CN106866379B - Method for preparing phenol acetone by CHP (CHP) through reactive distillation decomposition - Google Patents
Method for preparing phenol acetone by CHP (CHP) through reactive distillation decomposition Download PDFInfo
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- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/08—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by decomposition of hydroperoxides, e.g. cumene hydroperoxide
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Abstract
The invention relates to a method for preparing phenol acetone by performing reactive distillation decomposition on CHP (CHP), which mainly solves the problems of low product selectivity, high investment and large occupied area in the prior art. The invention adopts a method for preparing phenol acetone by CHP (CHP) through reactive distillation decomposition, wherein a CHP raw material containing 25-80 wt% is fed into a reactive distillation tower for decomposition reaction to generate phenol acetone, and the catalyst is in a flowing state by utilizing the reaction heat to gasify and boil the material so as to keep high activity; meanwhile, the acetone product is rectified and separated, so that the selectivity of phenol is improved to 99.35-99.55%, the selectivity of acetone is improved to 99.25-99.45%, and the purity of the acetone product is more than or equal to 99.9 wt%.
Description
Technical Field
The invention relates to a method for preparing phenol acetone by CHP through reactive distillation decomposition.
Background
Phenol and acetone are basic organic chemical raw materials with wide application, and the market demand is very vigorous at home and abroad. The phenol-acetone device for producing phenol-acetone firstly adopts cumene raw material and air to prepare cumene hydroperoxide CHP in an oxidation reaction tower, then the CHP is decomposed under the action of catalyst to generate phenol and acetone, and finally phenol products and acetone products are obtained by rectification, separation, refining and purification.
The patent application No. CN201210512571.4 in the prior art is used for a novel reaction rectification process for producing phenol and acetone, and discloses that three processes of CHP decomposition, cumene separation and phenol crude separation are coupled to a rectification tower, so that the reaction heat utilization rate is improved. Patent application No. CN201410337795.5 discloses a method for decomposing phenol/acetone by cumene hydroperoxide, which adopts fine-particle-size solid acid as a catalyst, adopts a multistage series reaction kettle, and further controls the conversion rate and temperature rise by controlling the reaction temperature, the catalyst dosage and the residence time. Patent application No. CN201510026002.2 discloses a reactive distillation method for preparing methyl chloroacetate, which adopts a reactive distillation tower to carry out gas-liquid-solid three-phase reaction, and has the advantages of simple flow, reduced investment, reduced energy consumption, high conversion rate and high selectivity. Patent application No. CN201510654488.4 discloses a method for preparing phenol acetone by adopting a moving bed reactor, in which CHP raw material enters the top of the moving bed reactor, contacts with a solid catalyst to generate decomposition reaction and release heat in a large amount, and liquid phase acetone is evaporated into vapor phase acetone and is discharged from the top of the moving bed reactor so as to improve the selectivity of phenol and acetone.
In the prior art, the patent application number CN201210512571.4 is only a method for preparing phenol acetone in a laboratory scale, 2 rectifying tower systems are required to be arranged, and the problems of large equipment quantity, high engineering investment, large occupied area and the like exist; moreover, in large-scale industrial applications, there is a problem of "amplification effect"; meanwhile, liquid-phase cumene and CHP enter the reactor together, the cumene is gasified and then flows out from the gas phase at the top of the reaction rectifying tower, and then flows out from the liquid phase at the bottom of the acetone rectifying tower after being condensed, so that the problem of high energy consumption is solved. Patent application No. CN201410337795.5 has that reaction equipment area is big, and the control process is complicated, especially the reaction later stage, and catalyst activity descends, and phenol acetone's selectivity further descends, and the accessory substance increases, and main product yield descends scheduling problem. The patent application No. CN201510026002.2 is only a method for preparing methyl chloroacetate products, the heating temperature of a tower kettle is 100-140 ℃, and phenol acetone products cannot be prepared. Patent application No. 201510654488.4 removes the reaction heat through acetone gasification-condensation, and acetone is only used for heat transfer process, and liquid phase acetone flows out from the reactor tower cauldron, is unfavorable for CHP decomposition reaction to generate phenol acetone product, and similarly, there are the equipment quantity many, and the engineering investment is high, and area is big scheduling problem.
Disclosure of Invention
The invention aims to solve the technical problems of low product selectivity, high investment and large occupied area in the prior art, and provides a novel method for preparing phenol acetone by performing reactive distillation decomposition on CHP. The method has the advantages of high product selectivity, low investment and small occupied area.
In order to solve the problems, the technical scheme adopted by the invention is as follows: a method for preparing phenol acetone by CHP through reactive distillation decomposition, cumene hydroperoxide CHP raw material (11) enters a reactive distillation tower (1), enters a reaction section at the lower part of the reactive distillation tower (1) along with gravity flow to contact with a solid catalyst, CHP decomposition reaction is carried out to generate phenol acetone and generate a large amount of reaction heat, all liquid phase acetone, a small amount of raw material CHP and a small amount of cumene are evaporated into gas phase and discharged from the upper part of the reaction section, liquid phase material without acetone is led out from the lower part of the reaction section of the reactive distillation tower (1), heat exchange is carried out with circulating cooling water in an intercooler and decomposition reaction heat is removed, liquid phase phenol product and unreacted raw material CHP and cumene (15) flow out of the tower bottom of the reactive distillation tower (1); gas-phase materials discharged from the reaction section of the reaction rectifying tower (1) enter the rectifying section at the upper part of the reaction rectifying tower (1) to be in gas-liquid contact, high-purity acetone materials (12) are obtained at the top of the reaction rectifying tower (1), and are condensed by a condenser (2) at the top of the tower, one part of liquid-phase acetone is taken as a product (14) to be sent out, and the other part of liquid-phase acetone is taken as reflux liquid (13) to return to the reaction rectifying tower (1) so as to keep the gas-liquid contact of the rectifying section.
In the above technical scheme, preferably, the catalyst is a resin catalyst, a macroporous styrene ion exchange resin polymerization production process is adopted, a (meth) acrylic fluoroalkyl ester monomer and phenol are added to participate in polymerization, and the catalyst is prepared by sulfonation, wherein the (meth) acrylic fluoroalkyl ester monomer is hexafluorobutyl acrylate, dodecafluoroheptyl acrylate and/or tridecafluoroctyl acrylate.
In the above technical solution, preferably, the process parameters of the reaction section of the reactive distillation column are as follows: the operation temperature is 75-100 ℃, the operation pressure is 110-195 kPaA, and the equipment parameters of the reaction section of the reactive distillation tower are as follows: the length-diameter ratio is 16: and 1, filling n sections of solid catalyst beds in the reaction section, wherein n is 1-12.
In the above technical solution, more preferably, the process parameters of the reaction section of the reactive distillation column are as follows: the operation temperature is 80-95 ℃, the operation pressure is 125-180 kPaA, and the equipment parameters of the reaction section of the reactive distillation tower are as follows: the length-diameter ratio is 6: and 1, filling n sections of solid catalyst beds in the reaction section, wherein n is 2-11.
In the above technical solution, most preferably, the process parameters of the reaction section of the reactive distillation column are as follows: the operation temperature is 85-90 ℃; the operating pressure is 140-165 kPaA; the parameters of the reaction section equipment of the reactive distillation tower are as follows: the length-diameter ratio is 2: 1; and n sections of solid catalyst bed layers are filled in the reaction section, wherein n is 2-10.
In the above technical scheme, preferably, the process parameters of the rectifying section of the reactive rectifying tower are as follows: the operation temperature is 45-70 ℃, the operation pressure is 68-156 kPaA, the reflux ratio is 0.55-0.95, the number of the rectification tower plates is 40-48, and the position of the feed plate is 38-46 tower plates from top to bottom.
In the above technical solution, more preferably, the process parameters of the rectifying section of the reactive rectifying tower are as follows: the operation temperature is 50-65 ℃, and the operation pressure is 83-141 kPaA.
In the above technical solution, most preferably, the process parameters of the rectifying section of the reactive rectifying tower are as follows: the operation temperature is 55-60 ℃; the operation pressure is 98-126 kPaA.
In the above technical scheme, preferably, each section of catalyst bed layer of the reaction section of the reactive distillation column is provided with a channel interconnected with the catalyst regeneration system, and the catalyst in a flowing state can realize online regeneration and online replacement.
On a large-scale commercial phenol-acetone production device, 25-80 wt% of CHP raw material is fed into a reaction rectifying tower for decomposition reaction to generate phenol-acetone, and the material is gasified and boiled by utilizing reaction heat to enable a catalyst to be in a flowing state so as to keep high activity; and simultaneously, rectifying and separating the acetone product. Therefore, the selectivity of phenol is improved to 99.35-99.55%, the selectivity of acetone is improved to 99.25-99.45%, the purity of acetone products is more than or equal to 99.9 wt%, and a good technical effect is achieved.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention.
In the figure 1, a reaction rectifying tower, 2, an overhead condenser, 3, an intercooler, 4, an intercooler, 5, an intercooler, 11, a liquid phase CHP raw material, 12, gas phase overhead acetone, 13, a liquid phase acetone reflux, 14, a liquid phase acetone product and 15, a liquid phase tower bottom material.
The present invention will be further illustrated by the following examples, but is not limited to these examples.
Detailed Description
Comparative example 1
In the prior art, the phenol-acetone production device firstly carries out decomposition reaction on CHP raw materials under the action of a catalyst to generate phenol and acetone, and then the phenol product and the acetone product are obtained by rectification, separation, refining and purification. Therefore, 2 CHP decomposition reactors and 2 acetone rectifying towers are required, the number of the devices is large, the engineering investment is high, and the occupied area is large.
[ example 1 ]
A method for preparing phenol acetone by CHP through reactive distillation decomposition is shown in figure 1, taking the example of filling 3 sections of solid catalyst bed layers, cumene hydroperoxide CHP raw material (11) enters a reactive distillation tower (1) from the middle part, enters a reaction section along with gravity flow to contact with a solid catalyst, generates a CHP decomposition reaction to generate phenol acetone and generate a large amount of reaction heat, and all liquid phase acetone, a small amount of raw material CHP and a small amount of cumene are evaporated into a gas phase and discharged from the upper part of the reaction section; the liquid phase material without acetone is led out from the lower part of the reaction section of the reactive distillation column (1), and is subjected to heat exchange with circulating cooling water and removal of decomposition reaction heat in an intercooler (3), an intercooler (4) and an intercooler (5), and liquid phase phenol products, unreacted raw materials CHP and isopropyl benzene (15) flow out of the bottom of the reactive distillation column (1). Gas-phase materials discharged from the reaction section of the reaction rectifying tower (1) enter the rectifying section of the reaction rectifying tower (1) to be in gas-liquid contact, the materials are separated in a mass transfer mode, the acetone content in the gas-phase materials is gradually increased, high-purity acetone materials (12) are obtained at the top of the reaction rectifying tower (1), and are condensed by a tower top condenser (2), one part of liquid-phase acetone is taken as a product (14) to be sent out, and the other part of liquid-phase acetone is taken as reflux liquid (13) to return to the reaction rectifying tower (1) so as to keep the gas-liquid contact of the rectifying section.
Taking a production scale phenol acetone device of 10 ten thousand tons/year as an example, the method for preparing phenol acetone by using the reaction, rectification and decomposition CHP integrates a moving bed reactor filled with a solid catalyst and a rectification tower for separating materials into a reaction rectification tower (1), thereby reducing the number of equipment, reducing the engineering investment and reducing the occupied area.
Cumene Hydroperoxide (CHP) raw material (11) enters a reaction rectifying tower (1) from the middle part and enters a reaction section along with gravity flow to contact with a catalyst to react to generate phenol acetone and generate reaction heat, and all the acetone, a small amount of CHP and a small amount of cumene are evaporated into a gas phase and are discharged from the upper part of the reaction section; the liquid phase material without acetone is led out from the lower part of the reaction section, and exchanges heat with circulating cooling water in an intermediate cooler and removes reaction heat, and liquid phase phenol products, unreacted CHP and isopropyl benzene (15) flow out from the tower bottom of the reactive distillation tower. And (3) the gas-phase material discharged from the reaction section enters a rectification section, the material is subjected to mass transfer separation, the acetone content in the gas-phase material is gradually increased, a high-purity acetone material (12) is obtained at the top of the reaction rectification tower, and is condensed by a condenser (2) at the top of the tower, one part of acetone is taken as a product (14) to be sent out, and the other part of acetone is taken as a reflux liquid (13) to return to the reaction rectification tower. The CHP feedstock composition was as follows:
the technological parameters are as follows: the operation temperature of the reaction section of the reactive distillation tower is 82 ℃, and the operation pressure is 132 kPaA; the length-diameter ratio of the reactor is 6: 1, filling 4 sections of catalyst in the reactor. The catalyst is a resin catalyst, a macroporous styrene ion exchange resin polymerization production process is adopted, fluoroalkyl (meth) acrylate monomers and phenol are added to participate in polymerization, and the catalyst is prepared by sulfonation, wherein: the fluoroalkyl (meth) acrylate monomer is hexafluorobutyl acrylate. The operation temperature of the rectifying section of the reactive rectifying tower is 53 ℃, the operation pressure is 98kPaA, and the reflux ratio is 0.71; the number of the rectifying trays is 46, and the position of the feed plate is 44 trays from top to bottom.
Thus, the selectivity to phenol was 99.50%, the selectivity to acetone was 99.35%, and the purity of the acetone product was 99.91 wt%. Compared with the comparative example 1, the number of the devices is reduced from 2 to 1, the engineering investment is reduced to 75 percent, and the occupied area is reduced to 50 percent.
[ example 2 ]
According to the conditions and the steps described in the example 1, except that the production scale of the phenol-acetone device is changed to 20 ten thousand tons/year, the method for preparing phenol-acetone by using the reactive distillation decomposition CHP of the invention has the following process parameters: the operation temperature of the reaction section of the reactive distillation tower is 82 ℃, and the operation pressure is 132 kPaA; the length-diameter ratio of the reactor is 6: 1, filling 4 sections of catalyst in the reactor. The operation temperature of the rectifying section of the reactive rectifying tower is 53 ℃, the operation pressure is 98kPaA, and the reflux ratio is 0.71; the number of the rectifying trays is 46, and the position of the feed plate is 44 trays from top to bottom.
Thus, the selectivity to phenol was 99.50%, the selectivity to acetone was 99.35%, and the purity of the acetone product was 99.91 wt%. Compared with the comparative example 1, the number of the devices is reduced from 2 to 1, the engineering investment is reduced to 74 percent, and the occupied area is reduced to 50 percent.
[ example 3 ]
According to the conditions and the steps described in the embodiment 1, the method for preparing the phenol acetone by using the reactive distillation decomposition CHP has the following process parameters, except that the production scale of the phenol acetone device is changed to 35 ten thousand tons/year: the operation temperature of the reaction section of the reactive distillation tower is 82 ℃, and the operation pressure is 132 kPaA; the length-diameter ratio of the reactor is 6: 1, filling 4 sections of catalyst in the reactor. The operation temperature of the rectifying section of the reactive rectifying tower is 53 ℃, the operation pressure is 98kPaA, and the reflux ratio is 0.71; the number of the rectifying trays is 46, and the position of the feed plate is 44 trays from top to bottom.
Thus, the selectivity to phenol was 99.45%, the selectivity to acetone was 99.30%, and the purity of the acetone product was 99.91 wt%. Compared with the comparative example 1, the number of the devices is reduced from 2 to 1, the engineering investment is reduced to 72 percent, and the occupied area is reduced to 50 percent.
[ example 4 ]
According to the conditions and the steps described in the embodiment 1, the method for preparing the phenol acetone by using the reactive distillation decomposition CHP has the following process parameters, except that the production scale of the phenol acetone device is changed to 40 ten thousand tons/year: the operation temperature of the reaction section of the reactive distillation tower is 82 ℃, and the operation pressure is 132 kPaA; the length-diameter ratio of the reactor is 6: 1, filling 4 sections of catalyst in the reactor. The operation temperature of the rectifying section of the reactive rectifying tower is 53 ℃, the operation pressure is 98kPaA, and the reflux ratio is 0.71; the number of the rectifying trays is 46, and the position of the feed plate is 44 trays from top to bottom.
Thus, the selectivity to phenol was 99.45%, the selectivity to acetone was 99.30%, and the purity of the acetone product was 99.91 wt%. Compared with the comparative example 1, the number of the devices is reduced from 2 to 1, the engineering investment is reduced to 72 percent, and the occupied area is reduced to 50 percent.
[ example 5 ]
According to the conditions and the steps described in the example 1, except that the production scale of the phenol-acetone device is changed to 60 ten thousand tons/year, the method for preparing phenol-acetone by using the reactive distillation decomposition CHP of the invention has the following process parameters: the operation temperature of the reaction section of the reactive distillation tower is 82 ℃, and the operation pressure is 132 kPaA; the length-diameter ratio of the reactor is 6: 1, filling 4 sections of catalyst in the reactor. The operation temperature of the rectifying section of the reactive rectifying tower is 53 ℃, the operation pressure is 98kPaA, and the reflux ratio is 0.71; the number of the rectifying trays is 46, and the position of the feed plate is 44 trays from top to bottom.
Thus, the selectivity to phenol was 99.45%, the selectivity to acetone was 99.30%, and the purity of the acetone product was 99.91 wt%. Compared with the comparative example 1, the number of the devices is reduced from 2 to 1, the engineering investment is reduced to 70 percent, and the occupied area is reduced to 50 percent.
[ example 6 ]
According to the conditions and steps described in example 3, the production scale of the phenol acetone plant is still 35 ten thousand tons/year, only the process operating conditions are changed, the CHP is prepared by the method for preparing phenol acetone by using the reactive distillation decomposition of CHP, and the CHP raw material composition is as follows:
the technological parameters are as follows: the operation temperature of the reaction section of the reactive distillation tower is 75 ℃, and the operation pressure is 110 kPaA; the length-diameter ratio of the reactor is 2: 1, filling 1 section of catalyst in the reactor. The catalyst is a resin catalyst, a macroporous styrene ion exchange resin polymerization production process is adopted, fluoroalkyl (meth) acrylate monomers and phenol are added to participate in polymerization, and the catalyst is prepared by sulfonation; wherein: the (methyl) acrylic fluoroalkyl ester monomer is acrylic dodecafluoro heptyl ester. The operating temperature of the rectifying section of the reactive rectifying tower is 45 ℃, the operating pressure is 68kPaA, and the reflux ratio is 0.55; the number of the rectifying trays is 48, and the position of the feed plate is the 46 th tray from top to bottom.
Thus, the selectivity to phenol was 99.35%, the selectivity to acetone was 99.25%, and the purity of the acetone product was 99.92 wt%. Compared with the comparative example 1, the number of the devices is reduced from 2 to 1, the engineering investment is reduced to 73 percent, and the occupied area is reduced to 50 percent.
[ example 7 ]
According to the conditions and steps described in example 3, the production scale of the phenol acetone plant is still 35 ten thousand tons/year, only the process operating conditions are changed, the CHP is prepared by the method for preparing phenol acetone by using the reactive distillation decomposition of CHP, and the CHP raw material composition is as follows:
the technological parameters are as follows: the operation temperature of the reaction section of the reactive distillation tower is 100 ℃, and the operation pressure is 195 kPaA; the length-diameter ratio of the reactor is 16: 1, filling 12 sections of catalyst in the reactor. The catalyst is a resin catalyst, a macroporous styrene ion exchange resin polymerization production process is adopted, fluoroalkyl (meth) acrylate monomers and phenol are added to participate in polymerization, and the catalyst is prepared by sulfonation; wherein: the (methyl) acrylic acid fluoroalkyl ester monomer is tridecafluorooctyl acrylate. The operation temperature of the rectifying section of the reactive rectifying tower is 70 ℃, the operation pressure is 156kPaA, and the reflux ratio is 0.95; the number of the rectifying trays is 40, and the position of the feed plate is 38 trays from top to bottom.
Thus, the selectivity to phenol was 99.55%, the selectivity to acetone was 99.45%, and the purity of the acetone product was 99.92 wt%. Compared with the comparative example 1, the number of the devices is reduced from 2 to 1, the engineering investment is reduced to 73 percent, and the occupied area is reduced to 50 percent.
Claims (5)
1. A method for preparing phenol acetone by CHP through reactive distillation decomposition, cumene hydroperoxide CHP raw material (11) enters a reactive distillation tower (1), enters a reaction section at the lower part of the reactive distillation tower (1) along with gravity flow to contact with a solid catalyst, CHP decomposition reaction is carried out to generate phenol and acetone and generate a large amount of reaction heat, all liquid phase acetone, a small amount of raw material CHP and a small amount of cumene are evaporated into gas phase and discharged from the upper part of the reaction section, liquid phase material without acetone is led out from the lower part of the reaction section of the reactive distillation tower (1), heat exchange is carried out with circulating cooling water in an intercooler and the decomposition reaction heat is removed, liquid phase phenol product and unreacted raw material CHP and cumene (15) flow out from the bottom of the reactive distillation tower (1); gas-phase materials discharged from the reaction section of the reactive rectifying tower (1) enter a rectifying section at the upper part of the reactive rectifying tower (1) to be in gas-liquid contact, high-purity acetone materials (12) are obtained at the top of the reactive rectifying tower (1), and are condensed by a condenser (2) at the top of the reactive rectifying tower, one part of liquid-phase acetone is taken as a product (14) to be sent out, and the other part of liquid-phase acetone is taken as reflux liquid (13) to return to the reactive rectifying tower (1) so as to keep the gas-liquid contact of the rectifying section; the catalyst is a resin catalyst, a macroporous styrene ion exchange resin polymerization production process is adopted, fluoroalkyl (meth) acrylate monomers and phenol are added to participate in polymerization, and the catalyst is prepared by sulfonation, wherein the fluoroalkyl (meth) acrylate monomers are hexafluorobutyl acrylate, dodecafluoroheptyl acrylate and/or tridecafluoroctyl acrylate; the technological parameters of the reaction section of the reactive distillation column are as follows: the operation temperature is 75-100 ℃, the operation pressure is 110-195 kPaA, and the equipment parameters of the reaction section of the reactive distillation tower are as follows: the length-diameter ratio is 16: 1, filling n sections of solid catalyst beds in a reaction section, wherein n is 1-12; the technological parameters of the rectifying section of the reactive rectifying tower are as follows: the operation temperature is 45-70 ℃, the operation pressure is 68-156 kPaA, the reflux ratio is 0.55-0.95, the number of the rectification tower plates is 40-48, and the 38-46 tower plates are arranged at the position of the feed plate from top to bottom; each section of catalyst bed layer of the reaction section of the reaction rectifying tower is provided with a channel which is mutually connected with a catalyst regeneration system, and the catalyst in a flowing state can realize on-line regeneration and on-line replacement.
2. The method for preparing phenol acetone by reactive distillation decomposition (CHP) according to claim 1, wherein the process parameters of the reaction section of the reactive distillation column are as follows: the operation temperature is 80-95 ℃, the operation pressure is 125-180 kPaA, and the equipment parameters of the reaction section of the reactive distillation tower are as follows: the length-diameter ratio is 6: and 1, filling n sections of solid catalyst beds in the reaction section, wherein n is 2-11.
3. The method for preparing phenol acetone by reactive distillation decomposition (CHP) according to claim 2, wherein the process parameters of the reaction section of the reactive distillation column are as follows: the operation temperature is 85-90 ℃; the operating pressure is 140-165 kPaA; the parameters of the reaction section equipment of the reactive distillation tower are as follows: the length-diameter ratio is 2: 1; and n sections of solid catalyst bed layers are filled in the reaction section, wherein n is 2-10.
4. The method for preparing phenol acetone by reactive distillation decomposition (CHP) according to claim 1, wherein the technological parameters of the rectifying section of the reactive distillation column are as follows: the operation temperature is 50-65 ℃, and the operation pressure is 83-141 kPaA.
5. The method for preparing phenol acetone by reactive distillation decomposition (CHP) according to claim 4, wherein the technological parameters of the rectifying section of the reactive distillation column are as follows: the operation temperature is 55-60 ℃; the operation pressure is 98-126 kPaA.
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