CN114177641A - Crude phenol dehydration method - Google Patents
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- CN114177641A CN114177641A CN202111547851.4A CN202111547851A CN114177641A CN 114177641 A CN114177641 A CN 114177641A CN 202111547851 A CN202111547851 A CN 202111547851A CN 114177641 A CN114177641 A CN 114177641A
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- crude phenol
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- raw material
- boiling point
- dehydration
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 230000018044 dehydration Effects 0.000 title claims abstract description 65
- 238000006297 dehydration reaction Methods 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 65
- 239000002904 solvent Substances 0.000 claims abstract description 73
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000002994 raw material Substances 0.000 claims abstract description 45
- 238000009835 boiling Methods 0.000 claims abstract description 33
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims abstract description 22
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims description 21
- RWGFKTVRMDUZSP-UHFFFAOYSA-N cumene Chemical compound CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 claims description 14
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 10
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 10
- KVZJLSYJROEPSQ-UHFFFAOYSA-N 1,2-dimethylcyclohexane Chemical compound CC1CCCCC1C KVZJLSYJROEPSQ-UHFFFAOYSA-N 0.000 claims description 8
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 claims description 8
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 claims description 8
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 claims description 8
- SGVUHPSBDNVHKL-UHFFFAOYSA-N 1,3-dimethylcyclohexane Chemical compound CC1CCCC(C)C1 SGVUHPSBDNVHKL-UHFFFAOYSA-N 0.000 claims description 6
- DMEGYFMYUHOHGS-UHFFFAOYSA-N cycloheptane Chemical compound C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 6
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethylcyclohexane Chemical compound CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 claims description 6
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methylcycloheptane Chemical compound CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 claims description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 4
- 238000005191 phase separation Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 229940078552 o-xylene Drugs 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 2
- 230000011218 segmentation Effects 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 48
- 239000012071 phase Substances 0.000 description 37
- 238000010992 reflux Methods 0.000 description 16
- 239000000463 material Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000010533 azeotropic distillation Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 241001120493 Arene Species 0.000 description 1
- 238000000998 batch distillation Methods 0.000 description 1
- -1 carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- KSSNXJHPEFVKHY-UHFFFAOYSA-N phenol;hydrate Chemical compound O.OC1=CC=CC=C1 KSSNXJHPEFVKHY-UHFFFAOYSA-N 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a crude phenol dehydration method, which is to add a solvent with the weight of 0.02-0.2 times of that of a crude phenol raw material into the crude phenol raw material for rectification; wherein the solvent is at least one of alkane with a boiling point of 115-155 ℃ and arene with a boiling point of 118-155 ℃. The method greatly reduces the using amount of the solvent, obviously reduces the rectification load, the energy consumption in the dehydration process and the dehydration cost, has lower volatile loss of the solvent, higher speed of water produced by rectification, greatly shortens the required operation time, and obviously reduces the subsequent treatment difficulty of the separated water.
Description
Technical Field
The invention relates to the technical field of crude phenol dehydration, in particular to a crude phenol dehydration method.
Background
The dehydration of the crude phenol is an essential step in the refining process of the coking crude phenol. The traditional crude phenol dehydration method is to directly rectify the crude phenol raw material, distill off the water in the crude phenol raw material and finish the dehydration. The main problems of the traditional crude phenol dehydration method are that: in the dehydration process, phenol in the crude phenol and water form an azeotrope, and the azeotrope is distilled out from the top of the tower, so that the content of phenol in the water obtained by dehydration reaches 2-4%, and the COD reaches 60000-120000 mg/L. Because the phenol content of the water is high, an extracting agent is required to be additionally added for extraction treatment so as to recover crude phenol (such as CN107739299A in China), a series of problems such as solvent regeneration process and equipment are involved, and the equipment investment and the production cost are obviously increased.
The document entitled azeotropic distillation separation of phenol-water mixture (from Qilu petrochemical industry 2005,33(4): 271-272) discloses that the dehydration of raw materials such as industrial continuous crude phenol is achieved by adopting a method of azeotropic distillation of toluene and water. This technique has at least the following problems: firstly, the technology mainly aims at the continuous dehydration process of crude phenol, and the crude phenol is basically a batch dehydration process at present; secondly, the azeotropic effect of toluene is not ideal, the amount of toluene required to be added in the rectification process is more than half of that of crude phenol raw materials, the treatment load, the treatment energy consumption and the treatment cost of a device can be obviously increased, and the economic benefit in the actual production is not good.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a crude phenol dehydration method to solve the technical problems in the prior art. The method greatly reduces the using amount of the solvent, obviously reduces the rectification load, the energy consumption in the dehydration process and the dehydration cost, has lower volatile loss of the solvent, higher speed of water produced by rectification, greatly shortens the required operation time, and obviously reduces the subsequent treatment difficulty of the separated water.
The purpose of the invention is realized by the following technical scheme:
a crude phenol dehydration process comprising: according to the weight of a crude phenol raw material, adding a solvent which is 0.02-0.2 times of the weight of the crude phenol raw material into the crude phenol raw material for rectification; wherein the solvent is at least one of alkane with a boiling point of 115-155 ℃ and arene with a boiling point of 118-155 ℃.
Preferably, a crude phenol raw material is added into a batch rectifying still, a solvent which is 0.02-0.2 times of the weight of the crude phenol raw material is added into the crude phenol raw material according to the weight of the crude phenol raw material, then rectification is carried out, a distillate at the top of a rectifying tower firstly enters a phase separator, and then sectional operation is carried out according to the fact that whether the distillate can be subjected to phase separation or not: the first stage is a dehydration process, when the distillate can be separated into phases, the solvent phase is totally refluxed, and the water phase is totally extracted until the anhydrous phase is discharged; the second stage is a solvent removal process, when the distillate can not be separated, the distillate partially flows back, the collector is switched, and the mixture of the solvent and the phenol is separately collected until the distillation process is stopped when the kettle liquid does not contain the solvent.
Preferably, the number of theoretical plates of the rectifying tower is 20-60, and the operating pressure is normal pressure-10 kPa (absolute pressure).
Preferably, the alkane with the boiling point of 115-155 ℃ comprises at least one of 1, 2-dimethylcyclohexane, 1, 3-dimethylcyclohexane, ethylcyclohexane, cycloheptane, methylcycloheptane and n-octane.
Preferably, the aromatic hydrocarbon with the boiling point of 118-155 ℃ is aromatic hydrocarbon with two methyl groups or an ethyl group or an isopropyl group. Preferably, the aromatic hydrocarbon with the boiling point of 118-155 ℃ comprises but is not limited to at least one of cumene, ortho-xylene, meta-xylene, para-xylene and ethylbenzene.
Compared with the prior art, the crude phenol dehydration method provided by the invention adopts at least one of alkane with a boiling point of 115-155 ℃ and aromatic hydrocarbon with a boiling point of 115-155 ℃ as a solvent to replace toluene in the prior art, and combines a specific crude phenol dehydration method, so that the use amount of the solvent can be greatly reduced, the rectification load, the dehydration energy consumption and the dehydration cost are remarkably reduced, the volatility loss of the solvent is lower, the rectification dehydration speed is higher, the required operation time is greatly shortened, and the subsequent treatment difficulty of the separated water is remarkably reduced.
Detailed Description
The technical scheme in the embodiment of the invention is clearly and completely described below; it is to be understood that the described embodiments are merely exemplary of the invention, and are not intended to limit the invention to the particular forms disclosed. 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 terms that may be used herein are first described as follows:
the terms "comprising," "including," "containing," "having," or other similar terms of meaning should be construed as non-exclusive inclusions. For example: including a feature (e.g., material, component, ingredient, carrier, formulation, material, dimension, part, component, mechanism, device, process, procedure, method, reaction condition, processing condition, parameter, algorithm, signal, data, product, or article of manufacture), is to be construed as including not only the particular feature explicitly listed but also other features not explicitly listed as such which are known in the art.
When concentrations, temperatures, pressures, dimensions, or other parameters are expressed as ranges of values, the ranges are to be understood as specifically disclosing all ranges formed from any pair of upper, lower, and preferred values within the range, regardless of whether ranges are explicitly recited; for example, if a numerical range of "2 ~ 8" is recited, then the numerical range should be interpreted to include ranges of "2 ~ 7", "2 ~ 6", "5 ~ 7", "3 ~ 4 and 6 ~ 7", "3 ~ 5 and 7", "2 and 5 ~ 7", and the like. Unless otherwise indicated, the numerical ranges recited herein include both the endpoints thereof and all integers and fractions within the numerical range.
The process for dehydrating crude phenol provided by the present invention is described in detail below. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art. Those not specifically mentioned in the examples of the present invention were carried out according to the conventional conditions in the art or conditions suggested by the manufacturer. The reagents or instruments used in the examples of the present invention are not specified by manufacturers, and are all conventional products available by commercial purchase.
The invention provides a crude phenol dehydration method, which comprises the following steps: and adding a solvent which is 0.02-0.2 times of the weight of the crude phenol raw material into the crude phenol raw material according to the weight of the crude phenol raw material, and rectifying.
The solvent is at least one of alkane with a boiling point of 115-155 ℃ and arene with a boiling point of 118-155 ℃, namely the solvent can be single alkane with a boiling point of 115-155 ℃ or single arene with a boiling point of 118-155 ℃, can also be a plurality of alkanes with a boiling point of 115-155 ℃ or a plurality of arenes with a boiling point of 118-155 ℃, and can also be a mixture of alkane with a boiling point of 115-155 ℃ and arene with a boiling point of 118-155 ℃. The alkane with the boiling point of 115-155 ℃ comprises but is not limited to 1, 2-dimethylcyclohexane, 1, 3-dimethylcyclohexane, ethylcyclohexane, cycloheptane, methylcycloheptane or n-octane. The aromatic hydrocarbon with the boiling point of 118-155 ℃ can adopt aromatic hydrocarbon with two methyl groups or an ethyl group or an isopropyl group, such as: cumene, ortho-xylene, meta-xylene, para-xylene or ethylbenzene.
Specifically, the crude phenol dehydration method provided by the invention can be implemented by adding a crude phenol raw material into an intermittent rectification kettle, adding a solvent which is 0.02-0.2 times of the weight of the crude phenol raw material into the crude phenol raw material according to the weight of the crude phenol raw material, rectifying, feeding distillate at the top of a rectification tower (the number of theoretical plates of the rectification tower for dehydration is 20-60, and the operation pressure is normal pressure-10 kPa (absolute)) into a phase separator, and then performing segmentation operation according to the phase separation possibility of the distillate: the first stage is a dehydration process, when the distillate can be separated into phases, the solvent phase is totally refluxed, and the water phase is totally extracted until the anhydrous phase is discharged; and the second stage is a solvent removal process, when the distillate is not subjected to phase separation, partial distillate flows back, the collector is switched, the mixture of the solvent and the phenol is separately collected, the rectification process is stopped until the kettle liquid does not contain the solvent, and the solvent recovered from the tower top is added into the kettle for recycling when the crude phenol raw material is rectified and dehydrated next time.
Compared with the prior art, the crude phenol dehydration method provided by the invention at least has the following advantages:
(1) the crude phenol dehydration method provided by the invention adopts at least one of alkane with a boiling point of 115-155 ℃ and arene with a boiling point of 118-155 ℃ as a solvent to replace toluene in the prior art, and the solvent can be a single pure solvent or a mixture, so that a better azeotropic effect than toluene can be obtained; the solvent adopted by the invention has higher boiling point, less volatilization loss and better azeotropic dehydration effect, and the proportion of the added solvent is reduced by more than half compared with the toluene in the documents in the background technology, namely, the using amount of the solvent is greatly reduced, so that the rectification load is obviously reduced, and the energy consumption and the cost in the dehydration process are obviously reduced.
For example, the azeotropic mass ratio of toluene to water is 0.81:0.19 and the azeotropic mass ratio of cumene to water is 0.58:0.42, meaning that 1 part of water requires 4.3 parts toluene to carry over, whereas if cumene is used, only 1.4 parts toluene to 0.58/0.42 is sufficient, thus requiring much less solvent to be added.
Of course, as for batch distillation, since the solvent is operated under total reflux and the aqueous phase is fully extracted, the amount of the solvent used in the actual operation does not need to comply with the above ratio, but when the high boiling point azeotropic agent is used, the water carrying capacity of the solvent is stronger, which means that the water is distilled out at a higher speed and the required operation time is greatly shortened.
(2) The crude phenol dehydration method provided by the invention adopts at least one of alkane with a boiling point of 115-155 ℃ and aromatic hydrocarbon with a boiling point of 118-155 ℃ as a solvent to replace toluene in the prior art, wherein the boiling point (118-155 ℃) of the selected solvent is higher than that (110 ℃) of the selected solvent, and the volatility loss is lower.
(3) The solvent selected in the crude phenol dehydration method provided by the invention is alkane or aromatic hydrocarbon with two methyl groups or an ethyl group or an isopropyl group, compared with the toluene with only one methyl group described in the above documents in the background art, the solvent has lower solubility in water and smaller loss, and the difficulty of the subsequent treatment of the separated water is also obviously reduced; for example, the solubility of toluene in water is 0.05g/100mL (20-25 ℃), and the solubility of o-xylene in water is 0.01g/100mL (20-25 ℃), with the difference being about 5 times; and the alkane and the cumene are basically insoluble in water; this significantly reduces solvent losses and the subsequent treatment of the separated water is significantly less difficult.
(4) In the prior art, a rectification dehydration mode without adding a solvent is adopted, and the content of phenol in the separated water is 2-4% (industrial actual data); in contrast, in the embodiment of the invention, the phenol content in the water separated by the azeotropic distillation of the added solvent is within 200ppm, and the difficulty of subsequent treatment is obviously reduced.
(5) The crude phenol dehydration method provided by the invention adopts at least one of alkane with a boiling point of 115-155 ℃ and aromatic hydrocarbon with a boiling point of 118-155 ℃ as a solvent to replace toluene in the prior art, and is combined with a specific crude phenol dehydration method, so that the use amount of the solvent can be greatly reduced, the rectification load, the dehydration energy consumption and the dehydration cost are remarkably reduced, the volatility loss of the solvent is lower, the water rectification speed is higher, the required operation time is greatly shortened, and the subsequent treatment difficulty of the separated water is remarkably reduced.
In conclusion, the embodiment of the invention greatly reduces the usage amount of the solvent, obviously reduces the rectification load, the energy consumption in the dehydration process and the dehydration cost, has lower volatile loss of the solvent, higher speed of water produced by rectification, greatly shortens the required operation time, and obviously reduces the difficulty of the subsequent treatment of the separated water.
In order to more clearly show the technical scheme and the technical effects provided by the present invention, the following detailed description of the crude phenol dehydration method provided by the embodiment of the present invention is provided by specific examples.
Example 1
A crude phenol dehydration process comprising: adding 2.0kg of crude phenol raw material containing 10.0% of water into a 3L batch rectifying still, adding 0.04kg (equivalent to 0.02 times of the weight of the crude phenol raw material) of isopropyl benzene into the crude phenol raw material, then rectifying at a constant heating rate of 500w, feeding distillate at the top of a rectifying tower (the number of theoretical plates of the rectifying tower is 60, carrying out negative pressure rectification all the time, and the absolute pressure is 10kPa) into a phase separator, refluxing all solvent phases, and extracting all water phases until an anhydrous phase is discharged to obtain 0.19kg of water phase and 19ppm of phenol; when the distillate at the top of the rectifying tower does not split phases any more, the reflux ratio is 10, and 0.08kg of mixture of the solvent, the phenol and the water is distilled off from the top of the rectifying tower (the materials are not layered), and the mixture can be used for rectifying and dehydrating the crude phenol raw material next time; anhydrous crude phenol is obtained in the batch rectifying kettle; the time for the dehydration process was 0.7 hours, starting with reflux at the top of the column.
Example 2
A crude phenol dehydration process comprising: adding 1.0kg of a crude phenol raw material containing 10.0% of water into a 2L batch rectifying still, adding 0.10kg (equivalent to 0.10 times of the weight of the crude phenol raw material) of an aromatic hydrocarbon mixture (the mass ratio of the components of the aromatic hydrocarbon mixture is that o-xylene, m-xylene, p-xylene and ethylbenzene is 1:1:1:1), rectifying, wherein the heating rate is constant at 250w, the number of theoretical plates of a rectifying tower is 40, performing negative pressure rectification, and the distillate at the top of the tower with the absolute pressure of 20kPa enters a phase separator, wherein the solvent phase completely refluxes, the water phase completely withdraws until the anhydrous phase is discharged, and the water phase is 0.09kg and the phenol content is 14 ppm; when the distillate at the top of the rectifying tower does not split phases any more, the reflux ratio is 15, and 0.13kg of mixture of the solvent, the phenol and the water is distilled off from the top of the rectifying tower (the materials are not layered), and the mixture can be used for rectifying and dehydrating the crude phenol raw material next time; anhydrous crude phenol is obtained in the batch rectifying kettle; the time for the dehydration process was 0.8 hours, starting with reflux at the top of the column.
Example 3
A crude phenol dehydration process comprising: adding 1.0kg of a crude phenol raw material containing 10.0% of water into a 2L batch rectifying still, adding 0.12kg (equivalent to 0.12 times of the weight of the crude phenol raw material) of an alkane mixture (the mass ratio of each component of the alkane mixture is 1, 2-dimethylcyclohexane: n-octane is 1:1) into the crude phenol raw material, then carrying out normal-pressure rectification, keeping the heating rate constant at 250w, feeding a distillate at the top of a rectifying tower (the theoretical plate number of the rectifying tower is 20) into a phase separator, completely refluxing a solvent phase, completely extracting a water phase until an anhydrous phase is discharged, and obtaining 0.09kg of a water phase and 4ppm of phenol; when the distillate at the top of the rectifying tower does not split phases any more, adopting negative pressure rectification with absolute pressure of 20kPa and reflux ratio of 5, distilling out 0.16kg of mixture of solvent, phenol and water (the material is not layered) at the top of the rectifying tower, and being used for rectifying and dehydrating crude phenol raw materials next time; anhydrous crude phenol is obtained in the batch rectifying kettle; the time for the dehydration process was 0.8 hours, starting with reflux at the top of the column.
Example 4
A crude phenol dehydration process comprising: adding 1.0kg of crude phenol raw material containing 10.0% of water into a 2L batch rectifying still, adding 0.20kg (equivalent to 0.20 times of the weight of the crude phenol raw material) of n-octane into the crude phenol raw material, then carrying out normal pressure rectification, keeping the heating rate constant at 250w, feeding distillate at the top of a rectifying tower (the number of theoretical plates of the rectifying tower is 20) into a phase separator, completely refluxing a solvent phase, completely extracting a water phase until the water-free phase is discharged, and obtaining 0.09kg of water phase and 6ppm of phenol; when the distillate at the top of the rectifying tower does not split phases any more, adopting negative pressure rectification with absolute pressure of 30kPa and reflux ratio of 5, distilling out 0.27kg of mixture of solvent, phenol and water (the material is not layered) at the top of the rectifying tower, and being used for rectifying and dehydrating crude phenol raw materials next time; anhydrous crude phenol is obtained in the batch rectifying kettle; the time for the dehydration process was 0.8 hours, starting with reflux at the top of the column.
Reference 1
A crude phenol dehydration method was substantially the same as that in example 3 of the present invention except that no solvent was added to the crude phenol raw material, the rectification pressure was constant at 20kPa (absolute pressure), the reflux ratio was 1:1, and 0.10kg of an aqueous phase obtained at the top of the rectification column and 3.8% of phenol were contained. The time for the dehydration process was 0.8 hours, starting with reflux at the top of the column.
Compared with the embodiment 3 of the invention, the solvent is not added in the comparative example 1 for the rectification and dehydration of the crude phenol, the separated water phase phenol content is very high, and the extraction treatment needs to be additionally added, while the solvent is added in the embodiment 3 of the invention for the rectification and dehydration of the crude phenol, the separated water phase phenol content is very low, and the extraction treatment does not need to be additionally added, which obviously reduces the equipment investment and the production cost.
Reference document 2
A crude phenol dehydration method which is substantially the same as that of example 3 of the present invention except that the solvent used was toluene instead of the alkane mixture (the mass ratio of each component of the alkane mixture was 1: 2; when the distillate at the top of the rectifying tower does not split phases any more, distilling out a mixture of 0.15kg of solvent, phenol and water (materials are not layered) at the top of the rectifying tower, and using the mixture for rectifying and dehydrating the crude phenol raw material next time; anhydrous crude phenol is obtained in the batch rectifying kettle; the time for the dehydration process was 1.3 hours, starting with reflux at the top of the column.
Compared with the embodiment 3 of the invention, in the comparative example 2, the toluene is added as the solvent to carry out rectification dehydration on the crude phenol, so that the time of the dehydration process is obviously prolonged, and the energy consumption is obviously increased, which shows that under the condition of equal solvent usage amount, the speed of the distilled water of the embodiment 3 of the invention is faster, the time of the dehydration process is greatly shortened, and the energy consumption is greatly reduced.
In conclusion, the embodiment of the invention greatly reduces the usage amount of the solvent, obviously reduces the rectification load, the energy consumption in the dehydration process and the dehydration cost, has lower volatile loss of the solvent, higher speed of water produced by rectification, greatly shortens the required operation time, and obviously reduces the difficulty of the subsequent treatment of the separated water.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Claims (6)
1. A method for dehydrating crude phenol, comprising: according to the weight of a crude phenol raw material, adding a solvent which is 0.02-0.2 times of the weight of the crude phenol raw material into the crude phenol raw material for rectification;
wherein the solvent is at least one of alkane with a boiling point of 115-155 ℃ and arene with a boiling point of 118-155 ℃.
2. The crude phenol dehydration method according to claim 1, characterized in that a crude phenol raw material is added into a batch still, a solvent which is 0.02 to 0.2 times the weight of the crude phenol raw material is added into the crude phenol raw material according to the weight of the crude phenol raw material, then rectification is carried out, a distillate at the top of a rectification tower firstly enters a phase separator, and then segmentation operation is carried out according to the phase separation possibility of the distillate: the first stage is a dehydration process, when the distillate can be separated into phases, the solvent phase is totally refluxed, and the water phase is totally extracted until the anhydrous phase is discharged; the second stage is a solvent removal process, when the distillate can not be separated, the distillate partially flows back, the collector is switched, and the mixture of the solvent and the phenol is separately collected until the distillation process is stopped when the kettle liquid does not contain the solvent.
3. The method for dehydrating crude phenol according to claim 2, wherein the number of theoretical plates of the rectifying tower is 20 to 60, and the operating pressure is normal pressure to 10kPa (absolute).
4. The method for dehydrating crude phenol according to any one of claims 1 to 3, wherein the alkane having a boiling point of 115 to 155 ℃ is at least one selected from the group consisting of 1, 2-dimethylcyclohexane, 1, 3-dimethylcyclohexane, ethylcyclohexane, cycloheptane, methylcycloheptane, and n-octane.
5. The method for dehydrating crude phenol according to any one of claims 1 to 3, wherein the aromatic hydrocarbon having a boiling point of 118 to 155 ℃ is an aromatic hydrocarbon having two methyl groups or one ethyl group or one isopropyl group.
6. The method for dehydrating crude phenol according to any one of claims 1 to 3, wherein the aromatic hydrocarbon having a boiling point of 118 to 155 ℃ is at least one of cumene, o-xylene, m-xylene, p-xylene, and ethylbenzene.
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| CN202111547851.4A CN114177641A (en) | 2021-12-16 | 2021-12-16 | Crude phenol dehydration method |
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| CN202111547851.4A Pending CN114177641A (en) | 2021-12-16 | 2021-12-16 | Crude phenol dehydration method |
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| CN111097191A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Method for recovering organic solvent by extraction-rectification method |
| CN113480412A (en) * | 2021-07-20 | 2021-10-08 | 广东锦昱材料科技有限公司 | Method for recovering phenol in alkylphenol production wastewater |
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2021
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| US4298765A (en) * | 1980-03-26 | 1981-11-03 | Allied Corporation | Purification of phenol with reduced energy consumption |
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| CN102942509A (en) * | 2012-10-17 | 2013-02-27 | 山东方明药业集团股份有限公司 | Synthetic method of etamsylate |
| CN107739299A (en) * | 2017-11-23 | 2018-02-27 | 魏艳娟 | The refining spearation combined dehydration method and device of mixed phenol |
| CN111097191A (en) * | 2018-10-25 | 2020-05-05 | 中国石油化工股份有限公司 | Method for recovering organic solvent by extraction-rectification method |
| CN113480412A (en) * | 2021-07-20 | 2021-10-08 | 广东锦昱材料科技有限公司 | Method for recovering phenol in alkylphenol production wastewater |
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Application publication date: 20220315 |