Water-containing non-polar solvent refining device and water-containing non-polar solvent refining method
By performing two-phase separation in the solvent refining device and using molecular sieve dehydration membrane treatment alone, the problem of low dehydration efficiency in the existing technology is solved, efficient solvent dehydration and recovery are achieved, and the moisture control requirements of high-end polyolefin materials are met.
Patent Information
- Application Number
- CN202510659886.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-21
- Publication Date
- 2025-09-09
AI Technical Summary
The dehydration efficiency of the refining device in the existing technology is low, resulting in a high water content in the solvent after dehydration, which cannot meet the strict control requirements of high-end new polyolefin materials on moisture content.
A water-containing non-polar solvent refining device is used, including a thermal energy processor, a two-phase separator, a heavy phase pervaporation component and a light phase pervaporation component. A molecular sieve dehydration membrane is used to separate the two phases of the solvent and dehydrate it separately, and deep dehydration is carried out in combination with vacuum operation and a density stratifier.
The dehydration efficiency of the solvent is improved, the water content in the solvent is reduced, the moisture content requirements of high-end new polyolefin materials are met, and the overall recovery rate and thermal energy utilization rate of the solvent are improved.
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Figure CN120605616A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of solvent refining, and in particular to an aqueous non-polar solvent refining device and an aqueous non-polar solvent refining method. Background Art
[0002] High-boiling-point organic solvents are often used in industrial processes such as petrochemicals and fine chemicals, and are used in solvents, solution polymerization processes, absorption separations, and other applications. Many of these high-boiling-point organic solvents are non-polar solvents, and while their mutual solubility in water is relatively poor, they still have a certain degree of solubility.
[0003] In recent years, with the gradual rise of high-end new polyolefin materials, some polymerization reaction processes have extremely strict control over the water content in the medium involved in the reaction to avoid the presence of water affecting the catalytic system and reaction effect. Generally, refining equipment is used to refine the water content in the reaction raw materials or solvent system.
[0004] However, the dehydration efficiency of the refining device in the related art is low, and there is a case where the water content of the solvent after dehydration is high. Summary of the Invention
[0005] The embodiments of the present invention provide an aqueous non-polar solvent refining device and an aqueous non-polar solvent refining method to improve the above technical problems.
[0006] The embodiments of the present invention achieve the above-mentioned objectives through the following technical solutions.
[0007] In a first aspect, an embodiment of the present invention provides an aqueous non-polar solvent refining device, which includes a thermal energy processor, a two-phase separator, a heavy phase pervaporation component, and a light phase pervaporation component. The inlet end of the two-phase separator is connected to the outlet end of the thermal energy processor, the first outlet end of the two-phase separator is connected to the inlet end of the heavy phase pervaporation component, and the second outlet end of the two-phase separator is connected to the inlet end of the light phase pervaporation component; wherein both the heavy phase pervaporation component and the light phase pervaporation component use molecular sieve dehydration membranes for dehydration.
[0008] In some embodiments, the aqueous non-polar solvent refining device includes a first heat recovery loop and a second heat recovery loop, the first heat recovery loop is connected to the collecting end of the heavy phase pervaporation component and the first collecting end of the thermal energy processor, and the second heat recovery loop is connected to the collecting end of the light phase pervaporation component and the second collecting end of the thermal energy processor.
[0009] In some embodiments, the aqueous non-polar solvent refining device further comprises a vacuum device, and the outlet end of the heavy phase pervaporation module and the outlet end of the light phase pervaporation module are both connected to the inlet end of the vacuum device.
[0010] In some embodiments, the aqueous non-polar solvent refining device further comprises a density separator, and the density separator is connected to the outlet end of the vacuum device.
[0011] In some embodiments, the aqueous non-polar solvent refining device includes a reflux loop connected to a reflux end of the density stratifier and an inlet end of the thermal processor.
[0012] In a second aspect, an embodiment of the present invention provides a method for refining an aqueous non-polar solvent, which comprises: introducing an aqueous non-polar solvent into a thermal energy processor for heating; introducing the heated aqueous non-polar solvent into a two-phase separator for two-phase separation; introducing the separated heavy phase component into a heavy phase pervaporation assembly, and dehydrating it using a molecular sieve dehydration membrane; introducing the separated light phase component into a light phase pervaporation assembly, and dehydrating it using a molecular sieve dehydration membrane.
[0013] In some embodiments, introducing an aqueous non-polar solvent into a thermal processor to increase the temperature comprises:
[0014] An aqueous non-polar solvent is introduced into a thermal processor and heated to 50°C-200°C.
[0015] In some embodiments, the method for refining an aqueous non-polar solvent further includes: introducing the solution at the outlet end of the heavy phase pervaporation component into a vacuum device for vacuum operation, maintaining the vacuum side pressure of the vacuum device less than 100 Pa; introducing the solution at the outlet end of the light phase pervaporation component into a vacuum device for vacuum operation, maintaining the vacuum side pressure of the vacuum device less than 100 Pa.
[0016] In some embodiments, the method for refining an aqueous non-polar solvent further includes: introducing the solution at the outlet of the vacuum device into a density separator for separation; refluxing the light phase obtained after separation in the density separator to a thermal energy processor; and discharging the aqueous phase obtained after separation in the density separator from the density separator.
[0017] In a third aspect, an embodiment of the present invention provides a method for refining an aqueous non-polar solvent, which comprises: introducing the aqueous non-polar solvent into a thermal energy processor to increase the temperature; introducing the heated aqueous non-polar solvent into a two-phase separator for two-phase separation; introducing the separated heavy phase component into a heavy phase pervaporation assembly, and dehydrating the component using a molecular sieve dehydration membrane.
[0018] The embodiments of the present invention provide an aqueous non-polar solvent refining device and an aqueous non-polar solvent refining method. The inlet end of the two-phase separator of the aqueous non-polar solvent refining device is connected to the outlet end of the thermal energy processor, the first outlet end of the two-phase separator is connected to the inlet end of the heavy phase pervaporation component, and the second outlet end of the two-phase separator is connected to the inlet end of the light phase pervaporation component. The heavy phase pervaporation component and the light phase pervaporation component both use molecular sieve dehydration membranes for dehydration. In this way, the aqueous non-polar solvent can be separated before dehydration, which helps to reduce the presence of mixed phases in the aqueous non-polar solvent, helps to reduce the impact of mixed phases in the aqueous non-polar solvent on the dehydration performance of the aqueous non-polar solvent refining device, helps to improve the dehydration efficiency of the aqueous non-polar solvent refining device for the aqueous non-polar solvent, and helps to reduce the water content of the aqueous non-polar solvent. Since the mass transfer resistance between water and other components in a single phase is small, water is more easily adsorbed by the molecular sieve dehydration membrane. The aqueous non-polar solvent refining device of the present application separates the aqueous non-polar solvent into two phases before dehydration, and dehydrates the separated heavy phase component and light phase component separately using molecular sieve dehydration membranes through heavy phase pervaporation components and light phase pervaporation components, which helps to improve the single-pass dehydration efficiency of the heavy phase component and light phase component of the aqueous non-polar solvent refining device, thereby helping to improve the dehydration efficiency of the aqueous non-polar solvent refining device for the aqueous non-polar solvent, and helping to reduce the water content of the aqueous non-polar solvent. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative work.
[0020] Figure 1 A simplified structural diagram of an aqueous non-polar solvent refining device provided in an embodiment of the present invention is shown.
[0021] Figure 2 A schematic flow chart of a method for refining an aqueous non-polar solvent provided in an embodiment of the present invention is shown.
[0022] Figure 3 A schematic flow chart of a method for refining an aqueous non-polar solvent provided in another embodiment of the present invention is shown.
[0023] Figure 4 A schematic flow chart of a method for refining an aqueous non-polar solvent provided in another embodiment of the present invention is shown.
[0024] Figure 5A schematic flow chart of a method for refining an aqueous non-polar solvent provided in another embodiment of the present invention is shown.
[0025] Figure 6 A schematic flow chart of a method for refining an aqueous non-polar solvent provided in another embodiment of the present invention is shown.
[0026] Figure 7 A schematic flow chart of a method for refining an aqueous non-polar solvent provided in another embodiment of the present invention is shown. DETAILED DESCRIPTION
[0027] In order to enable those skilled in the art to better understand the embodiments of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments in the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative work are within the scope of protection of the embodiments of the present invention.
[0028] The technical solutions in the embodiments of the present invention will be described clearly and completely below with reference to the accompanying drawings in the embodiments of the present invention.
[0029] See also Figure 1 An embodiment of the present invention provides an aqueous non-polar solvent refining device 100, which includes a thermal energy processor 11, a two-phase separator 12, a heavy-phase pervaporation component 13, and a light-phase pervaporation component 14. The inlet end 121 of the two-phase separator 12 is connected to the outlet end 111 of the thermal energy processor 11, the first outlet end 122 of the two-phase separator 12 is connected to the inlet end 131 of the heavy-phase pervaporation component 13, and the second outlet end 123 of the two-phase separator 12 is connected to the inlet end 141 of the light-phase pervaporation component 14; wherein, both the heavy-phase pervaporation component 13 and the light-phase pervaporation component 14 use molecular sieve dehydration membranes for dehydration.
[0030] In this way, the aqueous non-polar solvent can be separated before dehydration, which helps to reduce the presence of mixed phases in the aqueous non-polar solvent, helps to reduce the impact of the mixed phases in the aqueous non-polar solvent on the dehydration performance of the aqueous non-polar solvent refining device 100, helps to improve the dehydration efficiency of the aqueous non-polar solvent refining device 100 for the aqueous non-polar solvent, and helps to reduce the water content of the aqueous non-polar solvent.
[0031] Since the mass transfer resistance between water and other components in a single phase is small, water is more easily adsorbed by the molecular sieve dehydration membrane. The aqueous non-polar solvent refining device 100 of the present application separates the aqueous non-polar solvent into two phases before dehydration, and dehydrates the separated heavy phase component and light phase component separately using molecular sieve dehydration membranes through the heavy phase pervaporation component 13 and the light phase pervaporation component 14, respectively. This helps to improve the single-pass dehydration efficiency of the heavy phase component and the light phase component of the aqueous non-polar solvent refining device 100, thereby helping to improve the dehydration efficiency of the aqueous non-polar solvent refining device 100 for the aqueous non-polar solvent, and helps to reduce the water content of the aqueous non-polar solvent.
[0032] In addition, since the molecular sieve dehydration membrane has a high specific surface area and porosity, it can provide a large number of adsorption sites, which helps to achieve rapid and efficient water removal from the components. The use of molecular sieve dehydration membrane for dehydration helps to improve the dehydration efficiency of heavy phase components and light phase components in aqueous non-polar solvents, and helps to improve the dehydration efficiency of the aqueous non-polar solvent refining device 100.
[0033] Among them, the thermal energy processor 11 may include a raw material preheater and a heater. The thermal energy processor 11 heats the incoming aqueous non-polar solvent so that the aqueous non-polar solvent can enter the two-phase separator 12 at a suitable temperature for separation. The temperature of the aqueous non-polar solvent after treatment by the thermal energy processor 11 can be 50-200°C.
[0034] The two-phase processor may be a gas-liquid separator, a liquid-liquid separator (for liquids with different solubility properties) or other separators, and may be specifically configured according to actual conditions.
[0035] Among them, the heavy phase pervaporation component 13 and the light phase pervaporation component 14 can both be separation devices filled with dehydration membrane materials. For example, the heavy phase pervaporation component 13 and the light phase pervaporation component 14 are both membrane separation devices filled with inorganic molecular sieve dehydration membrane materials. The specific settings can be made according to actual conditions.
[0036] Among them, the heavy phase pervaporation component 13 may include steam permeation and a pervaporation membrane dehydrator, for example, the heavy phase pervaporation component 13 may include a pervaporation membrane dehydrator for liquid phase dehydration; the light phase pervaporation component 14 may include steam permeation and a pervaporation membrane dehydrator, for example, the light phase pervaporation component 14 may include a steam permeation membrane dehydrator for vapor phase dehydration.
[0037] In some embodiments, the aqueous non-polar solvent in the aqueous non-polar solvent refining apparatus 100 is generated in the polymerization reaction section. The aqueous non-polar solvent may originate from the polymer synthesis reaction section and may comprise a single solvent or a mixed solvent containing soluble components. In other embodiments, the aqueous non-polar solvent may also include other components, which may be adjusted based on actual circumstances.
[0038] The aqueous non-polar solvent may include a hydrocarbon solvent having 6-12 carbon atoms, such as a saturated normal / isoalkane solvent having 8-10 carbon atoms. The aqueous non-polar solvent may also include a hydrocarbon solvent having 2-8 carbon atoms, such as a low-boiling light component of alkanes or olefins having 2-4 carbon atoms. In other embodiments, the aqueous non-polar solvent may also include other components, which may be specifically configured according to actual circumstances.
[0039] In some embodiments, the aqueous non-polar solvent refining device 100 includes a first heat recovery loop 17 and a second heat recovery loop 18, the first heat recovery loop 17 connects the collection end 132 of the heavy phase pervaporation component 13 and the first collection end 112 of the thermal energy processor 11, and the second heat recovery loop 18 connects the collection end 142 of the light phase pervaporation component 14 and the second collection end 113 of the thermal energy processor 11.
[0040] Since the temperature of the components after dehydration by the heavy phase pervaporation component 13 and the light phase pervaporation component 14 is relatively high and it is not convenient to use them directly, the aqueous non-polar solvent refining device 100 can collect the dehydrated components to the thermal energy processor 11 through the first heat recovery loop 17 and the second heat recovery loop 18, so that the thermal energy processor 11 can cool the dehydrated components, which helps to ensure that the components after dehydration by the heavy phase pervaporation component 13 and the light phase pervaporation component 14 can have a suitable temperature, which is convenient for users to collect, and also helps the thermal energy processor 11 to recover heat energy, which helps to improve the thermal energy utilization rate of the thermal energy processor 11, and makes it convenient for the thermal energy processor 11 to have sufficient heat energy to heat the aqueous non-polar solvent that enters next time.
[0041] In some embodiments, the aqueous non-polar solvent refining device 100 further includes a vacuum device 15 , and the outlet end 133 of the heavy phase pervaporation module 13 and the outlet end 143 of the light phase pervaporation module 14 are both connected to the inlet end 151 of the vacuum device 15 .
[0042] In this way, the solvent at the outlet end 143 of the heavy phase pervaporation component 13 and the light phase pervaporation component 14, that is, the solvent at the permeation side of the heavy phase pervaporation component 13 and the light phase pervaporation component 14, can enter the vacuum device 15 for vacuum operation to preliminarily separate the water in the solvent at the permeation side of the heavy phase pervaporation component 13 and the light phase pervaporation component 14 from the solvent raw material, thereby achieving preliminarily dehydrating the solvent at the permeation side of the heavy phase pervaporation component 13 and the light phase pervaporation component 14, and facilitating the recycling of the dehydrated solvent raw material at the outlet end 143 of the heavy phase pervaporation component 13 and the light phase pervaporation component 14.
[0043] The vacuum device 15 may include a vacuum condenser and a vacuum pump. The vacuum device 15 may separate the solvents at the outlet 143 of the heavy phase pervaporation component 13 and the light phase pervaporation component 14 by means of osmotic pressure difference. The specific settings may be made according to actual conditions.
[0044] The pressure on the vacuum side of the vacuum device 15 is less than 100 Pa, which helps to ensure that the vacuum side of the vacuum device 15 has a suitable pressure environment and helps to ensure that the vacuum device 15 has a dehydration effect on the incoming solvent.
[0045] In some embodiments, the aqueous non-polar solvent refining device 100 further includes a density stratifier 16 , which is connected to the outlet end 152 of the vacuum device 15 .
[0046] In this way, the solvent at the outlet end 152 of the vacuum device 15, that is, the solvent on the permeate side of the outlet end 152 of the vacuum device 15, can enter the density stratifier 16 for separation operation to separate the water in the solvent on the permeate side of the heavy phase pervaporation component 13 and the light phase pervaporation component 14 from the solvent raw material again, thereby achieving deep dehydration of the solvent on the permeate side of the heavy phase pervaporation component 13 and the light phase pervaporation component 14, and facilitating the recycling of the dehydrated solvent raw material at the outlet end 143 of the heavy phase pervaporation component 13 and the light phase pervaporation component 14.
[0047] Among them, the solvent at the outlet end 152 of the vacuum device 15 can be condensed and collected and then sent to the density stratifier 16, for example, to enter the water phase / solvent phase separation equipment for static stratification through density difference to achieve interfacial stratification of light and heavy components, wherein the water phase is transported to the outside of the boundary area for treatment, and the solvent phase returns to the raw material tank for further dehydration treatment to obtain a higher overall solvent recovery rate.
[0048] In some embodiments, the aqueous non-polar solvent refining apparatus 100 includes a reflux loop 19 , which connects a reflux end 161 of the density stratifier 16 and an inlet end 114 of the thermal processor 11 .
[0049] In this way, the solvent raw material processed by the density stratifier 16 can be refluxed to the thermal energy processor 11 through the reflux loop 19 to re-dehydrate the discharged solvent raw material, which helps to improve the utilization rate of the aqueous non-polar solvent, and also helps to improve the dehydration rate of the aqueous non-polar solvent, and also helps the thermal energy processor 11 to recover heat energy, which helps to improve the thermal energy utilization rate of the thermal energy processor 11.
[0050] See also Figure 2 An embodiment of the present invention provides a method for refining an aqueous non-polar solvent, and the method for refining an aqueous non-polar solvent includes step 010, step 020, step 031 and step 032.
[0051] Step 010: Introduce an aqueous non-polar solvent into the thermal energy processor 11 to increase the temperature.
[0052] The thermal energy processor 11 can heat the incoming aqueous non-polar solvent to ensure that the aqueous non-polar solvent has a suitable temperature and can enter the next stage to participate in the reaction at a suitable temperature. The thermal energy processor 11 can include a raw material preheater and a heater.
[0053] Step 020: Introduce the heated aqueous non-polar solvent into the two-phase separator 12 for two-phase separation.
[0054] The two-phase separator 12 can separate the aqueous non-polar solvent before dehydration, for example, separating the aqueous non-polar solvent into a gas phase and a liquid phase, or separating the aqueous non-polar solvent into liquid phases with different solubility properties. The specific setting can be based on actual conditions.
[0055] Since the mass transfer resistance between water and other components in a single phase is small, water is more easily adsorbed by the molecular sieve dehydration membrane. The aqueous non-polar solvent refining device 100 of the present application separates the aqueous non-polar solvent into two phases before dehydration, which helps to reduce the presence of mixed phases in the aqueous non-polar solvent, helps to reduce the influence of the mixed phase in the aqueous non-polar solvent on the dehydration performance of the aqueous non-polar solvent refining device 100, helps to improve the dehydration efficiency of the aqueous non-polar solvent refining device 100 for the aqueous non-polar solvent, and helps to reduce the water content of the aqueous non-polar solvent.
[0056] The two-phase processor may be a gas-liquid separator, a liquid-liquid separator (for liquids with different solubility properties) or other separators, and may be specifically configured according to actual conditions.
[0057] Step 031: The separated heavy phase components are introduced into the heavy phase pervaporation assembly 13 and dehydrated using a molecular sieve dehydration membrane.
[0058] In this way, the separated heavy phase component can be dehydrated separately using a molecular sieve dehydration membrane through the heavy phase pervaporation component 13, which helps to improve the single-pass dehydration efficiency of the heavy phase component of the aqueous non-polar solvent refining device 100 and helps to reduce the water content of the heavy phase component in the aqueous non-polar solvent.
[0059] In addition, since the molecular sieve dehydration membrane has a high specific surface area and porosity, it can provide a large number of adsorption sites, which helps to achieve rapid and efficient water removal from the components. The use of molecular sieve dehydration membrane for dehydration helps to improve the dehydration efficiency of heavy phase components in aqueous non-polar solvents, and helps to improve the dehydration efficiency of the aqueous non-polar solvent refining device 100.
[0060] Step 032: The separated light phase components are introduced into the light phase pervaporation assembly 14 and dehydrated using a molecular sieve dehydration membrane.
[0061] In this way, the separated light phase component can be dehydrated separately using a molecular sieve dehydration membrane through the light phase pervaporation assembly 14, which helps to improve the single-pass dehydration efficiency of the light phase component of the aqueous non-polar solvent refining device 100 and helps to reduce the water content of the light phase component in the aqueous non-polar solvent.
[0062] In addition, since the molecular sieve dehydration membrane has a high specific surface area and porosity, it can provide a large number of adsorption sites, which helps to achieve rapid and efficient water removal from the components. The use of molecular sieve dehydration membrane for dehydration helps to improve the dehydration efficiency of the light phase components in the aqueous non-polar solvent, and helps to improve the dehydration efficiency of the aqueous non-polar solvent refining device 100.
[0063] In this way, the aqueous non-polar solvent refining device 100 of the present application separates the aqueous non-polar solvent into two phases before dehydration, and dehydrates the separated heavy phase component and light phase component separately using molecular sieve dehydration membranes through the heavy phase pervaporation component 13 and the light phase pervaporation component 14, respectively. This helps to improve the single-pass dehydration efficiency of the heavy phase component and the light phase component of the aqueous non-polar solvent refining device 100, thereby helping to improve the dehydration efficiency of the aqueous non-polar solvent refining device 100 for the aqueous non-polar solvent, and helping to reduce the water content of the aqueous non-polar solvent.
[0064] See also Figure 2 and Figure 3 In some embodiments, introducing an aqueous non-polar solvent into the thermal energy processor 11 to increase the temperature includes step 011 , that is, step 010 includes step 011 .
[0065] Step 011: Introduce an aqueous non-polar solvent into the thermal processor 11 and heat it to 50°C-200°C.
[0066] The aqueous non-polar solvent needs to have a certain temperature when entering the two-phase separator 12 for separation. If the temperature is too high or too low, the two-phase separator 12 will not be able to effectively separate the entering solution.
[0067] By arranging a thermal energy processor 11 at the front end of the two-phase separator 12 and heating the aqueous non-polar solvent to a suitable temperature before entering the two-phase separator 12, it helps to ensure that the two-phase separator 12 can effectively separate the entering aqueous non-polar solvent and ensure the normal operation of the aqueous non-polar solvent refining device 100.
[0068] Illustratively, the thermal energy processor 11 can heat the aqueous non-polar solvent to 50°C, 60°C, 70°C, 85°C, 90°C, 100°C, 120°C, 1350°C, 150°C, 180°C, 200°C or other temperatures, which can be set according to actual conditions.
[0069] See also Figure 4 In some embodiments, the method for refining with an aqueous non-polar solvent further includes steps 041 and 042.
[0070] Step 041: Introduce the solution at the outlet of the heavy phase pervaporation assembly 13 into the vacuum device 15 for vacuum operation, and maintain the vacuum side pressure of the vacuum device 15 less than 100 Pa.
[0071] In this manner, the solvent at outlet port 133 of heavy-phase pervaporation module 13, i.e., the solvent on the permeate side of heavy-phase pervaporation module 13, can enter vacuum device 15 for vacuum operation to initially separate the water in the solvent on the permeate side of heavy-phase pervaporation module 13 from the solvent feedstock, thereby achieving preliminary dehydration of the solvent on the permeate side of heavy-phase pervaporation module 13 and facilitating the recycling of the dehydrated solvent feedstock at outlet port 133 of heavy-phase pervaporation module 13. The vacuum side pressure of vacuum device 15 is less than 100 Pa, which helps ensure that the vacuum side of vacuum device 15 has a suitable pressure environment and helps ensure that vacuum device 15 effectively dehydrates the incoming solvent.
[0072] The vacuum device 15 may include a vacuum condenser and a vacuum pump. The vacuum device 15 may separate the solvent at the outlet 133 of the heavy phase pervaporation component 13 by using an osmotic pressure difference. The specific settings may be made according to actual conditions.
[0073] Step 042: Introduce the solution at the outlet of the light phase pervaporation assembly 14 into the vacuum device 15 for vacuum operation, and maintain the vacuum side pressure of the vacuum device 15 less than 100 Pa.
[0074] In this manner, the solvent at outlet port 143 of light-phase pervaporation module 14, i.e., the solvent on the permeate side of light-phase pervaporation module 14, can enter vacuum device 15 for vacuum operation to initially separate the water in the solvent on the permeate side of light-phase pervaporation module 14 from the solvent feedstock, thereby achieving preliminary dehydration of the solvent on the permeate side of light-phase pervaporation module 14 and facilitating the recycling of the dehydrated solvent feedstock at outlet port 143 of light-phase pervaporation module 14. The vacuum side pressure of vacuum device 15 is less than 100 Pa, which helps ensure a suitable pressure environment on the vacuum side of vacuum device 15 and helps ensure that vacuum device 15 effectively dehydrates the incoming solvent.
[0075] The vacuum device 15 may include a vacuum condenser and a vacuum pump. The vacuum device 15 may separate the solvent at the outlet 143 of the light phase pervaporation component 14 by using an osmotic pressure difference. The specific settings may be made according to actual conditions.
[0076] In this way, the vacuum device 15 can perform vacuum operation on the solvent on the permeation side of the heavy phase pervaporation component 13 and the light phase pervaporation component 14 to preliminarily separate the water in the solvent on the permeation side of the heavy phase pervaporation component 13 and the light phase pervaporation component 14 from the solvent raw material, thereby achieving preliminary dehydration of the solvent on the permeation side of the heavy phase pervaporation component 13 and the light phase pervaporation component 14.
[0077] See also Figure 5 In some embodiments, the method for refining with an aqueous non-polar solvent further includes step 051, step 052 and step 053.
[0078] Step 051: Introduce the solution at the outlet of the vacuum device 15 into the density stratifier 16 for separation.
[0079] In this way, the solvent at the outlet end 152 of the vacuum device 15, that is, the solvent on the permeate side of the outlet end 152 of the vacuum device 15, can enter the density stratifier 16 for separation operation to separate the water in the solvent on the permeate side of the heavy phase pervaporation component 13 and the light phase pervaporation component 14 from the solvent raw material again, thereby achieving deep dehydration of the solvent on the permeate side of the heavy phase pervaporation component 13 and the light phase pervaporation component 14, and facilitating the recycling of the dehydrated solvent raw material at the outlet end 143 of the heavy phase pervaporation component 13 and the light phase pervaporation component 14.
[0080] Step 052: The light phase obtained after separation in the density stratifier 16 is refluxed to the thermal energy processor 11.
[0081] In this way, the solvent raw material processed by the density stratifier 16 can be refluxed to the thermal energy processor 11 through the reflux loop 19 to re-dehydrate the discharged solvent raw material, which helps to improve the utilization rate of the aqueous non-polar solvent, and also helps to improve the dehydration rate of the aqueous non-polar solvent, and also helps the thermal energy processor 11 to recover heat energy, which helps to improve the thermal energy utilization rate of the thermal energy processor 11.
[0082] Step 053: The water phase obtained after separation in the density separator 16 is discharged from the density separator 16.
[0083] In this way, the solvent on the permeate side of the outlet end 152 of the vacuum device 15 can be separated again in the density separator 16, thereby achieving deep dehydration of the solvent on the permeate side of the heavy phase pervaporation component 13 and the light phase pervaporation component 14, and the dehydrated water phase is discharged from the density separator 16, reducing the situation where the water phase remains in the density separator 16 and redissolves in the solvent.
[0084] See also Figure 6 In some embodiments, introducing the solution at the outlet of the vacuum device 15 into the density stratifier 16 for separation includes step 054 and step 055, that is, step 051 includes step 054 and step 055.
[0085] Step 054: Condensing the solution at the outlet of the vacuum device 15.
[0086] Before entering the density stratifier 16 , the solution at the outlet of the vacuum device 15 is condensed into a liquid phase to ensure the separation effect of the density stratifier 16 on the solution.
[0087] Step 055: The condensed solution is introduced into the density stratifier 16 for static stratification.
[0088] The condensed solution can be introduced into a water / solvent phase separation device, where it is allowed to stand and separate by density difference, achieving interfacial separation of the light and heavy components. The water phase is transported to the outer boundary for processing, while the solvent phase is returned to the feed tank for further dehydration, thereby achieving a higher overall solvent recovery rate. The density separator 16 has a simple separation method and is easy to operate.
[0089] In Example 1, an aqueous non-polar solvent, such as a solvent feedstock with 8-10 carbon atoms, is introduced into a thermal processor 11 for heating. The solvent feedstock with 8-10 carbon atoms is a mixed solvent system obtained from a front-end polymerization reactor after separation of the solvent and product. It contains unreacted monomers with a low boiling point, which dissolve in the solvent at a certain temperature and pressure, resulting in a liquid phase. Specific raw material parameters are shown in the table below.
[0090]
[0091] The temperature of the introduced aqueous non-polar solvent is then raised to 70°C, preheated to 115°C by a steam heater, and maintained at this temperature before entering two-phase separator 12. By increasing the temperature at a constant pressure, the low-boiling light hydrocarbon components, ethylene and butene, in the solvent liquid phase are mostly separated from the liquid phase in the vapor phase. The compositions of the gas and liquid phases are shown in the following table.
[0092]
[0093]
[0094] The light phase enters the light phase pervaporation module 14, where it is dehydrated using a molecular sieve membrane. The light phase, a vapor phase rich in light hydrocarbons, primarily butene, enters the molecular sieve dehydration membrane and is dehydrated in the vapor phase. The moisture content of the non-permeable material produced from the molecular sieve membrane unit is reduced to below 5 ppm.
[0095] The heavy phase enters the heavy phase pervaporation module 13, where it is dehydrated using a molecular sieve membrane. The heavy phase, primarily composed of a solvent containing a small amount of dissolved olefins, enters the molecular sieve dehydration membrane and is dehydrated as a liquid. The moisture content of the non-permeable material produced from the molecular sieve membrane device is reduced to below 5 ppm.
[0096] The permeate sides of the light-phase pervaporation module 14 and the heavy-phase pervaporation module 13 are connected to a vacuum unit 15, which operates under vacuum to separate the permeate-side water from the solvent feed. To ensure the ultimate dehydration of the solvent feed, the vacuum side pressure of the vacuum unit 15 is maintained at less than 100 Pa.
[0097] The permeate from the permeate side is further separated by density separator 16, with the light phase returned to the solvent feed side and the aqueous phase discharged as wastewater. The water and a small amount of solvent components from the permeate side are condensed and collected before being sent to a water / solvent phase separation device. Static separation is achieved by density difference, achieving interfacial separation of the light and heavy components. The aqueous phase is transported to the outer boundary for processing, while the solvent phase is returned to the feed tank for further dehydration, achieving a higher overall solvent recovery rate.
[0098] The solvent on the non-permeated side of the light phase pervaporation module 14 and the heavy phase pervaporation module 13 is cooled by the thermal energy processor 11 to obtain an ultra-low water content solvent product, wherein the water content in the final product is less than 1ppm, meeting the high moisture requirement for the polymerization reaction.
[0099] The entire device adopts a continuous operation mode, with single-pass in and single-pass out, and the solvent recovery rate can reach more than 99%.
[0100] See also Figure 7The embodiment of the present invention provides a method for refining an aqueous non-polar solvent, the method comprising steps 010, 020 and 031.
[0101] Step 010: Introduce an aqueous non-polar solvent into the thermal energy processor 11 to increase the temperature.
[0102] Step 020: Introduce the heated aqueous non-polar solvent into the two-phase separator 12 for two-phase separation.
[0103] Step 031: The separated heavy phase components are introduced into the heavy phase pervaporation assembly 13 and dehydrated using a molecular sieve dehydration membrane.
[0104] Step 010, step 020 and step 031 are the same as those in the above embodiment and are not described in detail here.
[0105] In this way, when no light phase component exists when the aqueous non-polar solvent passes through the two-phase separator 12, the light phase pervaporation component 14 can be separated from the two-phase separator 12 and the vacuum device 15, and the aqueous non-polar solvent refining process does not need to pass through the light phase pervaporation component 14, which helps to reduce the dehydration path of the aqueous non-polar solvent, helps to improve the dehydration efficiency of the aqueous non-polar solvent, and also helps to reduce the energy consumption of the aqueous non-polar solvent refining device 100.
[0106] In this way, the aqueous non-polar solvent refining device 100 can selectively connect or separate the light phase pervaporation component 14 according to the introduced aqueous non-polar solvent components, which helps to improve the flexibility of the aqueous non-polar solvent refining device 100 to better meet actual production needs.
[0107] In summary, the aqueous non-polar solvent refining device 100 and the aqueous non-polar solvent refining method provided in the embodiment of the present invention are as follows: the inlet end 121 of the two-phase separator 12 of the aqueous non-polar solvent refining device 100 is connected to the outlet end 111 of the thermal energy processor 11, the first outlet end 122 of the two-phase separator 12 is connected to the inlet end 131 of the heavy phase pervaporation component 13, and the second outlet end 123 of the two-phase separator 12 is connected to the inlet end 141 of the light phase pervaporation component 14; wherein, both the heavy phase pervaporation component 13 and the light phase pervaporation component 14 use molecular sieve dehydration membranes for dehydration. In this way, the aqueous non-polar solvent can be separated before dehydration, which helps to reduce the presence of mixed phases in the aqueous non-polar solvent, helps to reduce the impact of the mixed phases in the aqueous non-polar solvent on the dehydration performance of the aqueous non-polar solvent refining device 100, helps to improve the dehydration efficiency of the aqueous non-polar solvent refining device 100 for the aqueous non-polar solvent, and helps to reduce the water content of the aqueous non-polar solvent. Since the mass transfer resistance between water and other components in a single phase is small, water is more easily adsorbed by the molecular sieve dehydration membrane. The aqueous non-polar solvent refining device 100 of the present application separates the aqueous non-polar solvent into two phases before dehydration, and dehydrates the separated heavy phase component and light phase component separately using molecular sieve dehydration membranes through the heavy phase pervaporation component 13 and the light phase pervaporation component 14, respectively. This helps to improve the single-pass dehydration efficiency of the heavy phase component and the light phase component of the aqueous non-polar solvent refining device 100, thereby helping to improve the dehydration efficiency of the aqueous non-polar solvent refining device 100 for the aqueous non-polar solvent, and helps to reduce the water content of the aqueous non-polar solvent.
[0108] In the embodiments of the present invention, unless otherwise expressly specified or limited, terms such as "assembly" should be interpreted broadly. For example, they can refer to fixed connections, removable connections, or integral connections; mechanical connections; direct connections, indirect connections through an intermediary, internal communication between two components, surface contact only, or surface contact connections through an intermediary. Those skilled in the art will understand the specific meanings of these terms in the embodiments of the present invention based on the specific circumstances.
[0109] In addition, the terms "first", "second", etc. are only used to distinguish the description and cannot be understood as a specific reference or special structure. The description of the term "some embodiments" means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the embodiment of the present invention. In the embodiments of the present invention, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in a suitable manner in any one or more embodiments or examples. In addition, those skilled in the art can combine and combine the different embodiments or examples described in the embodiments of the present invention and the features of the different embodiments or examples, unless they are contradictory.
[0110] The above embodiments are only used to illustrate the technical solutions of the embodiments of the present invention, rather than to limit them. Although the embodiments of the present invention are described in detail with reference to the above embodiments, ordinary technicians in this field should understand that they can still modify the technical solutions recorded in the above embodiments, or replace some of the technical features therein with equivalents. These modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention, and should all be included in the protection scope of the embodiments of the present invention.
Claims
1. A device for refining an aqueous non-polar solvent, characterized in that: include: A thermal energy processor, a two-phase separator, a heavy-phase pervaporation assembly, and a light-phase pervaporation assembly, wherein the inlet end of the two-phase separator is connected to the outlet end of the thermal energy processor, the first outlet end of the two-phase separator is connected to the inlet end of the heavy-phase pervaporation assembly, and the second outlet end of the two-phase separator is connected to the inlet end of the light-phase pervaporation assembly; wherein both the light-phase pervaporation assembly and the heavy-phase pervaporation assembly use molecular sieve dehydration membranes for dehydration.
2. The aqueous non-polar solvent refining device according to claim 1, characterized in that: The aqueous non-polar solvent refining device includes a first heat recovery circuit and a second heat recovery circuit. The first heat recovery circuit is connected to the collecting end of the heavy phase pervaporation component and the first collecting end of the thermal energy processor, and the second heat recovery circuit is connected to the collecting end of the light phase pervaporation component and the second collecting end of the thermal energy processor.
3. The aqueous non-polar solvent refining device according to claim 1, characterized in that: The aqueous non-polar solvent refining device further includes a vacuum device, and the outlet end of the heavy phase pervaporation component and the outlet end of the light phase pervaporation component are both connected to the inlet end of the vacuum device.
4. The aqueous non-polar solvent refining device according to claim 3, characterized in that: The aqueous non-polar solvent refining device further comprises a density stratifier, which is connected to the outlet end of the vacuum device.
5. The aqueous non-polar solvent refining device according to claim 4, characterized in that: The aqueous non-polar solvent refining device includes a reflux loop, which is connected to the reflux end of the density stratifier and the inlet end of the thermal energy processor.
6. A method for refining an aqueous non-polar solvent, characterized in that: include: introducing an aqueous non-polar solvent into a thermal energy processor to increase the temperature; introducing the heated aqueous non-polar solvent into a two-phase separator for two-phase separation; The separated heavy phase components are introduced into a heavy phase pervaporation assembly and dehydrated using a molecular sieve dehydration membrane; The separated light phase components are introduced into the light phase pervaporation assembly and dehydrated using a molecular sieve dehydration membrane.
7. The method for refining aqueous non-polar solvent according to claim 6, characterized in that: The step of introducing the aqueous non-polar solvent into the thermal energy processor to increase the temperature comprises: An aqueous non-polar solvent is introduced into a thermal processor and heated to 50°C-200°C.
8. The method for refining aqueous non-polar solvent according to claim 6, characterized in that: The method for refining the aqueous non-polar solvent further comprises: Introduce the solution at the outlet of the heavy phase pervaporation component into a vacuum device for vacuum operation, and maintain the pressure on the vacuum side of the vacuum device less than 100 Pa; The solution at the outlet of the light phase pervaporation component is introduced into a vacuum device for vacuum operation, and the pressure on the vacuum side of the vacuum device is maintained at less than 100 Pa.
9. The method for refining aqueous non-polar solvent according to claim 8, characterized in that: The method for refining the aqueous non-polar solvent further comprises: The solution at the outlet of the vacuum device is introduced into a density stratifier for separation; The light phase obtained after separation in the density separator is refluxed to the thermal energy processor; The water phase obtained after separation in the density separator is discharged from the density separator.
10. A method for refining an aqueous non-polar solvent, characterized in that: include: introducing an aqueous non-polar solvent into a thermal energy processor to increase the temperature; introducing the heated aqueous non-polar solvent into a two-phase separator for two-phase separation; The separated heavy phase components are introduced into a heavy phase pervaporation assembly and dehydrated using a molecular sieve dehydration membrane.
Citation Information
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