Fractional distillation system and method

The fractional distillation system with a corrosion-resistant mesh and controlled diverter enhances separation efficiency and purity by using a corrosion-resistant mesh and multiple vacuums, addressing inefficiencies in existing systems.

JP2025537819APending Publication Date: 2025-11-20ENTEGRIS INC
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Patent Information

Application Number
JP2025528494
Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Priority Date
2022-11-15
Filing Date
2023-10-26
Publication Date
2025-11-20

AI Technical Summary

Technical Problem

Existing fractional distillation systems are inefficient and unable to meet purity requirements for separating components of liquid mixtures.

Method used

A fractional distillation system comprising a distillation vessel, a column with a corrosion-resistant mesh, a magnetically actuated diverter controlled by a timer, and multiple conduits connected to vacuums, which allows for efficient separation and collection of fractions.

Benefits of technology

The system enhances separation efficiency, reduces start-up time, and ensures stable distillation procedures by using a corrosion-resistant mesh and multiple vacuums, improving the reproducibility and purity of the distillation process.

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Abstract

The apparatus includes a distillation vessel configured to receive the mixture. The apparatus includes a column fluidly connected to the distillation vessel. A mesh is disposed in the column. The apparatus includes a plurality of conduits fluidly connected to respective vacuums. A fractionation top is fluidly connected to the column. The column is fluidly connected between the distillation vessel and the fractionation top.
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Description

[Technical Field]

[0001] The present disclosure relates to the field of distillation. More particularly, the present disclosure relates to systems and methods for fractional distillation. [Background technology]

[0002] Fractional distillation is a technique for separating the individual components or constituents of a mixture or composition. Fractional distillation takes advantage of the fact that each component of a composition or mixture (made up of several different components) has a unique boiling point or vaporization point that is different from the other components that make up the composition.

[0003] overview In some embodiments, the apparatus includes a distillation vessel configured to receive the mixture. In some embodiments, the apparatus includes a column fluidly connected to the distillation vessel. In some embodiments, a mesh is disposed in the column. In some embodiments, the apparatus includes a plurality of conduits fluidly connected to respective vacuums. In some embodiments, the fractionation overhead is fluidly connected to the column. In some embodiments, the column is fluidly connected between the distillation vessel and the fractionation overhead.

[0004] In some embodiments, the fractionation top comprises a magnetically actuated diverter.

[0005] In some embodiments, the magnetically actuated diverter is configured to be controlled by a timer.

[0006] In some embodiments, the device includes a pressure relief valve.

[0007] In some embodiments, the device includes a collection vessel configured to receive a first fraction of the mixture.

[0008] In some embodiments, a first conduit of the plurality of conduits is fluidly connected to the fractionation head.

[0009] In some embodiments, the mesh is made of a corrosion-resistant metal, hi some embodiments, the corrosion-resistant metal comprises at least one of stainless steel, a corrosion-resistant nickel alloy, or a combination thereof.

[0010] In some embodiments, the method includes obtaining a liquid mixture. In some embodiments, the method includes separating the liquid mixture by heating the liquid mixture in a distillation vessel. In some embodiments, the separating includes flowing vapor of the liquid mixture through a fraction overhead fluidly connected to the tower so as to contact a column having a mesh. In some embodiments, the method includes collecting a first fraction of the as-separated liquid mixture.

[0011] In some embodiments, the method includes controlling the fraction head via a timer to control the separation.

[0012] In some embodiments, the fractionation top includes a magnetically actuated diverter controlled by a timer.

[0013] In some embodiments, the method includes collecting a second fraction of the liquid mixture that remains separated.

[0014] In some embodiments, the method includes evacuating the top of the fractionation via a plurality of conduits fluidly connected to respective vacuums.

[0015] In some embodiments, the liquid mixture comprises a compound of the formula: TIFF2025537819000002.tif58170[where, R 1 and R 2 are each independently hydrogen, a straight chain alkyl, or a branched alkyl, and M is a metal. Includes.

[0016] In some embodiments, the device comprises a compound of the formula: TIFF2025537819000003.tif58170[where, R 1 and R 2 are each independently hydrogen, a straight chain alkyl, or a branched alkyl, and M is a metal. In some embodiments, the apparatus includes a distillation vessel configured to receive a liquid mixture comprising: a distillation vessel configured to receive a liquid mixture comprising: a distillation vessel; a column fluidly connected to the distillation vessel and configured to receive vapor from the distillation vessel; a corrosion-resistant mesh disposed within the column; a plurality of conduits fluidly connected to respective vacuums; a magnetically actuated diverter fluidly connected to the column and configured to receive vapor from the column.

[0017]

[0021] In some embodiments, the magnetically actuated diverter is configured to be controlled by a timer.

[0018] In some embodiments, the apparatus includes a collection vessel configured to receive a first fraction of the liquid mixture.

[0019] In some embodiments, a first conduit of the plurality of conduits is fluidly connected to a magnetically actuated diverter.

[0020] In some embodiments, the corrosion-resistant mesh is made of a corrosion-resistant metal.

[0021] In some embodiments, the corrosion-resistant metal comprises at least one of stainless steel, a corrosion-resistant nickel alloy, or a combination thereof.

[0022] Several embodiments of the present disclosure are described herein, by way of example only, with reference to the accompanying drawings. With specific reference to the drawings in detail, it is emphasized that the illustrated embodiments are intended by way of example and for illustrative discussion of the disclosed embodiments. In this regard, the description taken together with the drawings will make apparent to those skilled in the art how the disclosed embodiments may be made. [Brief explanation of the drawings]

[0023] [Figure 1] 1 illustrates a fractional distillation system according to some embodiments. [Figure 2] 1 shows a flow chart for a method for fractional distillation according to some embodiments.

[0024] Detailed Description Fractional distillation is a technique for separating the individual components or constituents that make up a mixture or composition. Fractional distillation takes advantage of the fact that each component that makes up a composition or mixture (composed of several different components) has a unique boiling point or vaporization point that is different from the other components that make up the composition. Existing fractional distillation systems can be inefficient, unable to meet purity requirements, or both. Embodiments of the present disclosure relate to improved fractional distillation systems that, in some embodiments, are efficient and able to meet purification requirements for distilling liquid mixtures.

[0025] 1 shows a fractional distillation system 100 according to some embodiments. The fractional distillation system 100 comprises a distillation vessel 102, a column 104, a mesh 106, a plurality of conduits 108 configured to be fluidly connected to respective vacuums, and a fractionation top 110.

[0026]

[0031] In some embodiments, the distillation vessel 102 is configured to receive a mixture (e.g., a liquid mixture). In some embodiments, the distillation vessel 102 can be, for example, a round-bottom flask, an Erlenmeyer flask, or a similar vessel capable of receiving and heating a liquid mixture. In some embodiments, heat can be applied, for example, via a Bunsen burner or the like. It should be appreciated that this is by way of example only and that the manner in which heat may be applied to the distillation vessel 102 is not limited thereto.

[0027] According to some embodiments, column 104 is fluidly connected to distillation vessel 102 at first end 112. According to some embodiments, column 104 is fluidly connected to fractionation overhead 110 at second end 114. Between first end 112 and second end 114, column 104 includes mesh 106.

[0028] In some embodiments, column 104 has a length L1. Length L1 can be selected based, for example, on the particular application of the liquid mixture being fractionated.

[0029] In some embodiments, mesh 106 spans length L2. In some embodiments, length L2 is less than length L1. In some embodiments, length L2 can be selected based on, for example, the particular application of the liquid mixture being fractionated. In some embodiments, length L2 can be selected based on length L2.

[0030] In some embodiments, the mesh 106 is formed from a corrosion-resistant metal. In some embodiments, the corrosion-resistant metal includes at least one of stainless steel, a corrosion-resistant nickel alloy, or a combination thereof. It should be appreciated that these materials are exemplary. In some embodiments, non-metallic materials may be utilized for the mesh 106. For example, in some embodiments, the mesh may be made from glass, ceramic, a combination thereof, or the like.

[0031] In some embodiments, the mesh 106 can have a large surface area and a high porosity. As a result, in some embodiments, the large surface area and high porosity can result in a low pressure drop across the column. As a result, in some embodiments, the column length and separation efficiency can be increased without increasing the temperature to which the distillation vessel 102 must be heated to perform the distillation.

[0032] In some embodiments, the mesh 106 can be formed from multiple flat ribbons of material. In some embodiments, the flat ribbons of material can be a corrosion-resistant metal or other metal (e.g., glass, ceramic, combinations thereof, etc.). In some embodiments, a configuration including interwoven flat ribbons of material can increase the surface area of ​​the mesh 106 compared to the volume of the mesh 106 (i.e., increase the surface area to volume ratio). It should be appreciated that this geometry is an example and that other geometries, such as tubular, can be used in accordance with the principles described herein.

[0033] Fractionation top 110 is fluidly connected to a second end 114 of column 104. According to some embodiments, fractionation top 110 includes a flow diverter 116. In some embodiments, flow diverter 116 is a magnetically actuated flow diverter. A magnetically actuated flow diverter allows for reduced variability between distillations and better reproducibility based on control of the magnetically actuated flow diverter. Fractionation top 110 may include a timer that indicates the position of flow diverter 116. In some embodiments, the timer may be part of flow diverter 116. In some embodiments, the timer may be configured in electronic communication with flow diverter 116, such that the flow diverter changes position upon expiration of the timer.

[0034] In some embodiments, fractional distillation system 100 is configured to receive a liquid mixture for distillation. In some embodiments, the liquid mixture contains a compound of the formula: TIFF2025537819000004.tif58170[where, R 1 and R 2are each independently hydrogen, a straight chain alkyl, or a branched alkyl, and M is a metal. In some embodiments, the metal is tungsten. It should be appreciated that fractional distillation system 100 can be used to distill liquid mixtures having compounds other than the examples above.

[0035]

[0042] The fractional distillation system 100 includes conduits 108 fluidly connected to respective vacuums. A first vacuum 118 is fluidly connected to a first conduit of the plurality of conduits 108 located at an end 120 of the fractionation top 110. A second vacuum 122 is fluidly connected to a second conduit of the plurality of conduits 108 located at an end 124 of the fractionation top 110. In some embodiments, the second vacuum 122 is fluidly connected adjacent to a flow diverter 116. In some embodiments, the conduits 108 are wide bore conduits. In some embodiments, wide bore conduits include conduits having a diameter sufficient for the size of the fractional distillation system 100 to compensate for tail gases. In some embodiments, the wide bore conduits may have a diameter of at least 0.5 inches for a fractional distillation system 100 having a capacity of 12 L.

[0036] In some embodiments, a collection vessel 126 is fluidly connected to the fractionation head 110. In some embodiments, more than one collection vessel 126 may be included, for example, to collect multiple fractions from the liquid mixture being distilled.

[0037] In some embodiments, a pressure relief valve 128 is fluidly connected to the fraction top 110 at the end 120 .

[0038] In some embodiments, including multiple conduits 108 fluidly connected to respective vacuums can reduce the time required to evacuate fractional distillation system 100, thereby, for example, reducing the start-up time for use of fractional distillation system 100. In some embodiments, multiple conduits 108 can reduce the time it takes for a vacuum to be restored if operation of the vacuum is interrupted. In some embodiments, the multiple conduits 108 and their fluid connections to the respective vacuums allow for a stable distillation procedure without cycling of the distillation rate.

[0039] 2 shows a flow chart for a method 150 for fractional distillation according to some embodiments. In some embodiments, the method 150 can be performed using the fractional distillation system 100 of FIG.

[0040] At block 152, the method 150 includes obtaining a liquid mixture. In some embodiments, the liquid mixture comprises a compound of the formula: Includes TIFF2025537819000005.tif58170. R 1 and R 2 are each independently hydrogen, a straight chain alkyl, or a branched alkyl. M is a metal. In some embodiments, the metal is tungsten.

[0041] At block 154, the method 150 includes separating the liquid mixture by heating the liquid mixture in a distillation vessel (e.g., distillation vessel 102 of FIG. 1 ). In some embodiments, the separation includes flowing vapor of the liquid mixture through a fractionation top (e.g., fractionation top 110 of FIG. 1 ) fluidly connected to a column (e.g., column 104 of FIG. 1 ) having a mesh (e.g., mesh 106 of FIG. 1 ) so as to contact the column. In some embodiments, the fractionation top includes a timer and a magnetically actuated diverter for controlling the fractionation top. In some embodiments, a timer is used to control the magnetically actuated diverter.

[0042] At block 156, the method 150 includes collecting a first fraction of the liquid mixture that remains separated. In some embodiments, optionally, a second fraction may be collected of the liquid mixture that remains separated. It should be appreciated that one or more additional fractions of the liquid mixture may also be collected.

[0043]

[0050] In some embodiments, the fractional distillation system may be evacuated using multiple wide-bore vacuums. In some embodiments, the inclusion of multiple wide-bore vacuum agents allows for faster evacuation of the distillation chamber than conventional methods.

[0044] Aspects Various aspects are described below. It should be understood that any one or more of the features mentioned in one or more of the following aspects can be combined with any other one or more aspects.

[0045] Aspect 1: 1. An apparatus comprising: a distillation vessel configured to receive a mixture; a column fluidly connected to the distillation vessel; a mesh disposed within the column; a plurality of conduits fluidly connected to respective vacuums; and a fractionation head fluidly connected to the column, wherein the column is fluidly connected between the distillation vessel and the fractionation head.

[0046] Aspect 2: 2. The apparatus of embodiment 1, wherein the fractionating top comprises a magnetically actuated diverter.

[0047] Aspect 3: 3. The apparatus of embodiment 2, wherein the magnetically actuated diverter is configured to be controlled by a timer.

[0048] Aspect 4: 4. The apparatus of any one of aspects 1 to 3, comprising a pressure relief valve.

[0049] Aspect 5: 5. The apparatus of any of aspects 1-4, comprising a collection vessel configured to receive a first fraction of the mixture.

[0050] Aspect 6: 6. The apparatus of any of aspects 1-5, wherein a first conduit of a plurality of conduits fluidly connected to a respective vacuum is fluidly connected to the fractionation head.

[0051] Aspect 7: 7. The device of any one of aspects 1 to 6, wherein the mesh is made of a corrosion-resistant metal.

[0052] Aspect 8: 8. The apparatus of embodiment 7, wherein the corrosion-resistant metal comprises at least one of stainless steel, a corrosion-resistant nickel alloy, or a combination thereof.

[0053] Aspect 9: Obtaining a liquid mixture, Separating the liquid mixture by heating the liquid mixture in a distillation vessel, the separation comprising flowing vapor of the liquid mixture into contact with a column having a mesh through a fractionation overhead fluidly connected to the column; and collecting a first fraction of said liquid mixture as separated; A method comprising:

[0054] Aspect 10: 10. The method of embodiment 9, comprising controlling the fractionation top head via a timer to control the separation.

[0055] Aspect 11: 11. The method of claim 10, wherein the fractionation top comprises a magnetically actuated diverter controlled by the timer.

[0056] Aspect 12: 12. The method of any one of embodiments 10 to 11, comprising collecting a second fraction of the liquid mixture that remains separated.

[0057] Aspect 13: 13. The method of any of aspects 10-12, comprising evacuating the fractionation heads via a plurality of conduits fluidly connected to respective vacuums.

[0058] Aspect 14: The liquid mixture comprises a compound of the formula: TIFF2025537819000006.tif58170[In the formula, R 1 and R 2 are each independently hydrogen, linear alkyl, or branched alkyl; M is a metal] 14. The method of any of embodiments 10 to 13, comprising:

[0059] Aspect 15: 1. An apparatus comprising: a distillation vessel configured to receive a liquid mixture comprising a compound of the formula: TIFF2025537819000007.tif58170[In the formula, R 1 and R 2 are each independently hydrogen, linear alkyl, or branched alkyl; M is a metal] a column fluidly connected to the distillation vessel and configured to receive vapor from the distillation vessel; a corrosion-resistant mesh disposed within the tower; a plurality of conduits fluidly connected to respective vacuums; and a magnetically actuated diverter fluidly connected to the column and configured to receive vapor from the column; An apparatus comprising:

[0060] Aspect 16: 16. The apparatus of embodiment 15, wherein the magnetically actuated diverter is configured to be controlled by a timer.

[0061] Aspect 17: 17. The apparatus of any one of aspects 15 to 16, comprising a collection vessel configured to receive a first fraction of the liquid mixture.

[0062] Aspect 18: 18. The apparatus of any of aspects 15-17, wherein a first conduit of a plurality of conduits fluidly connected to a respective vacuum is fluidly connected to the magnetically actuated diverter.

[0063] Aspect 19: Aspect 19. The apparatus of any of aspects 15-18, wherein the corrosion-resistant mesh is made of a corrosion-resistant metal.

[0064] Aspect 20: 20. The apparatus of embodiment 19, wherein the corrosion-resistant metal comprises at least one of stainless steel, a corrosion-resistant nickel alloy, or a combination thereof.

[0065] Among these disclosed benefits and improvements, other objects and advantages of the present disclosure will become apparent from the following description taken in conjunction with the accompanying drawings. Detailed embodiments of the present disclosure are disclosed herein. However, it should be understood that the disclosed embodiments are merely exemplary of the disclosure, which may be embodied in various forms. Additionally, examples given with respect to various embodiments of the disclosure are intended to be illustrative and not limiting.

[0066] All prior patents and publications referenced herein are incorporated by reference in their entirety.

[0067] Throughout the specification and claims, the following terms shall have the meanings expressly associated therewith, unless the context clearly dictates otherwise. As used herein, the phrases "in one embodiment," "in an embodiment," and "in some embodiments" do not necessarily refer to the same embodiment or embodiments, although they may. Additionally, as used herein, the phrases "in another embodiment" and "in some other embodiments" do not necessarily refer to different embodiments, although they may. It is intended that all disclosed embodiments may be combined without departing from the scope or spirit of the disclosure.

[0068] As used herein, the term "based on" is not exclusive and allows for based on additional unrecited elements unless the context clearly dictates otherwise. Additionally, throughout this specification, the meanings of "a," "an," and "the" include plural references. The meaning of "in" includes "in" and "on."

[0069] As used herein, the term "between" does not necessarily require being located immediately adjacent to another element. The term generally refers to a configuration in which something is sandwiched between two or more other things. At the same time, the term "between" can describe something that is immediately adjacent to two opposing things. Thus, in any one or more of the embodiments disclosed herein, a particular structural component that is located between two other structural elements may be: · A particular structural component is located directly between both of two other structural elements so that it is in direct contact with both of the other two structural elements; · A particular structural element is located immediately adjacent to only one of two other structural elements so that it is in direct contact with only one of the other two structural elements; · A particular structural element is indirectly located on only one of the other two structural elements, so that it is not in direct contact with only one of the other two structural elements, and there is another element that juxtaposes the particular structural element with one of the other two structural elements; · A particular structural component may be indirectly located between both of two other structural elements, such that it is not in direct contact with both of the other two structural elements, and other features may be located in between; Or any combination of these.

[0070] As used herein, "embedded" means that a first material is distributed throughout a second material.

[0071] It should be understood that changes can be made in details, particularly in relation to the materials of construction used and the shape, size and arrangement of parts, without departing from the scope of the present disclosure. The specification and described embodiments are examples, the true scope and spirit of the present disclosure being indicated by the following claims.

Claims

1. a distillation vessel configured to receive the mixture; a column fluidly connected to the distillation vessel; a mesh disposed within the tower; a plurality of conduits fluidly connected to respective vacuums; and a fractionation overhead in fluid connection with said column; An apparatus comprising: the column is fluidly connected between the distillation vessel and the fractionation overhead; Device.

2. The apparatus of claim 1 , wherein the fractionating top comprises a magnetically actuated diverter.

3. The apparatus of claim 2 , wherein the magnetically actuated diverter is configured to be controlled by a timer.

4. The apparatus of claim 1 comprising a pressure relief valve.

5. The apparatus of claim 1 , comprising a collection vessel configured to receive a first fraction of the mixture.

6. 10. The apparatus of claim 1, wherein a first of a plurality of conduits fluidly connected to a respective vacuum is fluidly connected to the fractionation head.

7. The device of claim 1 , wherein the mesh is made of a corrosion-resistant metal.

8. The apparatus of claim 7 , wherein the corrosion-resistant metal comprises at least one of stainless steel, a corrosion-resistant nickel alloy, or a combination thereof.

9. Obtaining a liquid mixture, separating the liquid mixture by heating the liquid mixture in a distillation vessel, the separation comprising flowing vapor of the liquid mixture into contact with a column having a mesh through a fractionation overhead fluidly connected to the column; and collecting a first fraction of said liquid mixture as separated; A method comprising:

10. 10. The method of claim 9, comprising controlling the fractionation top head via a timer to control the separation.

11. 11. The method of claim 10, wherein the fractionating top comprises a magnetically actuated diverter controlled by the timer.

12. 11. The method of claim 10, further comprising collecting a second fraction of the liquid mixture that remains separated.

13. 11. The method of claim 10, comprising evacuating the fractionation heads through a plurality of conduits fluidly connected to respective vacuums.

14. 10. The method of claim 1, wherein the liquid mixture comprises a compound of the formula: [In the formula, R 1 and R 2 are each independently hydrogen, linear alkyl, or branched alkyl; M is a metal. The method of claim 10, comprising:

15. 1. An apparatus comprising: A compound of the formula: [In the formula, R 1 and R 2 are each independently hydrogen, linear alkyl, or branched alkyl; M is a metal. a distillation vessel configured to receive a liquid mixture comprising: a column fluidly connected to the distillation vessel and configured to receive vapor from the distillation vessel; a corrosion-resistant mesh disposed within the tower; a plurality of conduits fluidly connected to respective vacuums; and a magnetically actuated diverter fluidly connected to the column and configured to receive vapor from the column; An apparatus comprising:

16. 16. The apparatus of claim 15, wherein the magnetically actuated diverter is configured to be controlled by a timer.

17. 16. The apparatus of claim 15, comprising a collection vessel configured to receive a first fraction of the liquid mixture.

18. 16. The apparatus of claim 15, wherein a first of a plurality of conduits fluidly connected to a respective vacuum is fluidly connected to the magnetically actuated diverter.

19. 16. The device of claim 15, wherein the corrosion-resistant mesh is made of a corrosion-resistant metal.

20. 20. The apparatus of claim 19, wherein the corrosion-resistant metal comprises at least one of stainless steel, a corrosion-resistant nickel alloy, or a combination thereof.

Citation Information

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