Production process for synthetic bisphenol a by resin process and device
By using a dual-effect liquid film drop evaporator and an external circulation heat exchange device in the bisphenol A production process, combined with multi-stage crystallization, washing and melting processes, the problems of high temperature reaction suppression, high energy consumption and low separation efficiency are solved, and high purity and high efficiency bisphenol A production is achieved.
Patent Information
- Application Number
- JP2024171248
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-10-16
- Filing Date
- 2024-09-30
- Publication Date
- 2025-04-28
- Estimated Expiration
- 2044-09-30
AI Technical Summary
During the existing bisphenol A production process, there are problems such as high temperatures leading to reaction suppression, high energy consumption, low separation efficiency and insufficient heat exchange, which affects product purity and energy utilization efficiency.
The dual-effect liquid film drop evaporator and external circulation heat exchange device are used to combine the multi-stage crystallization, washing and melting process to convert poor products through high-pressure separation and isomer reactions to improve the selectivity and purity of bisphenol A.
It significantly improves the purity and selectivity of bisphenol A, reduces energy consumption, improves separation efficiency and heat exchange effect, and improves overall production efficiency.
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Figure 2025068595000001_ABST
Abstract
Description
[Technical field]
[0001] The present invention relates to a method and apparatus for producing bisphenol A, and more particularly to a method and apparatus for producing synthetic bisphenol A by a resin method. [Background technology]
[0002] The molecular formula of bisphenol A (BPA) is C 15 H 16 O 2 , the molecular weight is 228.29, and the chemical structural formula is as follows:
[0003] [ka]
[0004] Bisphenol A is a white crystal that is soluble in ethanol, ether, and acetic anhydride, has very low solubility in water (1:2820 by weight), and is slightly soluble in boiling water (1:130 by weight). Bisphenol A can form crystalline adducts with various inorganic and organic substances (phenol, isopropyl alcohol, amines, ammonia, etc.) in equimolar ratios of components. These adducts are very unstable and may cause decomposition when washed with water, or heated under normal pressure, vacuum, or with inert gas bubbling.
[0005] Bisphenol A is an important industrial chemical and is the main raw material for the production of epoxy resins and polycarbonates, as well as for the production of other polymeric materials, such as polysulfone resins, phenolic unsaturated resins, polyarylates, polyetherimides, heat stabilizers for polyvinyl chloride, and antioxidants for rubber.
[0006] Currently, bisphenol A is usually produced by condensation reaction of excess phenol and acetone in the presence of an acid catalyst, and the most common acid catalyst is a strongly acidic cation exchange resin. The resulting reaction mixture contains bisphenol A, as well as unreacted phenol, acetone, by-product water, bisphenol A isomers, triphenols, chromanols, and more than 10 other substances. The reaction mixture obtained by the condensation reaction is generally crystallized, solid-liquid separated, the crude crystals are washed, and then the phenol is removed to recover bisphenol A.
[0007] Patent Document 1 discloses a method for increasing the concentration of bisphenol A by recycling the reaction liquid in order to reduce energy consumption. In this method, after removing acetone, water and a part of the phenol from the reaction liquid, the reaction liquid is sent to a vacuum evaporation system to remove the phenol, and a high-purity bisphenol A melt is obtained through multiple crystallization and melt circulations, and the material after vacuum dehydration is returned to the reaction inlet.
[0008] Patent Document 2 discloses an optimization method for producing bisphenol A reaction system, which includes a step of sequentially subjecting a mother liquor obtained by treating at least a part of a reaction liquid to an isomerization reaction-concentration-partial preconcentration-decomposition-rearrangement reaction step, and a step of operating a reaction system for producing bisphenol A, in which the isomerization reaction and the rearrangement reaction are simultaneously carried out in an isomerization-rearrangement reactor to form a circulating operation system, and isopropylphenol produced in the decomposition process enters a phenol recovery system together with light fractions in the partial preconcentration step and is separated from phenol together with mixed polyphenols.
[0009] Patent Document 3 discloses a method for reducing isopropylphenol in the production of a bisphenol A reaction system, which comprises: obtaining a rearrangement liquid by isomerizing-decomposing-rearrangement at least a part of a reaction liquid obtained after catalytic condensation reaction of an excess amount of phenol with acetone in a condensation reactor; subjecting the rearrangement liquid containing isopropylphenol to a concentration process to allow isopropylphenol to enter a phenol recovery system, and allowing it to leave phenol together with mixed polyphenols, thereby making the mass percent content of isopropylphenol in the condensation reactor 0.25% or less.
[0010] To sum up the above and other references, in the current bisphenol A production process, most of the reaction systems are one- or two-stage tubular reactors connected in series. As the reaction proceeds, the reaction heat is released, causing the temperature of the system to continue to rise, and the content of by-product water also continues to increase. The high temperature and the presence of water inhibit the forward reaction, and the equilibrium conversion rate also decreases, making it impossible to obtain an ideal reaction rate and conversion rate.
[0011] From the viewpoint of the reaction system, currently, there is a method to increase the conversion rate of phenol by returning the stream from the separation section to the reactor, but no effective method has been proposed to solve the problem of the temperature inside the reactor being too high. A rectification tower is used after the reactor to extract light fractions, and water is involved in the reaction throughout the entire process, which is not helpful for the forward reaction. The energy consumption of the rectification tower is high and it is not suitable for material separation at this point. From the perspective of the separation system, there are currently multiple stages of crystallization-washing-melting process, and the process is long and overlapping. The fundamental reason is that the efficiency of the solid-liquid separation equipment is low, which makes it difficult to achieve the separation goal of the system. From the perspective of overall energy utilization, the entire process includes many endothermic and dissipative processes, including preheating, condensation, evaporation, etc., among which, different evaporation methods have a large difference in energy utilization efficiency. The ones used in many industrial examples and patents are basically simple one-stage evaporation or one-stage rising film / falling film evaporation, which does not fully utilize the energy gradient and has little heat exchange between streams, resulting in significant energy waste. From the perspective of the overall material circulation, the layout of the circulation streams between the various zones is unreasonable, which leads to serious back-mixing of materials and increases the burden on the separation equipment and power equipment.
[0012] In short, the current bisphenol A production method has more or less defects from part to the whole, and it is necessary to adjust the direction of some circulation streams in the whole process, increase the heat exchange between process streams in the whole process, and focus on improving some processes and equipment, in order to improve the purity of the product and reduce energy consumption. [Prior art documents] [Patent documents]
[0013] [Patent Document 1] Chinese Patent No. CN200910030415.2 [Patent Document 2] Chinese Patent No. CN202111654111.0 [Patent Document 3] Chinese Patent No. CN202111165633.9 Summary of the Invention [Problem to be solved by the invention]
[0014] The present invention provides a method and apparatus for synthesizing bisphenol A, which includes a reactor external circulation heat exchanger, a tank for removing light components between the two-stage reaction, a pressurized separator, a double-effect falling film evaporator, and an isomerization reactor, and adjusts the direction of a part of the circulation stream in the entire process to increase the heat exchange between process streams in the entire process, thereby achieving the objectives of improving the purity of products and circulation materials, reducing energy consumption, and improving bisphenol A selectivity. [Means for solving the problem]
[0015] A method for producing synthetic bisphenol A by a resin method, comprising the following steps: (1) A process for providing a condensation reaction unit for producing bisphenol A by catalytic condensation reaction of phenol and acetone under the action of a resin catalyst, the reactor of the unit comprising a first-stage reactor and a second-stage reactor, and providing an external circulation heat transfer to the first-stage reactor and a flash evaporation dehydration between the first-stage reactor and the second-stage reactor; (2) A process for mixing the condensation reaction concentrate with the recovered adduct crystals after melting, followed by crystallization of the adduct, and then adding phenol to the adduct crystal-containing solution after pressurization, drum rotation, and filtration, followed by uniform stirring and washing, and then centrifuging to obtain the adduct crystals, comprising a first adduct crystallization unit, and separating the solid phase and the liquid phase with a pressurized separator; (3) a liquid-phase dephenolization unit for extracting the phenol from the adduct melt, granulating and packaging to obtain a bisphenol A product; (4) a secondary adduct crystallization unit for recovering phenol and bisphenol A from the mother liquor, separating phenol and bisphenol A by double-effect falling film evaporation, and converting the by-product to bisphenol A in an isomerization reactor; (5) a solvent recovery unit for recovering unreacted phenol and acetone and sending the phenol-containing wastewater to wastewater treatment; (6) A decomposition and rearrangement unit to remove impurities produced during the manufacturing process, recover phenol from the mother liquor, and first decompose and rearrange the bisphenol A and 2,4-bisphenol A contained in the mother liquor, converting it into bisphenol A and returning it to the system.
[0016] In the manufacturing method for realizing the synthetic bisphenol A by the resin method of the present invention, the raw material acetone, recovered acetone, and recycled phenol are sent to the condensation reaction unit (100#) to react, and after the product and unreacted raw materials are simply separated, the reaction liquid is sent to the adduct crystallization unit (200#), and the hydrous phenol is sent to the solvent recovery unit (500#). A part of the raw material phenol is added from the adduct crystallization unit and used to wash the upstream reaction liquid, the recovered phenol from the dephenolization purification unit (300#), and the adduct crystal melt from the mother liquor recovery unit (400#). After washing, the first-stage centrifugal separation mother liquor / washing liquid and the second-stage centrifugal separation mother liquor are sent to the mother liquor recovery unit (400#), and the adduct crystal melt is used for dephenolization purification. The phenol is then sent to the dephenolation unit, the final product BPA is produced in the dephenolation unit, and the hydrous phenol is sent to the solvent recovery unit. A part of the raw phenol is added from the mother liquor recovery unit and used to wash the mother liquor, washing liquid, recovered phenol, and recovered BPA from the decomposition and rearrangement unit (600#). Then the mother liquor from the second stage of centrifugation is sent to the decomposition and rearrangement unit, ethylbenzene is added as an azeotropic agent to the solvent recovery unit, the recovered acetone is sent to the condensation reaction unit, the recovered phenol is sent to the mother liquor recovery unit, and the wastewater is discharged outside the system. The decomposition and rearrangement unit receives the mother liquor from the second stage of centrifugation and decomposes it, returns the recovered BPA to the mother liquor recovery unit, and sends isopropyl phenol and waste liquid out of the system.
[0017] In the condensation reaction unit (100#), fresh acetone after purification with a flow rate of 14000-16000 kg / h is metered and fed proportionally to the first-stage reactor (102) and the second-stage reactor (112), respectively. The acetone fed to the reactor (102) is mixed with the recovered phenol from the cracking feed preheater (601) and the material from the first-stage circulation pump (105), enters the first-stage cooler (101), and is cooled by the circulating water, after which it enters the first-stage reactors (102-104). A part of the reaction liquid flowing out of the first-stage reactor (104) is fed to the first-stage circulation pump (105). The remaining part is circulated by a circulation pump (105) and returned to the first-stage reactor (102), with a circulation flow rate of 455,000 to 520,000 kg / h. The remaining part is heated by a dehydration flash heater (106) and then enters a dehydration flash evaporator (107) to remove some of the moisture. The flash steam from the dehydration flash evaporator (107) is condensed and cooled by a flash evaporation first condenser (108) and a flash evaporation second condenser (109). The condensate containing water, acetone, and phenol flows into the light fraction receiving tank (124), and the tail gas is sent to a vacuum system. The dehydrated material from the dehydration flash evaporator (107) is mixed with the recovered acetone and fresh acetone from the second stream, and then pumped by the second-stage feed pump (110) to the second-stage cooler (111), where it is cooled with circulating water and then enters the second-stage reactors (112-114). The condensation reaction liquid discharged from the second-stage reactor (114) is mixed with the bottom liquid from the phenol absorption tower (306) and then enters the adsorption column (115), and is then heated by heat exchange with the bottom liquid of the light fraction removal tower (117) in the preheater (116), and then enters the light fraction removal tower (117). The water, unreacted acetone, and a part of the phenol in the reaction liquid evaporate from the top of the column and are condensed in the condenser (122) and the aftercooler (123). The tail gas then enters the vacuum system, and the condensate flows into the light fraction receiving tank (124) and is sent to the solvent recovery unit (500#) by the discharge pump (125) to recover the phenol and acetone. The light fraction removal column reboiler (118) is heated with low-pressure steam to concentrate the column bottoms, which are then sent out by the discharge pump (119) and, after being heat-exchanged in the preheater (116) to lower the temperature, are sent to the condensation reaction liquid receiving tank (120).
[0018] The adduct crystallization unit (200#): The reaction concentrate from the condensation reaction liquid discharge pump (121) and the adduct crystal melt recovered from the mother liquor recovery unit (400#) of the crystal melting device circulation pump (427) are mixed in the crystallization supply buffer tank (201), then sent out by the crystallization supply pump (202), cooled by the supply cooler (203), and then entered into the main circulation type crystallizer (204). The crystal slurry is then pumped into the main circulation type crystallizer (204) by the crystallization circulation pump (205). After being pumped out from the crystallizer (204), it enters the crystallization cooler (206) where the heat of crystallization is removed under the cooling action of deionized water. The crystal slurry flowing out from the main circulation type crystallizer (204) is continuously sent to the pressurized main separator (207) by the flow control valve to carry out solid-liquid separation. The phenol for washing the filter cake is the filtrate from the second stage centrifuge of the slurry mixed washing mother liquor pump (214). The separated mother liquor and washing liquid are sent to the main separator mother liquor / washing liquid tank (206). The phenol from the main separator and the phenol discharge pump (311) is mixed with the filtered adduct crystals in the slurry mixing and washing tank (210) and washed. The crystal slurry after the slurry mixing is sent to the second stage pressurized main separator (212) by the corresponding crystal slurry pump (211) and undergoes solid-liquid separation. The filtrate is fed to the slurry mixing centrifuge mother liquor tank (401) and then to the slurry mixing centrifuge mother liquor tank (402). The slurry enters the liquid tank (213), is pumped out by the slurry mixed washing mother liquor pump (214), and is sent to the pressurized main separator (207) and the pressurized secondary separator (423), respectively, for use in phenol washing. The filter cake is removed by a centrifuge and enters the crystal melter (215). The material in the crystal melter (215) is sent to the heater (217) by the corresponding crystal melt circulation pump (216) to be heated, and then returned to the crystal melter (215).
[0019] The phenol removal purification unit (300#): The adduct melt from the phenol removal supply pump (218) enters the liquid film falling type phenol removal device (301), where it is evaporated by heating with steam and enters the gas-liquid separation tank (302), the liquid phase enters the top of the steam stripping phenol removal device (305), the gas phase is condensed by the condenser (303), the tail gas enters the vacuum system, the condensate enters the phenol tank (310), fresh phenol with a flow rate of 42756-48864 kg / h from the tank area enters the fresh phenol tank (313) and is pumped out by the fresh phenol pump (314), a part of it is metered and then pumped into the phenol tank (310), and the rest is sent to the recovery phenol tank (416), the phenol in the phenol tank (310) is pumped out by the phenol discharge pump (311), cooled to a set value by the washing phenol cooler (312), and then mixed with the slurry. The water vapor is sent to a washing tank (210) to produce washed phenol, and the water vapor is heated by an electric steam superheater (304) and then enters the bottom of the steam stripping dephenolization unit (305) as steam for steam stripping. The liquid bisphenol A obtained at the bottom of the tower is pumped out by a BPA melt pump (315) and then molded, granulated, and packaged in a packaging machine (316) to produce a bisphenol A product. The gas phase at the top of the tower enters the bottom of the phenol absorption tower (306) and undergoes gas-liquid mass transfer with the absorbed phenol added from the top of the tower. The gas coming out of the top of the tower enters the phenol absorption tower condenser (309), the tail gas enters a vacuum system, the condensate is hydrous phenol, and enters an ethylbenzene tank (526). The bottom liquid is a bisphenol A phenol solution, and is sent to a cooler (308) by a phenol circulation pump (307) to be cooled, and then returned to the top of the phenol absorption tower (306).
[0020] In the mother liquor recovery unit (400#), the material from the mother liquor receiving tank (401) is successively sent by the feed pump (402) to the first feed preheater (403) and the second feed preheater (404). The first feed preheater (403) is a thermally coupled heat exchanger, and the heat medium is the gas phase material from the gas-liquid separation tank (411). The second feed preheater (404) is also a thermally coupled heat exchanger, and the heat medium is phenol from the recovery phenol pump (419). After the two-stage preheating, the material is metered and divided into two parts. One part enters the high pressure falling film evaporator (406), The vapor is heated by the steam and evaporates. The gas and liquid phases flowing out from the bottom of the high-pressure falling film evaporator (406) enter the first-stage gas-liquid separation tank (407). The liquid phase is pumped by the pump (410) into the gas-liquid separation tank (411). The gas phase enters the low-pressure falling film evaporator (405) as a heat medium. After condensation, the gas and liquid phases are separated in the second-stage gas-liquid separation tank (408). The liquid phase enters the phenol recovery tank (416). The gas phase enters the tail gas condenser (409) and is further condensed by circulating water. The condensate enters the phenol recovery tank (416) and the tail gas condenser (409) is further condensed by circulating water. The gas is sent to the vacuum system, and the other part of the preheated mother liquor is heated and evaporated in the low pressure falling film evaporator (405). The gas-liquid two-phase material flowing out from the bottom of the low pressure falling film evaporator (405) enters the third stage gas-liquid separation tank (411). Part of the gas phase material enters the first stage supply preheater (403) as a heat medium, and the rest is condensed in the condenser (414) under the action of circulating water. The tail gas of the first stage supply preheater (403) and the condenser (414) are merged and then enter the aftercooler (415), where it is further condensed under the action of circulating water. The tail gas is then discharged into the vacuum system. The condensate from the first-stage feed (403), condenser (414) and aftercooler (415) flows into the recovered phenol tank (416), and the material in the recovered phenol tank (416) is pumped into the recovered phenol storage tank (418) by the phenol discharge pump (417), and then pumped out by the recovered phenol pump (419). The temperature is lowered by heat exchange in the second-stage feed preheater (404) and the decomposition feed preheater (601), and then the material is sent to the first-stage cooler (101) of the condensation reactor and the discharge port of the phenol circulation pump (307), respectively.The liquid phase material in the third-stage gas-liquid separation tank (411) is a concentrated bisphenol A phenol solution, which is pumped out by a crystallization feed pump (412), passed through a crystallization feed cooler (413) and cooled with circulating water before entering a recovery crystallizer (420). The adduct crystal slurry is pumped out of the recovery crystallizer (420) by a crystallization circulation pump (422), and then enters a crystallization cooler (421) where the heat of crystallization is cooled by deionized water. The crystal slurry discharged from the recovery crystallizer (420) is continuously sent to the pressure sub-separator (423) for solid-liquid separation, and the phenol for washing the filter cake is the filtrate from the second stage centrifuge of the slurry mixing washing mother liquor pump (214). The mother liquor separated from the pressure sub-separator (423) enters the mother liquor receiving tank (429) and is pumped out by the mother liquor discharge pump (430). After being preheated by the mother liquor heater (431), a part of it is subjected to an isomerization reaction. The reaction liquid is sent to the pressure secondary separator (423) and sent to the washing liquid receiving tank (424) and sent to the mother liquor receiving tank (401) by the washing liquid discharge pump (425). A part of the reaction liquid introduced from the main separator and metered by the condensation reaction concentrated liquid discharge pump (121) is mixed with the adduct crystals filtered in the tail gas condenser (409). The material in the tail gas condenser (409) is sent to the heater (428) by the corresponding crystal melt circulation pump (427) to be heated and then returned to the tail gas condenser (409). The material in the tail gas condenser (409) is sent to the crystallization supply buffer tank (201) by the crystal melt circulation pump (427).
[0021] The solvent recovery unit (500#): the dehydration tower (502) is an azeotropic distillation tower, and ethylbenzene is the azeotropic agent. The material from the light fraction discharge pump (125) is mixed with the material from the ethylbenzene supply pump (527), and then preheated by low-pressure steam in the dehydration tower supply preheater (501) before entering the dehydration tower (502). The overhead gas directly enters the acetone recovery tower (504), and the bottom liquid is phenol containing ethylbenzene, which is sent to the phenol recovery tower (519) by the tower pot discharge pump (518). The overhead gas of the acetone recovery tower (504) is condensed through the acetone tower condenser (506) and the aftercooler (507), and the tail gas is sent to the vacuum system. The condensate enters the acetone tower reflux tank (508) and is sent out by the acetone tower reflux pump (509).One strand is sent as reflux to the top of the acetone recovery tower, and the other strand is sent as recovered acetone to the suction port of the second stage feed pump (110) of the condensation reaction unit (100#) reactor. The tower bottoms enter the phase separator (510) where an aqueous phase and an organic phase are formed. The aqueous phase material is pumped out by the aqueous phase discharge pump (511) and cooled by coolers (512, 513) before entering the phase separator (514) where further phase separation takes place. The organic phase flows into the phase separator (510), The aqueous phase is discharged from the boundary region as wastewater of the apparatus by the wastewater pump (516) and is subjected to biochemical treatment. The organic phase of the phase separator (510) is discharged by the ethylbenzene discharge pump (515), a part of which is returned to the top of the dehydration tower (502) as reflux liquid, and the remainder is cooled by the ethylbenzene cooler (517) and then enters the vacuum pump as the auxiliary working liquid of the ethylbenzene liquid ring vacuum pump. By adjusting the flow rate of the heating steam in the reboiler (505), the ascending steam in the tower is increased. The amount of gas flowing through the dehydration tower (502) is controlled, and the material from the tower tank discharge pump (518) enters the phenol recovery tower (519). The overhead gas is condensed through the phenol tower condenser (522) and aftercooler (523). The tail gas enters the vacuum system, and the condensate enters the reflux tank (524). A portion of it is returned to the top of the tower as reflux by the reflux pump (525). The remainder overflows into the ethylbenzene tank (526), which is used as reflux for the phenol absorption tower condensate. The dehydration tower (502) receives the hydrous phenol from the condenser (309), the substituted ethylbenzene from the vacuum system, and the make-up ethylbenzene. The material in the ethylbenzene tank (526) is fed to the dehydration tower (502) through the ethylbenzene feed pump (527). The bottom liquid is phenol that does not contain ethylbenzene, and is sent to the recovered phenol storage tank (416) through the tower bottom discharge pump (521). The amount of rising steam in the tower is controlled by adjusting the flow rate of the heating steam in the reboiler (520).
[0022] In the cracking and rearrangement unit (600#), the mother liquor from the mother liquor discharge pump (430) is preheated by the cracking and feed preheater (601) and then enters the falling film evaporator (602). The cracking and feed preheater (601) is a thermally coupled heat exchanger, and the heat medium is the recovered phenol from the second feed preheater (404). The mother liquor is evaporated in the falling film evaporator (602) by heating with steam. The gas-liquid two-phase material enters the gas-liquid separation tank (603), the liquid phase enters the kettle section of the cracking reactor (610), and the gas phase enters the p-isopropylphenol decomposition tower (612). The bottom liquid of the p-isopropylphenol removal tower (604) is a heavy fraction containing p-isopropylphenol, which is discharged to the outside of the system via a discharge pump (606) and incinerated. The overhead gas is condensed and cooled by a condenser (607). The tail gas enters a vacuum system, and the condensate enters a reflux tank (608) and is then pumped out by a reflux pump (609). A portion of it is returned to the top of the p-isopropylphenol removal tower (604) as reflux, and the other portion is used as reflux for the decomposition reaction in the decomposition reactor (610). The material flows into the top of the decomposition reactor (610), and the material that overflows from the reflux tank (608) flows into the decomposition product tank (614). The amount of rising steam in the column is controlled by adjusting the flow rate of the heated steam in the reboiler (605). The material from the gas-liquid separation tank (603) flows into the kettle section of the decomposition reactor (610), and is then sent by the decomposition reaction circulation pump (611) to the decomposition reaction heater (612) where it is heated. After that, a certain amount of alkaline liquid is added as a catalyst for the decomposition reaction, and the material is returned to the kettle section of the decomposition reactor (610). The tar thus produced is discharged outside the system via the cracking reaction circulation pump (611) and incinerated, the overhead gas of the cracking reactor (610) is condensed and cooled in the cracking product condenser (613), the tail gas enters the vacuum system, and the condensate enters the cracking product tank (614) and is then sent by the rearrangement reaction supply pump (615) to the circulation cooler (616) where it is cooled, a portion of which is circulated back to the cracking product tank (614), while the other portion is used as the feed for the rearrangement reactor (617), and the rearranged material is returned to the mother liquor receiving tank (401).
[0023] Apparatus for implementing the method for producing synthetic bisphenol A (1): The cooling side outlet of the cracking supply preheater (601) merges with the discharge port of the first-stage circulation pump (105) and is then connected to the cooling side inlet of the first-stage cooler (101), the cooling side outlet of the first-stage cooler (101) is connected to the inlet of the first-stage reactor (102), the outlet of the first-stage reactor (102) is connected to the inlet of the first-stage reactor (103), the outlet of the first-stage reactor (103) is connected to the inlet of the first-stage reactor (104), the outlet of the first-stage reactor (104) is branched into two, each of which is fed to the first-stage circulation pump (105) The suction port of the second-stage supply pump (110) is connected to the inlet of the second-stage condenser (104) and the heating side inlet of the dehydration flash evaporative heater (106), the heating side outlet of the dehydration flash evaporative heater (106) is connected to the inlet of the dehydration flash evaporator (107), the vapor phase outlet of the dehydration flash evaporator (107) is connected to the cooling side inlet of the flash evaporation first condenser (108), and the liquid phase outlet merges with the discharge port of the acetone tower reflux pump (509) and is connected to the suction port of the second-stage supply pump (110), the discharge port of the second-stage supply pump (110) is connected to the cooling side inlet of the second-stage cooler (111), and the cooling side outlet of the second-stage cooler (111) is connected to the suction port of the second-stage supply pump (110). The outlet of the first stage reactor (112) is connected to the inlet of the second stage reactor (113), the outlet of the second stage reactor (113) is connected to the inlet of the second stage reactor (114), the gas phase outlet on the cooling side of the flash evaporation first condenser (108) is connected to the cooling side inlet of the flash evaporation second condenser (109), the liquid phase outlet of the flash evaporation first condenser (108) joins with the liquid phase outlet on the cooling side of the flash evaporation second condenser (109) and is then connected to the inlet of the light fraction receiving tank (124), and the gas phase outlet on the cooling side of the flash evaporation second condenser (109) is connected to the inlet of the vacuum unit. the outlet of the second-stage reactor (114) is joined to the discharge port of a phenol circulating pump (307) and then connected to the inlet of an adsorption column (115); the outlet of the adsorption column (115) is connected to the heating side inlet of a light fraction removal column supply preheater (116); the heating side outlet of the light fraction removal column supply preheater (116) is connected to the inlet of a light fraction removal column (117); the outlet of the light fraction removal column (117) is connected to the suction port of a light fraction removal column pot discharge pump (119); and the discharge port of the light fraction removal column pot discharge pump (119) is connected to the cooling side inlet of the light fraction removal column supply preheater (116).The cooling side outlet of the light fraction removal column supply preheater (116) is connected to the inlet of a condensation reaction liquid receiving tank (120), the outlet of the condensation reaction liquid receiving tank (120) is connected to the suction port of a condensation reaction liquid discharge pump (121), the discharge port of the condensation reaction liquid discharge pump (121) is branched into two and is connected to the filter cake outlet of the pressurized sub-separator (423) and the inlet of the crystallization supply buffer tank (201), respectively, and the top outlet of the light fraction removal column (117) is connected to the light fraction removal column condenser The cooling side gas phase outlet of the light fraction removal column condenser (122) is connected to the cooling side inlet of the light fraction removal column aftercooler (123), the cooling side gas phase outlet of the light fraction removal column aftercooler (123) is connected to a vacuum unit, and the cooling side liquid phase outlet of the light fraction removal column condenser (122) merges with the cooling side liquid phase outlet of the light fraction removal column aftercooler (123) and is then connected to the inlet of the light fraction receiving tank (124).
[0024] Apparatus for implementing the method for producing synthetic bisphenol A (2): The discharge port of the condensation reaction liquid discharge pump (121) is connected to the discharge port of the circulation pump (427) of the crystal melting device, and then connected to the inlet of the crystallization supply buffer tank (201). The outlet of the crystallization supply buffer tank (201) is connected to the suction port of the main crystallizer supply pump (202). The discharge port of the main crystallizer supply pump (202) is connected to the cooling side inlet of the supply cooler (203) of the main crystallizer. The cooling side outlet of the supply cooler (203) of the main crystallizer and the cooling side outlet of the external circulation crystallization cooler (206) are both main circulation type crystallizers. The outlet of the main circulation type crystallizer (204) is connected to the suction port of the crystallization circulation pump (205) and the mother liquor inlet of the first-stage pressurized main separator (207). The discharge port of the crystallization circulation pump (205) is connected to the cooling-side inlet of the external circulation crystallization cooler (206). The mother liquor / washing liquid outlet of the first-stage pressurized main separator (207) is connected to the inlet of the first-stage main separator mother liquor / washing liquid tank (208). The outlet of the first-stage main separator mother liquor / washing liquid tank (208) is connected to the suction port of the washing phenol pump (209). is connected to the inlet of the mother liquor receiving tank (401), the discharge port of the phenol discharge pump (311) is connected to the filter cake outlet of the first-stage pressurized main separator (207) and the inlet of the slurry mixing and washing tank (210), the outlet of the slurry mixing and washing tank (210) is connected to the suction port of the crystal slurry pump (211), the discharge port of the crystal slurry pump (211) is connected to the mother liquor inlet of the second-stage pressurized main separator (212), the mother liquor outlet of the second-stage pressurized main separator (212) is connected to the inlet of the second-stage main separator mother liquor tank (213), and the outlet of the second-stage main separator mother liquor tank (213) is connected to the suction port of the crystal slurry pump (211). is connected to the suction port of a slurry mixed washing mother liquor pump (214), the discharge port of the slurry mixed washing mother liquor pump (214) is branched into two, which are respectively connected to the washing liquid inlet of the pressurized secondary separator (423) and the washing liquid inlet of the first-stage pressurized main separator (207), the filter cake outlet of the second-stage main separator mother liquor tank (213) and the heating side outlet of the melting heater (217) are both connected to the inlet of a crystal melting device (215), the outlet of which is connected to the suction port of the circulating pump (216) of the crystal melting device and the suction port of the dephenol supply pump (218),The discharge port of the circulation pump (216) of the crystal melting device is connected to the inlet of the heating side of the melting heater (217), and the discharge port of the phenol removal supply pump (218) is connected to the inlet of the liquid film falling type phenol removal device (301).
[0025] Apparatus for implementing the method for producing synthetic bisphenol A (3): the discharge port of the phenol removal supply pump (218) is connected to the inlet of a liquid film falling type phenol removal apparatus (301), the outlet of the liquid film falling type phenol removal apparatus (301) is connected to the inlet of a gas-liquid separation tank (302), the gas phase outlet of the gas-liquid separation tank (302) is connected to the cooling side inlet of a condenser (303) of a steam stripping dephenol removal tower, the gas phase outlet of the condenser (303) of the steam stripping dephenol removal tower is connected to a vacuum unit, and the liquid phase outlet is connected to a phenol tank (31 The outlet of the phenol tank (310) is connected to the inlet of a phenol discharge pump (311), the discharge outlet of the phenol discharge pump (311) is connected to the cooling side inlet of a phenol cooler (312), the liquid phase outlet of the liquid separation tank (302) is connected to the top inlet of a steam stripping phenol removal tower (305), the top outlet of the steam stripping phenol removal tower (305) is connected to the inlet of the kettle section of the phenol absorption tower (306), the outlet of the kettle section is connected to the suction port of the BPA melting pump (315), and the inlet of the kettle section is connected to the steam The phenol absorber (306) is connected to the heating side outlet of the stripping steam superheater (304), the discharge port of the BPA melt pump (315) is connected to the inlet of the packaging machine (316), the top outlet of the phenol absorber (306) is connected to the cooling side inlet of the phenol absorber condenser (309), the outlet of the kettle section is connected to the suction port of the phenol circulation pump (307), the top inlet is connected to the cooling side outlet of the spray phenol cooler (308), the gas phase outlet of the cooling side of the phenol absorber condenser (309) is connected to a vacuum unit, the liquid phase outlet is connected to the inlet of an ethylbenzene tank (526), and the phenol absorber (306) is connected to the heating side outlet of the phenol absorber condenser (309). The discharge port of the phenol circulation pump (307) is branched into two, one of which is joined with the outlet of the second-stage reactor (114) and then connected to the inlet of the adsorption column (115); the other is joined with one stream of the cooling side outlet of the decomposition supply preheater (601) and then connected to the cooling side inlet of the spray phenol cooler (308); the outlet of the fresh phenol tank (313) is connected to the suction port of the fresh phenol pump (314); the discharge port of the fresh phenol pump (314) is branched into two, one of which is connected to the inlet of the recovered phenol tank (416);The other one merges with the cooling side outlet of the phenol cooler (312) and then connects to the filter cake outlet of the first stage pressurized main separator (207).
[0026] Apparatus for implementing the method for producing synthetic bisphenol A (3): The inlet of the mother liquor receiving tank (401) is connected to the discharge port of the washing phenol pump (209), the outlet of the rearrangement reactor (617), the discharge port of the washing liquid discharge pump (425), and the outlet of the isomerization reactor (432), respectively. The outlet of the mother liquor receiving tank (401) is connected to the suction port of the feed pump (402) of the falling film evaporator. The feed pump (402) of the falling film evaporator is connected to the inlet of the heating side of the first-stage feed preheater (403). The heating side outlet of the first-stage feed preheater (403) is connected to the heating side outlet of the second-stage feed preheater (404). The second-stage supply preheater (404) has a heating side outlet branched into two, which are connected to the heating side inlets of the low-pressure liquid film falling evaporator (405) and the pressurized liquid film falling evaporator (406), respectively. The heating side outlet of the pressurized liquid film falling evaporator (406) is connected to the inlet of the first-stage gas-liquid separation tank (407). The gas phase outlet of the first-stage gas-liquid separation tank (407) is connected to the cooling side inlet of the low-pressure liquid film falling evaporator (405). The liquid phase outlet is connected to the suction port of the discharge pump (410) of the first-stage separation tank. The discharge port of the discharge pump (410) of the first-stage separation tank is connected to the gas phase inlet of the third-stage gas-liquid separation tank (406). The low-pressure falling film evaporator (405) has a heating side outlet connected to the inlet of the third-stage gas-liquid separation tank (411), a cooling side outlet connected to the inlet of the second-stage gas-liquid separation tank (408), a gas phase outlet of the second-stage gas-liquid separation tank (408) connected to the inlet of the tail gas condenser (409), and a liquid phase outlet merges with the liquid phase outlet of the tail gas condenser (409) and is then connected to the inlet of the recovered phenol tank (416), and a liquid phase outlet of the third-stage gas-liquid separation tank (411) connected to the suction port of the crystallizer supply pump (412), resulting in two gas phase outlets. The first-stage supply preheater (403) is branched and connected to the cooling-side inlet of the first-stage supply preheater (403) and the cooling-side inlet of the condenser (414), respectively. The cooling-side gas phase outlet of the first-stage supply preheater (403) is joined to the cooling-side gas phase outlet of the condenser (414) and then connected to the cooling-side inlet of the aftercooler (415). The cooling-side liquid phase outlets of the first-stage supply preheater (403), the condenser (414), and the aftercooler (415) are joined to each other and then connected to the inlet of the recovered phenol tank (416). The discharge outlet of the crystallizer supply pump (412) is connected to the cooling-side inlet of the crystallizer supply cooler (413).The discharge port of the fresh phenol pump (313) and the discharge port of the tank discharge pump (521) of the phenol recovery tower are both connected to the inlet of a recovered phenol tank (416), the outlet of the recovered phenol tank (416) is connected to the inlet of a recovered phenol storage tank (418), the outlet of the recovered phenol storage tank (418) is connected to the suction port of a recovered phenol pump (419), the discharge port of the recovered phenol pump (419) is connected to the cooling side inlet of a second-stage supply preheater (404), and the discharge port of the recovered phenol pump (419) is connected to the cooling side inlet of a second-stage supply preheater (404). The cooling side outlet of the recovery crystallizer (420) is connected to the cooling side inlet of the cracking feed preheater (601), the inlet of the recovery crystallizer (420) is connected to the cooling side outlet of the feed cooler (413) of the crystallizer and the cooling side outlet of the external circulation crystallization cooler (421), and the outlet of the recovery crystallizer (420) is connected to the mother liquor inlet of the crystallization circulation pump (422) and the pressurized sub-separator (423). The discharge of the crystallization circulation pump (422) is connected to the cooling side inlet of the external circulation crystallization cooler (421), and the discharge of the slurry mixing washing mother liquor pump (214) is connected to the cooling side inlet of the pressurized sub-separator (423). The mother liquor outlet of the pressurized sub-separator (423) is connected to the inlet of the mother liquor receiving tank (429), the outlet of the mother liquor receiving tank (429) is connected to the suction port of the mother liquor discharge pump (430), the discharge port of the mother liquor discharge pump (430) is branched into two, one of which is connected to the heating side inlet of the mother liquor heater (431) and the other is further branched into two, which are connected to the inlet of the isomerization reactor (432) and the heating side inlet of the cracking feed preheater (601), respectively, and the wash liquid outlet of the pressurized sub-separator (432) is connected to the inlet of the wash liquid receiving tank (424). The filter cake outlet is connected to the discharge port of the condensation reaction liquid discharge pump (121) and the inlet of the crystal melting device (426), the outlet of the crystal melting device (426) is connected to the suction port of the circulating pump (427) of the crystal melting device, the discharge port of the circulating pump (427) of the crystal melting device is branched into two, which are respectively connected to the inlet of the crystallization supply buffer tank (201) and the heating side inlet of the heater (428) of the crystal melting device, and the heating side outlet of the heater (428) of the crystal melting device is connected to the inlet of the crystal melting device (426).
[0027] An apparatus for implementing the method for producing synthetic bisphenol A (5): the discharge outlet of the light fraction discharge pump (125) is joined to the discharge outlet of an ethylbenzene supply pump (527) and then connected to the heating side inlet of a dehydrating tower preheater (501), the heating side outlet of the dehydrating tower preheater (501) is connected to the inlet of a dehydrating tower (502), the top outlet of the dehydrating tower (502) is connected to the inlet of an acetone recovery tower (504), the top inlet of the tower is connected to the discharge outlet of an ethylbenzene discharge pump (515), the tower pot outlet is connected to the suction port of a tower pot discharge pump (518) of the dehydrating tower, and the top outlet of the acetone recovery tower (504) is connected to the discharge port of an ethylbenzene discharge pump (515). The acetone tower reflux tank (508) is connected to the inlet of the cooling side of the acetone tower condenser (506), its top inlet is connected to the discharge outlet of the acetone tower reflux pump (509), its outlet of the tower pot is connected to the inlet of the phase separator (510), its cooling-side gas phase outlet of the acetone tower condenser (506) is connected to the cooling-side inlet of the acetone tower aftercooler (507), its liquid phase outlet is connected to the inlet of the acetone tower reflux tank (508), its cooling-side gas phase outlet of the acetone tower aftercooler (507) is connected to a vacuum unit, its liquid phase outlet is connected to the inlet of the acetone tower reflux tank (508), and its outlet of the acetone tower reflux tank (508) is connected to the inlet of the acetone tower reflux pump (509). The outlet of the phase separator (510) is connected to the suction port of the aqueous phase discharge pump (511) and the suction port of the ethylbenzene discharge pump (515). The outlet of the aqueous phase discharge pump (511) is connected to the suction port of the ethylbenzene discharge pump (515). The outlet of the aqueous phase discharge pump (511) is connected to the cooling side inlet of the phenol-containing water cooler (512). The cooling side outlet of the phenol-containing water cooler (512) is connected to the cooling side inlet of the phenol-containing water cooler (513). The cooling side outlet of the phenol-containing water cooler (513) is connected to the inlet of the phase separator (514). The outlet of the phase separator (514) is connected to the inlet of the phase separator (510) and the suction port of the wastewater pump (516), the discharge port of the ethylbenzene discharge pump (515) is also connected to the cooling side inlet of the ethylbenzene cooler (517), the cooling side outlet of the ethylbenzene cooler (517) is connected to a vacuum unit, the outlet of the column pot discharge pump (518) of the dehydration tower is connected to the inlet of the phenol recovery tower (519), the top outlet of the phenol recovery tower (519) is connected to the cooling side inlet of the phenol tower condenser (522), and the top inlet is connected to the discharge port of the reflux pump (525) of the phenol recovery tower,The outlet of the tank section is connected to the suction port of the tank discharge pump (521) of the phenol recovery tower, the gas phase outlet on the cooling side of the phenol tower condenser (522) is connected to the cooling side inlet of the phenol tower aftercooler (523), the liquid phase outlet is connected to the inlet of the phenol tower reflux tank (524), the gas phase outlet on the cooling side of the phenol tower aftercooler (523) is connected to a vacuum unit, and the liquid phase outlet is connected to the inlet of the phenol tower reflux tank (524).
[0028] Apparatus for implementing the method for producing synthetic bisphenol A (6): the discharge port of the mother liquor discharge pump (430) is connected to the heating side inlet of a cracking feed preheater (601), the heating side outlet of the cracking feed preheater (601) is connected to the inlet of a falling film evaporator (602), the outlet of the falling film evaporator (602) is connected to the inlet of a gas-liquid separation tank (603), the gas phase outlet of the gas-liquid separation tank (603) is connected to the inlet of a de-p-isopropylphenol tower (604), the liquid phase outlet of the gas-liquid separation tank (603) is connected to the inlet of a de-p-isopropylphenol tower (604), and the liquid phase outlet of the gas-liquid separation tank (603) is connected to the inlet of a de-p-isopropylphenol tower (604). The top outlet of the isopropylphenol tower (604) is connected to the cooling side inlet of the condenser (607), the tower pot outlet is connected to the suction port of the tower pot discharge pump (606), the discharge port of the reflux pump (609) is branched into three and is connected to the top inlet of the de-p-isopropylphenol tower (604), the inlet of the decomposition product tank (614), and the top inlet of the decomposition reactor (610), respectively, the gas phase outlet on the cooling side of the condenser (607) is connected to a vacuum unit, and the liquid phase outlet is connected to the inlet of the reflux tank (608), and the reflux tank (608 The outlet of the decomposition reaction heater (612) is connected to the inlet of the decomposition reaction heater (612) and the incinerator. The outlet of the decomposition reaction heater (612) is connected to the inlet of ... The gas phase outlet of the cooling side is connected to a vacuum unit, the liquid phase outlet is connected to the inlet of a cracked product tank (614), the outlet of the cracked product tank (614) is connected to the suction port of a rearrangement supply pump (615), the suction port of the rearrangement supply pump (615) is connected to the cooling side inlet of a circulating cooler (616), the cooling side outlet of the circulating cooler (616) is branched into two, which are respectively connected to the inlet of the cracked product tank (614) and the inlet of the rearrangement reactor (617), and the outlet of the rearrangement reactor (617) is connected to the inlet of the mother liquor recovery tank (401).
[0029] The cooling side outlet temperature of the first-stage cooler (101) is 65 to 70°C, the heating side outlet temperature of the dehydration flash heater (106) is 85 to 87°C, the operation pressure of the dehydration flash evaporator (107) is 6 to 8 kPaA, the cooling side outlet temperature of the second-stage cooler (111) is 70 to 75°C, the operation pressure of the first-stage pressurized main separator (207) is 300 to 550 kPaA, the operation pressure of the second-stage pressurized main separator (212) is 350 to 600 kPaA, the operating temperature of the high-pressure falling film evaporator (406) is 150 to 154°C, and the operation pressure is 33 to 35 kPaA, the operating temperature of the low-pressure falling film evaporator (405) is 112 to 114°C, and the operation pressure is 6 to 8 kPaA, and the inlet temperature of the isomerization reactor (432) is 70 to 75°C.
[0030] The present invention relates to a method and apparatus for producing synthetic bisphenol A by a resin method, which comprises a condensation reaction unit for producing bisphenol A by catalytic condensation reaction of phenol and acetone under the action of a resin catalyst, an adduct crystallization unit for mixing the condensation reaction concentrate with the recovered adduct crystals after melting and then carrying out crystallization of the adduct, a liquid-phase dephenolization unit for melting the adduct to obtain a bisphenol A product, a secondary adduct crystallization unit for recovering phenol and bisphenol A in the mother liquor, a solvent recovery unit for recovering unreacted phenol and acetone and sending the phenol-containing wastewater to wastewater treatment, and a decomposition and rearrangement unit for recovering phenol in the mother liquor, first decomposing bisphenol A and 2,4-bisphenol A therein, then rearranging them, converting them into bisphenol A, and returning them to the system. In order to improve the yield and purity of phenol and reduce energy consumption, external circulation of the first-stage reactor, flash evaporation dehydration between the second-stage reactor, solid-liquid separation in a high-pressure separator, double-effect falling film evaporation and conversion of an isomerization reactor are introduced into the process. Through the application of these processes, the purity of the final bisphenol A product is more than 99.97 wt%, with free phenol less than 10 ppm, 2,4-bisphenol A less than 60 ppm, triphenol less than 25 ppm, water less than 480 ppm, and the consumption of standard oil per ton of bisphenol A product is less than 198 kg. Effect of the Invention
[0031] The advantages and benefits of the present invention are as follows: 1. The advantages of the synthetic bisphenol A production method and apparatus of the present invention are that a unique catalytic dehydration condensation reaction process is developed, which realizes high one-pass conversion rate of acetone and high selectivity of bisphenol A production; the process of two serial packed beds is used, and the first-stage reactor uses external circulation heat transfer, which reduces the average temperature in the reactor, inhibits the progress of reverse reaction, and improves the one-pass conversion rate; 2. The advantage of the method and apparatus for producing synthetic bisphenol A according to the present invention is that water can be removed in a timely manner from the front of the second-stage reactor by using flash evaporation, eliminating the chemical balance inhibition effect of water on the condensation reaction for producing bisphenol A and the activity inhibition effect of water on the condensation reaction resin catalyst, thereby realizing a higher one-pass conversion rate of the second-stage reactor; 3. The advantage of the synthetic bisphenol A production method and apparatus of the present invention is that the main and sub-flows are both using rotary drum type pressurized centrifuges to carry out solid-liquid phase separation, which greatly improves the separation driving force and separation effect, and reduces the difficulty and energy consumption of removing and recovering phenol from the products in the downstream areas. 4. The advantage of the synthetic bisphenol A production method and equipment of the present invention is that by applying thermal coupling technology and double effect falling film evaporation technology, the steam consumption can be greatly reduced, and the steam consumption index is advanced. 5. The advantages of the synthetic bisphenol A production method and apparatus of the present invention are that the by-products are converted into bisphenol A using an isomerization reactor, which increases the yield of bisphenol A, reduces the proportion of heavy fractions required for incineration, and reduces pollution. [Brief description of the drawings]
[0032] [Figure 1] FIG. 1 is a block diagram of a method for synthesizing bisphenol A by a resin method. [Diagram 2] FIG. 1 is a process diagram of condensation reaction unit 100#. [Diagram 3] FIG. 1 is a process diagram of adduct crystallization unit 200#. [Figure 4] FIG. 1 is a process diagram of liquid phase dephenolation unit 300#. [Diagram 5] FIG. 1 is a process diagram of secondary adduct crystallization unit 400#. [Figure 6] FIG. 13 is a process diagram of solvent recovery unit 500#. [Figure 7] FIG. 13 is a process diagram of the decomposition and rearrangement unit 600#. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0033] Example 1 Fresh acetone with a flow rate of 16000 kg / h after purification was measured and fed proportionally to the first-stage reactor 102 and the second-stage reactor 112, respectively. The acetone fed to the reactor 102 was mixed with the recovered phenol from the decomposition feed preheater 601 and the material from the first-stage circulation pump 105, entered the first-stage cooler 101, and was cooled to 65°C by the circulating water, and then entered the first-stage reactors 102-104. A part of the reaction liquid flowing out from the first-stage reactor 104 was circulated by the first-stage circulation pump 105 and returned to the first-stage reactor 102, with a circulation flow rate of 520000 kg / h. The remaining part was heated to 85°C by the dehydration flash heater 106, and then entered the dehydration flash evaporator 107 to remove some of the moisture. The operating pressure of the flash evaporator was 6 kPaA. The flash steam from the dehydration flash evaporator 107 is condensed and cooled by the flash evaporation first condenser 108 and the flash evaporation second condenser 109, and then the condensate containing water, acetone, and phenol flows into the light fraction receiving tank 124, and the tail gas is sent to the vacuum system. The dehydrated material from the dehydration flash evaporator 107 is mixed with the recovered acetone and fresh acetone from the second stream, and then sent to the second stage cooler 111 by the second stage supply pump 110. After being cooled to 70°C with circulating water, it enters the second stage reactors 112 to 114. The condensation reaction liquid discharged from the second stage reactor 114 is mixed with the bottom liquid from the phenol absorption tower 306 and then adsorbed. The reaction mixture enters the column 115, and is then heated by heat exchange with the bottom liquid of the light fraction removal tower 117 in the preheater 116, and then enters the light fraction removal tower 117. The water, unreacted acetone, and a part of the phenol in the reaction mixture evaporate from the top of the tower, and are condensed in the condenser 122 and the aftercooler 123. The tail gas enters the vacuum system, and the condensate flows into the light fraction receiving tank 124, and is sent to the solvent recovery unit 500# by the discharge pump 125 to recover phenol and acetone. The light fraction removal tower reboiler 118 is heated using low-pressure steam, and the bottom product is concentrated and sent out by the discharge pump 119. The temperature is lowered by heat exchange in the preheater 116, and then sent to the condensation reaction liquid receiving tank 120.
[0034] The reaction concentrate from the condensation reaction liquid discharge pump 121 and the recovery adduct crystal melt from the mother liquor recovery unit 400# of the crystal melting device circulation pump 427 are mixed in the crystallization supply buffer tank 201, then sent out by the crystallization supply pump 202, cooled by the supply cooler 203, and then enters the main circulation type crystallizer 204. The crystal slurry is pumped out of the main circulation type crystallizer 204 by the crystallization circulation pump 205, then enters the crystallization cooler 206, and removes the crystallization heat under the cooling action of deionized water. The crystal slurry flowing out of the main circulation type crystallizer 204 is continuously sent to the pressurized main separator 207 by the flow control valve to carry out solid-liquid separation. The phenol for washing the filter cake is the filtrate from the second stage centrifuge of the slurry mixing washing mother liquor pump 214. The separated mother liquor and washing liquid enter the main separator mother liquor / washing liquid tank 208, and then discharged. The phenol is introduced from the main separator and sent to the mother liquor receiving tank 401 by the discharge pump 218, and the phenol from the phenol discharge pump 311 is mixed with the filtered adduct crystals in the slurry mixing and washing tank 210, and the crystal slurry after the slurry mixing is sent to the second stage pressurized main separator 212 by the corresponding crystal slurry pump 211, and solid-liquid separation is performed. The filtrate enters the slurry mixing centrifuge mother liquor tank 213, and is sent by the slurry mixing and washing mother liquor pump 214 to the pressurized main separator 207 and the pressurized sub-separator 423, respectively, and is used for phenol washing. The filter cake is taken out by the centrifuge and enters the crystal melting device 215, and the material in the crystal melting device 215 is sent to the heater 217 by the corresponding crystal melting circulation pump 216 to be heated, and then returned to the crystal melting device 215. The operating pressures of the first stage pressurized main separator 207 and the second stage pressurized main separator 212 were 300 kPaA and 350 kPaA, respectively.
[0035] The adduct melt from the dephenolization supply pump 218 enters the falling film type dephenolization device 301, evaporates by heating with steam, and enters the gas-liquid separation tank 302. The liquid phase enters the top of the steam stripping dephenolization device 305, the gas phase is condensed by the condenser 303, the tail gas enters the vacuum system, the condensate enters the phenol tank 310, and fresh phenol with a flow rate of 48,864 kg / h from the tank area enters the fresh phenol tank 313 and is pumped out by the fresh phenol pump 314, a part of it is metered and then pumped into the phenol tank 310, and the rest is sent to the recovery phenol tank 416. The phenol in the phenol tank 310 is pumped out by the phenol discharge pump 311, cooled to a set value by the washing phenol cooler 312, and then sent to the slurry mixing washing tank 210 for washing. The water vapor is heated by the electric steam superheater 304 and enters the bottom of the steam stripping dephenolization device 305 as steam stripping steam. The liquid bisphenol A obtained at the bottom is pumped out by the BPA melting pump 315, then molded, granulated, and packaged in the packaging machine 316 to obtain a bisphenol A product. The gas phase at the top enters the bottom of the phenol absorption tower 306 and undergoes gas-liquid mass transfer with the absorbed phenol added from the top. The gas coming out of the top enters the phenol absorption tower condenser 309, the tail gas enters the vacuum system, the condensate is hydrous phenol and enters the ethylbenzene tank 526, the bottom liquid is a bisphenol A phenol solution, which is sent to the cooler 308 by the phenol circulation pump 307 to be cooled, and then returned to the top of the phenol absorption tower 306.
[0036] The material from the mother liquor receiving tank 401 is sequentially sent to the first-stage feed preheater 403 and the second-stage feed preheater 404 by the feed pump 402. The first-stage feed preheater 403 is a thermally coupled heat exchanger, and the heat medium is the gas phase material from the third-stage gas-liquid separation tank 411. The second-stage feed preheater 404 is also a thermally coupled heat exchanger, and the heat medium is phenol from the recovery phenol pump 419. After the material has been preheated in two stages, it is weighed and divided into two parts. One part enters the high-pressure falling film evaporator 406, where it is evaporated by the heating of steam, and the other part is discharged from the bottom of the high-pressure falling film evaporator 406. The outflowing gas and liquid phase materials enter the first stage gas-liquid separation tank 407, and the operating temperature and operating pressure of the high pressure falling film evaporator 406 are 150°C and 33kPaA, respectively. The liquid phase material is pumped to the third stage gas-liquid separation tank 411 by the pump 410, and the gas phase material enters the low pressure falling film evaporator 405 as a heat medium. After condensation, the gas and liquid phases are separated in the second stage gas-liquid separation tank 408, and the liquid phase enters the recovery phenol tank 416, and the gas phase enters the tail gas condenser 409, where it is further condensed by circulating water. The condensate enters the recovery phenol tank 416, and the tail gas condenser 409 is further condensed by circulating water. The remaining part of the preheated mother liquor is sent to the vacuum system, and the remaining part of the preheated mother liquor is heated and evaporated in the low-pressure falling film evaporator 405. The gas-liquid two-phase material flowing out from the bottom of the low-pressure falling film evaporator 405 enters the third-stage gas-liquid separation tank 411. The operating temperature and operating pressure of the low-pressure falling film evaporator 405 are 112°C and 6kPaA, respectively. A part of the gas phase material enters the feed preheater 403 as a heat medium, and the remaining part is condensed in the condenser 414 under the action of circulating water. After the tail gas of the feed preheater 403 and the condenser 414 are combined, it enters the aftercooler 415, and the circulating water The tail gas is further condensed under the action of the vacuum system, and the condensate of the raw material preheater 403, the condenser 414 and the aftercooler 415 flows into the recovered phenol tank 416, and the material in the recovered phenol tank 416 is pumped into the recovered phenol storage tank 418 by the phenol discharge pump 417, and then pumped out by the recovered phenol pump 419, and after the temperature is lowered by heat exchange in the second-stage supply preheater 404 and the decomposition supply preheater 601, it is sent to the outlet of the first-stage cooler 101 of the condensation reactor and the phenol circulation pump 307, respectively.The liquid phase material in the third-stage gas-liquid separation tank 411 is a concentrated bisphenol A phenol solution, which is sent out by the crystallization supply pump 412 and cooled by circulating water via the crystallization feed material cooler 413, and then enters the recovery crystallizer 420. The adduct crystal slurry is pumped out of the recovery crystallizer 420 by the crystallization circulation pump 422, then enters the crystallization cooler 421, where the heat of crystallization is cooled and removed by deionized water. The crystal slurry flowing out of the recovery crystallizer 420 is continuously sent to the pressure sub-separator 423 for solid-liquid separation. The phenol for washing the filter cake is the filtrate from the second-stage centrifuge of the slurry mixing washing mother liquor pump 214. The mother liquor separated from the pressure sub-separator 423 enters the mother liquor receiving tank 429, is sent out by the mother liquor discharge pump 430, is preheated by the mother liquor heater 431, and then part of it is sent to the isomerization reactor 432. The inlet temperature is 70°C, and some of the 2,4-bisphenol A, triphenol, chromanol, etc. are converted to bisphenol A before entering the mother liquor receiving tank 401, and the other part is sent to the cracking and rearrangement unit 600# for cracking and rearrangement. The washing liquid from the pressurized secondary separator 423 enters the washing liquid receiving tank 424 and is sent to the mother liquor receiving tank 401 by the washing liquid discharge pump 425. A part of the reaction liquid introduced from the main separator and metered by the condensation reaction concentrated liquid discharge pump 121 is mixed with the adduct crystals filtered in the tail gas condenser 409. The material in the tail gas condenser 409 is sent to the heater 428 by the corresponding crystal melt circulation pump 427 to be heated and then returned to the tail gas condenser 409. The material in the tail gas condenser 409 is sent to the crystallization supply buffer tank 201 by the crystal melt circulation pump 427.
[0037] The dehydration tower 502 is an azeotropic distillation tower, and ethylbenzene is the azeotropic agent. The material from the light fraction discharge pump 121 is mixed with the material from the ethylbenzene supply pump 527, and then preheated by low pressure steam in the dehydration tower supply preheater 501, and then enters the dehydration tower 502. The overhead gas directly enters the acetone recovery tower 504, and the bottom liquid is phenol containing ethylbenzene, which is sent to the phenol recovery tower 519 by the tower pot discharge pump 518. The overhead gas of the acetone recovery tower 504 is condensed through the acetone tower condenser 506 and the aftercooler 507, and then the tail gas is sent to the vacuum system. The condensate enters the acetone tower reflux tank 508 and is sent out by the acetone tower reflux pump 509.One strand is sent to the top of the acetone recovery tower as reflux, and the other strand is sent to the suction port of the second stage feed pump 110 of the condensation reaction unit 100# reactor as recovered acetone. The bottom product enters the phase separator 510 to form an aqueous phase and an organic phase. The aqueous phase material is sent out by the aqueous phase discharge pump 511 and cooled by the coolers 512 and 513, then enters the phase separator 514 for further phase separation. The organic phase flows to the phase separator 510, and the aqueous phase is sent out from the boundary region by the wastewater pump 516 as the wastewater of this device to carry out biochemical treatment. The organic phase of the phase separator 510 is sent out by the ethylbenzene discharge pump 515, a part of which is returned to the top of the dehydration tower 502 as a reflux liquid, and the remaining part is cooled by the ethylbenzene cooler 517 and then enters the vacuum pump as the auxiliary working liquid of the ethylbenzene liquid ring vacuum pump. By adjusting the heating steam flow rate of the reboiler 505, the rising The amount of steam is controlled, and the material from the column pot discharge pump 518 of the dehydration column 502 enters the phenol recovery column 519, the column top gas is condensed through the phenol column condenser 522 and the aftercooler 523, the tail gas enters the vacuum system, the condensate enters the reflux tank 524, a part of it is returned to the top of the column as reflux by the reflux pump 525, and the rest overflows into the ethylbenzene tank 526, which receives the hydrous phenol from the phenol absorption column condenser 309, the substituted ethylbenzene from the vacuum system, and the make-up ethylbenzene. The material in the ethylbenzene tank 526 is sent to the dehydration column 502 by the ethylbenzene supply pump 527 and charged. The column bottom liquid is phenol not containing ethylbenzene, and is sent to the recovered phenol storage tank 416 by the column pot discharge pump 521. The amount of rising steam in the column was controlled by adjusting the heating steam flow rate of the reboiler 520.
[0038] The mother liquor from the mother liquor discharge pump 430 is preheated by the cracking feed preheater 601 and then enters the falling film evaporator 602. The cracking feed preheater 601 is a thermally coupled heat exchanger, and the heat medium is the recovered phenol from the second stage feed preheater 404. The mother liquor is evaporated by heating with steam in the falling film evaporator 602. The gas-liquid two-phase material enters the gas-liquid separation tank 603. The liquid phase enters the decomposition reactor 610. The gas phase enters the de-p-isopropylphenol tower 604. The bottom liquid of the isopropylphenol column 604 is a heavy fraction containing p-isopropylphenol, which is discharged to the outside of the system via a discharge pump 606 and incinerated. The overhead gas is condensed and cooled by a condenser 607. The tail gas enters a vacuum system, and the condensate enters a reflux tank 608 and is then pumped out by a reflux pump 609. A portion of the liquid is returned to the top of the column as a reflux for the p-isopropylphenol removal column 604, and the other portion is returned to the top of the column as a reflux for the decomposition reactor 610. The material that enters the top and overflows from the reflux tank 608 enters the decomposition product tank 614, and the amount of rising steam in the tower is controlled by adjusting the flow rate of the heated steam in the reboiler 605. The material from the gas-liquid separation tank 603 enters the tower kettle of the decomposition reactor 610, and is then sent to the decomposition reaction heater 612 by the decomposition reaction circulation pump 611 to heat the material. After that, a certain amount of alkaline liquid is added as a catalyst for the decomposition reaction, and the material is returned to the tower kettle of the decomposition reactor 610, and the decomposition product is used as a catalyst for the decomposition reaction. Tar is discharged outside the system via a cracking reaction circulation pump 611 and incinerated, the overhead gas of the cracking reactor 610 is condensed and cooled by a cracking product condenser 613, the tail gas enters a vacuum system, the condensate enters a cracking product tank 614, and is then sent to a circulation cooler 616 by a rearrangement reaction supply pump 615 where it is cooled, a part of it is circulated back to the cracking product tank 614, the other part is used as the feed for a rearrangement reactor 617, and the material after rearrangement is returned to the mother liquor receiving tank 401.
[0039] The purity of the final bisphenol A product is more than 99.97 wt%, with free phenol less than 10 ppm, 2,4-bisphenol A less than 60 ppm, triphenol less than 25 ppm, water less than 480 ppm, and the consumption of standard oil per ton of bisphenol A product is less than 193 kg.
[0040] Example 2 Fresh acetone with a flow rate of 15000 kg / h after purification was measured and fed proportionally to the first-stage reactor 102 and the second-stage reactor 112, respectively. The acetone fed to the reactor 102 was mixed with the recovered phenol from the cracking supply preheater 601 and the material from the first-stage circulation pump 105, entered the first-stage cooler 101, and was cooled to 67°C by the circulating water, and then entered the first-stage reactors 102-104. A part of the reaction liquid flowing out from the first-stage reactor 104 was circulated by the first-stage circulation pump 105 and returned to the first-stage reactor 102, with a circulation flow rate of 487500 kg / h. The remaining part was heated to 86°C by the dehydration flash heater 106, and then entered the dehydration flash evaporator 107 to remove some of the moisture. The operating pressure of the flash evaporator was 7 kPaA. The flash steam from the dehydration flash evaporator 107 is condensed and cooled by the flash evaporation first condenser 108 and the flash evaporation second condenser 109, and then the condensate containing water, acetone, and phenol flows into the light fraction receiving tank 124, and the tail gas is sent to the vacuum system. The dehydrated material from the dehydration flash evaporator 107 is mixed with the recovered acetone and fresh acetone from the second stream, and then sent to the second stage cooler 111 by the second stage supply pump 110. After being cooled to 72°C with circulating water, it enters the second stage reactors 112 to 114. The condensation reaction liquid discharged from the second stage reactor 114 is mixed with the bottom liquid from the phenol absorption tower 306 and then adsorbed. The reaction mixture enters the column 115, and is then heated by heat exchange with the bottom liquid of the light fraction removal tower 117 in the preheater 116, and then enters the light fraction removal tower 117. The water, unreacted acetone, and a part of the phenol in the reaction mixture evaporate from the top of the tower, and are condensed in the condenser 122 and the aftercooler 123. The tail gas enters the vacuum system, and the condensate flows into the light fraction receiving tank 124, and is sent to the solvent recovery unit 500# by the discharge pump 125 to recover phenol and acetone. The light fraction removal tower reboiler 118 is heated using low-pressure steam, and the bottom product is concentrated and sent out by the discharge pump 119. The temperature is lowered by heat exchange in the preheater 116, and then sent to the condensation reaction liquid receiving tank 120.
[0041] The reaction concentrate from the condensation reaction liquid discharge pump 121 and the recovery adduct crystal melt from the mother liquor recovery unit 400# of the crystal melting device circulation pump 427 are mixed in the crystallization supply buffer tank 201, then sent out by the crystallization supply pump 202, cooled by the supply cooler 203, and then enters the main circulation type crystallizer 204. The crystal slurry is pumped out of the main circulation type crystallizer 204 by the crystallization circulation pump 205, then enters the crystallization cooler 206, and removes the crystallization heat under the cooling action of deionized water. The crystal slurry flowing out of the main circulation type crystallizer 204 is continuously sent to the pressurized main separator 207 by the flow control valve to carry out solid-liquid separation. The phenol for washing the filter cake is the filtrate from the second stage centrifuge of the slurry mixing washing mother liquor pump 214. The separated mother liquor and washing liquid enter the main separator mother liquor / washing liquid tank 208, and then discharged. The phenol is introduced from the main separator and sent to the mother liquor receiving tank 401 by the discharge pump 218, and the phenol from the phenol discharge pump 311 is mixed with the filtered adduct crystals in the slurry mixing and washing tank 210, and the crystal slurry after the slurry mixing is sent to the second stage pressurized main separator 212 by the corresponding crystal slurry pump 211, and solid-liquid separation is performed. The filtrate enters the slurry mixing centrifuge mother liquor tank 213, and is sent by the slurry mixing and washing mother liquor pump 214 to the pressurized main separator 207 and the pressurized sub-separator 423, respectively, and is used for phenol washing. The filter cake is taken out by the centrifuge and enters the crystal melting device 215, and the material in the crystal melting device 215 is sent to the heater 217 by the corresponding crystal melting circulation pump 216 to be heated, and then returned to the crystal melting device 215. The operating pressures of the first stage pressurized main separator 207 and the second stage pressurized main separator 212 were 450 kPaA and 500 kPaA, respectively.
[0042] The adduct melt from the dephenolization supply pump 218 enters the falling film type dephenolization device 301, evaporates by heating with steam, and enters the gas-liquid separation tank 302. The liquid phase enters the top of the steam stripping dephenolization device 305, the gas phase is condensed by the condenser 303, the tail gas enters the vacuum system, the condensate enters the phenol tank 310, and fresh phenol with a flow rate of 45,810 kg / h from the tank area enters the fresh phenol tank 313 and is pumped out by the fresh phenol pump 314, a part of it is metered and then pumped into the phenol tank 310, and the rest is sent to the recovery phenol tank 416. The phenol in the phenol tank 310 is pumped out by the phenol discharge pump 311, cooled to a set value by the washing phenol cooler 312, and then sent to the slurry mixing washing tank 210 for washing. The water vapor is heated by the electric steam superheater 304 and enters the bottom of the steam stripping dephenolization device 305 as steam stripping steam. The liquid bisphenol A obtained at the bottom is pumped out by the BPA melting pump 315, then molded, granulated, and packaged in the packaging machine 316 to obtain a bisphenol A product. The gas phase at the top enters the bottom of the phenol absorption tower 306 and undergoes gas-liquid mass transfer with the absorbed phenol added from the top. The gas coming out of the top enters the phenol absorption tower condenser 309, the tail gas enters the vacuum system, the condensate is hydrous phenol and enters the ethylbenzene tank 526, the bottom liquid is a bisphenol A phenol solution, which is sent to the cooler 308 by the phenol circulation pump 307 to be cooled, and then returned to the top of the phenol absorption tower 306.
[0043] The material from the mother liquor receiving tank 401 is sent by the supply pump 402 to the first-stage supply preheater 403 and the second-stage supply preheater 404 in sequence. The first-stage preheater 403 is a thermally coupled heat exchanger, and the heat medium is the gas phase material from the third-stage gas-liquid separation tank 411. The second-stage supply preheater 404 is also a thermally coupled heat exchanger, and the heat medium is phenol from the recovery phenol pump 419. After the two-stage preheating, the material is weighed and divided into two parts. One part enters the high-pressure falling film evaporator 406, where it is evaporated by the heating of steam and flows out from the bottom of the high-pressure falling film evaporator 406. The gas and liquid phase materials enter the first-stage gas-liquid separation tank 407, and the operating temperature and operating pressure of the high-pressure falling film evaporator 406 are 152°C and 34kPaA, respectively. The liquid phase material is pumped into the third-stage gas-liquid separation tank 411 by the pump 410, and the gas phase material enters the low-pressure falling film evaporator 405 as a heat medium. After condensation, the gas and liquid phases are separated in the second-stage gas-liquid separation tank 408, and the liquid phase enters the recovery phenol tank 416. The gas phase enters the tail gas condenser 409 and is further condensed by circulating water. The condensate enters the recovery phenol tank 416, and the tail gas is pumped to the vacuum suction system. The other part of the preheated mother liquor is heated and evaporated in the low-pressure falling film evaporator 405. The gas-liquid two-phase material flowing out from the bottom of the low-pressure falling film evaporator 405 enters the third-stage gas-liquid separation tank 411. The operating temperature and operating pressure of the low-pressure falling film evaporator 405 are 113°C and 7kPaA, respectively. A part of the gas phase material enters the first-stage supply preheater 403 as a heat medium, and the remaining part is condensed in the condenser 414 under the action of circulating water. After the tail gas of the first-stage supply preheater 403 and the condenser 414 are combined, it enters the aftercooler 415, and the circulating water is The condensate is further condensed under the action of the condenser, and the tail gas is sent to the vacuum system. The condensate of the first-stage feed preheater 403, the condenser 414 and the aftercooler 415 flows into the recovered phenol tank 416. The material in the recovered phenol tank 416 is pumped into the recovered phenol storage tank 418 by the phenol discharge pump 417, and then pumped out by the recovered phenol pump 419. After the temperature is lowered by the heat exchange of the second-stage feed preheater 404 and the decomposition feed preheater 601, the material is sent to the outlet of the first-stage cooler 101 of the condensation reactor and the outlet of the phenol circulation pump 307.The liquid phase material in the third-stage gas-liquid separation tank 411 is a concentrated bisphenol A phenol solution, which is sent out by the crystallization supply pump 412 and cooled by circulating water via the crystallization feed material cooler 413, and then enters the recovery crystallizer 420. The adduct crystal slurry is pumped out of the recovery crystallizer 420 by the crystallization circulation pump 422, then enters the crystallization cooler 421, where the heat of crystallization is cooled and removed by deionized water. The crystal slurry flowing out of the recovery crystallizer 420 is continuously sent to the pressure sub-separator 423 for solid-liquid separation. The phenol for washing the filter cake is the filtrate from the second-stage centrifuge of the slurry mixing washing mother liquor pump 214. The mother liquor separated from the pressure sub-separator 423 enters the mother liquor receiving tank 429, is sent out by the mother liquor discharge pump 430, is preheated by the mother liquor heater 431, and then part of it is sent to the isomerization reactor 432. The inlet temperature is 72°C, and some of the 2,4-bisphenol A, triphenol, chromanol, etc. are converted to bisphenol A before entering the mother liquor receiving tank 401, and the other part is sent to the cracking and rearrangement unit 600# for cracking and rearrangement. The washing liquid from the pressurized secondary separator 423 enters the washing liquid receiving tank 424 and is sent to the mother liquor receiving tank 401 by the washing liquid discharge pump 425. A part of the reaction liquid introduced from the main separator and metered by the condensation reaction concentrated liquid discharge pump 121 is mixed with the adduct crystals filtered in the tail gas condenser 409. The material in the tail gas condenser 409 is sent to the heater 428 by the corresponding crystal melt circulation pump 427 to be heated and then returned to the tail gas condenser 409. The material in the tail gas condenser 409 is sent to the crystallization supply buffer tank 201 by the crystal melt circulation pump 427.
[0044] The dehydration tower 502 is an azeotropic distillation tower, and ethylbenzene is the azeotropic agent. The material from the light fraction discharge pump 121 is mixed with the material from the ethylbenzene supply pump 527, and then preheated by low pressure steam in the dehydration tower supply preheater 501, and then enters the dehydration tower 502. The overhead gas directly enters the acetone recovery tower 504, and the bottom liquid is phenol containing ethylbenzene, which is sent to the phenol recovery tower 519 by the tower pot discharge pump 518. The overhead gas of the acetone recovery tower 504 is condensed through the acetone tower condenser 506 and the aftercooler 507, and then the tail gas is sent to the vacuum system. The condensate enters the acetone tower reflux tank 508 and is sent out by the acetone tower reflux pump 509.One strand is sent to the top of the acetone recovery tower as reflux, and the other strand is sent to the suction port of the second stage feed pump 110 of the condensation reaction unit 100# reactor as recovered acetone. The bottom product enters the phase separator 510 to form an aqueous phase and an organic phase. The aqueous phase material is sent out by the aqueous phase discharge pump 511 and cooled by the coolers 512 and 513, then enters the phase separator 514 for further phase separation. The organic phase flows to the phase separator 510, and the aqueous phase is sent out from the boundary region by the wastewater pump 516 as the wastewater of this device to carry out biochemical treatment. The organic phase of the phase separator 510 is sent out by the ethylbenzene discharge pump 515, a part of which is returned to the top of the dehydration tower 502 as a reflux liquid, and the remaining part is cooled by the ethylbenzene cooler 517 and then enters the vacuum pump as the auxiliary working liquid of the ethylbenzene liquid ring vacuum pump. By adjusting the heating steam flow rate of the reboiler 505, the rising The amount of steam is controlled, and the material from the column pot discharge pump 518 of the dehydration column 502 enters the phenol recovery column 519, the column top gas is condensed through the phenol column condenser 522 and the aftercooler 523, the tail gas enters the vacuum system, the condensate enters the reflux tank 524, a part of it is returned to the top of the column as reflux by the reflux pump 525, and the rest overflows into the ethylbenzene tank 526, which receives the hydrous phenol from the phenol absorption column condenser 309, the substituted ethylbenzene from the vacuum system, and the make-up ethylbenzene. The material in the ethylbenzene tank 526 is sent to the dehydration column 502 by the ethylbenzene supply pump 527 and charged. The column bottom liquid is phenol not containing ethylbenzene, and is sent to the recovered phenol storage tank 416 by the column pot discharge pump 521. The amount of rising steam in the column was controlled by adjusting the heating steam flow rate of the reboiler 520.
[0045] The mother liquor from the mother liquor discharge pump 430 is preheated by the cracking feed preheater 601 and then enters the falling film evaporator 602. The cracking feed preheater 601 is a thermally coupled heat exchanger, and the heat medium is the recovered phenol from the second stage feed preheater 404. The mother liquor is evaporated by heating with steam in the falling film evaporator 602. The gas-liquid two-phase material enters the gas-liquid separation tank 603. The liquid phase enters the decomposition reactor 610. The gas phase enters the de-p-isopropylphenol tower 604. The bottom liquid of the isopropylphenol column 604 is a heavy fraction containing p-isopropylphenol, which is discharged to the outside of the system via a discharge pump 606 and incinerated. The overhead gas is condensed and cooled by a condenser 607. The tail gas enters a vacuum system, and the condensate enters a reflux tank 608 and is then pumped out by a reflux pump 609. A portion of the liquid is returned to the top of the column as a reflux for the p-isopropylphenol removal column 604, and the other portion is returned to the top of the column as a reflux for the decomposition reactor 610. The material that enters the top and overflows from the reflux tank 608 enters the decomposition product tank 614, and the amount of rising steam in the tower is controlled by adjusting the flow rate of the heated steam in the reboiler 605. The material from the gas-liquid separation tank 603 enters the tower kettle of the decomposition reactor 610, and is then sent to the decomposition reaction heater 612 by the decomposition reaction circulation pump 611 to heat the material. After that, a certain amount of alkaline liquid is added as a catalyst for the decomposition reaction, and the material is returned to the tower kettle of the decomposition reactor 610, and the decomposition product is used as a catalyst for the decomposition reaction. Tar is discharged outside the system via a cracking reaction circulation pump 611 and incinerated, the overhead gas of the cracking reactor 610 is condensed and cooled by a cracking product condenser 613, the tail gas enters a vacuum system, the condensate enters a cracking product tank 614, and is then sent to a circulation cooler 616 by a rearrangement reaction supply pump 615 where it is cooled, a part of it is circulated back to the cracking product tank 614, the other part is used as the feed for a rearrangement reactor 617, and the material after rearrangement is returned to the mother liquor receiving tank 401.
[0046] The purity of the final bisphenol A product is more than 99.97 wt%, with free phenol less than 10 ppm, 2,4-bisphenol A less than 60 ppm, triphenol less than 25 ppm, water less than 480 ppm, and the consumption of standard oil per tonne of bisphenol A product is less than 196 kg.
[0047] Example 3 Fresh acetone with a flow rate of 14000 kg / h after purification was measured and fed proportionally to the first-stage reactor 102 and the second-stage reactor 112, respectively. The acetone fed to the reactor 102 was mixed with the recovered phenol from the decomposition feed preheater 601 and the material from the first-stage circulation pump 105, entered the first-stage cooler 101, and was cooled to 70°C by the circulating water, and then entered the first-stage reactors 102-104. A part of the reaction liquid flowing out from the first-stage reactor 104 was circulated by the first-stage circulation pump 105 and returned to the first-stage reactor 102, with a circulation flow rate of 520000 kg / h. The remaining part was heated to 87°C by the dehydration flash heater 106, and then entered the dehydration flash evaporator 107 to remove some of the moisture. The operating pressure of the flash evaporator was 8 kPaA. The flash steam from the dehydration flash evaporator 107 is condensed and cooled by the flash evaporation first condenser 108 and the flash evaporation second condenser 109, and then the condensate containing water, acetone, and phenol flows into the light fraction receiving tank 124, and the tail gas is sent to the vacuum system. The dehydrated material from the dehydration flash evaporator 107 is mixed with the recovered acetone and fresh acetone from the second stream, and then sent to the second stage cooler 111 by the second stage supply pump 110. After being cooled to 75°C with circulating water, it enters the second stage reactors 112 to 114. The condensation reaction liquid discharged from the second stage reactor 114 is mixed with the bottom liquid from the phenol absorption tower 306 and then adsorbed. The reaction mixture enters the column 115, and is then heated by heat exchange with the bottom liquid of the light fraction removal tower 117 in the preheater 116, and then enters the light fraction removal tower 117. The water, unreacted acetone, and a part of the phenol in the reaction mixture evaporate from the top of the tower, and are condensed in the condenser 122 and the aftercooler 123. The tail gas enters the vacuum system, and the condensate flows into the light fraction receiving tank 124, and is sent to the solvent recovery unit 500# by the discharge pump 125 to recover phenol and acetone. The light fraction removal tower reboiler 118 is heated using low-pressure steam, and the bottom product is concentrated and sent out by the discharge pump 119. The temperature is lowered by heat exchange in the preheater 116, and then sent to the condensation reaction liquid receiving tank 120.
[0048] The reaction concentrate from the condensation reaction liquid discharge pump 121 and the recovery adduct crystal melt from the mother liquor recovery unit 400# of the crystal melting device circulation pump 427 are mixed in the crystallization supply buffer tank 201, then sent out by the crystallization supply pump 202, cooled by the supply cooler 203, and then enters the main circulation type crystallizer 204. The crystal slurry is pumped out of the main circulation type crystallizer 204 by the crystallization circulation pump 205, then enters the crystallization cooler 206, and removes the crystallization heat under the cooling action of deionized water. The crystal slurry flowing out of the main circulation type crystallizer 204 is continuously sent to the pressurized main separator 207 by the flow control valve to carry out solid-liquid separation. The phenol for washing the filter cake is the filtrate from the second stage centrifuge of the slurry mixing washing mother liquor pump 214. The separated mother liquor and washing liquid enter the main separator mother liquor / washing liquid tank 208, and then discharged. The phenol is introduced from the main separator and sent to the mother liquor receiving tank 401 by the discharge pump 218, and the phenol from the phenol discharge pump 311 is mixed with the filtered adduct crystals in the slurry mixing and washing tank 210, and the crystal slurry after the slurry mixing is sent to the second stage pressurized main separator 212 by the corresponding crystal slurry pump 211, and solid-liquid separation is performed. The filtrate enters the slurry mixing centrifuge mother liquor tank 213, and is sent by the slurry mixing and washing mother liquor pump 214 to the pressurized main separator 207 and the pressurized sub-separator 423, respectively, and is used for phenol washing. The filter cake is taken out by the centrifuge and enters the crystal melting device 215, and the material in the crystal melting device 215 is sent to the heater 217 by the corresponding crystal melting circulation pump 216 to be heated, and then returned to the crystal melting device 215. The operating pressures of the first stage pressurized main separator 207 and the second stage pressurized main separator 212 were 550 kPaA and 600 kPaA, respectively.
[0049] The adduct melt from the dephenolization supply pump 218 enters the falling film type dephenolization device 301, evaporates by heating with steam, and enters the gas-liquid separation tank 302. The liquid phase enters the top of the steam stripping dephenolization device 305, the gas phase is condensed by the condenser 303, the tail gas enters the vacuum system, the condensate enters the phenol tank 310, and the fresh phenol with a flow rate of 442756 kg / h from the tank area enters the fresh phenol tank 313 and is pumped out by the fresh phenol pump 314, a part of it is metered and then pumped into the phenol tank 310, and the rest is sent to the recovery phenol tank 416. The phenol in the phenol tank 310 is pumped out by the phenol discharge pump 311, cooled to a set value by the washing phenol cooler 312, and then sent to the slurry mixing washing tank 210 for washing. The water vapor is heated by the electric steam superheater 304 and enters the bottom of the steam stripping dephenolization device 305 as steam stripping steam. The liquid bisphenol A obtained at the bottom is pumped out by the BPA melting pump 315, then molded, granulated, and packaged in the packaging machine 316 to obtain a bisphenol A product. The gas phase at the top enters the bottom of the phenol absorption tower 306 and undergoes gas-liquid mass transfer with the absorbed phenol added from the top. The gas coming out of the top enters the phenol absorption tower condenser 309, the tail gas enters the vacuum system, the condensate is hydrous phenol and enters the ethylbenzene tank 526, the bottom liquid is a bisphenol A phenol solution, which is sent to the cooler 308 by the phenol circulation pump 307 to be cooled, and then returned to the top of the phenol absorption tower 306.
[0050] The material from the mother liquor receiving tank 401 is sequentially sent to the first-stage feed preheater 403 and the second-stage feed preheater 404 by the feed pump 402. The first-stage feed preheater 403 is a thermally coupled heat exchanger, and the heat medium is the gas phase material from the third-stage gas-liquid separation tank 411. The second-stage feed preheater 404 is also a thermally coupled heat exchanger, and the heat medium is phenol from the recovery phenol pump 419. After the material has been preheated in two stages, it is weighed and divided into two parts. One part enters the high-pressure falling film evaporator 406, where it is evaporated by the heating of steam and flows out from the bottom of the high-pressure falling film evaporator 406. The gas and liquid phase materials enter the first-stage gas-liquid separation tank 407, and the operating temperature and operating pressure of the high-pressure falling film evaporator 406 are 154°C and 35kPaA, respectively. The liquid phase material is pumped into the gas-liquid separation tank 411 by the pump 410, and the gas phase material enters the low-pressure falling film evaporator 405 as a heat medium. After condensation, the gas and liquid phases are separated in the second-stage gas-liquid separation tank 408, and the liquid phase enters the recovery phenol tank 416. The gas phase enters the tail gas condenser 409 and is further condensed by circulating water. The condensate enters the recovery phenol tank 416, and the tail gas is passed through the vacuum system. The other part of the preheated mother liquor is heated and evaporated in the low pressure falling film evaporator 405. The gas-liquid two-phase material flowing out from the bottom of the low pressure falling film evaporator 405 enters the third stage gas-liquid separation tank 411. The operating temperature and operating pressure of the low pressure falling film evaporator 405 are 114°C and 8kPaA, respectively. A part of the gas phase material enters the first stage supply preheater 403 as a heat medium, and the remaining part is condensed in the condenser 414 under the action of circulating water. The tail gases of the first stage supply preheater 403 and the condenser 414 are joined together, and then enter the aftercooler 415, where the circulating water acts to condense the gas. The condensate from the first-stage feed preheater 403, the condenser 414 and the aftercooler 415 flows into the recovered phenol tank 416. The material in the recovered phenol tank 416 is pumped into the recovered phenol storage tank 418 by the phenol discharge pump 417, and then pumped out by the recovered phenol pump 419. After the temperature is lowered by heat exchange in the second-stage feed preheater 404 and the decomposition feed preheater 601, the material is sent to the outlet of the first-stage cooler 101 of the condensation reactor and the phenol circulation pump 307, respectively.The liquid phase material in the third stage gas-liquid separation tank 411 is a concentrated bisphenol A phenol solution, which is sent out by the crystallization supply pump 412 and cooled by circulating water via the crystallization feed material cooler 413, and then enters the recovery crystallizer 420. The adduct crystal slurry is pumped out of the recovery crystallizer 420 by the crystallization circulation pump 422, then enters the crystallization cooler 421, where the heat of crystallization is cooled and removed by deionized water. The crystal slurry flowing out of the recovery crystallizer 420 is continuously sent to the pressure sub-separator 423 for solid-liquid separation. The phenol for washing the filter cake is the filtrate from the second stage centrifuge of the slurry mixing washing mother liquor pump 214. The mother liquor separated from the pressure sub-separator 423 enters the mother liquor receiving tank 429, is sent out by the mother liquor discharge pump 430, is preheated by the mother liquor heater 431, and then part of it is subjected to an isomerization reaction. The 2,4-bisphenol A, triphenol, chromanol, etc. are converted into bisphenol A and then enter the mother liquor receiving tank 401, and the other parts are sent to the decomposition and rearrangement unit 600# for decomposition and rearrangement. The washing liquid from the pressurized secondary separator 423 enters the washing liquid receiving tank 424 and is sent to the mother liquor receiving tank 401 by the washing liquid discharge pump 425. A part of the reaction liquid introduced from the main separator and metered by the condensation reaction concentrated liquid discharge pump 121 is mixed with the adduct crystals filtered in the crystal melting device 426. The material in the crystal melting device 426 is sent to the heater 428 by the corresponding crystal melting circulation pump 427 to be heated and then returned to the crystal melting device 426. The material in the crystal melting device 426 is sent to the crystallization supply buffer tank 201 by the crystal melting circulation pump 427.
[0051] The dehydration tower 502 is an azeotropic distillation tower, and ethylbenzene is the azeotropic agent. The material from the light fraction discharge pump 121 is mixed with the material from the ethylbenzene supply pump 527, and then preheated by low pressure steam in the dehydration tower supply preheater 501, and then enters the dehydration tower 502. The overhead gas directly enters the acetone recovery tower 504, and the bottom liquid is phenol containing ethylbenzene, which is sent to the phenol recovery tower 519 by the tower pot discharge pump 518. The overhead gas of the acetone recovery tower 504 is condensed through the acetone tower condenser 506 and the aftercooler 507, and then the tail gas is sent to the vacuum system. The condensate enters the acetone tower reflux tank 508 and is sent out by the acetone tower reflux pump 509.One strand is sent to the top of the acetone recovery tower as reflux, and the other strand is sent to the suction port of the second stage feed pump 110 of the condensation reaction unit 100# reactor as recovered acetone. The bottom product enters the phase separator 510 to form an aqueous phase and an organic phase. The aqueous phase material is sent out by the aqueous phase discharge pump 511 and cooled by the coolers 512 and 513, then enters the phase separator 514 for further phase separation. The organic phase flows to the phase separator 510, and the aqueous phase is sent out from the boundary region by the wastewater pump 516 as the wastewater of this device to carry out biochemical treatment. The organic phase of the phase separator 510 is sent out by the ethylbenzene discharge pump 515, a part of which is returned to the top of the dehydration tower 502 as a reflux liquid, and the remaining part is cooled by the ethylbenzene cooler 517 and then enters the vacuum pump as the auxiliary working liquid of the ethylbenzene liquid ring vacuum pump. By adjusting the heating steam flow rate of the reboiler 505, the rising The amount of steam is controlled, and the material from the column pot discharge pump 518 of the dehydration column 502 enters the phenol recovery column 519, the column top gas is condensed through the phenol column condenser 522 and the aftercooler 523, the tail gas enters the vacuum system, the condensate enters the reflux tank 524, a part of it is returned to the top of the column as reflux by the reflux pump 525, and the rest overflows into the ethylbenzene tank 526, which receives the hydrous phenol from the phenol absorption column condenser 309, the substituted ethylbenzene from the vacuum system, and the make-up ethylbenzene. The material in the ethylbenzene tank 526 is sent to the dehydration column 502 by the ethylbenzene supply pump 527 and charged. The column bottom liquid is phenol not containing ethylbenzene, and is sent to the recovered phenol storage tank 416 by the column pot discharge pump 521. The amount of rising steam in the column was controlled by adjusting the heating steam flow rate of the reboiler 520.
[0052] The mother liquor from the mother liquor discharge pump 430 is preheated by the cracking feed preheater 601 and then enters the falling film evaporator 602. The cracking feed preheater 601 is a thermally coupled heat exchanger, and the heat medium is the recovered phenol from the second stage feed preheater 404. The mother liquor is evaporated by heating with steam in the falling film evaporator 602. The gas-liquid two-phase material enters the gas-liquid separation tank 603. The liquid phase enters the decomposition reactor 610. The gas phase enters the de-p-isopropylphenol tower 604. The bottom liquid of the isopropylphenol column 604 is a heavy fraction containing p-isopropylphenol, which is discharged to the outside of the system via a discharge pump 606 and incinerated. The overhead gas is condensed and cooled by a condenser 607. The tail gas enters a vacuum system, and the condensate enters a reflux tank 608 and is then pumped out by a reflux pump 609. A portion of the liquid is returned to the top of the column as a reflux for the p-isopropylphenol removal column 604, and the other portion is returned to the top of the column as a reflux for the decomposition reactor 610. The material that enters the top and overflows from the reflux tank 608 enters the decomposition product tank 614, and the amount of rising steam in the tower is controlled by adjusting the flow rate of the heated steam in the reboiler 605. The material from the gas-liquid separation tank 603 enters the tower kettle of the decomposition reactor 610, and is then sent to the decomposition reaction heater 612 by the decomposition reaction circulation pump 611 to heat the material. After that, a certain amount of alkaline liquid is added as a catalyst for the decomposition reaction, and the material is returned to the tower kettle of the decomposition reactor 610, and the decomposition product is used as a catalyst for the decomposition reaction. Tar is discharged outside the system via a cracking reaction circulation pump 611 and incinerated, the overhead gas of the cracking reactor 610 is condensed and cooled by a cracking product condenser 613, the tail gas enters a vacuum system, the condensate enters a cracking product tank 614, and is then sent to a circulation cooler 616 by a rearrangement reaction supply pump 615 where it is cooled, a part of it is circulated back to the cracking product tank 614, the other part is used as the feed for a rearrangement reactor 617, and the material after rearrangement is returned to the mother liquor receiving tank 401.
[0053] The purity of the final bisphenol A product is more than 99.97 wt%, with free phenol less than 10 ppm, 2,4-bisphenol A less than 60 ppm, triphenol less than 25 ppm, water less than 480 ppm, and the consumption of standard oil per tonne of bisphenol A product is less than 195 kg.
[0054] The technical means disclosed and proposed by the present invention can be achieved by those skilled in the art by referring to the contents of this specification and appropriately changing the parts of the conditions, etc. The method and manufacturing technology of the present invention have been described through preferred embodiments, but those skilled in the art can obviously modify or recombine the methods and technical means described herein to achieve the final manufacturing technology without departing from the content, spirit and scope of the present invention. It should be noted that all similar replacements and modifications are obvious to those skilled in the art, and such replacements and modifications are deemed to be within the spirit, scope and content of the present invention. [Explanation of symbols]
[0055] 101 1st stage cooler 102 First stage reactor 103 First stage reactor 104 First stage reactor 105 1st stage circulation pump 106 Dehydration flash evaporative heater 107 Dehydration flash evaporator 108 Flash evaporation first condenser 109 Flash evaporation secondary condenser 110 Second stage supply pump 111 Second stage cooler 112 Second stage reactor 113 Second stage reactor 114 Second stage reactor 115 Adsorption Column 116 Light fraction removal column supply preheater 117 Light fraction removal tower 118 Light fraction removal tower reboiler 119 Light fraction removal tower tank discharge pump 120 Condensation reaction liquid receiving tank 121 Condensation reaction concentrated liquid output pump 122 Light fraction removal column condenser 123 Light fraction removal tower aftercooler 124 Light separation tank 201 Crystallization supply buffer tank 202 Main crystallizer feed pump 203 Main Crystallizer Feed Cooler 204 Main circulation type crystallizer 205 Crystallization Circulation Pump 206 External circulation crystallization cooler 207 First stage pressurized main separator 208 1st stage main separator mother liquor / washing tank 209 Cleaning Phenol Pump 210 Slurry mixing and cleaning tank 211 Crystal Slurry Pump 212 Second stage pressurized main separator 213 Second stage main separator mother liquor tank 214 Slurry Mixing Washing Mother Liquor Pump 215 Crystal Melting Apparatus 216 Circulation pump for crystal melting equipment 217 Melting Heater 218 Phenol-free supply pump 301 Liquid film falling type dephenolization device 302 Gas-liquid separation tank 303 Condenser of steam stripping dephenol tower 304 Steam Stripping Steam Superheater 305 Steam stripping dephenol tower 306 Phenol Absorption Tower (306) 307 Phenol Circulation Pump 308 Spray Phenol Cooler 309 Phenol absorber condenser 310 Phenol Tank 311 Phenol Dispensing Pump 312 Phenol Cooler 313 Fresh Phenol Tank 314 Fresh Phenol Pump 315 BPA Melt Pump 316 Packaging Machine 401 Mother liquor receiving tank 402 Feed pump for falling film evaporator 403 1st stage supply preheater 404 2nd stage supply preheater 405 Low pressure falling film evaporator 406 Pressurized falling film evaporator 407 First stage gas-liquid separation tank 408 Second stage gas-liquid separation tank 409 Tail Gas Condenser 410 Discharge pump for first stage separation tank 411 3rd stage gas-liquid separation tank 412 Crystallizer Feed Pump 413 Crystallizer Feed Cooler 414 Condenser 415 Aftercooler 416 Phenol recovery tank 417 Phenol Dispensing Pump 418 Recovered phenol storage tank 419 Phenol recovery pump(419) 420 Recovery Crystallizer 421 External circulation crystallization cooler 422 Crystallization Circulation Pump 423 Pressurized Secondary Separator 424 Cleaning fluid receiving tank 425 Cleaning solution pump 426 Crystal Melting Apparatus 427 Circulation pump for crystal melting equipment 428 Heater for crystal melting device 429 Mother liquor receiver tank 430 Mother liquor discharge pump 431 Mother Liquor Heater 432 Isomerization Reactor 501 Dehydration tower preheater 502 Dehydration tower 503 Dehydration tower reboiler 504 Acetone recovery tower 505 Acetone tower reboiler 506 Acetone tower condenser 507 Acetone tower aftercooler 508 Acetone tower reflux tank 509 Acetone tower reflux pump 510 Phase Separator 511 Water phase discharge pump 512 Phenol-containing water cooler 513 Phenol-containing water cooler 514 Phase Separator 515 Ethylbenzene Pump 516 Wastewater Pump 517 Ethylbenzene Cooler 518 Dehydration tower tank discharge pump 519 Phenol recovery tower 520 Phenol tower reboiler 521 Phenol recovery tower tank discharge pump 522 Phenol column condenser 523 Phenol tower aftercooler 524 Phenol tower reflux tank 525 Reflux pump for phenol recovery tower 526 Ethylbenzene Tank 527 Ethylbenzene Supply Pump 601 Decomposition supply preheater 602 Falling film evaporator 603 Gas-liquid separation tank 604 p-Isopropylphenol Desorption Tower 605 Reboiler 606 Tower kettle discharge pump 607 Condenser 608 Reflux Tank 609 Circulation Pump 610 Decomposition Reactor 611 Decomposition reaction circulation pump 612 Decomposition reaction heater 613 Decomposition product condenser 614 Decomposition Products Tank 615 Displacement Supply Pump 616 Circulating cooler 617 Rearrangement Reactor
Claims
1. A method for producing synthetic bisphenol A by a resin method, comprising the steps of: (1) A process for producing bisphenol A by catalytically condensing phenol and acetone under the action of a resin catalyst in a condensation reaction unit, the reactor of the unit comprising a first-stage reactor and a second-stage reactor, the first-stage reactor being provided with an external circulation heat transfer and the second-stage reactor being provided with a flash evaporation dehydration step; (2) A process for mixing the condensation reaction concentrate with the recovered adduct crystals after melting, followed by crystallization of the adduct, followed by pressurization, drum rotation, filtration, adding phenol to the adduct crystal-containing solution, uniformly stirring and washing, and then centrifuging to obtain the adduct crystals, comprising a first adduct crystallization unit, and separating the solid phase and the liquid phase with a pressurized separator; (3) a liquid phase dephenolization unit for extracting phenol from the adduct melt, granulating and packaging to obtain a bisphenol A product; (4) a step of providing a secondary adduct crystallization unit for recovering phenol and bisphenol A in the mother liquor, separating phenol and bisphenol A by double-effect falling film evaporation, and converting the by-product into bisphenol A in an isomerization reactor; (5) a solvent recovery unit for recovering unreacted phenol and acetone and sending the phenol-containing wastewater to wastewater treatment; (6) a decomposition and rearrangement unit for removing impurities generated during the production process, recovering phenol in the mother liquor, and first decomposing and rearranging bisphenol A and 2,4-bisphenol A in the mother liquor, and then converting them into bisphenol A and returning them to the system; A method for producing synthetic bisphenol A by a resin method, characterized by having the above-mentioned features.
2. A method for realizing synthetic bisphenol A by the resin method according to claim 1, comprising: feeding raw acetone, recovered acetone, and recycled phenol into a condensation reaction unit (100#) for reaction; after simple separation of the product and unreacted raw materials, feeding the reaction liquid into an adduct crystallization unit (200#), feeding the hydrous phenol into a solvent recovery unit (500#); a part of the raw phenol is added from the adduct crystallization unit and used to wash the upstream reaction liquid, the recovered phenol from the dephenolization purification unit (300#), and the adduct crystal melt from the mother liquor recovery unit (400#); after washing, the first-stage centrifugal separation mother liquor / washing liquid and the second-stage centrifugal separation mother liquor are fed into the mother liquor recovery unit (400#), the adduct crystal melt is fed into the dephenolization purification unit, and the dephenolization is carried out. The method is characterized in that the final product BPA is produced in the phenol unit, and hydrous phenol is sent to the solvent recovery unit, a part of the raw phenol is added from the mother liquor recovery unit and used to wash the mother liquor, washing liquid, recovered phenol and recovered BPA from the decomposition and rearrangement unit (600#), then the second stage centrifuged mother liquor is sent to the decomposition and rearrangement unit, ethylbenzene is added as an azeotropic agent to the solvent recovery unit, recovered acetone is sent to the condensation reaction unit, recovered phenol is sent to the mother liquor recovery unit and waste water is discharged outside the system, the decomposition and rearrangement unit receives the second stage centrifuged mother liquor and decomposes and rearranges it, the recovered BPA is returned to the mother liquor recovery unit, and isopropyl phenol and waste liquid are sent out of the system.
3. Condensation reaction unit (100#): Fresh acetone after purification is measured and fed proportionally to the first stage reactor (102) and the second stage reactor (112), respectively. The acetone fed to the reactor (102) is mixed with the recovered phenol from the decomposition feed preheater (601) and the material from the first stage circulation pump (105), enters the first stage cooler (101), and is cooled by the circulating water, after which it enters the first stage reactors (102-104). A part of the reaction liquid flowing out from the first stage reactor (104) is circulated by the first stage circulation pump (105). The remaining part is heated by a dehydration flash heater (106) and then flows into a dehydration flash evaporator (107) to remove some of the moisture. The flash steam from the dehydration flash evaporator (107) is condensed and cooled by a flash evaporation first condenser (108) and a flash evaporation second condenser (109). The condensate containing water, acetone and phenol flows into a light fraction receiving tank (124), and the tail gas is sent to a vacuum system. The dehydrated material from the dehydration flash evaporator (107) is collected by a recovery tank (124). The condensation reaction liquid discharged from the second-stage reactor (114) is mixed with the bottom liquid from the phenol absorption tower (306) and then enters the adsorption column (115). The condensation reaction liquid is then heated by heat exchange with the bottom liquid of the light fraction removal tower (117) in the preheater (116) and enters the light fraction removal tower (117), where the water, unreacted acetone and some of the phenols in the reaction liquid are removed.
3. The method according to claim 2, characterized in that after the phenol evaporates from the top of the column and is condensed in the condenser (122) and the aftercooler (123), the tail gas enters a vacuum system, the condensate flows into the light fraction receiving tank (124), and is sent to the solvent recovery unit (500#) by the discharge pump (125) to recover phenol and acetone, the light fraction removal column reboiler (118) is heated with low pressure steam, the column bottom is concentrated, and sent out by the discharge pump (119), and the temperature is lowered by heat exchange in the preheater (116), and then sent to the condensation reaction liquid receiving tank (120).
4. The adduct crystallization unit (200#): The reaction concentrate from the condensation reaction liquid discharge pump (121) and the adduct crystal melt recovered from the mother liquor recovery unit (400#) of the crystal melting device circulation pump (427) are mixed in the crystallization supply buffer tank (201), then sent out by the crystallization supply pump (202), cooled by the supply cooler (203), and then enters the main circulation type crystallizer (204). The crystal slurry is then pumped by the crystallization circulation pump (205) to the main circulation type crystallizer (205). After being pumped out from the main circulation type crystallizer (204), it enters the crystallization cooler (206) and removes the heat of crystallization under the cooling action of deionized water. The crystal slurry flowing out of the main circulation type crystallizer (204) is continuously sent to the pressurized main separator (207) by the flow control valve to carry out solid-liquid separation. The phenol for washing the filter cake is the filtrate from the second stage centrifuge of the slurry mixed washing mother liquor pump (214). The separated mother liquor and washing liquid enter the main separator mother liquor / washing liquid tank (208) and are discharged by the discharge pump. The phenol introduced from the main separator and the phenol discharge pump (311) is mixed with the filtered adduct crystals in the slurry mixing and washing tank (210) and washed. The crystal slurry after the slurry mixing is sent to the second stage pressurized main separator (212) by the corresponding crystal slurry pump (211) and undergoes solid-liquid separation. The filtrate enters the slurry mixing centrifuge mother liquor tank (213), and the slurry The method according to claim 2, characterized in that the mixed washing mother liquor is pumped out by the mixed washing mother liquor pump (214) and sent to the pressurized main separator (207) and the pressurized secondary separator (423) respectively for phenol washing, the filter cake is taken out by the centrifuge and enters the crystal melter (215), the material in the crystal melter (215) is sent to the heater (217) by the corresponding crystal melt circulation pump (216) for heating, and then returned to the crystal melter (215).
5. The phenol removal purification unit (300#): the adduct melt from the phenol removal supply pump (218) enters the liquid film falling type phenol removal device (301), is evaporated by heating with steam, and enters the gas-liquid separation tank (302), the liquid phase enters the top of the steam stripping phenol removal device (305), the gas phase is condensed by the condenser (303), the tail gas enters the vacuum system, the condensate enters the phenol tank (310), fresh phenol from the tank area enters the fresh phenol tank (313) and is pumped out by the fresh phenol pump (314), a part of it is metered and then pumped into the phenol tank (310), and the rest is sent to the recovery phenol tank (416), the phenol in the phenol tank (310) is pumped out by the phenol discharge pump (311), cooled to a set value by the washing phenol cooler (312), and then sent to the slurry mixing washing tank (210) for washing phenol.
5. The method according to claim 4, characterized in that: the bisphenol A is phenol, the water vapor is heated by an electric steam superheater (304) and then enters the bottom of the steam stripping dephenolization unit (305) as steam for steam stripping; the liquid bisphenol A obtained at the bottom is pumped out by a BPA melting pump (315) and then molded, granulated, and packaged in a packaging machine (316) to obtain a bisphenol A product; the vapor phase at the top enters the bottom of the phenol absorption tower (306) and performs gas-liquid mass transfer with the absorbed phenol added from the top; the gas coming out of the top enters the phenol absorption tower condenser (309), the tail gas enters a vacuum system, the condensate is hydrous phenol and enters an ethylbenzene tank (526); the bottom liquid is a bisphenol A phenol solution, which is sent to a cooler (308) by a phenol circulation pump (307) to be cooled, and then returned to the top of the phenol absorption tower (306).
6. The mother liquor recovery unit (400#): the material from the mother liquor receiving tank (401) is successively sent to the first stage supply preheater (403) and the second stage supply preheater (404) by the supply pump (402). The preheater (403) is a thermally coupled heat exchanger, and the heat medium is the gas phase material from the third stage gas-liquid separation tank (411). The second stage supply preheater (404) is also a thermally coupled heat exchanger, and the heat medium is phenol from the recovery phenol pump (419). After the two stages of preheating, the material is weighed and divided into two parts, and one part is fed to the high pressure falling film evaporator (406). The gas and liquid phases flowing out from the bottom of the high pressure falling film evaporator (406) enter the first stage gas-liquid separation tank (407), the liquid phase is pumped to the third stage gas-liquid separation tank (411) by a pump (410), the gas phase enters the low pressure falling film evaporator (405) as a heat medium, and after condensation, the gas and liquid phases are separated in the second stage gas-liquid separation tank (408), the liquid phase enters the recovery phenol tank (416), the gas phase enters the tail gas condenser (409) and is further condensed by circulating water, and the condensate is fed to the recovery phenol tank (416). The remaining part of the preheated mother liquor is heated and evaporated in the low pressure liquid film falling evaporator (405), the gas-liquid two-phase material flowing out from the bottom of the low pressure liquid film falling evaporator (405) flows into the third stage gas-liquid separation tank (411), a part of the gas phase material flows into the first stage supply preheater (403) as a heat medium, the remaining part is condensed in the condenser (414) under the action of circulating water, the tail gas of the first stage supply preheater (403) and the tail gas of the condenser (414) are merged and then flow into the aftercooler (415). The phenol is further condensed under the action of circulating water, and the tail gas is sent to a vacuum system. The condensates of the first stage supply preheater (403), the condenser (414) and the aftercooler (415) flow into the recovered phenol tank (416). The material in the recovered phenol tank (416) is pumped into the recovered phenol storage tank (418) by the phenol discharge pump (417), and then pumped out by the recovered phenol pump (419). The temperature is lowered by heat exchange in the second stage supply preheater (404) and the decomposition supply preheater (601), and thenThe liquid phase material in the third-stage gas-liquid separation tank (411) is a concentrated bisphenol A phenol solution, which is pumped out by a crystallization feed pump (412), passed through a crystallization feed cooler (413) and cooled with circulating water, and then enters a recovery crystallizer (420). The adduct crystal slurry is pumped out of the recovery crystallizer (420) by a crystallization circulating pump (422). After being pumped out, the phenol enters a crystallization cooler (421) where it is cooled and removed by deionized water. The crystal slurry flowing out of the recovery crystallizer (420) is continuously sent to a pressure sub-separator (423) for solid-liquid separation. The phenol for washing the filter cake is the filtrate from the second stage centrifuge of the slurry mixed washing mother liquor pump (214). The mother liquor separated from the pressure sub-separator (423) enters a mother liquor receiving tank (429) and is pumped out by a mother liquor discharge pump (430). After being preheated by the liquid heater (431), a part of the liquid is sent to the isomerization reactor (432), where a part of 2,4-bisphenol A, triphenol, chromanol, etc. contained therein is converted to bisphenol A and then enters the mother liquor receiver (401), and the other part is sent to the cracking and rearrangement unit (600#) for cracking and rearrangement. The wash liquid from the pressurized secondary separator (423) enters the wash liquid receiver (424) and is sent to the mother liquor receiver (401) by the wash liquid discharge pump (425), and the main separator is The method according to claim 5, characterized in that a part of the reaction liquid introduced and metered by the condensation reaction liquid discharge pump (121) is mixed with the filtered adduct crystals in the crystal melter 426, the material in the crystal melter 426 is sent to the heater (428) by the corresponding crystal melt circulating pump (427) to be heated and then returned to the crystal melter 426, and the material in the crystal melter 426 is sent to the crystallization supply buffer tank (201) by the crystal melt circulating pump (427).
7. The solvent recovery unit (500#): the dehydration tower (502) is an azeotropic distillation tower, ethylbenzene is the azeotropic agent, the material from the light fraction discharge pump (125) is mixed with the material from the ethylbenzene supply pump (527), and then preheated by low pressure steam in the dehydration tower supply preheater (501) before entering the dehydration tower (502), the overhead gas directly enters the acetone recovery tower (504), the tower bottom liquid is phenol containing ethylbenzene, and is sent to the phenol recovery tower (519) by the tower pot discharge pump (518), the overhead gas of the acetone recovery tower (504) is condensed through the acetone tower condenser (506) and the aftercooler (507), and the tail gas is sent to the vacuum system, the condensate enters the acetone tower reflux tank (508) and is sent out by the acetone tower reflux pump (509);One strand is sent as reflux to the top of the acetone recovery tower, and the other strand is sent as recovered acetone to the suction port of the second stage feed pump (110) of the condensation reaction unit (100#). The bottom product enters the phase separator (510) and forms an aqueous phase and an organic phase. The aqueous phase material is pumped out by the aqueous phase discharge pump (511) and cooled by coolers (512) and (513), and then enters the phase separator (514) for further phase separation. The organic phase flows to the phase separator (510) and the aqueous phase flows to the main reactor. The organic phase of the phase separator (510) is discharged by an ethylbenzene discharge pump (515), a part of which is returned to the top of the dehydration tower (502) as a reflux liquid, and the remainder is cooled by an ethylbenzene cooler (517) and then enters the vacuum pump as an auxiliary working liquid for the ethylbenzene liquid ring vacuum pump. The amount of rising steam in the tower is controlled by adjusting the flow rate of the heating steam in the reboiler (505), and the amount of rising steam in the tower is then supplied to the dehydration tower (502) as a reflux liquid. The material from the column bottom discharge pump (518) of the column (502) enters the phenol recovery column (519), the column top gas is condensed through the phenol column condenser (522) and the aftercooler (523), the tail gas enters the vacuum system, and the condensate enters the reflux tank (524), a part of which is returned to the top of the column as reflux by the reflux pump (525), and the remaining part overflows into the ethylbenzene tank (526), which is filled with the water-containing phenol from the phenol absorption column condenser (309). The method according to claim 2, characterized in that the ethylbenzene tank (526) receives the ethylbenzene from the dehydration tower (502) and the ethylbenzene supply pump (527) sends the material in the ethylbenzene tank (526) to the dehydration tower (502) for charging, the bottom liquid is phenol not containing ethylbenzene, which is sent to the recovered phenol storage tank (416) by the tower bottom discharge pump (521), and the amount of rising steam in the tower is controlled by adjusting the flow rate of heating steam in the reboiler (520).
8. The cracking and rearrangement unit (600#): the mother liquor from the mother liquor discharge pump (430) is preheated by the cracking and supply preheater (601) and then enters the falling film evaporator (602). The cracking and supply preheater (601) is a thermally coupled heat exchanger, and the heat medium is the recovered phenol from the second-stage supply preheater (404). The mother liquor is evaporated in the falling film evaporator (602) by heating with steam. The gas-liquid two-phase material enters the gas-liquid separation tank (603). The liquid phase enters the tower pot of the cracking reactor (610), and the gas phase enters the p-isopropylphenol removal tower (604). The bottom liquid of the p-isopropylphenol removal tower (604) is a heavy fraction containing p-isopropylphenol, which is discharged to the outside of the system via a discharge pump (606) and incinerated. The overhead gas is condensed and cooled by a condenser (607). The tail gas enters a vacuum system. The condensate enters a reflux tank (608) and is then pumped out by a reflux pump (609). A portion of the liquid is returned to the top of the p-isopropylphenol removal tower (604) as a reflux for the tower, and the other portion is fed to the top of the decomposition reactor (610) as a reflux for the decomposition reactor (610). The material overflowing from the reflux tank (608) enters the decomposition product tank (614), and the amount of rising steam in the tower is controlled by adjusting the flow rate of the heated steam in the reboiler (605). The material from the gas-liquid separation tank (603) enters the tower kettle of the decomposition reactor (610), and is then sent to the decomposition reaction heater (612) by the decomposition reaction circulation pump (611) to heat the material. After that, a certain amount of alkaline liquid is added as a catalyst for the decomposition reaction, and the material is returned to the tower kettle of the decomposition reactor (610). The tar generated by the decomposition is returned to the tower kettle of the decomposition reactor (610). the rearrangement reactor (617) is charged with the rearrangement reactor (618), the rearrangement reactor (619) is charged with the rearrangement reactor (620), and the rearrangement reactor (621) is charged with the rearrangement reactor (622). The rearrangement reactor (623) is charged with the rearrangement reactor (623), and the rearrangement reactor (624) is charged with the rearrangement reactor (625). The rearrangement reactor (626) is charged with the rearrangement reactor (626). The rearrangement reactor (627) is charged with the rearrangement reactor (628). The rearrangement reactor (629) is charged with the rearrangement reactor (630). The rearrangement reactor (631) is charged with the rearrangement reactor (632). The rearrangement reactor (631) is charged with the rearrangement reactor (63 ...
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