A method for producing butadiene and acid activated bleaching earth from a deteriorated sulfolane

Abstract

The application relates to a method for recycling deteriorated sulfolane to produce butadiene and acid active clay, which comprises a deteriorated sulfolane solvent cooler, a solvent decoloring tank, an extraction column feeding pump, an extraction column body, an extractant heater, an extractant pump, a butadiene flash tank body, a mixed acid tank, a mixed acid pump, an activation reactor, a filter, a dryer and a crushing collector, and the outlet of the deteriorated sulfolane solvent cooler is connected with the solvent decoloring tank through a first pipeline. In the method, butadiene gas is released from the top of the butadiene flash tank body, the extractant pump is used to send the extractant to the extraction column body for recycling from the bottom of the butadiene flash tank body, the acid liquid at the top of the extraction column body is self-pressurized to the mixed acid tank, the mixed acid pump is used to pressurize the mixed acid to the white clay activation reactor to perform an activation reaction with bentonite, and a series of operations such as filtering, drying and crushing are performed on the reaction product to obtain the acid active clay.

Description

Technical Field

[0001] This invention relates to the field of degraded sulfolane technology, specifically a method for reusing degraded sulfolane to produce butadiene and acidic activated clay. Background Technology

[0002] Degraded sulfolane is a colorless and transparent liquid, an excellent aprotic polar solvent, miscible with water, acetone, and toluene, and is also an ideal solvent in the aromatic hydrocarbon extraction process in petrochemicals. Sulfolane is easily decomposed at high temperatures. Below 220℃, the decomposition rate is relatively slow, but above 220℃, the decomposition rate increases sharply with increasing temperature. Excessively high temperatures will cause sulfolane to decompose into black polymers and sulfur dioxide. In the presence of air, due to the oxidation effect of air, the amount of sulfur dioxide released in the solvent system is greater than when no air is present. Butadiene is an organic compound, a colorless gas with a slightly aromatic odor, insoluble in water, but soluble in most organic solvents such as acetone, benzene, acetic acid, and esters. It is a raw material for manufacturing synthetic rubber, synthetic resins, and nylon. Acidic activated clay is a grayish-white granular powder with a large specific surface area and pore volume. It has special adsorption capacity and ion exchange performance, strong decolorization ability and activity, and good stability after decolorization.

[0003] In the process of reusing degraded sulfolane, butadiene and acid activated clay are usually processed to facilitate cooling and heating of butadiene and acid activated clay. However, in the extraction and distillation unit, which uses sulfolane solvent to extract aromatics, the solvent degrades and decomposes due to factors such as oxygen, acidic substances, and high temperature during recycling. This degrades and decomposes the sulfolane solvent, producing butadiene, sulfonic acid, and sulfuric acid, which are deposited at the bottom of the solvent regeneration tower and discharged as waste residue. This not only wastes sulfolane solvent but also pollutes the atmosphere and the surrounding environment, making it inconvenient to use and unable to meet the actual production needs of degraded sulfolane. Summary of the Invention

[0004] (a) Technical problems to be solved

[0005] To address the shortcomings of existing technologies, this invention provides a method for reusing degraded sulfolane to produce butadiene and acidic activated clay. This method offers advantages such as a series of operations including filtration, drying, and pulverization. It solves the problem that in extraction distillation units using sulfolane solvent to extract aromatics, the solvent degrades and decomposes during recycling due to factors such as oxygen, acidic substances, and high temperatures. This degrades and decomposes the solvent, producing butadiene, sulfonic acid, and sulfuric acid, which accumulate at the bottom of the solvent regeneration tower and are ultimately discharged as waste. This not only wastes sulfolane solvent but also pollutes the atmosphere and surrounding environment, making it inconvenient to use and unable to meet the actual production needs of degraded sulfolane.

[0006] (II) Technical Solution

[0007] To achieve the above objectives, the present invention provides the following technical solution: a method for reusing degraded sulfolane to produce butadiene and acidic activated clay, comprising a degraded sulfolane solvent cooler, a solvent decolorization tank, an extraction tower feed pump, an extraction tower body, an extractant heater, an extractant pump, a butadiene flash tank body, a mixed acid tank, a mixed acid pump, an activation reactor, a filter, a dryer, and a pulverizer collector. The outlet of the degraded sulfolane solvent cooler is connected to the solvent decolorization tank via a first pipeline. The outlet of the solvent decolorization tank is connected to the extraction tower feed pump via a second pipeline. The outlet of the extraction tower feed pump is connected to the extraction tower body via a third pipeline. The inlet of the extraction tower body... The extraction tower body is connected to the extractant heater via a fourth pipeline. The inlet of the extractant heater is connected to the extractant pump via a fifth pipeline. The outlet of the extraction tower body is connected to the butadiene flash tank via a sixth pipeline. The outlet of the extraction tower body is connected to the mixed acid tank via a seventh pipeline. The outlet of the mixed acid tank is connected to the mixed acid pump via an eighth pipeline. The outlet of the mixed acid pump is connected to the activation reactor via a ninth pipeline. The outlet of the activation reactor is connected to the filter via a tenth pipeline. The outlet of the filter is connected to the dryer via an eleventh pipeline. The outlet of the dryer is connected to the pulverizer collector via a twelfth pipeline.

[0008] Furthermore, the seventh pipeline is fixedly connected to the outside of the extraction tower top mixed acid outlet valve, the seventh pipeline is a mixed acid self-pressurized pipeline, and the fourth pipeline is an extractant circulation pipeline.

[0009] Furthermore, a gas phase pipeline on the top of the flash tank is fixedly connected to the outside of the butadiene flash tank body, and an external valve on the top of the flash tank is fixedly connected to the outside of the gas phase pipeline on the top of the flash tank.

[0010] Furthermore, a liquid phase pipeline at the bottom of the regeneration tower is fixedly connected to the outside of the degraded sulfolane solvent cooler, and a liquid phase outlet valve at the bottom of the regeneration tower is fixedly connected to the outside of the liquid phase pipeline at the bottom of the regeneration tower.

[0011] Furthermore, the outlet of the butadiene flash tank body is connected to the extractant pump through a first connecting pipe, and a solvent regeneration tower is fixedly connected to the outside of the gas phase pipeline on the top of the flash tank, and the gas phase pipeline on the top of the flash tank is connected to the solvent regeneration tower.

[0012] Furthermore, a flash tube is fixedly connected to the outside of the butadiene flash tank body, an extraction tube is fixedly connected to the outside of the extraction tower body, and a fixing tube is fixedly connected to the outside of the mixed acid tank.

[0013] Furthermore, the degraded sulfolane solvent cooler can be used to cool the degraded sulfolane mixture at the bottom of the regeneration tower to a suitable temperature, and the solvent decolorization tank can be used to decolorize the degraded sulfolane and filter out heavy polymers, mechanical impurities and suspended solids in the degraded sulfolane.

[0014] Furthermore, the extraction tower body can facilitate solvent extraction and separation of acidic substances such as sulfuric acid and sulfonic acid, as well as butadienes; the mixed acid tank can be used to recover acidic substances from degraded sulfolane; and the activation reactor can be used to react acidic substances with bentonite to generate activated clay.

[0015] Furthermore, the dryer can use infrared light to dry acidic activated clay and shape it, the pulverizer and collector is used to pulverize the clay into granules, and the butadiene flash tank body can use pressure flash evaporation to separate butadiene and extractant.

[0016] A method for reusing degraded sulfolane to produce butadiene and acidic activated clay includes the following steps:

[0017] 1) The 170-175℃ degraded sulfolane solvent flowing out from the bottom of the solvent regeneration tower by gravity and static pressure is cooled to 90-95℃ by the degraded sulfolane solvent cooler;

[0018] 2) After being supercooled, the degraded sulfolane solvent enters the solvent decolorization tank to remove suspended solids, mechanical impurities and heavy polymers. Then, it is pressurized by the extraction tower feed pump and sent to the middle of the extraction tower body at a pressure of 1.0-1.2MPa. The impurities accumulated in the decolorization tank are periodically discharged to the underground sludge tank.

[0019] 3) The extractant enters from the top of the extraction tower body, and after contacting the degraded sulfolane solvent, it absorbs butadiene-type extractants. Due to the large pressure difference between the pressurized extraction tower body and the butadiene flash tank body, it can enter the butadiene flash tank body by its own pressure.

[0020] 4) The rich solvent entering the butadiene flash tank body at a pressure of -30 to 0 kPa and a temperature of 60 to 70°C will be converted into a gas-liquid two-phase system due to flashing. After opening the external valve on the top of the butadiene flash tank, the butadiene will be discharged from the gas phase pipeline on the top of the flash tank.

[0021] 5) The liquid extractant in the butadiene flash tank is pressurized by the extractant pump and heated to 100-105℃ by the extractant heater through the extractant circulation pipeline before being sent to the extraction tower for recycling.

[0022] 6) The acidic liquid mixture that is not absorbed by the extractant accumulates at the top of the extraction tower. Open the mixed acid outlet valve at the top of the extraction tower, and the mixed acid enters the mixed acid tank through the mixed acid self-pressurization pipeline.

[0023] 7) The mixed acid in the mixing tank is pumped to the activation reactor. The activation reactor contains bentonite with a particle size of 10-15 μm. The solid-liquid ratio of bentonite to acid is 2-5:1. The activation reaction is carried out at a reaction temperature of 80-90℃ and a reaction pressure of 0.25 MPa for 0.5-1.5 hours. Acidic activated clay is produced after stirring during the activation reaction.

[0024] 8) The reaction products of the activated reactor are filtered to remove impurities using ceramic balls and ceramic sand, then enter an air dryer to remove moisture, and finally pass through a crusher and collector to produce qualified granular acidic activated clay.

[0025] (III) Beneficial Effects

[0026] Compared with the prior art, the technical solution of this application has the following beneficial effects:

[0027] 1. This method for reusing degraded sulfolane to produce butadiene and acidic activated clay utilizes the coordinated action of a degraded sulfolane solvent cooler, solvent decolorization tank, extraction tower feed pump, extraction tower body, extractant heater, extractant pump, butadiene flash tank body, mixed acid tank, mixed acid pump, activation reactor, filter, dryer, pulverizer collector, mixed acid outlet valve at the top of the extraction tower, external valve at the top of the butadiene flash tank, liquid phase outlet valve at the bottom of the regeneration tower, and the gas phase pipeline at the top of the flash tank and the liquid phase pipeline at the bottom of the regeneration tower. This allows the reaction products to undergo a series of operations including filtration, drying, and pulverization to obtain acidic activated clay. An extractant is then used to separate acidic substances and butadiene from the degraded sulfolane, producing acidic activated clay and butadiene, with high-purity butadiene as a byproduct.

[0028] 2. In this method of reusing degraded sulfolane to produce butadiene and acidic activated clay, the sulfolane solvent at the bottom of the solvent regeneration tower, after being cooled by a degraded sulfolane solvent cooler, enters a solvent decolorization tank to remove impurities, and then enters the pressurized extraction tower body. The bottom of the extraction tower body contains a rich liquid that has absorbed butadiene. The rich liquid enters the reduced pressure butadiene flash tank body under pressure. Butadiene gas is released from the top of the butadiene flash tank body. The extractant pump at the bottom of the butadiene flash tank body sends the extractant to the extraction tower body for recycling. The acidic liquid at the top of the extraction tower body is pressurized to a mixed acid tank. The mixed acid pump pressurizes the mixed acid and sends it to the clay activation reactor to activate it with bentonite. The reaction product is filtered, dried, and pulverized to obtain acidic activated clay. Attached Figure Description

[0029] Figure 1 This is a flowchart illustrating the structure of the present invention.

[0030] In the diagram: 1. Degraded sulfolane solvent cooler; 2. Solvent decolorization tank; 3. Extraction tower feed pump; 4. Extraction tower body; 5. Extractant heater; 6. Extractant pump; 7. Butadiene flash tank body; 8. Mixed acid tank; 9. Mixed acid pump; 10. Activation reactor; 11. Filter; 12. Dryer; 13. Pulverizer collector; 14. Mixed acid outlet valve at the top of the extraction tower; 15. External valve at the top of the butadiene flash tank; 16. Liquid phase outlet valve at the bottom of the regeneration tower; 17. Gas phase pipeline at the top of the flash tank; 18. Liquid phase pipeline at the bottom of the regeneration tower. Detailed Implementation

[0031] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0032] Please see Figure 1 This embodiment describes a method for reusing degraded sulfolane to produce butadiene and acidic activated clay, comprising a degraded sulfolane solvent cooler 1, a solvent decolorization tank 2, an extraction tower feed pump 3, an extraction tower body 4, an extractant heater 5, an extractant pump 6, a butadiene flash tank body 7, a mixed acid tank 8, a mixed acid pump 9, an activation reactor 10, a filter 11, a dryer 12, and a pulverizer collector 13. The outlet of the degraded sulfolane solvent cooler 1 is connected to the solvent decolorization tank 2 via a first pipeline. The outlet of the solvent decolorization tank 2 is connected to the extraction tower feed pump 3 via a second pipeline. The outlet of the extraction tower feed pump 3 is connected to the extraction tower body 4 via a third pipeline. The inlet of the extraction tower body 4 is... The extraction tower body 4 is connected to the extractant heater 5 via the fourth pipeline. The inlet of the extractant heater 5 is connected to the extractant pump 6 via the fifth pipeline. The outlet of the extraction tower body 4 is connected to the butadiene flash tank body 7 via the sixth pipeline. The outlet of the extraction tower body 4 is connected to the mixed acid tank 8 via the seventh pipeline. The outlet of the mixed acid tank 8 is connected to the mixed acid pump 9 via the eighth pipeline. The outlet of the mixed acid pump 9 is connected to the activation reactor 10 via the ninth pipeline. The outlet of the activation reactor 10 is connected to the filter 11 via the tenth pipeline. The outlet of the filter 11 is connected to the dryer 12 via the eleventh pipeline. The outlet of the dryer 12 is connected to the pulverizer collector 13 via the twelfth pipeline.

[0033] The seventh pipeline is fixedly connected to the outside of the mixed acid outlet valve 14 at the top of the extraction tower. The seventh pipeline is a self-pressurized mixed acid pipeline, and the fourth pipeline is an extractant circulation pipeline. By setting the mixed acid outlet valve 14 at the top of the extraction tower, the self-pressurized mixed acid pipeline can be opened or closed. The butadiene flash tank body 7 is fixedly connected to the outside of the flash tank top gas phase pipeline 17. The butadiene flash tank top external valve 15 is fixedly connected to the outside of the flash tank top gas phase pipeline 17. By setting the butadiene flash tank top external valve 15, the flash tank top gas phase pipeline 17 can be opened or closed.

[0034] The outer side of the degraded sulfolane solvent cooler 1 is fixedly connected to the bottom liquid phase pipeline 18 of the regeneration tower. The outer side of the bottom liquid phase pipeline 18 of the regeneration tower is fixedly connected to the bottom liquid phase outlet valve 16 of the regeneration tower. By setting the bottom liquid phase outlet valve 16 of the regeneration tower, the bottom liquid phase pipeline 18 of the regeneration tower can be opened or closed. The outlet of the butadiene flash tank body 7 is connected to the extractant pump 6 through the first connecting pipe. The outer side of the flash tank top gas phase pipeline 17 is fixedly connected to the solvent regeneration tower. The flash tank top gas phase pipeline 17 is connected to the solvent regeneration tower. The outer side of the butadiene flash tank body 7 is fixedly connected to the flash pipe. The outer side of the extraction tower body 4 is fixedly connected to the extraction pipe. The outer side of the mixed acid tank 8 is fixedly connected to the fixed pipe.

[0035] The degraded sulfolane solvent cooler 1 can be used to cool the degraded sulfolane mixture at the bottom of the regeneration tower to a suitable temperature. The solvent decolorization tank 2 can be used to decolorize the degraded sulfolane and filter heavy polymers, mechanical impurities and suspended solids in the degraded sulfolane. The extraction tower body 4 can facilitate solvent extraction and separation of acidic substances such as sulfuric acid and sulfonic acid and butadiene. The mixed acid tank 8 can be used to recover acidic substances in the degraded sulfolane. The activation reactor 10 can be used to react acidic substances and bentonite to generate activated clay. The dryer 12 can use infrared light to dry the acidic activated clay and shape it. The pulverizer collector 13 is used to pulverize the clay into granules. The butadiene flash evaporator body 7 can use pressure flash evaporation to separate butadiene and extractant.

[0036] Example 1: A method for reusing degraded sulfolane to produce butadiene and acidic activated clay, comprising the following steps:

[0037] 1) The 170°C degraded sulfolane solvent flowing out from the bottom of the solvent regeneration tower by gravity and static pressure is cooled to 90°C by the degraded sulfolane solvent cooler 1;

[0038] 2) After being cooled, the degraded sulfolane solvent enters the solvent decolorization tank 2 to remove suspended solids, mechanical impurities and heavy polymers. After being pressurized by the extraction tower feed pump 3, it is sent to the middle of the extraction tower body 4 with a pressure of 1.0 MPa. The impurities accumulated in the decolorization tank are periodically discharged to the underground sludge tank.

[0039] 3) The extractant enters from the top of the extraction tower body 4 and absorbs butadiene extractant after contacting the deteriorated sulfolane solvent. Due to the large pressure difference between the pressurized extraction tower body 4 and the butadiene flash tank body 7, it can enter the butadiene flash tank body 7 by its own pressure.

[0040] 4) The solvent-rich material entering the butadiene flash tank body 7 at a pressure of -30 kPa and a temperature of 60°C will be converted into a gas-liquid two-phase system due to flashing. The butadiene flash tank top external valve 15 will be opened, and the butadiene will be discharged from the gas phase pipeline 17 at the top of the flash tank.

[0041] 5) The liquid extractant in the butadiene flash tank body 7 is pressurized by the extractant pump 6 and heated to 100°C through the extractant circulation pipeline and the extractant heater 5 before being sent to the extraction tower body 4 for recycling.

[0042] 6) The acidic liquid mixture that is not absorbed by the extractant accumulates at the top of the extraction tower body 4. The mixed acid outlet valve 14 at the top of the extraction tower is opened, and the mixed acid enters the mixed acid tank 8 through the mixed acid self-pressurization pipeline.

[0043] 7) The mixed acid in the mixing acid tank 8 is sent to the activation reactor 10 via the mixing acid pump 9. The activation reactor 10 contains bentonite with a particle size of 10 μm. The solid-liquid ratio of bentonite to acid is 2:1. The activation reaction is carried out at a reaction temperature of 80℃ and a reaction pressure of 0.25 MPa for 0.5 h. The activation time varies depending on the acid concentration of the mixed acid. Acidic activated clay is produced by stirring during the activation reaction.

[0044] 8) The reaction product of the activated reactor 10 passes through the filter 11 to remove impurities using ceramic balls and ceramic sand, then enters the air dryer 12 to remove moisture, and finally passes through the crusher and collector 13 to produce qualified granular acidic activated clay.

[0045] Example 2: A method for reusing degraded sulfolane to produce butadiene and acidic activated clay, comprising the following steps:

[0046] 1) The 175°C degraded sulfolane solvent flowing out from the bottom of the solvent regeneration tower by gravity and static pressure is cooled to 95°C by the degraded sulfolane solvent cooler 1;

[0047] 2) After being cooled, the degraded sulfolane solvent enters the solvent decolorization tank 2 to remove suspended solids, mechanical impurities and heavy polymers. Then, it is pressurized by the extraction tower feed pump 3 and sent to the middle of the extraction tower body 4 at a pressure of 1.2 MPa. The impurities accumulated in the decolorization tank are periodically discharged to the underground sludge tank.

[0048] 3) The extractant enters from the top of the extraction tower body 4 and absorbs butadiene extractant after contacting the deteriorated sulfolane solvent. Due to the large pressure difference between the pressurized extraction tower body 4 and the butadiene flash tank body 7, it can enter the butadiene flash tank body 7 by its own pressure.

[0049] 4) The rich solvent entering the butadiene flash tank body 7 at a pressure of 0 kPa and a temperature of 70°C will be converted into a gas-liquid two-phase system due to flashing. The butadiene flash tank top external valve 15 will be opened, and the butadiene will be discharged from the gas phase pipeline 17 at the top of the flash tank.

[0050] 5) The liquid extractant in the butadiene flash tank body 7 is pressurized by the extractant pump 6 and heated to 105°C through the extractant circulation pipeline and the extractant heater 5 before being sent to the extraction tower body 4 for recycling.

[0051] 6) The acidic liquid mixture that is not absorbed by the extractant accumulates at the top of the extraction tower body 4. The mixed acid outlet valve 14 at the top of the extraction tower is opened, and the mixed acid enters the mixed acid tank 8 through the mixed acid self-pressurization pipeline.

[0052] 7) The mixed acid in the mixing acid tank 8 is sent to the activation reactor 10 via the mixing acid pump 9. The activation reactor 10 contains bentonite with a particle size of 15 μm. The solid-liquid ratio of bentonite to acid is 5:1. The activation reaction is carried out at a reaction temperature of 90℃ and a reaction pressure of 0.25 MPa for 1.5 hours. The activation time varies depending on the acid concentration of the mixed acid. Acidic activated clay is produced by stirring during the activation reaction.

[0053] 8) The reaction product of the activated reactor 10 passes through the filter 11 to remove impurities using ceramic balls and ceramic sand, then enters the air dryer 12 to remove moisture, and finally passes through the crusher and collector 13 to produce qualified granular acidic activated clay.

[0054] Example 3: A method for reusing degraded sulfolane to produce butadiene and acidic activated clay, characterized by comprising the following steps:

[0055] 1) The 173°C degraded sulfolane solvent flowing out from the bottom of the solvent regeneration tower by gravity is cooled to 93°C by the degraded sulfolane solvent cooler 1;

[0056] 2) After being cooled, the degraded sulfolane solvent enters the solvent decolorization tank 2 to remove suspended solids, mechanical impurities and heavy polymers. Then, it is pressurized by the extraction tower feed pump 3 and sent to the middle of the extraction tower body 4 at a pressure of 1.1 MPa. The impurities accumulated in the decolorization tank are periodically discharged to the underground sludge tank.

[0057] 3) The extractant enters from the top of the extraction tower body 4 and absorbs butadiene extractant after contacting the deteriorated sulfolane solvent. Due to the large pressure difference between the pressurized extraction tower body 4 and the butadiene flash tank body 7, it can enter the butadiene flash tank body 7 by its own pressure.

[0058] 4) The solvent-rich material entering the butadiene flash tank body 7 at a pressure of -15KPa and a temperature of 65℃ will be converted into a gas-liquid two-phase system due to flashing. The butadiene flash tank top external valve 15 will be opened, and the butadiene will be discharged from the gas phase pipeline 17 at the top of the flash tank.

[0059] 5) The liquid extractant in the butadiene flash tank body 7 is pressurized by the extractant pump 6 and heated to 103°C through the extractant circulation pipeline and the extractant heater 5 before being sent to the extraction tower body 4 for recycling.

[0060] 6) The acidic liquid mixture that is not absorbed by the extractant accumulates at the top of the extraction tower body 4. The mixed acid outlet valve 14 at the top of the extraction tower is opened, and the mixed acid enters the mixed acid tank 8 through the mixed acid self-pressurization pipeline.

[0061] 7) The mixed acid in the mixing acid tank 8 is sent to the activation reactor 10 via the mixing acid pump 9. The activation reactor 10 contains bentonite with a particle size of 13 μm. The solid-liquid ratio of bentonite to acid is 3:1. The activation reaction is carried out at a reaction temperature of 85℃ and a reaction pressure of 0.25 MPa for 1.0 h. The activation time varies depending on the acid concentration of the mixed acid. Acidic activated clay is produced by stirring during the activation reaction.

[0062] 8) The reaction product of the activated reactor 10 passes through the filter 11 to remove impurities using ceramic balls and ceramic sand, then enters the air dryer 12 to remove moisture, and finally passes through the crusher and collector 13 to produce qualified granular acidic activated clay.

[0063] The working principle of the above embodiments is as follows:

[0064] (1) Through the coordinated action of the deteriorated sulfolane solvent cooler 1, solvent decolorization tank 2, extraction tower feed pump 3, extraction tower body 4, extractant heater 5, extractant pump 6, butadiene flash tank body 7, mixed acid tank 8, mixed acid pump 9, activation reactor 10, filter 11, dryer 12, pulverizer collector 13, mixed acid outlet valve at the top of extraction tower 14, external valve at the top of butadiene flash tank 15, liquid phase outlet valve at the bottom of regeneration tower 16, gas phase pipeline at the top of flash tank 17 and liquid phase pipeline at the bottom of regeneration tower 18, the reaction product can be filtered, dried and pulverized to obtain acidic activated clay. The acidic substances and butadiene in the deteriorated sulfolane are separated by the extractant to produce acidic activated clay and butadiene, and high-purity butadiene is produced as a by-product.

[0065] (2) The sulfolane solvent at the bottom of the solvent regeneration tower, which has deteriorated at high temperature, is cooled by the sulfolane solvent cooler 1 and then enters the solvent decolorization tank 2 to remove impurities. After that, it enters the pressurized extraction tower body 4. The bottom of the extraction tower body 4 is a rich liquid that has absorbed butadiene. The rich liquid enters the reduced pressure butadiene flash tank body 7 by self-pressure. The top of the butadiene flash tank body 7 releases butadiene gas. The bottom of the butadiene flash tank body 7 is pumped by the extractant pump 6 to the extraction tower body 4 for recycling. The acidic liquid at the top of the extraction tower body 4 is pumped by self-pressure to the mixed acid tank 8. The mixed acid pump 9 pressurizes the mixed acid and sends it to the clay activation reactor 10 to activate the bentonite. The reaction product is filtered, dried and crushed to obtain acidic activated clay.

[0066] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0067] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for producing butadiene and acidic activated clay by reusing degraded sulfolane, comprising a degraded sulfolane solvent cooler (1), a solvent decolorization tank (2), an extraction tower feed pump (3), an extraction tower body (4), an extractant heater (5), an extractant pump (6), a butadiene flash tank body (7), a mixed acid tank (8), a mixed acid pump (9), an activation reactor (10), a filter (11), a dryer (12), and a pulverizer collector (13), characterized in that: The outlet of the degraded sulfolane solvent cooler (1) is connected to the solvent decolorization tank (2) via a first pipeline. The outlet of the solvent decolorization tank (2) is connected to the extraction tower feed pump (3) via a second pipeline. The outlet of the extraction tower feed pump (3) is connected to the extraction tower body (4) via a third pipeline. The inlet of the extraction tower body (4) is connected to the extractant heater (5) via a fourth pipeline. The inlet of the extractant heater (5) is connected to the extractant pump (6) via a fifth pipeline. The outlet of the extraction tower body (4) is connected to the butadiene flash tank body via a sixth pipeline. (7) The outlet of the extraction tower body (4) is connected to the mixing acid tank (8) through the seventh pipeline. The outlet of the mixing acid tank (8) is connected to the mixing acid pump (9) through the eighth pipeline. The outlet of the mixing acid pump (9) is connected to the activation reactor (10) through the ninth pipeline. The outlet of the activation reactor (10) is connected to the filter (11) through the tenth pipeline. The outlet of the filter (11) is connected to the dryer (12) through the eleventh pipeline. The outlet of the dryer (12) is connected to the pulverizer collector (13) through the twelfth pipeline. The seventh pipeline is fixedly connected to the outside of the mixed acid outlet valve (14) at the top of the extraction tower. The seventh pipeline is a self-pressurized mixed acid pipeline. The fourth pipeline is an extractant circulation pipeline. The butadiene flash tank body (7) is fixedly connected to the outer side of the flash tank top gas phase pipeline (17), and the butadiene flash tank top external valve (15) is fixedly connected to the outer side of the flash tank top gas phase pipeline (17). The degraded sulfolane solvent cooler (1) is fixedly connected to the outside of the bottom liquid phase pipeline (18) of the regeneration tower, and the bottom liquid phase outlet valve (16) of the regeneration tower is fixedly connected to the outside of the bottom liquid phase pipeline (18). The outlet of the butadiene flash tank body (7) is connected to the extractant pump (6) through a first connecting pipe. A solvent regeneration tower is fixedly connected to the outside of the gas phase pipeline (17) on the top of the flash tank. The gas phase pipeline (17) on the top of the flash tank is connected to the solvent regeneration tower.

2. The method for reusing degraded sulfolane to produce butadiene and acidic activated clay according to claim 1, characterized in that: A flash tube is fixedly connected to the outside of the butadiene flash tank body (7), an extraction tube is fixedly connected to the outside of the extraction tower body (4), and a fixed tube is fixedly connected to the outside of the mixed acid tank (8).

3. The method for reusing degraded sulfolane to produce butadiene and acidic activated clay according to claim 1, characterized in that: The degraded sulfolane solvent cooler (1) is used to cool the degraded sulfolane mixture at the bottom of the regeneration tower to a suitable temperature, and the solvent decolorization tank (2) is used to decolorize the degraded sulfolane and filter out heavy polymers, mechanical impurities and suspended solids in the degraded sulfolane.

4. The method for reusing degraded sulfolane to produce butadiene and acidic activated clay according to claim 1, characterized in that: The extraction tower body (4) is conducive to solvent extraction and separation of sulfuric acid, sulfonic acid and butadiene, the mixed acid tank (8) is used to recover acidic substances in deteriorated sulfolane, and the activation reactor (10) is used to react acidic substances and bentonite to generate activated clay.

5. The method for reusing degraded sulfolane to produce butadiene and acidic activated clay according to claim 1, characterized in that: The dryer (12) uses infrared light to dry acidic activated clay and shape it. The pulverizer (13) is used to pulverize the clay into granules. The butadiene flash tank body (7) uses pressure flash evaporation to separate butadiene and extractant.

6. The method for reusing degraded sulfolane to produce butadiene and acidic activated clay according to claim 1, characterized in that, Includes the following steps: 1) The 170-175℃ degraded sulfolane solvent flowing out from the bottom of the solvent regeneration tower by gravity is cooled to 90-95℃ by the degraded sulfolane solvent cooler (1); 2) After being cooled, the degraded sulfolane solvent enters the solvent decolorization tank (2) to remove suspended solids, mechanical impurities and heavy polymers. After being pressurized by the extraction tower feed pump (3), it is sent to the middle of the extraction tower body (4) with a pressure of 1.0-1.2MPa. The impurities accumulated in the decolorization tank are periodically discharged to the underground sludge tank. 3) The extractant enters from the top of the extraction tower body (4), and after contacting the deteriorated sulfolane solvent, it absorbs butadiene-type extractant. Due to the pressure difference between the pressurized extraction tower body (4) and the butadiene flash tank body (7), it enters the butadiene flash tank body (7) by self-pressure. 4) The rich solvent entering the butadiene flash tank body (7) at a pressure of -30-0KPa and a temperature of 60-70℃ will be transformed into a gas-liquid two-phase system due to flash evaporation. Open the external valve (15) on the top of the butadiene flash tank, and the butadiene will be discharged from the gas phase pipeline (17) on the top of the flash tank. 5) The liquid extractant in the butadiene flash tank body (7) is pressurized by the extractant pump (6) and heated to 100-105℃ through the extractant circulation pipeline and the extractant heater (5) before being sent to the extraction tower body (4) for recycling; 6) The acidic liquid mixture that was not absorbed by the extractant accumulates at the top of the extraction tower body (4). Open the mixed acid outlet valve (14) at the top of the extraction tower and the mixed acid enters the mixed acid tank (8) through the mixed acid self-pressurization pipeline. 7) The mixed acid in the mixed acid tank (8) is sent to the activation reactor (10) by the mixed acid pump (9). The activation reactor (10) contains bentonite with a particle size of 10-15um. The solid-liquid ratio of bentonite to acid is 2-5:

1. The activation reaction is carried out at a reaction temperature of 80-90℃ and a reaction pressure of 0.25MPa for 0.5-1.5h. Acidic activated clay is produced by stirring during the activation reaction. 8) The reaction product of the activated reactor (10) is filtered (11) to remove impurities using ceramic balls and ceramic sand, and then enters the air dryer (12) to remove moisture. Finally, it passes through the crusher and collector (13) to produce qualified granular acidic activated clay.

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