CN114230442A - Method for reducing isopropyl phenol in reaction system for preparing bisphenol A - Google Patents
Method for reducing isopropyl phenol in reaction system for preparing bisphenol A Download PDFInfo
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Abstract
The invention discloses a method for reducing isopropylphenol in a reaction system for preparing bisphenol A, at least one part of reaction liquid after excessive phenol and acetone are subjected to condensation reaction by a catalyst in a condensation reactor is subjected to isomerization-cracking-rearrangement to obtain heavy drainage liquid, and the heavy drainage liquid containing isopropylphenol is treated by a concentration process to ensure that the isopropylphenol enters a phenol recovery system and is separated from the phenol along with mixed polyphenol; the mass percentage content of the isopropyl phenol in the condensation reactor is less than or equal to 0.25 percent. According to the invention, the cracking rearrangement product containing the isopropylphenol is concentrated, so that the isopropylphenol enters the light component and is discharged along with the mixed polyphenol, and the content of the isopropylphenol in the phenol extracted from the tower top can be adjusted by means of adjusting the extraction amount of the tower kettle and the like, thereby solving the problem that the service life of the catalyst is shortened because the cracking liquid or the rearrangement liquid for generating the isopropylphenol directly enters the reaction system in the prior art.
Description
Technical Field
The invention relates to the technical field of bisphenol A production, in particular to a method for reducing isopropyl phenol in a reaction system for preparing bisphenol A.
Background
Bisphenol a (bpa), one of the most widely used industrial compounds in the world, is mainly used for synthesizing materials such as Polycarbonate (PC) and epoxy resin.
Bisphenol A is an important organic chemical raw material which is generally prepared by condensation of two molecules of phenol and one molecule of acetone in the presence of an acidic catalyst, the catalyst which is commonly used in the prior art is sulfonic acid type strong-acid ion exchange resin carrying aminothiol, and the process steps mainly comprise reaction, raw material recovery, crystallization purification, adduct decomposition, concentration and granulation. However, in the above process, cumene phenol is accumulated as an impurity in the system, and chinese patent No. CN101370761A discloses a process for producing bisphenol a, wherein it is described that, in order to avoid accumulation of isomers or high boiling point impurities in the reaction system, a part of the mother liquor is withdrawn and subjected to alkali addition cracking treatment, and cumene phenol is a by-product generated during the cracking treatment. The isopropylphenol causes the aminothiol compound as a cocatalyst in the reaction step to be modified to lose its effect, thereby decreasing the catalytic activity of the aminothiol-supported sulfonic acid type ion exchange resin catalyst. The process for the preparation of bisphenol a disclosed in this patent comprises: a reaction step, a low boiling point component separation step, a bisphenol A separation step, a light component separation step, and a recombination reaction step, wherein the content of isopropylphenol in the reaction liquid is controlled to be less than 4% by weight. The method is used for producing bisphenol A, wherein the content of isopropyl phenol still has great influence on the service life of the catalyst, and the method generates more tar, thereby consuming more raw materials.
Chinese patent CN104379546A discloses a process for preparing bisphenol a, which comprises separating solid from liquid after separating concentrated liquid after reaction, wherein at least a part of the mother liquor is isomerized, separating solid from liquid after crystallizing the solution after isomerization, cracking at least a part of the obtained mother liquor, and feeding the product to the reaction step without being combined with a reactor. By doing so, the amount of tar produced can be reduced, the raw material consumption can be reduced, but still most of the cumene phenol can enter the reaction system, the catalyst activity is affected, and the catalyst life is reduced.
Obviously, the prior art process for producing bisphenol A cannot better process p-isopropylphenol.
Disclosure of Invention
The invention aims to provide a method for reducing the content of isopropylphenol in a reaction system for preparing bisphenol A, which is characterized in that isopropylphenol is separated from pyrolysis liquid and/or heavy drainage liquid and is not directly returned to a condensation reactor, so that the content of isopropylphenol returned to the condensation reaction system is reduced, and the problem that the service life of a catalyst is influenced because the pyrolysis liquid and/or rearrangement liquid of isopropylphenol is returned to the condensation reaction system to reduce the activity of the condensation reaction catalyst is solved.
In order to achieve the purpose of the invention, the technical scheme of the invention is as follows:
a method for reducing isopropyl phenol in a reaction system for preparing bisphenol A comprises the steps of carrying out isomerization-cracking-rearrangement on at least one part of reaction liquid after excessive phenol and acetone are subjected to condensation reaction in a condensation reactor by a catalyst to obtain heavy drainage liquid, carrying out concentration process treatment on the heavy drainage liquid containing isopropyl phenol, and enabling isopropyl phenol to enter a phenol recovery system and be separated from phenol along with mixed polyphenol; the mass percentage content of the isopropyl phenol in the condensation reactor is less than or equal to 0.25 percent.
Further, carrying out condensation reaction on excessive phenol and acetone in the presence of a catalyst to obtain a reacted solution, concentrating the reacted solution to obtain a light component (I) and a concentrated solution (I), carrying out crystallization process on the concentrated solution (I), and carrying out solid-liquid separation to obtain a bisphenol A adduct and a mother solution (I);
at least one part of the mother liquor (I) is subjected to isomerization reaction to obtain an isomerization product, and at least one part of the isomerization product is subjected to a primary concentration process to obtain a concentrated solution (II) and a low-boiling-point component; crystallizing and filtering the concentrated solution (II) to obtain a solid phase component and a mother solution (II), and pre-concentrating the mother solution (II) to obtain a heavy component (II) and a light component (II); adding alkali into the heavy component (II) for cracking, carrying out rearrangement reaction on a light component (III) generated by cracking to obtain heavy liquid, and carrying out secondary concentration process treatment on the heavy liquid to obtain a heavy component (IV) and a light component (IV); the light component (IV) containing the isopropylphenol enters the phenol recovery system and is removed together with the mixed polyphenol; the mass percentage content of the isopropyl phenol in the removed mixed polyphenol is 10-30%.
Further, the solid phase component and the heavy component (IV) generated by the concentrated solution (II) through a crystallization process are diluted by at least a part of the mother liquor (I) to form a crystallization solution, and the crystallization solution is returned to the crystallization process of the concentrated solution (I).
And further, returning the light component (IV) and the light component (II) to an isomerization concentration system through a preconcentration tower to be mixed with a low-boiling-point component, condensing and recovering heat, and entering a phenol recovery system for dephenolization treatment.
Further, the phenol recovery system comprises a dehydration column and a phenol purification column, and at least a part of the light component (I) and the low boiling point component are sent to the dehydration column; and the gas phase at the top of the dehydrating tower enters an acetone recovery tower, the liquid phase in the tower kettle of the dehydrating tower enters the phenol refining tower, the refined phenol is extracted from the gas phase at the top of the phenol refining tower, and the mixed polyphenol containing the isopropyl phenol is discharged from the tower kettle.
And further, removing impurities from the supplemented phenol raw material in the condensation reaction, conveying the phenol raw material into the dehydration tower for dehydration, refining the phenol raw material by the phenol refining tower to obtain refined phenol, and conveying the refined phenol into the condensation reactor.
Further, the phenol recovery system also comprises an acetone recovery tower, wherein the top of the acetone recovery tower is used for recovering acetone, and the bottom product of the acetone recovery tower is subjected to oil-water separation to obtain an entrainer mainly containing ethylbenzene, and the entrainer is circularly returned to the dehydration tower for reuse.
Further, the technical scheme of the invention at least comprises the following steps:
(1) and (3) catalytic reaction: under the action of a strong acid cation exchange resin catalyst, carrying out condensation reaction on excessive phenol and acetone to generate bisphenol A, and obtaining bisphenol A and a reaction solution of unreacted raw materials and a small amount of impurities;
(2) concentration and liquid separation: concentrating the reverse solution obtained in the step (1) to obtain a light component (I) and a concentrated solution (I), and carrying out solid-liquid separation on the concentrated solution after crystallization to obtain a bisphenol A adduct and a mother solution (I); dephenolizing the bisphenol A adduct to obtain a bisphenol A product;
(3) isomerization: at least one part of the mother liquor (I) obtained in the step (2) is subjected to isomerization reaction, part of the isomerized reaction liquid is returned to the condensation reactor, and part of the isomerized reaction liquid is injected into an isomerization concentration system to be subjected to primary concentration process treatment, so that concentrated liquid (II) and low-boiling-point components are obtained;
(4) pre-concentration: crystallizing and filtering the concentrated solution (II) obtained in the step (3) to obtain a solid phase component and a mother solution (II), and pre-concentrating the mother solution (II) in a pre-concentration tower to obtain a heavy component (II) and a light component (II);
returning the light component (II) to the isomerization concentration system;
(5) splitting and rearranging: carrying out alkaline cracking on the heavy component (II) in the step (4), condensing a light component (III) generated by cracking, carrying out rearrangement reaction to obtain a rearrangement liquid containing isopropyl phenol, and carrying out secondary concentration process treatment on heavy discharge liquid to obtain a heavy component (IV) and a light component (IV); introducing a light component (IV) containing isopropyl phenol into a phenol recovery system, and removing the light component (IV) and mixed polyphenol together; the mass percentage content of the isopropyl phenol in the removed mixed polyphenol is 10-30 percent;
diluting the solid phase component and the heavy component (IV) by at least part of the mother liquor (I) in the step (4) to form a crystallization liquid, and returning the crystallization liquid to the crystallization process of the concentrated solution (I);
(6) and (3) recovering phenol: feeding at least a portion of said low boiling components of step (3) to said dehydration column; meanwhile, the light component (IV) returns to the pre-concentration tower, and is mixed with the low boiling point component in the isomerization concentration system together with the light component (II), condensed and recycled, and then enters the dehydration tower together;
gas phase at the top of the dehydrating tower enters an acetone recovery tower to obtain recovered acetone, and oil-water separation is carried out on a product at the bottom of the dehydrating tower to obtain an azeotropic agent mainly containing ethylbenzene; the liquid phase in the tower kettle of the dehydration tower enters a phenol refining tower, and the gas phase at the tower top of the phenol refining tower is refined recovered phenol and can return to the condensation reactor; discharging mixed polyphenol containing isopropyl phenol from the tower kettle;
the mass percentage content of the isopropyl phenol in the condensation reactor is less than or equal to 0.25 percent after the steps.
Further, the method also comprises the steps of melting and granulating: and (3) carrying out liquid phase dephenolization on the bisphenol A adduct obtained in the step (2), removing phenol, forming bisphenol A molten liquid, and granulating the molten liquid to obtain a bisphenol A product.
In the prior art, in order to avoid accumulation of isomers or high-boiling-point impurities in a reaction system, a part of mother liquor is extracted and subjected to alkali-adding cracking treatment, and the isopropyl phenol is a byproduct generated in the treatment process. This substance causes the aminothiol compound as a co-catalyst in the reaction step to be modified to lose its effect, thereby reducing the catalytic activity of the aminothiol-supported sulfonic acid type ion exchange resin catalyst. Obviously, to increase catalyst life, reducing the percentage of cumene phenol produced by cracking that is directly fed to the condensation reaction system is the most straightforward solution to increasing catalyst activity and maintaining catalyst life. In the prior art, at least a part of the mother liquor is subjected to isomerization treatment, the solution after the isomerization treatment is crystallized and then subjected to solid-liquid separation, at least a part of the obtained mother liquor is subjected to cracking treatment, and the product is supplied to the reaction step without being combined with a reactor. By doing so, the amount of tar (i.e., mixed polyphenols) produced can be reduced, reducing raw material consumption, but still allowing a significant portion of the cumene phenol to enter the reaction system, affecting catalyst activity, reducing catalyst life.
The invention adopts a cracking-rearrangement reaction step, and then the cracking-rearrangement product is concentrated, so that the isopropylphenol enters a light component IV and is separated from a heavy component IV containing bisphenol A, and the isopropylphenol enters a phenol recovery system, thereby controlling the amount of the isopropylphenol in the phenol along with the amount of the extracted mixed polyphenol. The concentrated solution after cracking-rearrangement is returned to the crystallization process system of the solution after reaction, so that the influence of isopropyl phenol on the activity of the strong-acid cation exchange resin catalyst is reduced, and the service life of the catalyst is prolonged.
In summary, the present invention adopts the above technical solutions to obtain the following technical effects:
1. by adopting the technical scheme of the invention, the cracking rearrangement product containing the isopropylphenol is subjected to a concentration process, so that the isopropylphenol enters the light component and is separated from the heavy components such as bisphenol A and the like, the light component enters the phenol recovery system, finally the isopropylphenol is discharged out of the system from the tower kettle of the phenol refining tower along with the mixed polyphenol, and the isopropylphenol content in the phenol extracted from the tower top can be adjusted by means of adjusting the extraction amount of the tower kettle and the like, thereby solving the problem that the service life of the catalyst is shortened because the cracking liquid or the rearrangement liquid which generates the isopropylphenol directly enters the reaction system in the prior art.
2. By adopting the technical scheme of the invention, the content of phenol in the mixed polyphenol extracted from the bottom of the phenol tower is low, and the total extracted amount at the bottom of the phenol tower is small. And the phenol content in the phenol tower bottom extracted in the prior art is high, and heavy components at the tower bottom are discharged in the form of solid waste such as tar, so that the phenol raw material consumption is low, the solid waste is less, and the phenol tower is more environment-friendly.
3. By adopting the technical scheme of the invention, the devices are reduced, and the operation steps are simplified. The method specifically comprises the following steps: firstly, light components obtained by treating a rearrangement solution obtained after rearrangement reaction through a concentration process need to be further rectified to reduce the content of heavy components, so that the light components are sent into a preconcentration tower of mother liquor obtained by treating an isomerization product concentration process and recrystallizing for solid-liquid separation, and are rectified at the same time, and the light components containing the isopropylphenol are extracted from the top of the tower, so that one rectifying tower can be reduced; secondly, the gas phase at the top of the pre-concentration tower is sent into an isomerization product concentration system to be condensed together, so that a condensation device of the pre-concentration tower can be reduced; finally, the original dehydration tower is utilized to simultaneously complete the dehydration process of recovering phenol and fresh supplementary phenol raw materials, so that the operation can be simplified, the equipment can be reduced, and the equipment investment can be saved.
4. By adopting the technical scheme of the invention, the technical effect of reducing energy consumption is achieved. Firstly, the gas phase of the rearrangement concentrated product enters a preconcentration tower, and the brought heat can reduce the energy consumption of a reboiler of the tower; secondly, in the process of condensing the isomerized product and the rearranged product after concentration, hot water at about 90 ℃ can be generated by utilizing the latent heat of the isomerized product and the rearranged product, and the hot water can be used for heating reaction materials entering a reactor, so that the heat is fully utilized. And thirdly, the gas phase at the top of the phenol refining tower is used as a heat source of a steam generator, hot water is converted into low-pressure steam while the phenol gas phase is condensed, the low-pressure steam is supplied to other equipment which needs the low-pressure steam as a heating medium, after heat balance, the low-pressure steam generated at the top of the phenol refining tower can meet the requirement without additionally providing the low-pressure steam, and the step can greatly reduce the energy consumption of the device.
Drawings
FIG. 1 is a schematic process flow diagram of example 1 of the present invention.
Fig. 2 is a schematic diagram of the connection of the apparatus according to embodiment 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the specific contents of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1:
referring to FIGS. 1 and 2, this example provides a process for reducing cumene phenol in a reaction system for the production of bisphenol A, comprising the steps of:
(1) and (3) catalytic reaction: under the action of a strong acid cation exchange resin catalyst, carrying out condensation reaction on excessive phenol and acetone in a condensation reactor to generate bisphenol A, and obtaining bisphenol A and a reaction solution of unreacted raw materials and a small amount of impurities; heating excessive recovered phenol or fresh phenol (a phenol raw material to be supplemented into a condensation reactor) to a proper temperature, mixing the excessive recovered phenol or fresh phenol with acetone in proportion, feeding at least a part of mother liquor I subjected to crystallization separation in the subsequent step (2) and a mixture returned in the subsequent isomerization step (4) into the condensation reactor, filling a strong-acid cation cross-linking resin catalyst into the condensation reactor, and finishing a condensation reaction between phenol and acetone, wherein the operation temperature of the condensation reactor is 55-85 ℃, and the operation pressure is 0.2-0.4 MPa (gauge pressure), so as to generate bisphenol A, excessive phenol, water and a small amount of impurities. The impurities mainly comprise: 2, 4-bisphenol a isomers, methyl bisphenol a, trisphenols, leuco dyes, isopropylphenol dimers, and the like.
(2) Concentration and liquid separation: and (2) concentrating the reaction solution obtained in the step (1) to obtain a light component I and a concentrated solution I, treating the concentrated solution I through a crystallization process, and performing solid-liquid separation to obtain a bisphenol A adduct and a mother liquor I.
(3) Melting and granulating: carrying out liquid phase dephenolization on the bisphenol A adduct obtained in the step (2), removing phenol, forming bisphenol A molten liquid, and granulating the molten liquid to obtain a bisphenol A product;
(4) isomerization: at least one part of the mother liquor I obtained in the step (2) is subjected to isomerization reaction to obtain an isomerization product, and the isomerization product is subjected to a primary concentration process to obtain a concentrated solution II and a low-boiling-point component.
(5) Pre-concentration: crystallizing and filtering the concentrated solution II obtained in the step (4) to obtain a solid phase component and a mother solution II; pre-concentrating the mother liquor (II) by a pre-concentration tower to obtain a light component II and a heavy component II; returning the light component II to the isomerization concentration system in the step (3), condensing, and then feeding the light component II into a phenol recovery system to remove water, isopropyl phenol and other polyphenols and then recovering phenol;
(6) splitting and rearranging: adding alkali into the heavy component II concentrated in the step (5) for cracking, condensing a light component III generated by cracking, performing rearrangement reaction to obtain a rearrangement solution containing the isopropylphenol, performing secondary concentration process treatment on heavy-discharge liquid to obtain a heavy component IV and a light component IV, feeding the heavy-discharge liquid containing the isopropylphenol and the concentrated light component IV into a dehydration tower of a phenol recovery system, and removing the heavy component IV and the light component IV together with mixed polyphenol; the content of isopropyl phenol in the removed mixed polyphenol is 10-30 percent (mass percentage).
(7) And (3) recovering phenol: returning at least one part of the low-boiling point components to the isomerization concentration system through the preconcentration tower, and allowing the low-boiling point components, together with the light component IV and the light component II returned to the preconcentration tower, to enter a dehydration tower and a phenol refining tower through the isomerization concentration system for dehydration and refining, so that the isopropylphenol and the mixed polyphenol are removed from the phenol together, and the obtained refined phenol is returned to the condensation reactor; the cumene phenol is discharged with the mixed polyphenols, thereby reducing the amount of cumene phenol in the condensation reactor and reducing the toxic effect of the cumene phenol on the catalyst. The cracking reactor generates isopropyl phenol, finally the isopropyl phenol enters a subsequent phenol refining tower, a small part of the isopropyl phenol exists in the recovered phenol at the top of the tower, and most of the isopropyl phenol is discharged out of the system along with the mixed polyphenol at the bottom of the phenol refining tower. The content of isopropylphenol is an important factor affecting the life of the catalyst in the reactor, and therefore the content of isopropylphenol in the condensation reactor can be controlled by controlling the content of isopropylphenol in the recovered phenol, and in this example, the content of isopropylphenol in the condensation reactor is set to 0.25 mass% or less, preferably 0.16 to 0.21 mass% based on the total amount of the reaction liquid in the condensation reactor.
Specifically, the reaction product enters a light component removal tower after heat exchange through a heat exchanger, a part of light components are removed through rectification, and water, a part of by-products, a part of unreacted excessive phenol and crude bisphenol A are separated. The material in the tower bottom is crude bisphenol A, mainly contains phenol, bisphenol A and impurities, and is sent to a crystallizer. The operation pressure of the light component removal column is-0.1 to 0.1MPa (gauge pressure), and in order to lower the operation temperature, vacuum operation is preferred. The concentrated solution in the light component removal tower enters a crystallizer for crystallization to generate a crystal of a bisphenol A adduct, a liquid phase (mother liquor I) obtained by the liquid-solid separation of the next stage is used for washing the crystal, the crystal and the mother liquor I are subjected to liquid-solid separation, and the processes of crystallization, washing and liquid-solid separation are repeated for 3 times; washing bisphenol A crystal for the third time by using phenol, then performing liquid-solid separation by using a centrifugal machine, and obtaining a purer bisphenol A adduct through the processes of crystallization, washing and solid-liquid separation for 3 times; wherein a part of the mother liquor I is returned to the step (1) for reuse.
And (3) centrifugally separating to obtain crystals (adduct of phenol and bisphenol A), sending a filter cake to a melting tank, heating, melting and then entering the step (3).
And (3): evaporating and stripping the phenol from the mixture of the molten phenol and the bisphenol A by using the bisphenol A adduct obtained in the step (2) under vacuum and at higher temperature to produce high-purity bisphenol A, forming bisphenol A molten liquid, and granulating the molten liquid to obtain a bisphenol A product.
The liquid phase dephenolizing equipment in the step (3) can adopt combination equipment such as a two-stage or multi-stage falling film evaporator, a steam stripping tower and the like, the operating temperature of the falling film evaporator is 170-190 ℃, the operating pressure is-0.1 to-0.02 MPa (gauge pressure), the operating temperature of the steam stripping tower is 170-200 ℃, and the operating pressure is-0.1 to-0.05 MPa (gauge pressure).
And (4): heating a part of the mother liquor I obtained in the step (2), then feeding the heated part of the mother liquor I into an isomerization reactor, carrying out isomerization reaction under the action of a catalyst, and converting a part of by-products into bisphenol A products. And concentrating at least one part of the isomerization product in a concentration tower system, separating out concentrated solution II and low boiling point components (including phenol and the like), condensing and recovering heat through the concentration tower system, and sending concentrated heavy components (including the isomerization product) to the step (5).
Specifically, the isomerization concentration system comprises a hot water generator and a flash tank, wherein the isomerization product is concentrated in the flash tank, then the light component obtained by gas-liquid separation is recycled in the hot water generator together with other light components and low boiling point components to generate hot water at about 90 ℃, and the hot water can be used for heating reaction materials entering the condensation reactor, so that the heat is fully utilized, and the effective utilization rate of energy is improved.
The isomerization reaction temperature in the step (4) is 50-90 ℃, the operation pressure is 0.2-0.4 MPa (gauge pressure), the operation temperature of the thickener is 170-200 ℃, and the operation pressure is-0.1-0.02 MPa (gauge pressure).
And (5): crystallizing the concentrated solution II obtained in the step (4) in a crystallizer, and then carrying out solid-liquid separation to separate the concentrated solution II into a solid component and a mother solution II; wherein the solid phase is diluted by at least one part of the mother liquor generated in the step (2), and then is sent to the step (2) for crystallization and solid-liquid separation; pre-concentrating the mother liquor II, and feeding the concentrated gas-phase light component into a concentration tower in the step (4) to be condensed and recovered together with the low-boiling-point component separated in the step (4).
And (5) operating the mother liquor pre-concentration equipment at the temperature of 110-180 ℃ and at the pressure of-0.1-0.02 MPa (gauge pressure).
The mother liquor II for crystallization, purification and solid-liquid separation in the step (5) contains 2, 4-bisphenol A, trisphenol, reaction byproducts and the like, and the concentration of the impurities and the concentration of the reaction byproducts need to be controlled in a proper range so as to ensure the quality of bisphenol A products. At least part of mother liquor II after crystallization, purification and solid-liquid separation is separated to obtain a light component II and a heavy component II, and then the heavy component II is sent to the step (6) for cracking and rearrangement to remove the impurities and reaction byproducts.
And (6): and (3) sending the heavy component II pre-concentrated in the step (5) to a cracking reactor, and cracking bisphenol A and partial side reaction products into phenol, isopropenylphenol and a small amount of isopropylphenol impurities under the action of a high temperature and a catalyst. Condensing gas phase generated by the cracking reactor, carrying out rearrangement reaction in the rearrangement reactor, reacting phenol and isopropenylphenol contained in the cracking liquid under the action of a catalyst to generate bisphenol A, and accumulating other impurities at the bottom of the reaction kettle to be discharged as mixed polyphenol. And (3) carrying out secondary concentration process treatment on the rearrangement liquid obtained by the rearrangement reaction, concentrating to obtain a light component IV and a heavy component IV of a gas phase containing the isopropyl phenol, feeding the light component IV into the preconcentration tower in the step (5), and finally into a dehydration tower of a phenol recovery system, and feeding the heavy component IV of a liquid phase into the mother liquor I in the step (5) for dilution.
Specifically, the solid phase component and the heavy component IV are diluted by at least a part of the mother liquor I to form a crystallization liquid, and the crystallization liquid is returned to the crystallization process of the concentrated solution I.
In this embodiment, a cracking rearrangement product containing the isopropylphenol is subjected to a concentration process, so that the isopropylphenol generated by cracking rearrangement enters a light component iv, is separated from a heavy component iv such as bisphenol a, and the light component iv enters a phenol recovery system, and is finally discharged out of the system from a tower kettle of a phenol refining tower along with mixed polyphenol, thereby solving the problem that a cracking solution or a rearrangement solution containing the isopropylphenol directly enters a reaction system, and the service life of a catalyst is shortened. Meanwhile, the gas phase (namely the light component IV) of the rearrangement concentrated product enters a preconcentration tower (a rectifying tower), and the energy consumption of a reboiler of the tower can be reduced by the introduced heat.
The operation temperature of the cracking reactor in the step (6) is 170-210 ℃, and the operation pressure is-0.1-0.02 MPa (gauge pressure); the operating temperature of the rearrangement reactor is 50-100 ℃, and the operating pressure is 0.1-0.5 MPa (gauge pressure).
Preferably, the method further comprises a phenol recovery process in addition to the steps 1 to 6, specifically comprises two parts of phenol dehydration and purification, which are respectively carried out in a dehydration tower and a phenol purification tower. And (3) rectifying the product obtained after the reaction in the step (2) in a light component removal tower, feeding the light component obtained at the top of the tower and the low boiling point component obtained by concentrating the isomerization product in the step (4) into a dehydration tower together, simultaneously adding a fresh phenol raw material supplemented after impurity removal into the dehydration tower, dehydrating and refining the fresh phenol raw material simultaneously, and returning the dehydrated and refined fresh phenol raw material to the condensation reactor.
Directly feeding the liquid phase at the top of the dehydrating tower into an acetone recovery tower to obtain recovered acetone at the top of the tower; oil-water separation is carried out on the tower bottom product to obtain the entrainer, and the entrainer is recycled to the dehydration tower for use; the liquid phase at the bottom of the dehydration tower enters a phenol refining tower. Extracting refined phenol from the gas phase at the top of the phenol refining tower, and extracting a byproduct mixed polyphenol containing isopropyl phenol from the tower kettle; the content of the isopropylphenol in the tower kettle mixed polyphenol is controlled to be 10-30% (mass content); and the isopropylphenol in the phenol recovered at the top of the tower can be controlled to be 100-300 ppm (mass content) by adjusting the yield at the bottom of the tower and other measures.
The top gaseous phase of phenol refining tower is as steam generator's heat source, converts hot water into low pressure steam when the condensation of phenol gaseous phase, and other needs low pressure steam of supplying this embodiment use as heating medium's equipment, through heat balance back, this embodiment need not additionally provide low pressure steam, and the low pressure steam that the top of phenol refining tower produced just can satisfy the requirement, and the energy consumption of device can be reduced by a wide margin to this step.
In the step (2), the operating temperature of the light component removal tower is 100-180 ℃, and the operating pressure is-0.1-0.02 MPa (gauge pressure);
and (3) feeding the fresh phenol subjected to impurity removal reaction in the step (3) into the dehydration tower in the step (2).
The operating temperature of the dehydration tower is 110-230 ℃, and the operating pressure is 0.01-0.4 MPa (gauge pressure); the dehydration tower is azeotropic distillation, and the selected azeotropic agent can be a chemical such as toluene or ethylbenzene and the like which can form an azeotrope with water, and preferably ethylbenzene.
And (4) feeding part of the low boiling point components after the isomerization product is concentrated in the step (4) into a dehydration tower in the phenol dehydration recovery process, and returning part of the low boiling point components to the step (5) for rearrangement reaction.
The purity of the bisphenol A product finally obtained in the embodiment is more than or equal to 99.93 percent (mass percent), the freezing point is 156.7-156.8 ℃, the phenol content is 20ppm (mass content), the water content is 500ppm (mass content), and the ash content is 1ppm (mass content).
Example 2:
a process for the preparation of bisphenol a comprising the steps of:
step (1): under the action of a strong acid cation exchange resin catalyst, 7.9kg/h of acetone and 25.15kg/h of supplemented phenol raw material, 64.78kg/h of mother liquor I separated in the subsequent crystallization step, and 38kg/h of a mixture of phenol and bisphenol A returned in the subsequent isomerization step are mixed and then enter a reactor for condensation reaction to generate bisphenol A, and 135.83kg/h of a reaction mixed solution of bisphenol A, unreacted raw materials and a small amount of impurities is obtained.
Step (2): rectifying and concentrating the reaction liquid obtained in the step (1) in a light component removal tower, removing 16.35kg/h of low boiling point components such as acetone, water and phenol and the like, and recovering in a dehydration tower of a raw material recovery system, thus obtaining 119.48kg/h of concentrated liquid at the tower bottom. Crystallizing the concentrated solution I to generate a crystal of an adduct of bisphenol A, cleaning and filtering the crystal, and repeating the processes of crystallization, cleaning and filtering for 3 times; through the crystallization solid-liquid separation process, purer bisphenol A adduct can be obtained; wherein a part of 64.78kg/h of the mother liquor I is returned to the step (1) for reuse.
And (3): and (3) carrying out liquid phase dephenolization on the bisphenol A adduct obtained in the step (2), removing phenol to form bisphenol A molten liquid, and granulating the molten liquid to obtain 15.15kg/h of bisphenol A product.
And (4): carrying out isomerization reaction on 50kg/h of the mother liquor I obtained in the step (2), concentrating 12kg/h of an isomerization product in an isomerization concentration system, introducing a gas-phase low-boiling-point component obtained by evaporation and a gas-phase light component II pre-concentrated in the step (5) together into the isomerization concentration system, separating 16.383kg/h of the low-boiling-point component, mostly consisting of phenol, and removing the phenol from a phenol recovery system after condensation and recovery; the concentrated solution after concentration is 6.643kg/h of an isomerized product and goes to the step (5).
And (5): crystallizing and carrying out solid-liquid separation on the concentrated solution II obtained in the step (4), wherein a solid phase is washed and diluted by using at least one part 6.477kg/h of mother liquor generated in the step (2), and the finally separated solid phase mainly comprises crude bisphenol A crystals and 7.56kg/h of phenol, and then feeding the crystals to the step (2) for solid-liquid separation; 5.65kg/h of mother liquor II as a separated liquid phase enters a preconcentration tower, preconcentration is carried out together with 5.19kg/h of gas-phase light components IV generated by the concentration of the rearrangement product in the step (6), 11.03kg/h of gas-phase light components at the top of the preconcentration tower enter an isomerization concentration system in the step (4) to be condensed with the low-boiling-point components separated in the step (4) and heat is recovered.
And (6): cracking and rectifying 1.37kg/h of heavy components at the bottom of the preconcentration tower in the step (5), diluting and refluxing the heavy components with 5.009kg/h of phenol separated by concentration in the step (4), generating 0.449kg/h of mixed polyphenol by-products at the bottom of the cracking tower, feeding 5.93kg/h of pyrolysis liquid at the top of the cracking and rectifying tower into a rearrangement reactor for rearrangement, concentrating the rearrangement products to obtain 5.19kg/h of gas phase containing the isopropylphenol, feeding the gas phase into the preconcentration tower in the step (5), and feeding 0.74kg/h of liquid phase heavy components into the crystallization liquid prepared in the step (5).
Preferably, the method further comprises a phenol recovery step in addition to the steps 1 to 6: concentrating the product obtained after the reaction in the step (2) in a light component removal tower, wherein the light component obtained at the top of the tower is 7.56kg/h and 9.818kg/h obtained by concentrating the isomerization product in the step (4) are sent to a dehydration tower together; the gas phase at the top of the dehydrating tower directly enters an acetone recovery tower, the recovered acetone is obtained at the top of the tower at a rate of 1.89kg/h, and the azeotropic agent mainly containing ethylbenzene is obtained after oil-water separation of the product at the bottom of the tower and is recycled to the dehydrating tower for use; the liquid phase at the tower bottom of the dehydration tower enters a phenol refining tower, 44.12kg/h of refined phenol is extracted from the gas phase at the tower top, 0.023kg/h of mixed polyphenol containing isopropyl phenol is extracted from the tower bottom, wherein the content of isopropyl phenol in the refined phenol at the tower top is 160ppm (mass content); the content of isopropylphenol in the tower bottom mixed polyphenol is 20 percent (mass content).
Preferably, in addition to the steps, 25.15kg/h of fresh phenol subjected to impurity removal reaction is returned to the dehydration tower in the phenol dehydration recovery process.
Preferably, 9.818kg/h of the low boiling point components 16.383kg/h after isomerization in step (4) are fed to the dehydration column of the phenol recovery process, another part of 5.009kg/h is fed to the rearrangement reaction in step (5), and the rest is fed to the preconcentration column in step (5) at 1.566 kg/h.
By this example, the cumene content in the condensation reactor in the step (1) was 0.18% (. ltoreq.0.21%), the purity of the finally obtained bisphenol A product was 99.93% (by mass), the phenol content was 20ppm, and the ash content was 1 ppm.
Example 3:
this example uses the process for making bisphenol a of example 1, which is data for a condensation reactor catalyst used at 13 months.
Under the action of a strong acid cation exchange resin catalyst, 79kg/h acetone and 252kg/h supplementary phenol, 648kg/h mother liquor separated in the subsequent crystallization step, and 380kg/h mixture of phenol and bisphenol A returned in the subsequent isomerization step are mixed and then enter a condensation reactor, and the composition (mass percentage) of materials at the inlet of the reactor is as follows: the phenol content was 78.61%, the bisphenol a content was 9.60%, the acetone content was 4.49%, the 2,4 bisphenol a content was 2.37%, the isopropyl phenol content was 0.18%, and the other impurities and heavy components content was 4.75%. The mixture enters a condensation reactor, and is subjected to condensation reaction under the action of a catalyst to generate bisphenol A, so that 1359kg/h of a reaction solution of bisphenol A, unreacted raw materials and a small amount of impurities is obtained. The composition (mass percent) of the after-reaction liquid is as follows: the phenol content was 66.14%, the bisphenol a content was 24.6%, the acetone content was 0.67%, the 2,4 bisphenol a content was 2.67%, the isopropyl phenol content was 0.18%, the other impurities and heavy components content was 5.74%, and the condensation reaction acetone conversion was 85%.
As can be seen from example 3: after the method is adopted, the content of the isopropyl phenol in the condensation reactor is lower and is only 0.18%, the influence of the isopropyl phenol on the activity of the strong-acid cation exchange resin catalyst is reduced, after the condensation reactor is operated for 13 months according to the process flow and the process conditions in the embodiment of the invention patent, the activity of the condensation reactor catalyst can still keep a higher level, the acetone conversion rate is 85% and is still higher than the designed value of the acetone conversion rate of the condensation reactor by 80%, the service life of the catalyst can be prolonged, and the operation cost of the device can be reduced.
Comparative example
In the comparative example, the method for preparing bisphenol a in the prior art is adopted, and the method is compared with the example 3, in the prior art, the cracking heavy-discharge liquid is directly returned to the condensation reaction system, the steps of concentrating the cracking rearrangement reaction liquid, introducing isopropyl phenol into a low-boiling-point component, separating the isopropyl phenol from heavy components such as bisphenol a and the like are lacked, and the like. The data for the condensation reactor catalyst at 13 months of use were compared to example 3 under prior art operating conditions.
Under the action of a strong acid cation exchange resin catalyst in a condensation reactor, 79kg/h acetone and 252kg/h supplementary phenol, 648kg/h mother liquor separated in the subsequent crystallization step and 380kg/h mixture returned by the subsequent cracking rearrangement procedure are mixed and then enter the condensation reactor, and the composition (mass percentage) of materials at the inlet of the condensation reactor is as follows: the phenol content was 78.23%, the bisphenol a content was 9.46%, the acetone content was 4.11%, the 2,4 bisphenol a content was 2.83%, the isopropyl phenol content was 0.40%, and the content of other impurities or heavy components was 4.97%. The mixture enters a condensation reactor, and is subjected to condensation reaction under the action of a catalyst to generate bisphenol A, so that 1359kg/h of a reaction solution of bisphenol A, unreacted raw materials and a small amount of impurities is obtained. The composition (mass percent) of the after-reaction liquid is as follows: the phenol content was 68.91%, the bisphenol a content was 19.07%, the acetone content was 1.23%, the 2,4 bisphenol a content was 2.99%, the isopropyl phenol content was 0.40%, the content of other impurities or heavy components was 7.4%, and the condensation reaction acetone conversion was 70%.
By adopting the comparative example, after the cumene phenol is produced in the cracking process, the cumene phenol enters low boiling point components due to lack of cracking rearrangement reaction liquid concentration, and is separated from bisphenol A and other heavy components. The isopropyl phenol generated by cracking directly enters a condensation reaction system, so that the content of isopropyl phenol in a reactor is high, the activity of the catalyst is influenced, the conversion rate of acetone to bisphenol A is reduced, the content of impurities in a reaction product is high, and the service life of the catalyst is shortened. The content of isopropyl phenol in the returned medium condensation reactor in the comparison example is 0.40%, after the process of the comparison example is operated for 13 months, the activity of the condensation reactor catalyst is greatly reduced, the acetone conversion rate is reduced to 70%, the acetone conversion rate is lower than the designed value of the acetone conversion rate of the condensation reactor by 80%, the contents of impurities and heavy components in the reaction product are high, the catalyst cannot meet the process requirements, and a new condensation reaction catalyst needs to be replaced; the condensation reactor according to the invention in example 3 has a content of cumene phenol of 0.18%, and after 13 months of operation according to the preparation method and the process conditions in the technology of the invention, the activity of the condensation reactor catalyst can still be kept at a high level, the acetone conversion is 85%, and the catalyst can still be used continuously.
The results of the examples and the comparative examples show that the invention adopts the steps of cracking-rearrangement reaction, and then the rearrangement solution after rearrangement reaction is concentrated, so that the isopropylphenol enters the light component with low boiling point to realize the separation with the heavy components such as bisphenol A, and the concentrated solution after cracking rearrangement reaction returns to the condensation reaction system again, thereby reducing the content of the isopropylphenol in the condensation reactor, reducing the influence of the isopropylphenol on the activity of the catalyst and prolonging the service life of the catalyst.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A method for reducing isopropylphenol in a reaction system for preparing bisphenol A is characterized in that at least one part of reaction liquid after excessive phenol and acetone are subjected to condensation reaction in a condensation reactor by a catalyst is subjected to isomerization-cracking-rearrangement to obtain heavy drainage liquid, and the heavy drainage liquid containing isopropylphenol is subjected to concentration process treatment, so that the isopropylphenol enters a phenol recovery system and is separated from the phenol along with mixed polyphenol; the mass percentage content of the isopropyl phenol in the condensation reactor is less than or equal to 0.25 percent.
2. The method for reducing cumene phenol in a reaction system for the production of bisphenol a according to claim 1, wherein said reacted liquid obtained by condensation reaction of excess phenol and acetone in the presence of a catalyst is concentrated to obtain a light component (i) and a concentrated liquid (i), said concentrated liquid (i) is subjected to a crystallization step and subjected to solid-liquid separation to obtain a bisphenol a adduct and a mother liquor (i);
at least one part of the mother liquor (I) is subjected to isomerization reaction to obtain an isomerization product, and at least one part of the isomerization product is subjected to a primary concentration process to obtain a concentrated solution (II) and a low-boiling-point component; crystallizing and filtering the concentrated solution (II) to obtain a solid phase component and a mother solution (II), and pre-concentrating the mother solution (II) to obtain a heavy component (II) and a light component (II); adding alkali into the heavy component (II) for cracking, carrying out rearrangement reaction on a light component (III) generated by cracking to obtain heavy liquid, and carrying out secondary concentration process treatment on the heavy liquid to obtain a heavy component (IV) and a light component (IV);
the light component (IV) containing the isopropylphenol enters the phenol recovery system and is removed together with the mixed polyphenol; the mass percentage content of the isopropyl phenol in the removed mixed polyphenol is 10-30%.
3. The method for reducing cumene phenol in a reaction system for the production of bisphenol a as recited in claim 2, wherein said solid phase component and said heavy component (iv) are diluted with at least a portion of said mother liquor (i) to form a crystallized liquid, and said crystallized liquid is returned to said step of crystallizing said concentrated liquid (i).
4. The process for producing bisphenol A as claimed in claim 2, wherein said light component (IV) is passed through a preconcentration column, returned to said isomerization concentration system together with said light component (II), mixed with a low boiling component, condensed and heat recovered, and introduced into said phenol recovery system for dephenolation.
5. The method for reducing cumene phenol in a reaction system for producing bisphenol A according to any one of claims 1 to 4, wherein said phenol recovery system comprises a dehydration column and a phenol purification column, and at least a part of said light component (II), said light component (IV) and said low boiling point component is fed to said dehydration column after being mixed in said isomerization concentration system, condensed and heat recovered; and the gas phase at the top of the dehydrating tower enters an acetone recovery tower, the liquid phase in the tower kettle of the dehydrating tower enters the phenol refining tower, the refined phenol is extracted from the gas phase at the top of the phenol refining tower, and the mixed polyphenol containing the isopropyl phenol is discharged from the tower kettle.
6. The method for reducing cumene phenol in a reaction system for the production of bisphenol a according to claim 5, wherein the phenol raw material supplemented in the condensation reaction is purified and then transferred to said dehydration column for dehydration, and further purified in said phenol purification column to obtain purified phenol, which is then transferred to said condensation reactor.
7. The method for reducing cumene phenol in a reaction system for the production of bisphenol a as recited in claim 5, wherein said phenol recovery system further comprises an acetone recovery column, wherein acetone is recovered from the top of said acetone recovery column, and the bottom product is subjected to oil-water separation to obtain an azeotropic agent mainly comprising ethylbenzene, which is recycled to said dehydration column for reuse.
8. The method of claim 7 for reducing cumene phenol in a reaction system for the production of bisphenol a comprising at least the steps of:
(1) and (3) catalytic reaction: under the action of a strong acid cation exchange resin catalyst, carrying out condensation reaction on excessive phenol and acetone to generate bisphenol A, and obtaining bisphenol A and a reaction solution of unreacted raw materials and a small amount of impurities;
(2) concentration and liquid separation: concentrating the reverse solution obtained in the step (1) to obtain a light component (I) and a concentrated solution (I), and carrying out solid-liquid separation on the concentrated solution after crystallization to obtain a bisphenol A adduct and a mother solution (I); dephenolizing the bisphenol A adduct to obtain a bisphenol A product;
(3) isomerization: at least one part of the mother liquor (I) obtained in the step (2) is subjected to isomerization reaction, part of the isomerized reaction liquid is returned to the condensation reactor, and part of the isomerized reaction liquid is injected into an isomerization concentration system to be subjected to primary concentration process treatment, so that concentrated liquid (II) and low-boiling-point components are obtained;
(4) pre-concentration: crystallizing and filtering the concentrated solution (II) obtained in the step (3) to obtain a solid phase component and a mother solution (II), and pre-concentrating the mother solution (II) in a pre-concentration tower to obtain a heavy component (II) and a light component (II);
returning the light component (II) to the isomerization concentration system;
(5) splitting and rearranging: carrying out alkaline cracking on the heavy component (II) in the step (4), condensing a light component (III) generated by cracking, carrying out rearrangement reaction to obtain a rearrangement liquid containing isopropyl phenol, and carrying out secondary concentration process treatment on heavy discharge liquid to obtain a heavy component (IV) and a light component (IV); introducing a light component (IV) containing isopropyl phenol into a phenol recovery system, and removing the light component (IV) and mixed polyphenol together; the mass percentage content of the isopropyl phenol in the removed mixed polyphenol is 10-30 percent;
diluting the solid phase component and the heavy component (IV) by at least part of the mother liquor (I) in the step (4) to form a crystallization liquid, and returning the crystallization liquid to the crystallization process of the concentrated solution (I);
(6) and (3) recovering phenol: feeding at least a portion of said low boiling components of step (3) to said dehydration column; meanwhile, the light component (IV) returns to the pre-concentration tower, and is mixed with the low boiling point component in the isomerization concentration system together with the light component (II), condensed and recycled, and then enters the dehydration tower together;
gas phase at the top of the dehydrating tower enters an acetone recovery tower to obtain recovered acetone, and oil-water separation is carried out on a product at the bottom of the dehydrating tower to obtain an azeotropic agent mainly containing ethylbenzene; the liquid phase in the tower kettle of the dehydration tower enters a phenol refining tower, the gas phase at the tower top of the phenol refining tower is condensed and the recovered heat is refined recovered phenol, and the refined recovered phenol can be returned to the condensation reactor; discharging mixed polyphenol containing isopropyl phenol from the tower kettle;
the mass percentage content of the isopropyl phenol in the condensation reactor is less than or equal to 0.25 percent after the steps.
9. The method for reducing cumene phenol in a reaction system for the production of bisphenol a of claim 8 further comprising the steps of melting and pelletizing: and (3) carrying out liquid phase dephenolization on the bisphenol A adduct obtained in the step (2), removing phenol, forming bisphenol A molten liquid, and granulating the molten liquid to obtain a bisphenol A product.
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