Reaction Liquid Transfer System
The reaction liquid transfer system addresses polymer clogging in ethylene oligomer reaction devices by using a sediment tank to settle and remove polymers, ensuring smooth transfer and reducing energy and time costs, thereby maintaining stable production.
Patent Information
- Application Number
- JP2023512771
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2022-07-01
- Filing Date
- 2022-07-25
- Publication Date
- 2025-02-03
- Estimated Expiration
- 2042-07-25
AI Technical Summary
The challenge is to prevent clogging and ensure smooth transfer of reaction solutions from ethylene oligomer reaction devices by addressing the issue of polymer formation in control valves during the transfer process, which leads to operational interruptions and increased cleaning and energy costs.
A reaction liquid transfer system is designed with a sediment tank and reactor emission piping that allows the reaction solution to overflow into the sediment tank, where polymers are settled and removed, preventing polymer-induced clogging and enabling smooth transfer to a storage container.
This system reduces energy costs and time required for polymer removal, maintains stable operation, and prevents fouling of control valves, ensuring continuous production by facilitating efficient transfer of reaction solutions.
Smart Images

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Abstract
Description
[Technical field]
[0001] This application claims the benefit of priority to Korean Patent Application No. 10-2021-0134020 filed on October 8, 2021 and Korean Patent Application No. 10-2022-0081412 filed on July 1, 2022, and all contents disclosed in the documents of the relevant Korean patent applications are incorporated herein by reference.
[0002] The present invention relates to a reaction liquid transport system, and more particularly to a method for smoothly transporting reaction liquid from an ethylene oligomerization reactor. [Background technology]
[0003] Alpha-olefins are widely used commercially as important substances used as comonomers, detergents, lubricants, plasticizers, etc. In particular, 1-hexene and 1-octene are widely used as comonomers to adjust the density of polyethylene in the production of linear low-density polyethylene (LLDPE).
[0004] Alpha olefins such as 1-hexene and 1-octene are typically produced by the oligomerization of ethylene. The oligomerization of ethylene is carried out by using ethylene as a reactant and oligomerizing ethylene (trimerization or tetramerization) in the presence of a catalyst. Through the above reaction, the desired products including 1-hexene and 1-octene are produced, but a small amount of polymer may be produced as a by-product during the catalytic reaction. The polymer suspended in the reaction liquid causes fouling of a control valve for maintaining a constant height of the reaction liquid in the reactor during the process of transferring the reaction liquid to a storage container using a reactor discharge pipe, and ultimately requires the operation of the reactor to be stopped and the pipes and valves to be cleaned. Summary of the Invention [Problem to be solved by the invention]
[0005] The object of the present invention is to provide a method for preventing a control valve from being clogged with polymers contained in a reaction liquid discharged from an ethylene oligomerization reactor and for smoothly transferring the reaction liquid, in order to solve the problems described in the Background of the Invention section above. [Means for solving the problem]
[0006] According to one embodiment of the present invention for solving the above problems, the present invention provides a reaction liquid transfer system including: a reactor for receiving a feed stream and reacting it to form a reaction liquid; a reactor discharge pipe provided on a side of the reactor at a position corresponding to a surface height of the reaction liquid in the reactor and connected to a precipitation tank for transferring the reaction liquid from the reactor to the precipitation tank; and a precipitation tank for precipitating a polymer contained in the reaction liquid. Effect of the Invention
[0007] According to the reaction liquid transfer system of the present invention, piping is designed to allow the reaction liquid to overflow from the reactor, and a settling tank is provided between the reactor and the storage vessel to remove polymers contained in the reaction liquid, and the reaction liquid is then transferred to the storage vessel through a settling tank discharge pipe equipped with a control valve, thereby preventing fouling caused by polymers contained in the reaction liquid and allowing the reaction liquid to be transferred smoothly.
[0008] In addition, by using the precipitation tank to remove the polymer contained in the reaction solution, it is possible to reduce the energy cost and time required for removing the polymer from the reaction solution and separating the product in a later stage. [Brief description of the drawings]
[0009] [Figure 1] FIG. 1 is a process flow diagram of a reaction liquid transfer system according to one embodiment of the present invention. [Diagram 2] FIG. 1 is a process flow diagram of a reaction liquid transport system according to a comparative example. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0010] The terms and words used in the description of the present invention and the claims should not be interpreted in a limited manner to their ordinary or dictionary meanings, but should be interpreted in a manner that is consistent with the technical idea of the present invention, based on the principle that the inventors can appropriately define the concepts of terms in order to best describe their invention.
[0011] In the present invention, the term "stream" refers to the flow of a fluid in a process, and may also refer to the fluid itself flowing in a transfer line (piping). Specifically, the term "stream" may refer to both the fluid itself flowing in the piping connecting each device and the flow of the fluid. Furthermore, the fluid may contain one or more components of gas, liquid, and solid.
[0012] In order that the present invention may be easily understood, the present invention will now be described in more detail with reference to the accompanying FIG.
[0013] According to the present invention, there is provided a reaction liquid transport system, which includes a reactor 10 that receives a feed stream, reacts with the feed stream to form a reaction liquid, a reactor discharge pipe 11 that is provided on the side of the reactor 10 at a position corresponding to the surface height of the reaction liquid in the reactor 10 and is connected to a precipitation tank 20 to transport the reaction liquid from the reactor 10 to the precipitation tank 20, and the precipitation tank 20 that precipitates a polymer contained in the reaction liquid.
[0014] According to one embodiment of the present invention, the type of the reactor 10 and the type of the reaction occurring in the reactor 10 are not particularly limited, and the reaction liquid transport system according to the present invention can be applied without limitation when the reaction occurring in the reactor 10 contains a polymer that may cause a fouling phenomenon in the reaction liquid.
[0015] The reactor 10 may be, for example, an ethylene oligomerization reactor. Specifically, alpha olefins are widely used commercially as important materials used as comonomers, detergents, lubricants, plasticizers, etc., and in particular, 1-hexene and 1-octene are widely used as comonomers for adjusting the density of polyethylene when producing linear low density polyethylene (LLDPE). Alpha olefins can be produced by the oligomerization reaction of ethylene.
[0016] The ethylene oligomerization reaction may be carried out by a trimerization reaction or a tetramerization reaction of ethylene using ethylene as a reactant in the presence of a catalyst.
[0017] The oligomerization reaction may refer to a reaction in which a monomer is polymerized. Depending on the number of monomers polymerized, it may be called trimerization or tetramerization, and these are collectively called multimerization.
[0018] The feed stream supplied to the reactor 10 may include, for example, ethylene as a reactant, a solvent, a catalyst, and a cocatalyst.
[0019] The catalyst used in the ethylene oligomerization reaction can include a transition metal source, which can be, for example, a compound including one or more selected from the group consisting of chromium (III) acetylacetonate, chromium (III) chloride tetrahydrofuran, chromium (III) 2-ethylhexanoate, chromium (III) tris(2,2,6,6-tetramethyl-3,5-heptanedionate), chromium (III) benzoylacetonate, chromium (III) hexafluoro-2,4-pentanedionate, chromium (III) acetate hydroxide, chromium (III) acetate, chromium (III) butyrate, chromium (III) pentanoate, chromium (III) laurate, and chromium (III) stearate.
[0020] The co-catalyst may include at least one selected from the group consisting of, for example, trimethylaluminium, triethylaluminium, triisopropylaluminium, triisobutylaluminium, ethylaluminum sesquichloride, diethylaluminum chloride, ethylaluminium dichloride, methylaluminoxane, modified methylaluminoxane, and borate.
[0021] The solvent may include, for example, one or more selected from the group consisting of n-pentane, n-hexane, n-heptane, cyclohexane, methylcyclohexane, octane, cyclooctane, decane, dodecane, benzene, xylene, 1,3,5-trimethylbenzene, toluene, ethylbenzene, chlorobenzene, dichlorobenzene, and trichlorobenzene.
[0022] In this way, in the process of oligomerizing ethylene monomer in the presence of a catalyst, a reaction liquid is formed, and in addition to the oligomer product, polymers such as polyethylene may be produced as by-products during the catalytic reaction in the reaction liquid. When the reaction liquid is transferred to a storage container through a reactor discharge pipe, the polymers floating in the reaction liquid cause serious polymer fouling in a control valve that maintains a constant height of the reaction liquid in the reactor, and the height of the reaction liquid gradually rises because the reaction liquid is not discharged. Eventually, the operation of the reactor must be stopped abnormally and the pipes and valves must be cleaned.
[0023] Conventionally, in order to clean a control valve that has become fouled by polymers, the piping and control valve must be dismantled, cleaned for a long time, and then reinstalled, which takes a lot of time. This leads to problems such as reduced production volume during shutdowns and increased cleaning costs, as well as increased time required to normalize the reaction after cleaning, resulting in reduced reaction stability.
[0024] In addition, an additional separation tower must be operated in order to separate and remove the polymer contained in the reaction solution at a later stage. When the reaction solution contains a large amount of polymer, the energy cost and time required to separate and remove the polymer increases.
[0025] In contrast, in the present invention, piping is designed to allow the reaction liquid to overflow from the reactor, and the reaction liquid is transferred to a precipitation tank to precipitate and remove the polymer, and then the reaction liquid is transferred to a storage container through a precipitation tank discharge piping equipped with a control valve, thereby preventing fouling of the control valve due to the polymer contained in the reaction liquid and enabling smooth transfer of the reaction liquid.
[0026] In addition, by removing the polymer contained in the reaction solution using the precipitation tank, it is possible to reduce the energy cost and time required for removing the polymer from the reaction solution and separating the product in a later stage.
[0027] According to one embodiment of the present invention, the reactor 10 may include a reactor discharge pipe 11 that is provided on the side of the reactor 10 at a position corresponding to the surface height of the reaction liquid in the reactor 10 and is connected to a settling tank 20 to transfer the reaction liquid from the reactor 10 to the settling tank 20.
[0028] As the reaction proceeds in the reactor 10, the surface height of the reaction liquid increases as a certain amount of product is produced. Therefore, the surface height of the reaction liquid to be maintained may vary depending on the type of the target product, process conditions, etc. Accordingly, the height at which the reactor discharge pipe 11 is installed may be adjusted.
[0029] The reactor 10 can receive a feed stream and react to form a reaction liquid containing a product, and unreacted materials can be discharged from the top of the reactor 10 and recovered in a subsequent process for reuse.
[0030] The reactor discharge pipe 11 is connected from a side of the reactor 10 at a position corresponding to the surface height of the reaction liquid in the reactor 10 to the settling tank 20, and in this case, the reactor discharge pipe 11 may be provided with a downward inclination from the reactor 10 to the settling tank 20. By designing the reactor discharge pipe 11 in this manner, when the reaction liquid in the reactor 10 reaches a certain height, it can overflow through the reactor discharge pipe 11 and be transferred to the settling tank 20.
[0031] The inclination of the reactor discharge pipe 11 extending from the reactor 10 may be, for example, 5° or more, 7° or more, or 8° or more, and 10° or less, 15° or less, 20° or less, or 30° or less. By designing the reactor discharge pipe 11 to have a downward inclination toward the settling tank 20, the reaction liquid can be discharged from the reactor 10 through the reactor discharge pipe 11 and smoothly transferred to the settling tank 20.
[0032] In addition, the reactor discharge pipe 11 may not include a control valve. Specifically, by not installing a control valve in the reactor discharge pipe 11, it is possible to prevent the occurrence of a fouling phenomenon in which the control valve is clogged by polymers contained in the reaction liquid transported through the reactor discharge pipe 11.
[0033] The operating pressure of the reactor 10 may be the same as the operating pressure of the settling tank 20. By maintaining the operating pressure of the reactor 10 and the operating pressure of the settling tank 20 at the same pressure, the reaction liquid in the reactor 10 can overflow through the reactor discharge pipe 11 and be transferred to the settling tank 20. On the other hand, if the operating pressure of the reactor 10 is lower than the operating pressure of the settling tank 20, the reaction liquid is not smoothly discharged, so that the height of the reaction liquid in the reactor 10 increases, and if the operating pressure of the reactor 10 is higher than the operating pressure of the settling tank 20, the flow of unreacted materials becomes unstable.
[0034] According to an embodiment of the present invention, the reaction solution is transferred to the precipitation tank 20 through the reactor discharge pipe 11, and in the precipitation tank 20, polymers contained in the reaction solution can be precipitated and removed.
[0035] The operating pressure of the settling tank 20 may vary depending on the operating pressure of the reactor 10. For example, the operating pressure of the settling tank 20 may be 20 kg / cm 2 .g or more, 25kg / cm 2 .g or more, or 30kg / cm 2 .g or more, and 40kg / cm 2 .g or less, 45kg / cm 2 .g or less, or 50kg / cm 2 It can be less than or equal to .g.
[0036] The operating temperature of the precipitation tank 20 may be appropriately adjusted to precipitate and remove the polymer contained in the reaction solution, for example, the operating temperature of the precipitation tank 20 may be 10° C. or more, 15° C. or more, or 20° C. or more, and 70° C. or less, 80° C. or less, or 90° C. or less.
[0037] In this way, by adjusting the operating conditions of the precipitation tank 20, the polymer contained in the reaction solution can be effectively removed in the precipitation tank 20, thereby reducing the energy cost and time required for separating the product from the reaction solution in the subsequent step. In this case, the polymer may have a weight average molecular weight of 80,000 g / mol to 300,000 g / mol, 100,000 g / mol to 200,000 g / mol, or 100,000 g / mol to 150,000 g / mol.
[0038] In the precipitation tank 20, a polymer precipitated in a solid state and an upper layer liquid including the reaction solution from which the polymer has been removed may be formed. Specifically, the upper layer liquid including the reaction solution from which the polymer has been removed may be transferred to a subsequent process, and in this case, by removing the polymer in advance in the precipitation tank 20, it is possible to reduce the energy cost and time required for separation in the subsequent product separation step.
[0039] A settling tank discharge pipe 21 may be provided at a side of the settling tank 20 at a height where the upper layer liquid is formed. Specifically, the settling tank discharge pipe 21 is formed at a side of the settling tank 20 at a height where the upper layer liquid is formed in the settling tank 20, and may discharge and transport the reaction liquid from which polymers have been removed from the settling tank 20.
[0040] The settling tank discharge pipe 21 may include a control valve 22. Specifically, the control valve 22 controls the flow rate of the reaction liquid discharged from the settling tank 20 and can maintain the height of the reaction liquid in the reactor 10.
[0041] The settling tank discharge pipe 21 may be installed at a position lower than the height at which the reactor discharge pipe 11 is connected to the settling tank 20. Specifically, by installing the settling tank discharge pipe 21 at a position lower than the height at which the reactor discharge pipe 11 is connected to the settling tank 20, it is possible to prevent the reaction solution from which the polymer has been removed in the settling tank 20 from flowing back into the reactor 10, and to allow the reaction solution to smoothly overflow from the reactor 10 to the settling tank 20, thereby maintaining the height of the reaction solution in the reactor 10.
[0042] According to an embodiment of the present invention, the present invention may further include a storage vessel 30 for receiving and storing the reaction solution from the settling vessel 20. The storage vessel 30 may be connected to the settling vessel 20 via the settling vessel discharge pipe 21.
[0043] The storage vessel 30 receives and stores the reaction solution from which polymers have been removed in the precipitation tank 20, and can control the transfer of the reaction solution to a subsequent process for separating a product.
[0044] The pressure in the storage vessel 30 may be lower than the pressure in the settling tank 20. For example, the pressure in the storage vessel 30 may be 1 kg / cm 2 lower than the pressure in the settling tank 20. 2 .g or more, 1.5kg / cm 2 .g or more, or 2kg / cm 2 .g or more, and 4kg / cm 2 .g or less, 4.5kg / cm 2 .g or less, or 5kg / cm 2 g or less. In this way, by adjusting the pressure of the storage vessel 30 to be lower than the pressure of the settling tank 20, the reaction liquid can be transferred from the settling tank 20 to the storage vessel 30 by using the pressure difference. In this case, the reaction liquid transferred from the settling tank 20 to the storage vessel 30 is transferred through a settling tank discharge pipe 21 equipped with a control valve 22, and by removing polymers from the reaction liquid in the settling tank 20, it is possible to prevent the occurrence of a fouling phenomenon in which the control valve is clogged by polymers during transfer.
[0045] The reaction liquid transfer system according to the present invention has been described and illustrated above. However, the above description and illustration only describe and illustrate the core configuration for understanding the present invention. In addition to the steps and devices described and illustrated above, steps and devices not described or illustrated can be appropriately applied and used to carry out the reaction liquid transfer system according to the present invention.
[0046] The present invention will be described in more detail with reference to the following examples. However, the following examples are merely for the purpose of illustrating the present invention, and it is obvious to those skilled in the art that various changes and modifications are possible within the scope of the scope and technical idea of the present invention, and the scope of the present invention is not limited to these examples.
[0047] Working Example Example 1 The reaction mixture was transferred according to the process flow diagram shown in attached FIG.
[0048] A feed stream was supplied to the reactor 10 to carry out an ethylene oligomerization reaction, which was also carried out in the following Examples 2 to 4 and Comparative Example 1.
[0049] In order to maintain the height of the reaction liquid in the reactor 10 at 1.4 m, a reactor discharge pipe 11 was installed on the side of the reactor 10 at a position corresponding to the surface height of the reaction liquid, and the reaction liquid was allowed to overflow into the settling tank 20 through the reactor discharge pipe 11. In this case, the reactor discharge pipe 11 was connected to the settling tank 20, had a downward inclination of 10° toward the settling tank 20, and did not have a control valve. In addition, the operating pressure of the reactor 10 and the settling tank 20 was set to 30 kg / cm. 2 .g were adjusted identically.
[0050] Under the condition that the temperature of the precipitation tank 20 was controlled at 20°C, the polymer in the reaction solution was precipitated in a solid state and removed, and an upper layer liquid containing the reaction solution from which the polymer was removed was formed. A precipitation tank discharge pipe 21 was provided at the height where the upper layer liquid was formed, and the reaction solution from which the polymer was removed was transferred to a storage vessel 30 through the precipitation tank discharge pipe 21. In this case, the precipitation tank discharge pipe 21 was provided at a position lower than the height of the reactor discharge pipe 11 connected to the precipitation tank 20, and a control valve 22 was provided on the precipitation tank discharge pipe 21. The operating pressure of the storage vessel 30 was 27 kg / cm 2 g, lower than the operating pressure of the settling tank 20.
[0051] In this manner, the reactor was operated for 10 hours, and the height of the reaction liquid in the reactor 10 was measured after the 10-hour operation. As a result, it was confirmed that the height of the reaction liquid in the reactor 10 was maintained at 1.4 m. This means that the control valve 22 provided in the settling tank discharge pipe 21 was not clogged with polymer, and the reaction liquid was smoothly discharged from the reactor 10, so that the height of the reaction liquid was maintained, and in this case, it was confirmed that the operation was sustainable.
[0052] Example 2 The reaction mixture was transferred according to the process flow diagram shown in attached FIG.
[0053] A feed stream was supplied to reactor 10 to carry out the ethylene oligomerization reaction.
[0054] In order to maintain the height of the reaction liquid in the reactor 10 at 1.4 m, a reactor discharge pipe 11 was installed on the side of the reactor 10 at a position corresponding to the surface height of the reaction liquid, and the reaction liquid was allowed to overflow into the settling tank 20 through the reactor discharge pipe 11. In this case, the reactor discharge pipe 11 was connected to the settling tank 20, had a downward inclination of 10° toward the settling tank 20, and did not have a control valve. In addition, the operating pressure of the reactor 10 and the settling tank 20 was set to 30 kg / cm. 2 .g were adjusted identically.
[0055] Under the condition that the temperature of the precipitation tank 20 was controlled at 50° C., the polymer contained in the reaction liquid was precipitated in a solid state and removed, and an upper layer liquid containing the reaction liquid from which the polymer was removed was formed. A precipitation tank discharge pipe 21 was provided at the height where the upper layer liquid was formed, and the reaction liquid from which the polymer was removed was transferred to a storage vessel 30 through the precipitation tank discharge pipe 21. In this case, the precipitation tank discharge pipe 21 was provided at a position lower than the height of the reactor discharge pipe 11 connected to the precipitation tank 20, and a control valve 22 was provided on the precipitation tank discharge pipe 21. The operating pressure of the storage vessel 30 was 27 kg / cm 2 g, lower than the operating pressure of the settling tank 20.
[0056] In this manner, the reactor was operated for 10 hours, and the height of the reaction liquid in the reactor 10 was measured after the 10-hour operation. As a result, it was confirmed that the height of the reaction liquid in the reactor 10 was maintained at 1.4 m. This means that the control valve 22 provided in the settling tank discharge pipe 21 was not clogged with polymer, and the reaction liquid was smoothly discharged from the reactor 10, so that the height of the reaction liquid was maintained, and in this case, it was confirmed that the operation was sustainable.
[0057] Example 3 The reaction mixture was transferred according to the process flow diagram shown in attached FIG.
[0058] A feed stream was supplied to reactor 10 to carry out the ethylene oligomerization reaction.
[0059] In order to maintain the height of the reaction liquid in the reactor 10 at 1.4 m, a reactor discharge pipe 11 was installed on the side of the reactor 10 at a position corresponding to the surface height of the reaction liquid, and the reaction liquid was allowed to overflow into the settling tank 20 through the reactor discharge pipe 11. In this case, the reactor discharge pipe 11 was connected to the settling tank 20, had a downward inclination of 10° toward the settling tank 20, and did not have a control valve. In addition, the operating pressure of the reactor 10 and the settling tank 20 was set to 30 kg / cm. 2 .g were adjusted identically.
[0060] Under the condition that the temperature of the precipitation tank 20 was controlled at 70°C, the polymer contained in the reaction liquid was precipitated in a solid state and removed, and an upper layer liquid containing the reaction liquid from which the polymer was removed was formed. A precipitation tank discharge pipe 21 was provided at the height where the upper layer liquid was formed, and the reaction liquid from which the polymer was removed was transferred to a storage vessel 30 through the precipitation tank discharge pipe 21. In this case, the precipitation tank discharge pipe 21 was provided at a position lower than the height of the reactor discharge pipe 11 connected to the precipitation tank 20, and a control valve 22 was provided on the precipitation tank discharge pipe 21. The operating pressure of the storage vessel 30 was 27 kg / cm 2 g, lower than the operating pressure of the settling tank 20.
[0061] In this manner, the reactor was operated for 10 hours, and the height of the reaction liquid in the reactor 10 was measured after the 10-hour operation. As a result, it was confirmed that the height of the reaction liquid in the reactor 10 was maintained at 1.4 m. This means that the control valve 22 provided in the settling tank discharge pipe 21 was not clogged with polymer, and the reaction liquid was smoothly discharged from the reactor 10, so that the height of the reaction liquid was maintained, and in this case, it was confirmed that the operation was sustainable.
[0062] Example 4 The reaction mixture was transferred according to the process flow diagram shown in attached FIG.
[0063] A feed stream was supplied to reactor 10 to carry out the ethylene oligomerization reaction.
[0064] In order to maintain the height of the reaction liquid in the reactor 10 at 1.4 m, a reactor discharge pipe 11 was installed on the side of the reactor 10 at a position corresponding to the surface height of the reaction liquid, and the reaction liquid was allowed to overflow into the settling tank 20 through the reactor discharge pipe 11. In this case, the reactor discharge pipe 11 was connected to the settling tank 20, had a downward inclination of 10° toward the settling tank 20, and did not have a control valve. In addition, the operating pressure of the reactor 10 and the settling tank 20 was set to 40 kg / cm. 2 .g were adjusted identically.
[0065] Under the condition that the temperature of the precipitation tank 20 was controlled at 50° C., the polymer contained in the reaction liquid was precipitated in a solid state and removed, and an upper layer liquid containing the reaction liquid from which the polymer was removed was formed. A precipitation tank discharge pipe 21 was provided at the height where the upper layer liquid was formed, and the reaction liquid from which the polymer was removed was transferred to a storage vessel 30 through the precipitation tank discharge pipe 21. In this case, the precipitation tank discharge pipe 21 was provided at a position lower than the height of the reactor discharge pipe 11 connected to the precipitation tank 20, and a control valve 22 was provided on the precipitation tank discharge pipe 21. The operating pressure of the storage vessel 30 was 37 kg / cm 2 g, lower than the operating pressure of the settling tank 20.
[0066] In this manner, the reactor was operated for 10 hours, and the height of the reaction liquid in the reactor 10 was measured after the 10-hour operation. As a result, it was confirmed that the height of the reaction liquid in the reactor 10 was maintained at 1.4 m. This means that the control valve 22 provided in the settling tank discharge pipe 21 was not clogged with polymer, and the reaction liquid was smoothly discharged from the reactor 10, so that the height of the reaction liquid was maintained, and in this case, it was confirmed that the operation was sustainable.
[0067] Comparative Example Comparative Example 1 The reaction mixture was transferred according to the process flow diagram shown in attached FIG.
[0068] A feed stream was supplied to reactor 10 to carry out the ethylene oligomerization reaction.
[0069] The reaction liquid was supplied to a storage vessel 30 through a reactor discharge pipe 12 provided on the side of the reactor 10 and equipped with a control valve 13. At this time, the operating pressure of the reactor 10 was 30 kg / cm. 2 g, and the operating pressure of the storage vessel 30 is adjusted to 27 kg / cm 2 The height of the reaction liquid in the reactor 10 was adjusted to 1.4 m using the control valve 13.
[0070] In this manner, the reactor was operated for 10 hours, and the height of the reaction liquid in the reactor 10 was measured after the 10-hour operation. As a result, it was confirmed that the height of the reaction liquid in the reactor 10 had risen to 3.0 m. This means that the control valve 13 provided in the reactor discharge pipe 12 was clogged with polymer, preventing the reaction liquid from being smoothly discharged from the reactor 10, causing the height of the reaction liquid to rise. In this case, it was confirmed that it was difficult to continue the operation, and therefore it was necessary to stop the operation and clean it. [Explanation of symbols]
[0071] 10. Reactor 11...Reactor discharge piping 12 Reactor discharge piping 13. Control valve 20. Settling tank 21...Settling tank discharge piping 22. Control valve 30 Storage container
Claims
1. a reactor for receiving and reacting a feed stream to form a reaction liquid; a reactor discharge pipe provided on a side of the reactor at a position corresponding to the surface height of the reaction liquid in the reactor, connected to a precipitation tank, and used to transfer the reaction liquid from the reactor to the precipitation tank; A precipitation tank for precipitating a polymer contained in the reaction solution, The polymer precipitated in the precipitation tank is removed without being fed to the reactor, The operating pressure of the reactor and the settling tank is the same; The reactor discharge pipe is provided so as to be inclined downward from the reactor to the settling tank, The reaction solution further includes a storage vessel for receiving and storing the reaction solution from the precipitation vessel, the pressure in the storage vessel is lower than the pressure in the settling tank; The reaction liquid delivery system, wherein the reactor is an ethylene oligomerization reactor.
2. 2. The reaction liquid transfer system of claim 1, wherein the reactor discharge piping does not include a control valve.
3. 2. The reaction liquid transport system according to claim 1, wherein the inclination of the reactor discharge pipe is 5° to 30°.
4. 2. The reaction liquid transport system according to claim 1, wherein the operating temperature of the precipitation tank is from 10°C to 90°C.
5. The operating pressure of the settling tank is 20 kg / cm 2 .g to 50 kg / cm 2 2. The reaction liquid transport system according to claim 1, wherein:
6. The pressure in the storage vessel is 1 kg / cm higher than the pressure in the settling tank. 2 .g to 5kg / cm 2 10. The reaction liquid transport system according to claim 1, wherein the reaction liquid transport system has a flow rate of 100 .001 g or less.
7. a settling tank discharge pipe connected from the settling tank to a storage vessel; 2. The reaction liquid transfer system according to claim 1, wherein the settling tank discharge pipe is formed on a side of the settling tank at a height where an upper layer liquid containing the reaction liquid from which the polymer has been removed is formed.
8. The reaction liquid transfer system according to claim 7 , wherein the settling tank discharge piping includes a control valve.
9. The reaction liquid transfer system according to claim 7 , wherein the settling tank discharge pipe is provided at a position lower than a height at which the reactor discharge pipe is connected to the settling tank.
Citation Information
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