Energy-saving material separation and purification device after hydroxylation reaction of phenol and hydrogen peroxide

Abstract

The utility model provides an energy-saving device for separating and purifying materials after hydroxylation reaction of phenol and hydrogen peroxide, and relates to the technical field of chemical synthesis. Materials obtained after phenol hydrogen peroxide hydroxylation reaction are separated and purified through the extraction tower, the extraction agent recovery tower, the first phenol removal tower, the tar removal tower, the second phenol removal tower, the catechol removal tower, the light component removal tower and the hydroquinone tower, the whole technological process is simple, the yield is high, and the high-purity hydroquinone product and the high-purity catechol product can be obtained; according to the utility model, the extraction tower is adopted to replace a dehydration rectifying tower in the traditional process to remove phenol-containing wastewater, so that the phenol recovery rate is improved, and the subsequent wastewater treatment burden is reduced; and the tar removal tower is arranged behind the phenol removal tower I, so that the retention time of tar impurities in the whole process system is shortened, and the process safety is improved. According to the utility model, the high-temperature waste heat at the top of the dephenolization tower I is recovered by combining waste heat recovery with a mechanical steam recompression energy-saving technology, so that the process energy consumption of the operation of the whole device is effectively reduced.

Description

TECHNICAL FIELD

[0001] The utility model relates to the field of chemical synthesis technology, concretely relates to an energy-saving phenol hydrogen peroxide hydroxylation post-material separation and purification device. BACKGROUND

[0002] Diphenol (including o-diphenol, p-diphenol) is an important fine chemical intermediate product, wherein, p-diphenol is mainly used for photosensitive material, rubber, dye, pharmaceutical industry. It can be used as a developer of film, a thermal inhibitor of photosensitive resin, an antioxidant, an anti-aging agent, an intermediate for producing anthraquinone, azo and other dyes; o-diphenol is mainly used as an intermediate for pesticide and dye, and is also an important intermediate for synthesizing perfume and medicine; in addition, it can be used for making hair dye, rubber hardener, electroplating tank additive and the like.

[0003] Among the synthesis methods of diphenol, the phenol hydrogen peroxide oxidation method has the most practical significance. This method uses phenol and hydrogen peroxide as raw materials to simultaneously generate o-diphenol and p-diphenol under the action of a catalyst. This method is widely used in the global range. In the actual production process, the separation of the mixed product after the phenol hydrogen peroxide hydroxylation reaction is a difficult problem that restricts the industrialized production of o-diphenol and p-diphenol. Specifically, the separation and purification process of separating and purifying through multiple rectifying towers will consume a large amount of energy, and thus cause problems of waste water and consumption of raw material phenol; in addition, the effective separation of tar is also one of the key difficulties, and the long-time retention of tar in the process system may cause the blockage of subsequent equipment and lead to operation risks. UTILITY MODEL CONTENTS

[0004] In view of the deficiencies in the prior art, the utility model discloses an energy-saving phenol hydrogen peroxide hydroxylation post-material separation and purification device, which can effectively reduce the process energy consumption of phenol hydrogen peroxide hydroxylation post-material separation and purification, reduce the phenol content in waste water, and reduce the residence time of tar impurities in the process system, thereby reducing the risk of subsequent operation.

[0005] In order to achieve the above technical purposes, the utility model provides an energy-saving phenol hydrogen peroxide hydroxylation post-material separation and purification device, which comprises an extraction tower, an extractant recovery tower, a dephenol I tower, a de-tar tower, a dephenol II tower, an o-diphenol tower, a light-removing tower and a p-diphenol tower, wherein:

[0006] The first feed inlet of the extraction column is connected to an input pipe of the material to be separated and purified, and the second feed inlet is connected to an input pipe of the extractant; the upper outlet of the extraction column is connected to the feed inlet of the extractant recovery column; the outlet of the column bottom of the extractant recovery column is connected to the feed inlet of the first dephenol column; the top of the extractant recovery column is connected to a first phase separation device; the water phase outlet of the first phase separation device is connected to the upper part of the extraction column, and the oil phase outlet outputs the recovered extractant; the outlet of the column bottom of the first dephenol column is connected to the feed inlet of the de-tar column; the top of the first dephenol column is connected to a second phase separation device; the oil phase outlet of the second phase separation device is connected to the upper part of the first dephenol column and is provided with a branch for outputting the recovered phenol; the upper outlet of the de-tar column is connected to the feed inlet of the second dephenol column; the outlet of the column bottom of the second dephenol column is connected to the feed inlet of the catechol column; the upper outlet of the second dephenol column outputs the recovered phenol; the upper outlet of the catechol column outputs the high-purity catechol product; the column bottom of the catechol column is connected to the feed inlet of the de-light column; the upper outlet of the de-light column outputs the light component impurities; the column bottom of the de-light column is connected to the feed inlet of the hydroquinone column; the upper outlet of the hydroquinone column outputs the high-purity hydroquinone product; and the column bottom of the hydroquinone column outputs the heavy component impurities.

[0007] The first gas-liquid separation tank is further connected to the coolant inlet of the overhead heat exchanger of the first dephenol column through a pipeline, and the feed inlet of the first gas-liquid separation tank is connected to the coolant outlet of the overhead heat exchanger of the first dephenol column; the gas phase outlet of the first gas-liquid separation tank is connected to the gas inlet of the first steam compressor, and the gas outlet of the first compressor outputs the secondary steam A.

[0008] The above technical solution extracts the material after the hydroxylation reaction of p-benzenediol and hydrogen peroxide in the extraction column; the oil phase containing p-benzenediol, o-benzenediol, phenol, water, tar, extractant and other components is output from the top of the extraction column; the oil phase is input into the extractant recovery column to recycle the extractant; the water phase containing a small amount of sodium sulfate, a small amount of extractant and water is collected from the column bottom of the extraction column. The extraction column is used to replace the dehydration rectification column in the traditional process to remove the phenol-containing wastewater in the material after the reaction, which greatly reduces the phenol content in the wastewater, improves the raw material recovery efficiency, and reduces the burden of subsequent wastewater treatment.

[0009] In the above technical solution, the column bottom of the de-tar column is connected to a tar post-treatment process, and the top of the de-tar column is connected to the second dephenol column. The de-tar column is arranged before the secondary phenol recovery in the second dephenol column, thereby effectively reducing the residence time of tar impurities in the device and reducing the risk of subsequent operation.

[0010] The technical scheme has the advantages that the phenol in the material after phenol-hydrogen peroxide hydroxylation reaction is fully recovered through the combination of the dephenolizing column, the de-tar column and the dephenolizing column II, the raw material utilization rate is improved, the process cost is reduced, and remarkable economic benefits are brought in large-scale production.

[0011] In addition, the high-temperature waste heat at the top of the dephenolizing column is recovered through the waste heat recovery combined with the mechanical steam re-compression energy-saving technology, the secondary steam obtained is 300-600kPa steam, which can be used for other links of the phenol-hydrogen peroxide oxidation process, the heating of the column kettle reboiler of other process columns (such as the extractant recovery column) in the separation and purification device, or the heating of the device pipeline, and the like, so that the process energy consumption of the overall device operation is effectively reduced.

[0012] Compared with the prior art, the separation and purification device has the advantages that:

[0013] The separation and purification device separates and purifies the material after phenol-hydrogen peroxide hydroxylation reaction through the extraction column, the extractant recovery column, the dephenolizing column, the de-tar column, the dephenolizing column II, the catechol column, the light component removal column and the p-benzenediol column, the overall process flow is simple and the yield is high, high-purity p-benzenediol products and catechol products can be obtained, the extraction column is used to replace the traditional dehydrating rectifying column to remove the phenol-containing wastewater, the phenol recovery rate is improved and the subsequent wastewater treatment burden is reduced, the de-tar column is arranged after the dephenolizing column, the residence time of tar impurities in the overall process system is reduced, the process safety is improved and the subsequent operation risk is reduced, the high-temperature waste heat at the top of the dephenolizing column is recovered through the waste heat recovery combined with the mechanical steam re-compression energy-saving technology, the process energy consumption of the overall device operation is effectively reduced, and the large-scale industrial application is facilitated. BRIEF DESCRIPTION OF DRAWINGS

[0014] The drawings accompanying the specification of this application form a part hereof, serve to provide further understanding of the present application, and together with the description of the exemplary embodiments of the present application, serve the purpose of explaining the present application, and do not constitute improper limitations on the present application. In the drawings:

[0015] Figure 1 A structure diagram of the energy-saving phenol-hydrogen peroxide hydroxylation reaction material separation and purification device is shown.

[0016] In the drawings, the following reference signs are used:

[0017] 1-extraction column, 11-material to be separated and purified input pipe, 12-extraction agent input pipe, 2-extraction agent recovery column, 21-first phase separation device, 22-extraction agent recycling pipe, 3-phenol removal column 1, 31-second phase separation device, 32-aqueous phase recycling pipe, 33-first phenol delivery pipe, 4-tar removal column, 41-tar delivery pipe, 5-phenol removal column 2, 51-second phenol delivery pipe, 6-catechol column, 61-catechol delivery pipe, 7-light component impurity removal column, 71-light component impurity delivery pipe, 8-hydroquinone column, 81-hydroquinone delivery pipe, 9-stripping column, 91-waste water output pipe, 10-1 first gas-liquid separation tank, 10-2 first steam compressor, 10-3 first steam buffer tank, 10-4 second steam compressor, 10-5 second steam buffer tank, 10-6 third steam compressor, 10-7 third steam buffer tank, 10-8 steam generator, 10-9 second gas-liquid separation tank, v1-secondary steam A, v2-recompressed steam, v3-third compressed steam, v4-secondary steam B. DETAILED DESCRIPTION

[0018] In order to facilitate the understanding of the present application, the present application will be described more fully below, and preferred embodiments of the present application are given. But it should be understood that these embodiments are only used for more detailed description, and should not be understood as limiting the present application in any form, that is, it is not intended to limit the protection scope of the present application.

[0019] Unless otherwise defined, the technical terms used in the following examples have the same meaning as generally understood by those skilled in the art to which the present application belongs. The test reagents used in the following examples, unless otherwise specified, are conventional biochemical reagents; the experimental methods, unless otherwise specified, are conventional methods.

[0020] In addition, the terms "first", "second", "third" are only for descriptive purposes, and should not be understood as indicating or implying relative importance or implicitly indicating the number of indicated technical features. Therefore, the features defined as "first", "second", "third" can explicitly or implicitly include one or more of the features. In the description of the present application, the meaning of "a plurality of" is two or more, unless otherwise specifically limited.

[0021] Example 1

[0022] An energy-saving phenol and hydrogen peroxide hydroxylation reaction post-material separation and purification device, the device comprises an extraction column 1, an extraction agent recovery column 2, a phenol removal column 1, a tar removal column 4, a phenol removal column 2, a catechol column 6, a light component impurity removal column 7 and a hydroquinone column, wherein:

[0023] The first feed inlet of the extraction tower 1 is connected with an input pipe 11 of the material to be separated and purified, and the second feed inlet is connected with an input pipe 12 of the extractant.

[0024] The bottom outlet of the extractant recovery tower 2 is connected with the feed inlet of the dephenolization tower 3, and the top of the extractant recovery tower 2 is connected with a first phase separation device 21; the water phase outlet of the first phase separation device 21 is connected with the upper part of the extraction tower 1, and the oil phase outlet outputs the recovered extractant. In the optional example of the utility model, the part of the recovered extractant is input into an extractant storage tank through an extractant recycling pipe 22 or directly returned to the extractant for recycling.

[0025] The bottom outlet of the dephenolization tower 3 is connected with the feed inlet of the de-tar tower 4; the top of the dephenolization tower 3 is connected with a second phase separation device 31, the oil phase outlet of the second phase separation device 31 is connected with the upper part of the dephenolization tower 3 and is provided with a branch for outputting the recovered phenol. In the optional example of the utility model, the recovered phenol is input into a phenol storage tank through a first phenol conveying pipe 33 or directly returned to the upstream reaction process. The water phase outlet of the second phase separation device outputs the recovered water, and in the optional example of the utility model, the part of the recovered water is input into a process water storage tank through a water phase recycling pipe 32 or directly input into the upstream extractant slurry preparation tank.

[0026] The upper outlet of the de-tar tower 4 is connected with the feed inlet of the dephenolization tower 5; the tar-containing impurities are output from the bottom of the de-tar tower 4, and in the optional example of the utility model, the part of the tar impurities is input into a subsequent tar treatment process through a tar conveying pipe 41.

[0027] The bottom outlet of the dephenolization tower 5 is connected with the feed inlet of the catechol tower 6, and the upper outlet of the dephenolization tower 5 outputs the recovered phenol; in the optional example of the utility model, the recovered phenol of the dephenolization tower 5 is input into a phenol storage tank through a second phenol conveying pipe 51 or directly returned to the upstream reaction process.

[0028] The upper outlet of the catechol tower 6 outputs high-purity catechol products, and the bottom thereof is connected with the feed inlet of the de-light tower 7; in the optional example of the utility model, the catechol products are input into a subsequent process through a catechol conveying pipe 61.

[0029] The upper outlet of the de-light tower 7 outputs light component impurities, and the bottom thereof is connected with the feed inlet of the hydroquinone tower; in the optional example of the utility model, the part of the light component impurities is sent to a subsequent treatment process through a light component impurity conveying pipe 71.

[0030] The upper outlet of the hydroquinone tower 8 outputs high-purity hydroquinone products, and the bottom thereof outputs heavy component impurities; in the optional example of the utility model, the hydroquinone products are input into a subsequent process through a hydroquinone conveying pipe 81.

[0031] Further comprising a first gas-liquid separation tank 10-1, the liquid phase outlet of the first gas-liquid separation tank 10-1 is connected with the refrigerant inlet of the overhead heat exchanger of the de-phenol one column 3 through a pipeline, and the feed inlet of the first gas-liquid separation tank 10-1 is connected with the refrigerant outlet of the overhead heat exchanger of the de-phenol one column 3; the gas phase outlet of the first gas-liquid separation tank 10-1 is connected with the gas inlet of the first steam compressor 10-2, and the secondary steam Av1 is output from the gas outlet of the first compressor. In the optional example of the utility model, the secondary steam AV1 is 300-600kPa A steam; further, the secondary steam can be used for raw material preheating of the phenol hydrogen peroxide hydroxylation reaction process, heating of the hydrogen peroxide decomposition process, and heating of the reboiler of the extractant recovery column 2 of the utility model and equipment and pipeline heating of the process, so as to reduce the process energy consumption of the overall device.

[0032] Embodiment 2

[0033] Based on the energy-saving phenol hydrogen peroxide hydroxylation reaction post material separation and purification device shown in embodiment 1, in the embodiment, the liquid phase outlet of the first gas-liquid separation tank 10-1 is connected with the refrigerant inlet of the overhead heat exchanger of the de-tar column 4 and / or the overhead heat exchanger of the de-phenol two column 5 through a pipeline, and the feed inlet of the first gas-liquid separation tank 10-1 is connected with the refrigerant outlet of the overhead heat exchanger of the de-tar column 4 and / or the de-phenol two column 5, thereby further recovering the overhead heat of the de-tar column 4 and / or the de-phenol two column 5 on the basis of recovering the overhead heat of the de-phenol one column 3, and improving the energy utilization rate.

[0034] It should be noted that in the actual process, the overhead heat of the de-phenol one column 3 and / or the de-tar column 4 and / or the de-phenol one column 3 can be recovered as needed.

[0035] Embodiment 3

[0036] Based on the energy-saving phenol hydrogen peroxide hydroxylation reaction post material separation and purification device shown in embodiment 1, in the embodiment, the gas outlet of the first steam compressor 10-2 is connected with the gas inlet of the second steam compressor 10-4, and the re-compressed steam v2 is output from the gas outlet of the second steam compressor 10-4, and through further steam compression, a steam of higher grade can be obtained, and the energy utilization efficiency is improved.

[0037] Optionally, the steam in the first steam buffer tank 10-3 can be input into the second steam buffer tank 10-5 after being compressed by the second steam compressor 10-4; in the optional example of the utility model, the re-compressed steam v2 is 1000-1500kPa A steam, and this part of the re-compressed steam v2 can be used for equipment and pipeline heating of the de-tar column 4, the de-phenol two column 5, the catechol column 6, the light removal column 7, and the hydroquinone column 8, or for equipment and pipeline heating of subsequent processes.

[0038] Further, the gas outlet of the second vapor compressor 10-4 is connected to the gas inlet of the third vapor compressor 10-6, and the third compressed vapor v3 is output from the gas outlet of the third vapor compressor 10-6, and through the re-compression of the re-compressed vapor v2, a vapor with higher grade can be obtained.

[0039] Optionally, the third compressed vapor v3 is input into the third vapor buffer tank 10-7; in the optional example of the utility model, 3500-4200kPaA, this part of vapor can be used for heating the reboiler of the de-phenol column 3, or other processes requiring high-pressure vapor. Optionally, the vapor obtained after heat exchange of the third compressed vapor v3 is input into the first vapor buffer tank 10-3, so as to realize more sufficient waste heat recovery and utilization.

[0040] Embodiment 4

[0041] Based on the energy-saving phenol-hydrogen peroxide hydroxylation post-material separation and purification device shown in embodiment 1, the embodiment further comprises a steam generator 10-8 and a second gas-liquid separation tank 10-9; the oil outlet pipe of the steam generator 10-8 is connected to the refrigerant inlet of the overhead heat exchanger of the de-light column 7 and the hydroquinone column 8, and the oil inlet pipe of the steam generator 10-8 is connected to the refrigerant outlet of the overhead heat exchanger of the de-light column 7 and the hydroquinone column 8; the discharge port of the steam generator 10-8 is connected to the feed inlet of the second gas-liquid separation tank 10-9, and the second vapor Bv4 is output from the gas phase outlet of the second gas-liquid separation tank 10-9.

[0042] In the optional example of the utility model, the secondary vapor Av1 is 300-600kPaA vapor. Optionally, the secondary vapor Bv4 can be used for raw material preheating of the phenol-hydrogen peroxide hydroxylation process, heating of the hydrogen peroxide decomposition process, reboiler heating of the extractant recovery column 2, and process equipment and pipeline heating. In the specific process, the prepared secondary vapor Bv4 can be input into the first vapor buffer tank 10-3 and combined with the secondary vapor Av1, and then input into other processes.

[0043] Further, the liquid phase outlet of the second gas-liquid separation tank 10-9 is connected with the coolant inlet of the overhead heat exchanger of the catechol column and / or the feed inlet of the steam generator 10-8 respectively; the coolant outlet of the overhead heat exchanger of the catechol column 6 is connected with the feed inlet of the second gas-liquid separation tank 10-9; thus, a branch one is obtained: the gas-liquid mixture generated by the steam generator 10-8 is returned to the second gas-liquid separation tank 10-9, the secondary steam Bv4 is obtained by gas-liquid separation, and the obtained liquid phase is returned to the steam generator 10-8; and / or, a branch two is obtained: the gas-liquid mixture generated by the overhead product of the catechol column 6 is returned to the second gas-liquid separation tank 10-9, the secondary steam Bv4 is obtained by gas-liquid separation, and the obtained liquid phase is returned to the overhead product of the catechol column 6; the liquid phase obtained by the second gas-liquid separation tank 10-9 is recycled by the branch one and the branch two.

[0044] Embodiment 5

[0045] Based on the energy-saving phenol-hydrogen peroxide hydroxylation post-material separation and purification device shown in Embodiment 1, in the present embodiment, the column bottom outlet of the hydroquinone column 8 is connected with the de-tar column 4, so that the heavy components in the overhead product of the hydroquinone column 8 can be concentrated and combined with the heavy components such as tar in the de-tar column for processing, the tar processing efficiency is improved by inputting the subsequent tar processing procedure, and the components such as catechol, hydroquinone and phenol contained in the column bottom overhead product of the hydroquinone column 8 can be fully recovered, and the process economic benefit is improved.

[0046] Embodiment 6

[0047] Based on the energy-saving phenol-hydrogen peroxide hydroxylation post-material separation and purification device shown in Embodiment 1, in the present embodiment, the de-phenol two-column 5 is provided with a side take-off port for outputting light component impurities, part of the light component impurities is discharged through the side take-off port, so that the rectification separation effect of the de-phenol two-column 5 is improved, which is beneficial to further separating and recovering phenol from the column top, and is also beneficial to reducing the impurity content of the column bottom overhead product, so that the separation and purification effect is improved.

[0048] In the optional example of the present utility model, the side take-off port of the de-phenol two-column 5 is connected with the pipeline connecting the upper take-off port of the de-light column 7, so that the light component impurities output from the de-phenol two-column 5 and the light component impurities output from the de-light column 7 can be combined for processing, and the processing efficiency of the subsequent light component impurity processing procedure is improved.

[0049] Embodiment 7

[0050] Based on the energy-saving phenol hydrogen peroxide hydroxylation reaction material separation and purification device shown in Example 1, the outlet of the tower kettle of the extraction column 1 is connected to the stripping column 9, and the outlet of the tower kettle of the stripping column 9 outputs waste water, so that the oil phase material (extractant and target product) in the water phase of the tower kettle of the extraction column 1 is separated by the stripping column 9, further reducing the difficulty of subsequent waste water treatment; and the oil phase material output from the upper part of the stripping column 9 can be recycled, improving the yield. In the optional example of the present application, the part of the waste water is input into the subsequent waste water treatment process through the waste water output pipe 91.

[0051] Further, the upper outlet of the stripping column 9 is connected to the first phase separation device 21, and the water phase outlet of the first phase separation device 21 is connected to the upper part of the stripping column 9, so that the extractant contained in the extracted material of the tower kettle of the extraction column 1 can be further recovered, and the recovery and utilization of the extractant can be realized after phase separation by the first phase separation device 21.

[0052] Example 8

[0053] The present embodiment shows the process of the energy-saving phenol hydrogen peroxide hydroxylation reaction material separation and purification device under the specific working condition of the present application, and it should be noted that the present embodiment is only a better display, and does not limit the protection scope of the present application.

[0054] An energy-saving phenol hydrogen peroxide hydroxylation reaction material separation and purification process, specifically:

[0055] In the upstream reaction process, the raw material phenol and 27.5% hydrogen peroxide and process water, with a temperature of 75℃ and a flow rate of 25000kg / h, undergo hydroxylation reaction in the reactor, wherein the mass ratio of phenol, hydrogen peroxide and catalyst is 1:0.33:0.025, and the mass ratio of catalyst to process water in the catalyst slurry is 0.02:1, and the reaction generates reaction after material containing catechol, hydroquinone, water, catalyst and tar, unreacted hydrogen peroxide and phenol. After the catalyst separation and hydrogen peroxide decomposition reaction, the part of the material is obtained.

[0056] The extracted material enters the middle and upper part of the extraction column 1, the extraction agent diisopropyl ether enters from the extraction agent input pipe 12 connected to the bottom of the extraction column 1, and the oil phase containing catechol, hydroquinone, diisopropyl ether and the like extracted from the top of the extraction column 1 enters the extraction agent recovery column 2; the water phase containing water, a small amount of diisopropyl ether and sodium sulfate and the like extracted from the tower kettle of the extraction column 1, and the part of the water phase enters the stripping column 9.

[0057] The operating parameters of the extraction column 1 are:

[0058] Name Operating parameters Operating temperature at top of column °C 39.2 Operating temperature at bottom of column °C 44.3 Operating pressure kPaA 150

[0059] The operating parameters of the stripping column 9 are:

[0060] Name Operating parameters Operating temperature at top of column °C 135.2 Operating temperature at bottom of column °C 136.8 Operating pressure kPaA 210

[0061] The oil phase output from the extraction column 1 is input into the extractant recovery column 2; the overhead product of the extractant recovery column 2 is subjected to phase separation treatment by the first phase separation device 21 to obtain the extractant, and the column bottom product is input into the first dephenolization column 3.

[0062] The operating parameters of the extractant recovery column 2 are as follows:

[0063] Name Operating parameters Operating temperature at top of column °C 112.3 Operating temperature at bottom of column °C 145.2 Operating pressure kPaA 230 Reflux ratio 0.3 Theoretical plates 15 Feed location 5

[0064] The gas phase of the overhead of the first dephenolization column 3 is exchanged with saturated water from the first steam buffer tank 10-3 to condense and produce a gas-liquid mixture, which is subjected to separation by the first gas-liquid separation tank 10-1 to obtain 50 kPaA steam, and the condensed liquid of the gas phase of the overhead of the first dephenolization column 3 is returned to the first dephenolization column 3 as the overhead reflux, and the remaining part is output to a phenol raw material tank or directly to a reaction process for phenol recycling; the column bottom product of the first dephenolization column 3 is input into a de-coke column, the column bottom reboiler of the extractant recovery column 2 is heated by 400 kPaA steam, and the tank equipment and pipelines containing phenol are heated by 400 kPaA steam.

[0065] The operating parameters of the first dephenolization column 3 are as follows:

[0066] Name Operating parameters Operating temperature at top of column °C 106.3 Operating temperature at bottom of column °C 185.2 Operating pressure kPaA 50 Reflux ratio 1.1 Theoretical plates 13 Feed location 5

[0067] The gas phase of the overhead of the de-coke column 4 is exchanged with saturated water from the first gas-liquid separation tank 10-1 to condense and produce a gas-liquid mixture, which is subjected to separation by the first gas-liquid separation tank 10-1 to obtain 50 kPaA steam; the column bottom product of the de-coke column 4 is input into the second dephenolization column 5, and the tank equipment and pipelines containing phenol are heated by 400 kPaA steam; the tar output from the column bottom of the de-coke column 4 is input into a subsequent tar treatment process through a tar conveying pipe 41, and the conveying pipe can be heated by 1200 kPaA steam generated by the second steam buffer tank 10-5.

[0068] The operating parameters of the de-coke column 4 are as follows:

[0069]

[0070]

[0071] The gas phase of the overhead of the second dephenolization column 5 is exchanged with saturated water from the first gas-liquid separation tank 10-1 to condense and produce a gas-liquid mixture, which is subjected to separation by the first gas-liquid separation tank 10-1 to obtain 50 kPaA steam; the column bottom product of the second dephenolization column 5 is input into a phenol raw material tank or directly returned to a reaction process; and the column bottom product of the second dephenolization column 5 is input into the catechol column 6, and the tank equipment and pipelines are heated by 400 kPaA steam.

[0072] The operating parameters of the second dephenolization column 5 are as follows:

[0073] Name Operating parameters Operating temperature at top of column °C 117.9 Operating temperature at bottom of column °C 204.0 Operating pressure kPaA 10 Reflux ratio 3 Theoretical plates 45 Feed location 30 Name 12

[0074] The overhead gas phase of the catechol column 6 exchanges heat with saturated water from the second gas-liquid separation tank 10-9 and condenses to produce a gas-liquid mixture, which is separated by the second gas-liquid separation tank 10-9 to obtain 400 kPaA steam; the catechol product extracted from the overhead has a mass fraction of greater than 99.8%, and a yield of greater than 98%, and the material extracted from the column bottom is introduced into the light component removal column 7.

[0075] The operating parameters of the catechol column 6 are as follows:

[0076] Operating parameters Operating temperature at top of column °C Operating temperature at bottom of column °C 162.3 Operating pressure kPaA 206.8 Reflux ratio 8 Theoretical plates 3 Feed location 16 Name 8

[0077] The overhead gas phase of the light component removal column 7 exchanges heat with a heat conducting oil exchanger and condenses, and the light component impurities extracted from the overhead are introduced into an impurity tank; the material extracted from the column bottom is introduced into the hydroquinone column 8. The operating parameters of the light component removal column 7 are as follows:

[0078] Operating parameters Operating temperature at top of column °C Operating temperature at bottom of column °C 192.3 Operating pressure kPaA 203.6 Reflux ratio 6.1 Theoretical plates 3.9 Feed location 51 Name 16

[0079] The overhead gas phase of the hydroquinone column 8 exchanges heat with a heat conducting oil exchanger and condenses, and the hydroquinone product extracted from the overhead has a mass fraction of greater than 99.8% and a yield of greater than 95%, and the material extracted from the column bottom is returned to the de-creosote column 4, wherein the equipment and pipelines are all heated by 1200 kPaA steam. The operating parameters of the hydroquinone column 8 are as follows:

[0080] Operating parameters Operating temperature at top of column °C Operating temperature at bottom of column °C 191.8 Operating pressure kPaA 200.6 Reflux ratio 5.6 Theoretical plates 3 Feed location 35 Name Operating parameters Operating temperature at top of column °C Operating temperature at bottom of column °C Operating pressure kPaA Reflux ratio Theoretical plates Feed location 20

[0081] The heat conducting oil exchanged with the overheads of the light component removal column 7 and the hydroquinone column 8 exchanges heat with saturated water from the second gas-liquid separation tank 10-9, and the heat recovered by the gas-liquid mixture of 400 kPaA is returned to the second gas-liquid separation tank 10-9.

[0082] The catechol and hydroquinone obtained from the catechol column 6 and the hydroquinone column 8 are introduced into a product tabletting and packaging process to obtain a final product. The equipment and pipelines of the product tabletting and packaging process are heated by 1200 kPaA steam.

[0083] In this embodiment, the catechol column 6 saves energy consumption of 0.524 Gcal / h, the light component removal column 7 saves energy consumption of 1.524 Gcal / h, and the hydroquinone column 8 saves energy consumption of 0.787 Gcal / h.

[0084] It should be noted that the above content is a further detailed description of the utility model made in combination with specific embodiments, and the specific implementation of the utility model cannot be limited to these descriptions. For ordinary skilled persons in the technical field to which the utility model belongs, a number of simple improvements can be made without departing from the concept of the utility model, and all of these should be regarded as falling within the scope of protection of the utility model.

Claims

1. An energy-saving device for separating and purifying materials after the hydroxylation reaction of phenol and hydrogen peroxide, characterized in that, It includes an extraction tower (1), an extractant recovery tower (2), a phenol removal tower (3), a tar removal tower (4), a phenol removal tower (5), a catechol tower (6), a light phenol removal tower (7), and a hydroquinone tower (8), wherein: The first inlet of the extraction tower (1) is connected to the input pipe (11) of the material to be separated and purified, and the second inlet is connected to the input pipe (12) of the extractant. The upper outlet of the extraction tower (1) is connected to the inlet of the extractant recovery tower (2). The bottom outlet of the extractant recovery tower (2) is connected to the inlet of the phenol removal tower (3). The top of the extractant recovery tower (2) is connected to the first phase separation device (21). The aqueous phase outlet of the first phase separation device (21) is connected to the upper part of the extraction tower (1) and the oil phase outlet outputs the recovered extractant. The bottom outlet of the phenol removal tower (3) is connected to the inlet of the tar removal tower (4); the top of the phenol removal tower (3) is connected to the second phase separation device (31), and the oil phase outlet of the second phase separation device (31) is connected to the upper part of the phenol removal tower (3) and a branch for outputting recovered phenol is provided. The upper outlet of the tar removal tower (4) is connected to the inlet of the phenol removal tower (5); The bottom outlet of the phenol removal tower (5) is connected to the inlet of the catechol tower (6), and the upper outlet of the phenol removal tower (5) outputs the recovered phenol. The upper outlet of the catechol tower (6) outputs high-purity catechol product, and its bottom is connected to the inlet of the light removal tower (7). The upper outlet of the light component removal tower (7) outputs light component impurities, and its bottom is connected to the inlet of the hydroquinone tower (8). The upper part of the hydroquinone tower (8) outputs high-purity hydroquinone product, while the bottom of the tower outputs heavy component impurities. It also includes a first gas-liquid separator (10-1), the liquid phase outlet of the first gas-liquid separator (10-1) is connected to the refrigerant inlet of the heat exchanger at the top of the phenol removal tower (3) via a pipeline, the feed inlet of the first gas-liquid separator (10-1) is connected to the refrigerant outlet of the heat exchanger at the top of the phenol removal tower (3); the gas phase outlet of the first gas-liquid separator (10-1) is connected to the air inlet of the first steam compressor (10-2), and secondary steam A (v1) is output from the air outlet of the first compressor.

2. The energy-saving phenol-hydrogen peroxide hydroxylation reaction material separation and purification device according to claim 1, characterized in that, The liquid outlet of the first gas-liquid separator (10-1) is connected via pipeline to the heat exchanger at the top of the tar removal tower (4) and / or the refrigerant inlet of the heat exchanger at the top of the phenol removal tower (5), and the feed inlet of the first gas-liquid separator (10-1) is connected to the refrigerant outlet of the heat exchanger at the top of the tar removal tower (4) and / or the heat exchanger at the top of the phenol removal tower (5).

3. The energy-saving phenol-hydrogen peroxide hydroxylation reaction material separation and purification device according to claim 1, characterized in that, The outlet of the first steam compressor (10-2) is connected to the inlet of the second steam compressor (10-4), and the outlet of the second steam compressor (10-4) outputs recompressed steam (v2).

4. The energy-saving phenol-hydrogen peroxide hydroxylation reaction post-material separation and purification device according to claim 3, characterized in that, The outlet of the second steam compressor (10-4) is connected to the inlet of the third steam compressor (10-6), and the outlet of the third steam compressor (10-6) outputs tertiary compressed steam (v3).

5. The energy-saving phenol-hydrogen peroxide hydroxylation reaction material separation and purification device according to claim 1, characterized in that, It also includes a steam generator (10-8) and a second gas-liquid separator (10-9); the oil outlet pipe of the steam generator (10-8) is connected to the refrigerant inlet of the heat exchanger at the top of the light-light removal tower (7) and the hydroquinone tower (8), and the oil inlet pipe of the steam generator (10-8) is connected to the refrigerant outlet of the heat exchanger at the top of the light-light removal tower (7) and the hydroquinone tower (8); the outlet of the steam generator (10-8) is connected to the inlet of the second gas-liquid separator (10-9), and secondary steam B (v4) is output from the gas phase outlet of the second gas-liquid separator (10-9).

6. The energy-saving phenol-hydrogen peroxide hydroxylation reaction post-material separation and purification device according to claim 5, characterized in that, The liquid phase outlet of the second gas-liquid separator (10-9) is connected to the refrigerant inlet of the top heat exchanger of the catechol column and / or the feed inlet of the steam generator (10-8); the refrigerant outlet of the top heat exchanger of the catechol column (6) is connected to the feed inlet of the second gas-liquid separator (10-9).

7. The energy-saving phenol-hydrogen peroxide hydroxylation reaction post-material separation and purification device according to claim 1, characterized in that, The bottom outlet of the hydroquinone tower (8) is connected to the tar removal tower (4).

8. The energy-saving phenol-hydrogen peroxide hydroxylation reaction material separation and purification device according to claim 1, characterized in that, The phenol removal tower (5) is equipped with a side sampling port for outputting light component impurities.

9. The energy-saving phenol-hydrogen peroxide hydroxylation reaction material separation and purification device according to claim 1, characterized in that, The bottom outlet of the extraction tower (1) is connected to the stripping tower (9), and the bottom outlet of the stripping tower (9) outputs wastewater.

10. The energy-saving phenol-hydrogen peroxide hydroxylation reaction material separation and purification device according to claim 9, characterized in that, The upper outlet of the stripping tower (9) is connected to the first phase separation device (21), and the water phase outlet of the first phase separation device (21) is connected to the upper part of the stripping tower (9).

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