum, the feed pump of the hydrogenated bisphenol A to be refined and the feed pump of the solvent B may not be set up, but a flow control valve needs to be set on the feed pipeline of the distillation tower to ensure that the hydrogenated bisphenol A to be refined and the solvent B enter the distillation tower smoothly and realize flow control.

[0069] The device for refining hydrogenated bisphenol A includes a discharge pump 9, which is connected to the discharge port b34. The discharge pump 9 is used to control the discharge of the discharge port d34 of the distillation tower.

[0070] Furthermore, the cooling component 4 includes a reaction kettle 41 , a cooler 42 and a temperature controller 43 .

[0071] Reactor 41 includes feed port e411 and discharge port f412. Reactor 41 is placed vertically, feed port e411 is located at the top of reactor 41, and discharge port f412 is located at the bottom of reactor 41. Feed port e411 is connected to discharge port c33 of distillation tower 3, and discharge port f412 is connected to solid-liquid separator.

[0072] Furthermore, the cooler 42 is a heating jacket disposed on the reactor 41 , and the temperature controller 43 is a temperature control circulator connected to the heating jacket for controlling the temperature of the heating jacket, thereby controlling the temperature of the reactor 41 .

[0073] Specifically, a stirring device with controllable speed is installed inside the reactor.

[0074] Specifically, the solid-liquid separator 5 is a centrifuge, which is used to separate the hydrogenated bisphenol A precipitated in the reaction kettle 41 from the solvent b.

[0075] Furthermore, the device for refining hydrogenated bisphenol A also includes a drying box 10, which is used to dry the hydrogenated bisphenol A obtained after separation by the centrifuge, and the hydrogenated bisphenol A is dried to obtain refined hydrogenated bisphenol A.

[0076] Example 2

[0077] The hydrogenated bisphenol A to be refined includes isopropanol (solvent a) and crude hydrogenated bisphenol A with a purity of 96.12%. The mass concentration of crude hydrogenated bisphenol A in the hydrogenated bisphenol A to be refined is 10%. The hydrogenated bisphenol A to be refined is pumped out by the hydrogenated bisphenol A feed pump and enters the distillation tower. After the liquid level in the bottom of the tower reaches 2 / 3, the distillation tower is heated until the gas phase temperature at the top of the distillation tower rises to 82-84°C. Solvent a is vaporized and discharged from the top of the distillation tower. The gaseous solvent a is condensed and refluxed in the condenser and then extracted to the solvent recovery tank. The medium temperature in the condenser is 15-20°C. When the remaining proportion of solvent a reaches 60% (the mass of solvent a not distilled out is 60% of the total mass of the solution in the distillation tower), the solvent b feed pump is turned on. Solvent b is p-xylene. The solvent b is gradually adjusted. The throttling amount is set, the feed flow rate of hydrogenated bisphenol A to be refined is set to 10 kg / h, the feed flow rate of p-xylene is set to 10 kg / h, the operating conditions of the distillation tower are adjusted, 8 kg / h of solvent a is produced, the remaining proportion of solvent a reaches 50% (the mass of undistilled solvent a is 50% of the total mass of the solution in the distillation tower) and the liquid level of the distillation tower is stable, the discharge pump is turned on, and the discharge flow rates of hydrogenated bisphenol A and solvent b are set to 12 kg / h. After the solvent is replaced, the newly formed hydrogenated bisphenol A and solvent b are pumped out from the bottom of the distillation tower by the discharge pump and enter the reactor equipped with a controllable speed stirring device. The reactor is operated intermittently, and the stirring is maintained at a constant speed of 30 to 50 rpm. The outer wall of the reactor is jacketed, and the jacket is filled with heat-conducting medium. The medium inlet and outlet pipelines are connected to a temperature control circulator. During the process of pumping hydrogenated bisphenol A and solvent b, the pipelines are insulated and heated to control the temperature in the reactor to be constant. When the liquid level of the reactor reaches 50 to 70% of the liquid level range, the feeding is stopped, and the temperature is lowered to 60°C at a cooling rate of 5°C per hour, and then from 60°C to 30°C at a cooling rate of 15°C per hour. The solid-liquid mixture is obtained by stirring at 30°C for 2 hours, and the solid-liquid mixture is discharged into a centrifuge. The centrifuge is operated for solid-liquid separation. After solid-liquid separation, the solid containing a certain amount of solvent is transferred to a drying box, and nitrogen is introduced into the drying box to remove the solvent at 100°C to obtain the refined hydrogenated bisphenol A. The composition of hydrogenated bisphenol A is analyzed, and the yield and purity of hydrogenated bisphenol A are investigated. The experimental results are shown in Table 1.

[0078] Example 3

[0079] The hydrogenated bisphenol A to be refined includes ethanol (solvent a) and crude hydrogenated bisphenol A with a mass purity of 96.12%. The mass concentration of crude hydrogenated bisphenol A in the hydrogenated bisphenol A to be refined is 30%. The hydrogenated bisphenol A to be refined is pumped out by the hydrogenated bisphenol A feed pump to be refined and enters the distillation tower. After the tower bottom reaches 2 / 3 of the liquid level, the distillation tower is heated until the gas phase temperature at the top of the distillation tower rises to 78-80°C. Solvent a is vaporized and discharged from the top of the distillation tower. The gaseous solvent a is condensed and refluxed by the condenser and then extracted to the solvent recovery tank. The medium temperature in the condenser is 15-20°C. When the remaining proportion of solvent a reaches 60% (the mass of solvent a that has not been distilled out is 60% of the total mass of the solution in the distillation tower), the solvent b feed pump is turned on. Solvent b is o-xylene and toluene. The mixed solution with a molar ratio of 1:1, gradually adjust the flow rate, set the feed flow rate of hydrogenated bisphenol A to be refined to 10 kg / h, set the feed flow rate of the mixed solution to 30 kg / h, adjust the operating conditions of the distillation tower, the remaining proportion of solvent a reaches 50% (the mass of undistilled solvent a is 50% of the total mass of the solution in the distillation tower) and the liquid level of the distillation tower is stable, start the discharge pump, set the discharge flow rates of hydrogenated bisphenol A and solvent b to 36 kg / h, and the newly formed hydrogenated bisphenol A and solvent b after solvent replacement are pumped out from the bottom of the distillation tower by the discharge pump and enter the reactor equipped with controllable speed stirring. The reactor is operated intermittently, and the stirring is maintained at a constant speed. The outer wall of the reactor is jacketed, and the jacket is filled with heat-conducting medium. The medium inlet and outlet pipelines are connected to a temperature control circulator. During the process of pumping hydrogenated bisphenol A and solvent b, the pipelines are insulated and heated to control the temperature in the reactor to be constant. When the liquid level of the reactor reaches 70% of the liquid level range, the feeding is stopped, and the temperature is cooled to 30°C at a cooling rate of 5°C per hour, and the temperature is maintained at 30°C for 2 hours. The solid-liquid mixture is discharged into a centrifuge, and the centrifuge is operated for solid-liquid separation. After solid-liquid separation, the solid containing a certain amount of solvent is transferred to a drying box, and nitrogen is introduced into the drying box to remove the solvent at 100°C to obtain refined hydrogenated bisphenol A. The composition of hydrogenated bisphenol A is analyzed, and the yield and purity of hydrogenated bisphenol A are investigated. The experimental results are shown in Table 1.

[0080] Example 4

[0081] The hydrogenated bisphenol A to be refined includes isopropanol (solvent a) and crude hydrogenated bisphenol A with a mass purity of 96.12%, and the mass concentration of crude hydrogenated bisphenol A in the hydrogenated bisphenol A to be refined is 20%. The hydrogenated bisphenol A to be refined is pumped out by the hydrogenated bisphenol A feed pump to be refined and enters the distillation tower. After the tower bottom reaches 2 / 3 of the liquid level, the vacuum pump is started, and the vacuum pump is connected to the solvent recovery tank to provide vacuum conditions for this process, and the vacuum degree is controlled at -0.02MPa. After the vacuum is established, the temperature of the distillation tower is increased until the gas phase temperature at the top of the distillation tower rises to 72-74°C. Solvent a is vaporized and discharged from the top of the distillation tower. The gas phase solvent a is condensed and refluxed by the condenser and then the solvent a is collected to the solvent recovery tank. The medium temperature in the condenser is 15-20°C. When the remaining proportion of solvent a reaches 60% (the mass of the undistilled solvent a is 60% of the total mass of the solution in the distillation tower), the solvent b feed pump is turned on. Solvent b is m-xylene. The flow rate is gradually adjusted and the hydrogenation to be refined is set. The feed flow rate of bisphenol A is 10 kg / h, the feed flow rate of meta-xylene is set to 6 kg / h, and the operating conditions of the distillation tower are adjusted. The remaining proportion of solvent a reaches 40% (the mass of undistilled solvent a is 40% of the total mass of the solution in the distillation tower) and the liquid level of the distillation tower is stable. The discharge pump is turned on, and the discharge flow rates of hydrogenated bisphenol A and solvent b are set to 9.4 kg / h. After the solvent is replaced, the newly formed hydrogenated bisphenol A and solvent b are pumped out from the bottom of the distillation tower by the discharge pump and enter the reactor equipped with controllable speed stirring. The reactor is operated intermittently, and the stirring is maintained at a constant speed. The outer wall of the reactor is jacketed, and the jacket is filled with heat-conducting medium. The medium inlet and outlet pipelines are connected to a temperature control circulator. During the process of pumping hydrogenated bisphenol A and solvent b, the pipelines are insulated and heated to control the temperature in the reactor to be constant. When the liquid level of the reactor reaches 70% of the liquid level range, the feeding is stopped, and the temperature is lowered to 60°C at a cooling rate of 10°C per hour, and then from 60°C to 30°C at a cooling rate of 15°C per hour. The temperature is kept at 30°C and stirred for 2 hours. The solid-liquid mixture is discharged into a centrifuge, and the centrifuge is operated for solid-liquid separation. After solid-liquid separation, the solid containing a certain amount of solvent is transferred to a drying box, and nitrogen is introduced into the drying box to remove the solvent at 100°C to obtain the refined hydrogenated bisphenol A. The composition of hydrogenated bisphenol A is analyzed, and the yield and purity of hydrogenated bisphenol A are investigated. The experimental results are shown in Table 1.

[0082] Example 5

[0083] The hydrogenated bisphenol A to be refined includes isobutyl alcohol (solvent a) and crude hydrogenated bisphenol A with a mass purity of 96.12%, and the mass concentration of crude hydrogenated bisphenol A in the hydrogenated bisphenol A to be refined is 15%. The hydrogenated bisphenol A to be refined is pumped out by the hydrogenated bisphenol A feed pump to be refined and enters the distillation tower. After the tower bottom reaches 2 / 3 of the liquid level, the vacuum pump is started to establish vacuum conditions. The vacuum pump is connected to the solvent recovery tank to provide vacuum conditions for this process, and the vacuum degree is controlled at -0.03MPa. After the vacuum is established, the temperature of the distillation tower is increased until the gas phase temperature at the top of the distillation tower rises to 73-75°C. Solvent a is vaporized and discharged from the top of distillation tower 3. The gas phase solvent a is condensed and refluxed through the condenser and then the solvent a is extracted to the solvent recovery tank. The medium temperature in the condenser is 15-20°C. When the remaining proportion of solvent a reaches 60% (the mass of undistilled solvent a is 60% of the total mass of the solution in the distillation tower), the solvent b feed pump is turned on. Solvent b is a mixed xylene containing p-xylene, m-xylene and o-xylene, and the flow rate is gradually adjusted. , set the feed flow rate of hydrogenated bisphenol A to be refined to 10 kg / h, set the feed flow rate of mixed xylene to 3 kg / h, adjust the operating conditions of the distillation tower, adjust the remaining proportion of solvent a to 35% (the mass of undistilled solvent a is 35% of the total mass of the solution in the distillation tower) and the liquid level of the distillation tower is stable, start the discharge pump, set the discharge flow rates of hydrogenated bisphenol A and solvent b to 5.3 kg / h, and after the solvent is replaced, the newly formed hydrogenated bisphenol A and solvent b are pumped out from the bottom of the distillation tower by the discharge pump and enter the reactor equipped with controllable speed stirring. The reactor is operated intermittently, and the stirring is maintained at a constant speed. The outer wall of the reactor is jacketed, and the jacket is filled with heat-conducting medium. The medium inlet and outlet pipelines are connected to a temperature control circulator. During the process of pumping hydrogenated bisphenol A and solvent b, the pipelines are insulated and heated to control the temperature in the reactor to be constant. When the liquid level of the reactor reaches 70% of the liquid level range, the feeding is stopped, and the temperature is lowered to 60°C at a cooling rate of 10°C per hour, and then from 60°C to 30°C at a cooling rate of 15°C per hour. The temperature is kept at 30°C and stirred for 2 hours. The solid-liquid mixture is discharged into a centrifuge, and the centrifuge is operated for solid-liquid separation. After solid-liquid separation, the solid containing a certain amount of solvent is transferred to a drying box, and nitrogen is introduced into the drying box to remove the solvent at 100°C to obtain the refined hydrogenated bisphenol A. The composition of hydrogenated bisphenol A is analyzed, and the yield and purity of hydrogenated bisphenol A are investigated. The experimental results are shown in Table 1.

[0084] Example 6

[0085] The hydrogenated bisphenol A to be refined includes isopropanol (solvent a) and crude hydrogenated bisphenol A with a purity of 95.76%. The mass concentration of crude hydrogenated bisphenol A in the hydrogenated bisphenol A to be refined is 10%. The hydrogenated bisphenol A to be refined is pumped out by the hydrogenated bisphenol A feed pump to be refined and enters the distillation tower 3. After the tower bottom reaches 2 / 3 of the liquid level, the distillation tower is heated until the gas phase temperature at the top of the distillation tower rises to 82-84°C. Solvent a is vaporized and discharged from the top of the distillation tower. The gaseous solvent a is condensed and refluxed by the condenser and then extracted to the solvent recovery tank. The medium temperature in the condenser is 15-20°C. When the remaining proportion of solvent a reaches 60% (the mass of the undistilled solvent a is 60% of the total mass of the solution in the distillation tower), the solvent b feed pump is turned on. Solvent b is Toluene, gradually adjust the flow rate, set the feed flow rate of hydrogenated bisphenol A to be refined to 10 kg / h, set the feed flow rate of toluene to 2 kg / h, adjust the operating conditions of the distillation tower 3, the remaining proportion of solvent a reaches 25% (the mass of undistilled solvent a is 25% of the total mass of the solution in the distillation tower) and the liquid level of the distillation tower 3 is stable, start the discharge pump, set the discharge flow rate of hydrogenated bisphenol A and solvent b to 3.3 kg / h, and the newly formed hydrogenated bisphenol A and solvent b after solvent replacement are pumped out from the bottom of the distillation tower by the discharge pump and enter the reactor equipped with controllable speed stirring. The reactor is operated intermittently, and the stirring is maintained at a constant speed. The coil design in the reactor contains a heat-conducting medium. The inlet and outlet of the coil are connected to an external temperature control circulator. During the process of pumping hydrogenated bisphenol A and solvent b, the pipeline is insulated and heated to control the temperature in the reactor to be constant. When the liquid level of the reactor reaches 70% of the liquid level range, the feeding is stopped, and the temperature is cooled to 30°C at a cooling rate of 5°C per hour. The temperature is maintained at 30°C and stirred for 2 hours. The solid-liquid mixture is discharged into a centrifuge, and the centrifuge is operated for solid-liquid separation. After solid-liquid separation, the solid containing a certain amount of solvent is transferred to a drying box, and nitrogen is introduced into the drying box to remove the solvent at 100°C to obtain refined hydrogenated bisphenol A. The composition of hydrogenated bisphenol A is analyzed, and the yield and purity of hydrogenated bisphenol A are investigated. The experimental results are shown in Table 1.

[0086] Example 7

[0087] The hydrogenated bisphenol A to be refined includes cyclohexanol (solvent a) and crude hydrogenated bisphenol A with a mass purity of 95.76%, and the mass concentration of crude hydrogenated bisphenol A in the hydrogenated bisphenol A to be refined is 15%. The hydrogenated bisphenol A to be refined is pumped out by the hydrogenated bisphenol A feed pump to be refined and enters the distillation tower 3. After the tower bottom reaches 2 / 3 of the liquid level, the vacuum pump is started to establish vacuum conditions. The vacuum pump is connected to the solvent recovery tank to provide vacuum conditions for this process, and the vacuum degree is controlled at -0.09MPa. After the vacuum is established, the temperature of the distillation tower is increased until the gas phase temperature at the top of the distillation tower rises to 65-68°C. Solvent a is vaporized and discharged from the top of the distillation tower. The gas phase solvent a is condensed and refluxed by the condenser and then the solvent a is collected to the solvent recovery tank. The medium temperature in the condenser is 15-20°C. When the remaining proportion of solvent a reaches 60% (the mass of the undistilled solvent a is 60% of the total mass of the solution in the distillation tower), the solvent b feed pump is turned on. Solvent b is durene. The flow rate is gradually adjusted and the hydrogenated bisphenol to be refined is set. The A feed flow rate is 10 kg / h, the tetramethylbenzene feed flow rate is set to 10 kg / h, and the operating conditions of the distillation tower are adjusted. The remaining proportion of solvent a reaches 30% (the mass of undistilled solvent a is 30% of the total mass of the solution in the distillation tower) and the liquid level of the distillation tower is stable. The discharge pump is turned on, and the discharge flow rates of hydrogenated bisphenol A and solvent b are set to 12.1 kg / h. After the solvent is replaced, the newly formed hydrogenated bisphenol A and solvent b are pumped out from the bottom of the distillation tower by the discharge pump and enter the reactor equipped with controllable speed stirring. The reactor is operated intermittently, and the stirring is maintained at a constant speed. The outer wall of the reactor is jacketed, and the jacket is filled with heat-conducting medium. The medium inlet and outlet pipelines are connected to a temperature control circulator. During the process of pumping hydrogenated bisphenol A and solvent b, the pipelines are insulated and heated to control the temperature in the reactor to be constant. When the liquid level of the reactor reaches 70% of the liquid level range, the feeding is stopped, and the temperature is cooled to 30°C at a cooling rate of 15°C per hour, and the temperature is maintained at 30°C for 2 hours. The solid-liquid mixture is discharged into a centrifuge, and the centrifuge is operated for solid-liquid separation. After solid-liquid separation, the solid containing a certain amount of solvent is transferred to a drying box, and nitrogen is introduced into the drying box to remove the solvent at 100°C to obtain refined hydrogenated bisphenol A. The composition of hydrogenated bisphenol A is analyzed, and the yield and purity of hydrogenated bisphenol A are investigated. The experimental results are shown in Table 1.

[0088] Example 8

[0089] The hydrogenated bisphenol A to be refined comprises isopropanol (solvent a) and crude hydrogenated bisphenol A with a mass purity of 95.76%, wherein the mass concentration of crude hydrogenated bisphenol A in the hydrogenated bisphenol A to be refined is 15%, and the hydrogenated bisphenol A to be refined is pumped out by a hydrogenated bisphenol A feed pump to be refined and enters a distillation tower. After the liquid level in the bottom of the tower reaches 2 / 3, the distillation tower is heated until the gas phase temperature at the top of the distillation tower rises to 82-84° C., and the solvent a is vaporized and discharged from the top of the distillation tower. The gaseous solvent a is condensed and refluxed by a condenser, and then the solvent a is extracted to a solvent recovery tank. The medium temperature in the condenser is 15-20° C. When the remaining proportion of the solvent a reaches 60% (the undistilled solvent The mass of solvent a is 60% of the total mass of the solution in the distillation tower), the solvent b feed pump is turned on, the solvent b is toluene, the flow rate is gradually adjusted, the feed flow rate of hydrogenated bisphenol A to be refined is set to 10 kg / h, the feed flow rate of toluene is set to 6 kg / h, the operating conditions of the distillation tower are adjusted, the remaining proportion of solvent a reaches 35% (the mass of undistilled solvent a is 35% of the total mass of the solution in the distillation tower) and the liquid level of the distillation tower is stable, the discharge pump is turned on, and the discharge flow rates of hydrogenated bisphenol A and solvent b are set to 7.5 kg / h. After the solvent is replaced, the newly formed hydrogenated bisphenol A and solvent b are pumped out from the bottom of the distillation tower by the discharge pump and enter the reactor equipped with a controllable speed stirrer. The reactor is operated intermittently, and the stirring is maintained at a constant speed. The outer wall of the reactor is jacketed, and the jacket is filled with heat-conducting medium. The medium inlet and outlet pipelines are connected to a temperature control circulator. During the process of pumping hydrogenated bisphenol A and solvent b, the pipelines are insulated and heated to control the temperature in the reactor to be constant. When the liquid level of the reactor reaches 70% of the liquid level range, the feeding is stopped, and the temperature is cooled to 30°C at a cooling rate of 5°C per hour, and the temperature is maintained at 30°C for 2 hours. The solid-liquid mixture is discharged into a centrifuge, and the centrifuge is operated for solid-liquid separation. After solid-liquid separation, the solid containing a certain amount of solvent is transferred to a drying box, and nitrogen is introduced into the drying box to remove the solvent at 100°C to obtain refined hydrogenated bisphenol A. The composition of hydrogenated bisphenol A is analyzed, and the yield and purity of hydrogenated bisphenol A are investigated. The experimental results are shown in Table 1.

[0090] Example 9

[0091] The hydrogenated bisphenol A to be refined includes isopropanol (solvent a) and crude hydrogenated bisphenol A with a mass purity of 95.76%, and the mass concentration of crude hydrogenated bisphenol A in the hydrogenated bisphenol A to be refined is 15%. The hydrogenated bisphenol A to be refined is pumped out by the hydrogenated bisphenol A feed pump to be refined and enters the distillation tower. After the tower bottom reaches 2 / 3 of the liquid level, the vacuum pump is started to establish vacuum conditions. The vacuum pump is connected to the solvent recovery tank to provide vacuum conditions for this process, and the vacuum degree is controlled at -0.07MPa. After the vacuum is established, the temperature of the distillation tower is increased until the gas phase temperature at the top of the distillation tower rises to 60-62°C. Solvent a is vaporized and discharged from the top of the distillation tower. The gas phase solvent a is condensed and refluxed by the condenser and then the solvent a is collected to the solvent recovery tank. The medium temperature in the condenser is 15-20°C. When the remaining proportion of solvent a reaches 60% (the mass of the undistilled solvent a is 60% of the total mass of the solution in the distillation tower), the solvent b feed pump is turned on. Solvent b is mesitylene. The flow rate is gradually adjusted and the hydrogenated dimethylbenzene to be refined is set. The feed flow rate of phenol A is 10 kg / h, the feed flow rate of mesitylene is set to 20 kg / h, and the operating conditions of the distillation tower are adjusted. The remaining proportion of solvent a reaches 45% (the mass of undistilled solvent a is 45% of the total mass of the solution in the distillation tower) and the liquid level of the distillation tower is stable. The discharge pump is turned on, and the discharge flow rates of hydrogenated bisphenol A and solvent b are set to 12 kg / h. After the solvent is replaced, the newly formed hydrogenated bisphenol A and solvent b are pumped out from the bottom of the distillation tower by the discharge pump and enter the reactor equipped with controllable speed stirring. The reactor is operated intermittently, and the stirring is maintained at a constant speed. The coil design in the reactor contains a heat-conducting medium. The inlet and outlet of the coil are connected to an external temperature control circulator. During the process of pumping hydrogenated bisphenol A and solvent b, the pipeline is insulated and heated to control the temperature of the reactor to be constant. When the liquid level of the reactor reaches 70% of the liquid level range, the feeding is stopped, and the temperature is cooled to 30°C at a cooling rate of 15°C per hour. The temperature is kept at 30°C and stirred for 2 hours. The solid-liquid mixture is discharged into a centrifuge, and the centrifuge is operated for solid-liquid separation. After solid-liquid separation, the solid containing a certain amount of solvent is transferred to a drying box, and nitrogen is introduced into the drying box to remove the solvent at 100°C to obtain refined hydrogenated bisphenol A. The composition of hydrogenated bisphenol A is analyzed, and the yield and purity of hydrogenated bisphenol A are investigated. The experimental results are shown in Table 1.

[0092] Example 10

[0093] The hydrogenated bisphenol A to be refined includes ethanol (solvent a) and crude hydrogenated bisphenol A with a purity of 95.76%, and the mass concentration of crude hydrogenated bisphenol A in the hydrogenated bisphenol A to be refined is 20%. This embodiment does not require the use of a distillation tower, and the hydrogenated bisphenol A to be refined is pumped into a reactor with controllable speed stirring by a feed pump of hydrogenated bisphenol A to be refined. The coil design in the reactor contains a heat-conducting medium, and the inlet and outlet of the coil are externally connected to a temperature control circulator. When the liquid level in the reactor is 70% of the reactor liquid level range, the reactor is heated, and the ethanol vaporization amount increases after the temperature reaches 78°C. The ethanol vapor is collected after condensation, and the solvent b feed pump is turned on to pump p-xylene into the reactor, and the temperature of the reactor is slowly increased to control the p-xylene. The benzene feed amount maintains the liquid level in the reactor at 70% of the reactor liquid level range. When the flow rate of the cooled ethanol is reduced to no ethanol distilled out, the solvent b feed pump is stopped, the reactor temperature is controlled, and the temperature is lowered to 30°C at a cooling rate of 10°C per hour, and maintained at 30°C for 2 hours. The solid-liquid mixture is discharged into the centrifuge, and the centrifuge is operated to separate the solid and liquid. After the solid-liquid separation, the solid containing a certain amount of solvent is transferred to the drying box 10, and the drying box 10 is passed with nitrogen to remove the solvent at 100°C to obtain the refined hydrogenated bisphenol A. The composition of hydrogenated bisphenol A is analyzed, and the yield and purity of hydrogenated bisphenol A are investigated. The experimental results are shown in Table 1.

[0094] Embodiment 11

[0095] The hydrogenated bisphenol A to be refined includes isobutyl alcohol (solvent a) and crude hydrogenated bisphenol A with a mass purity of 95.76%, and the mass concentration of crude hydrogenated bisphenol A in the hydrogenated bisphenol A to be refined is 20%. In this embodiment, the boiling points of isobutyl alcohol and toluene are close, and toluene is added after isobutyl alcohol is separated by distillation. The hydrogenated bisphenol A to be refined is pumped out by the hydrogenated bisphenol A feed pump to be refined and enters the distillation tower. After the tower bottom reaches 3 / 4 liquid level, the vacuum pump is started to establish vacuum conditions. The vacuum pump is connected to the solvent recovery tank to provide vacuum conditions for this process, and the vacuum degree is controlled at -0.08MPa. After the vacuum is established, the temperature of the distillation tower is increased until the gas phase temperature at the top of the distillation tower rises to 64-65°C, the feed pump of the hydrogenated bisphenol A to be refined is stopped, the solvent a is vaporized and discharged from the top of the distillation tower, the gaseous solvent a is condensed and refluxed through the condenser, and the solvent a is extracted to the solvent recovery tank, the medium temperature in the condenser is 15-20°C, and the isobutanol solvent is continuously extracted until the top temperature rises to above 75°C, the solvent b feed pump is turned on, the solvent b is toluene, the flow rate is adjusted to pump the solvent b until the liquid level at the bottom of the tower returns to 3 / 4, the solvent b feed pump is stopped, the distillation tower maintains the temperature in the tower at 75-80°C, and the solvent replacement is completed after continuous heating equilibrium for one hour. After the solvent is replaced, the newly formed hydrogenated bisphenol A and solvent b are pumped out from the bottom of the distillation tower by the discharge pump and enter the reactor equipped with a controllable speed stirrer. The reactor is operated intermittently, and the stirring is maintained at a constant speed. The coil design in the reactor contains a heat-conducting medium. The inlet and outlet of the coil are connected to an external temperature control circulator. During the process of pumping hydrogenated bisphenol A and solvent b, the pipeline is insulated and heated to control the temperature of the reactor to be constant. When the liquid level of the reactor reaches 70% of the liquid level range of the reactor, the feeding is stopped, and the temperature is cooled to 30°C at a cooling rate of 10°C per hour. The temperature is kept at 30°C and stirred for 2 hours. The solid-liquid mixture is discharged into a centrifuge, and the centrifuge is operated for solid-liquid separation. After solid-liquid separation, the solid containing a certain amount of solvent is transferred to a drying box, and nitrogen is introduced into the drying box to remove the solvent at 100°C to obtain the refined hydrogenated bisphenol A. The composition of hydrogenated bisphenol A is analyzed, and the yield and purity of hydrogenated bisphenol A are investigated. The experimental results are shown in Table 1.

[0096] Table 1 Refining effect of hydrogenated bisphenol A

[0097]

[0098] Note: (1) Crude hydrogenated bisphenol A is a homemade product.

[0099] (2) The mother liquor and the refined hydrogenated bisphenol A were analyzed by gas chromatography. The mother liquor was directly analyzed, and the refined bisphenol A was analyzed after being dissolved in methanol. The solvent was not integrated during the component analysis, and the results were obtained by gas chromatography. The mother liquor was the liquid separated in the centrifuge.

[0100] (3) Single-pass yield of refined bisphenol A = (mass of refined hydrogenated bisphenol A product / mass of crude hydrogenated bisphenol A input) × 100%.

[0101] 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 refining hydrogenated bisphenol A, characterized in that: It includes a supply end of hydrogenated bisphenol A to be refined, a supply end of solvent B, a distillation tower, a cooling component, a solid-liquid separator and a pipeline. The distillation tower is placed in a vertical direction, and comprises a feed port a, a feed port b, a discharge port c and a discharge port d, wherein the feed port a is higher than the feed port b, the supply end of the hydrogenated bisphenol A to be refined is connected to the feed port b, and the supply end of the solvent b is connected to the feed port a; The distillation tower, the cooling component, and the solid-liquid separator are connected in sequence through pipelines, and the cooling component is connected to the discharge port c of the distillation tower.

2. The device according to claim 1, characterized in that The hydrogenated bisphenol A to be refined comprises hydrogenated bisphenol A and solvent a; The distillation tower is used to replace the solvent a in the hydrogenated bisphenol A to be refined with the solvent b; The cooling component is used to precipitate hydrogenated bisphenol A from the solvent b; The solid-liquid separator is used to separate the hydrogenated bisphenol A precipitated in the cooling component from the solvent b; and / or, the boiling point of the solvent b is higher than the boiling point of the solvent a, and the difference between the boiling point of the solvent b and the boiling point of the solvent a is less than or equal to 30° C.; And / or, the device for refining hydrogenated bisphenol A further comprises a solvent recovery tank, and the solvent recovery tank is connected to the discharge port d of the distillation tower; And / or, a condenser is further provided between the solvent recovery tank and the discharge port d; And / or, the device for refining hydrogenated bisphenol A further comprises a vacuum pump, which is connected to the solvent recovery tank and is used to establish vacuum conditions in the device for refining hydrogenated bisphenol A.

3. The device according to claim 1 or 2, characterized in that: The hydrogenated bisphenol A to be refined supply end includes a hydrogenated bisphenol A to be refined storage tank and a hydrogenated bisphenol A to be refined feed pump; and / or, the solvent b supply end includes a solvent b storage tank and a solvent b feed pump.

4. The device according to any one of claims 1 to 3, characterized in that: The cooling component comprises a reaction kettle, a cooler and a temperature controller. The cooler is used to reduce the temperature inside the reaction kettle, and the temperature controller is used to control the cooling rate of the cooler.

5. A method for refining hydrogenated bisphenol A using the device according to any one of claims 1 to 4, characterized in that: The steps include: Step S1: introducing the hydrogenated bisphenol A to be purified into the distillation tower, the hydrogenated bisphenol A to be purified is separated into bisphenol A and solvent a in the distillation tower, and the solvent a is discharged from the distillation tower; Step S2: introducing solvent b into the distillation tower, and discharging solvent b from the distillation tower after mixing with hydrogenated bisphenol A; Step S3: precipitating hydrogenated bisphenol A from solution b; Step S4: Separating the hydrogenated bisphenol A precipitated in step S3 from the solvent b to obtain purified hydrogenated bisphenol A.

6. The method according to claim 5, characterized in that The method further comprises step S5 after step S4, wherein step S5 is drying the hydrogenated bisphenol A obtained after the solid-liquid separation in step S4.

7. The method according to claim 5 or 6, characterized in that: The solvent a includes at least one of ethanol, isopropanol, isobutanol, and cyclohexanol; and / or the solution b includes one or more of toluene, p-xylene, o-xylene, m-xylene, mixed xylenes, mesitylene, and tetramethylbenzene.

8. The method according to any one of claims 5 to 7, characterized in that: The amount of solvent b added to the distillation tower is 20% to 300% of the mass of the hydrogenated bisphenol A solution to be purified, preferably 40% to 100%; and / or, the amount of solvent b added to the distillation tower is 2 to 10 times, preferably 3 to 6 times, of the mass of hydrogenated bisphenol A in the hydrogenated bisphenol A solution to be purified; and / or, when the mass of the remaining solvent a in the distillation tower is 50% of the total mass of the solution in the distillation tower or the mass of the remaining solvent a in the distillation tower is less than 50% of the total mass of the solution in the distillation tower, the solvent b and hydrogenated bisphenol A are discharged; and / or, the pressure in the distillation tower is normal pressure or the pressure is controlled to be 0 to -0.09 MPaG; And / or, the step 3 is to place the mixture of hydrogenated bisphenol A and solution b in the reactor, and precipitate hydrogenated bisphenol A from solution b by lowering the temperature of the reactor; preferably, when the temperature of the mixture is above 60°C, the cooling rate of the reactor is 5-15°C / H1.

9. Use of the device according to any one of claims 1 to 4 or the method according to any one of claims 5 to 8 in refining hydrogenated bisphenol A.

10. A purified hydrogenated bisphenol A prepared by the device according to any one of claims 1 to 4 or the method according to any one of claims 5 to 8, characterized in that: The mass content of hydrogenated bisphenol A in the refined hydrogenated bisphenol A is greater than 98%.

Citation Information

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