Condensation pipe, condensation reflux reaction device and method for feeding materials above condensation pipe

Abstract

The invention relates to a condensation pipe, a condensation reflux reaction device and a method for feeding materials above the condensation pipe. The condensation pipe comprises an outer pipe and an inner pipe, the inner pipe penetrates through the outer pipe, the inner pipe is a Tesla valve pipeline, and the downstream direction of the Tesla valve pipeline is opposite to the steam flowing direction of the condensation pipe; the outer pipe is provided with a liquid inlet and a liquid outlet, and a condensing agent channel is formed in the space between the outer pipe and the inner pipe. Through the reversely arranged Tesla valve pipeline and the condensation pipe, the condensation effect can be ensured, liquid splashing or backflow solvent spewing after feeding is prevented, and meanwhile the problem of inaccurate feeding caused by gasification-condensation circulation of part of raw materials in the condensation pipe due to heat exchange in the feeding process of the condensation pipe is solved. By means of the condensation pipe, the feeding operation in the backflow experiment process can be simplified, and safety and accuracy can be both considered when feeding is conducted above the condensation pipe.

Description

Technical Field

[0001] The invention relates to the technical field of condensation instruments, and in particular to a condenser, a condensation reflux reaction device and a method for feeding above the condenser. Background Art

[0002] In the process of condensation and reflux in chemical experiments, in order to quickly add the reaction raw materials during the reaction, the materials are often added directly above the reflux condenser. The conventional serpentine condenser channel is too long / the solvent flow rate is slow, which is easy to accumulate distillate or feed raw materials, which will lead to delayed feeding time and incomplete feeding. Although the straight condenser and spherical condenser have no lag in feeding time, they have the problem of poor condensation effect. If the reaction is violent during feeding, it may also cause steam or reaction substrate to splash / spray out of the condenser.

[0003] The temperature of the steam in the inner tube of the condenser decreases from the boiling point of the reflux solvent to the temperature of the condensing agent. If a raw material with a lower boiling point than the reflux solvent is directly added during the use of a serpentine condenser, the longer inner tube channel and the non-vertical pipe will result in a slower flow rate, which will transfer part of the heat of the steam to the input raw material, causing part of the input raw material to vaporize and be driven up by the steam of the reflux solvent until it condenses and repeats the process of heat exchange and vaporization to form a "vaporization-condensation cycle", resulting in part of the input raw material remaining in the condenser and unable to reach the reaction system. The smaller the feed equivalent, the more obvious this phenomenon is.

[0004] Currently, feeding above the condenser is faced with the following three problems: "ensuring the condensation effect", "preventing liquid splashing or reflux solvent gushing after feeding", and "heat exchange during the feeding process of the condenser causes part of the raw materials to be vaporized in the condenser, resulting in 'vaporization-condensation cycle' and inaccurate feeding". Often, only individual problems can be solved, and all three problems cannot be solved at the same time.

[0005] Therefore, it is particularly important to propose a condenser, a condensation reflux reaction device and a method for feeding above the condenser, which can ensure the condensation effect during the condensation reflux process, prevent liquid splashing or reflux solvent gushing after feeding, and solve the problem of inaccurate feeding caused by the heat exchange of the condenser during the feeding process, which causes part of the raw materials to be vaporized in the condenser "gasification-condensation cycle". Summary of the invention

[0006] In order to overcome the defects of the prior art, the present invention proposes a condenser, a condensation reflux reaction device and a method for feeding above the condenser, which can ensure the condensation effect during the condensation reflux process, prevent liquid splashing or reflux solvent gushing after feeding, and solve the problem of inaccurate feeding caused by the heat exchange of the condenser during the feeding process, which causes part of the raw materials to be vaporized in the condenser in the "gasification-condensation cycle".

[0007] To achieve this object, the present invention adopts the following technical solutions: A condenser provided by the present invention comprises an outer tube and an inner tube; the inner tube runs through the outer tube, the inner tube is a Tesla valve pipe, and the downstream direction of the Tesla valve pipe is opposite to the steam flow direction of the condenser; the outer tube has a liquid inlet and a liquid outlet, and the space between the outer tube and the inner tube forms a condenser channel.

[0008] It should be noted that the reverse-set Tesla valve pipeline refers to the Tesla valve pipeline or the Tesla valve whose downstream direction is opposite to the direction of steam flow during the condensation reflux process. During the ordinary condensation reflux process, the steam flows from bottom to top, that is, the steam flows from the air inlet to the air outlet; that is, the downstream direction of the Tesla valve pipeline is from top to bottom.

[0009] The Tesla valve is a passive fluid control device with a fixed geometric shape. Its characteristic is that the fluid encounters only small resistance when flowing forward into the Tesla valve, while the fluid encounters great resistance when flowing reversely into the Tesla valve, making forward flow easier than reverse flow, thereby achieving unidirectional flow flow limitation.

[0010] The condenser according to the embodiment of the present invention has at least the following beneficial effects: compared with the serpentine condenser, which needs to pass through a longer serpentine pipeline, heat exchange during the feeding process of the condenser causes part of the raw materials to be vaporized in the condenser, resulting in a "gasification-condensation cycle" that causes inaccurate feeding; through the reversely arranged Tesla valve pipeline, during the condensation reflux process, the Tesla valve in the downstream direction has less resistance to the substrate directly fed from the air outlet above the condenser, and the flow path is less than that of the countercurrent, so that the fed substrate can quickly enter the reaction vessel below, and has a more accurate and rapid feeding effect; and the steam below rises upward, which is a countercurrent direction for the Tesla valve. At this time, the Tesla valve plays a role of a flow disturbance, which can make the steam stay in the Tesla valve for a longer time, and has a better condensation effect for straight condensers and spherical condensers; the sputtering liquid during the violent reaction is in the countercurrent direction for the Tesla valve, and at this time the Tesla valve can directly prevent the backflow. Therefore, the present invention proposes a condenser that can simultaneously solve the three problems existing in the background technology: it can ensure the condensation effect during the condensation and reflux process, prevent liquid splashing after feeding or gushing of reflux solvent, and solve the problem of inaccurate feeding caused by the heat exchange of the condenser during the feeding process, which causes part of the raw materials to be vaporized in the condenser in the "vaporization-condensation cycle".

[0011] In some embodiments of the present invention, air inlets and / or air outlets are respectively provided at both ends of the outer tube penetrated by the inner tube.

[0012] It should be noted that the air inlet is connected to the reaction vessel in the condensation reflux process, and the steam in the reaction vessel enters the inner tube through the air inlet.

[0013] Preferably, the downstream direction of the Tesla valve pipeline is from the air outlet to the air inlet.

[0014] In some embodiments of the present invention, the material of the inner tube includes glass and metal; preferably, the metal includes at least one of iron, copper and aluminum.

[0015] In some embodiments of the present invention, the diameter of the inner tube is 0.3-10 cm; preferably, the diameter of the inner tube is 0.3-3 cm; further preferably, the diameter of the inner tube is 0.3-1 cm.

[0016] It should be noted that the diameter of the inner tube is selected according to the size of the reaction system. For a ton-level reaction, the maximum diameter can be selected to be 10 cm; for a kilogram-level reaction, the maximum diameter can be selected to be 3 cm; for a gram-level reaction, the maximum diameter can be selected to be 1 cm. The length of the corresponding condenser tube is selected according to the tube diameter, production requirements and common knowledge in the field.

[0017] In some embodiments of the present invention, the Tesla valve pipeline is composed of multiple single-stage Tesla valve group pipelines; preferably, the Tesla valve pipeline is composed of 5-30 single-stage Tesla valve pipelines, and the single-stage Tesla valve pipeline includes a main channel and a branch channel; further preferably, the Tesla valve pipeline is composed of 5-20 single-stage Tesla valve pipelines; further preferably, the Tesla valve pipeline is composed of 5-15 single-stage Tesla valve pipelines.

[0018] In some embodiments of the present invention, the angle between the main channel and the branch channel is 30° to 60°; preferably, the angle between the main channel and the branch channel is 40° to 50°.

[0019] In some embodiments of the present invention, the ratio of the length of the main channel to the length of the branch channel is 1:1.2-3; preferably, the ratio of the length of the main channel to the length of the branch channel is 1:1.2-2.

[0020] In some embodiments of the present invention, the main channel is a straight channel.

[0021] In some embodiments of the present invention, the branch channel is an arc channel.

[0022] In a second aspect, another technical solution provided by the present invention is: a condensation reflux reaction device, which comprises any of the above-mentioned condensation tubes.

[0023] In a third aspect, another technical solution provided by the present invention is: a method for feeding materials above a condenser, wherein the method uses any of the above-mentioned condensers.

[0024] Beneficial effects of the present invention: The present invention proposes a condenser, which, compared with the serpentine condenser, needs to pass through a longer serpentine pipeline: during the feeding process of the condenser, heat exchange causes part of the raw materials to be vaporized in the condenser, and the "vaporization-condensation cycle" leads to the problem of inaccurate feeding; through the Tesla valve pipeline set in reverse, during the condensation reflux process, the Tesla valve in the downstream direction has less resistance to the substrate directly fed from the air outlet above the condenser, and the flow path is less than the countercurrent, so that the fed substrate can quickly enter the reaction vessel below, and has a more accurate and rapid feeding effect; and the steam below rises upward, which is a countercurrent direction for the Tesla valve. At this time, the Tesla valve plays a role of a flow disturbance, which can make the steam stay in the Tesla valve for a longer time, and has a better condensation effect for straight condensers and spherical condensers; the sputtering liquid during the violent reaction is in the countercurrent direction for the Tesla valve, and at this time the Tesla valve can directly prevent the backflow.

[0025] Therefore, the present invention proposes a condenser that can simultaneously solve the three problems existing in the background technology: it can ensure the condensation effect during the condensation and reflux process, prevent liquid splashing after feeding or gushing of reflux solvent, and solve the problem of inaccurate feeding caused by the heat exchange of the condenser during the feeding process, which causes part of the raw materials to be vaporized in the condenser in the "vaporization-condensation cycle". BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0027] Figure 1 is a schematic structural diagram of a condenser according to Embodiment 1 of the present invention; Figure 2 is a 3D effect schematic diagram of a condenser tube according to another embodiment of the present invention; Reference numerals: Glass outer tube 100 , glass inner tube 200 , liquid inlet 101 , liquid outlet 102 , gas inlet 103 , gas outlet 104 . DETAILED DESCRIPTION

[0028] Embodiments of the present invention are described in detail below, and examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and cannot be understood as limiting the present invention.

[0029] The present invention adopts the following technical solutions: The present invention provides a condenser, comprising an outer tube and an inner tube; the inner tube runs through the outer tube, the inner tube is a Tesla valve pipe, and the downstream direction of the Tesla valve pipe is opposite to the steam flow direction of the condenser; the outer tube has a liquid inlet and a liquid outlet, and the space between the outer tube and the inner tube forms a condenser channel.

[0030] According to some embodiments of the present invention, air inlets and / or air outlets are respectively provided at both ends of the outer tube penetrated by the inner tube.

[0031] It should be noted that the air inlet is connected to the reaction vessel in the condensation reflux process, and the steam in the reaction vessel enters the inner tube through the air inlet.

[0032] According to some embodiments of the present invention, the material of the inner tube includes glass and metal; preferably, the metal includes at least one of iron, copper and aluminum.

[0033] According to some embodiments of the present invention, the diameter of the inner tube is 0.3-10 cm; preferably, the diameter of the inner tube is 0.3-3 cm; further preferably, the diameter of the inner tube is 0.3-1 cm.

[0034] It should be noted that the diameter of the inner tube is selected according to the size of the reaction system. For a ton-level reaction, the maximum diameter can be selected to be 10 cm; for a kilogram-level reaction, the maximum diameter can be selected to be 3 cm; for a gram-level reaction, the maximum diameter can be selected to be 1 cm. The length of the corresponding condenser tube is selected according to the tube diameter, production requirements and common knowledge in the field.

[0035] According to some embodiments of the present invention, the Tesla valve pipeline is composed of multiple single-stage Tesla valve group pipelines; preferably, the Tesla valve pipeline is composed of 5-30 single-stage Tesla valve pipelines, and the single-stage Tesla valve pipeline includes a main channel and a branch channel; further preferably, the Tesla valve pipeline is composed of 5-20 single-stage Tesla valve pipelines; further preferably, the Tesla valve pipeline is composed of 5-15 single-stage Tesla valve pipelines.

[0036] According to some embodiments of the present invention, the angle between the main channel and the branch channel is 30° to 60°; preferably, the angle between the main channel and the branch channel is 40° to 50°.

[0037] According to some embodiments of the present invention, the ratio of the length of the main channel to the branch channel is 1:1.2-3; preferably, the ratio of the length of the main channel to the branch channel is 1:1.2-2.

[0038] According to some embodiments of the present invention, the main channel is a straight channel.

[0039] According to some embodiments of the present invention, the branch channel is an arc channel.

[0040] In a second aspect, another technical solution provided by the present invention is: a condensation reflux reaction device, which comprises any of the above-mentioned condensation tubes. Example 1

[0041] A condenser, such as Figure 1 , Figure 1 1 is a schematic structural diagram of a condenser tube according to Embodiment 1 of the present invention, comprising a glass outer tube 100 and a glass inner tube 200; The glass inner tube 200 penetrates the glass outer tube 100, and the glass inner tube 200 is a Tesla valve pipeline arranged in reverse direction (the downstream direction is from the air outlet to the air inlet); The glass outer tube 100 has a liquid inlet 101 and a liquid outlet 102, and the space between the glass outer tube 100 and the glass inner tube 200 forms a condensing agent channel; An air inlet 103 and an air outlet 104 are respectively provided at both ends of the glass outer tube 100 penetrated by the glass inner tube 200 .

[0042] The diameter of the glass inner tube 200 is 0.5 cm.

[0043] The Tesla valve pipeline is composed of 6 single-stage Tesla valve pipelines, and the outlet directions of each single-stage Tesla valve pipeline are arranged alternately. The single-stage Tesla valve pipeline includes a main channel and a branch channel. The main channel is a 1 cm straight channel, and the branch channel is a 2 cm long arc channel. The angle between the main channel and the branch channel is 45°, and the ratio of the length of the main channel to the branch channel is 1:2.

[0044] The heating reaction kettle is equipped with the above-mentioned condenser to form a condensation reflux reaction device.

[0045] Figure 2 It is a schematic diagram of the 3D effect of a condenser according to another embodiment of the present invention.

[0046] Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that the glass inner tube of Example 1 is replaced with a straight condenser tube with a diameter of 1 cm. The condenser tube of Comparative Example 1 has the same height as the condenser tube of Example 1.

[0047] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that the glass inner tube of Example 1 is replaced with a serpentine condenser tube having a diameter of 0.5 cm and a rotating outer diameter of 3 cm. The condenser tube of Comparative Example 2 has the same height as the condenser tube of Example 1.

[0048] Comparative Example 3 The condenser tube of comparative example 3 has two glass inner tubes, one inner tube is a glass straight tube with a diameter of 1 cm of comparative example 1, and the other inner tube is a glass serpentine tube with a diameter of 0.5 cm and a rotating outer diameter of 3 cm of comparative example 2. The condensation channel is selected by shielding the movable blades between the two inner tubes. The glass serpentine tube is selected during condensation, and the glass straight tube is selected during feeding. The condenser tube of comparative example 3 has the same height as the condenser tube of embodiment 1.

[0049] Although the straight condenser of Comparative Example 1 is convenient for feeding, its condensation effect is poor, and when additional reactants are added during the condensation reflux, if boiling occurs, the boiling solvent or splashes are easily sprayed out from the top of the straight condenser.

[0050] The serpentine condenser of Comparative Example 2 increases the efficiency of heat exchange by increasing the length of the condensation channel and the degree of tortuosity of the condensation channel, which can ensure the condensation effect and prevent liquid splashing during boiling to a certain extent; however, it cannot necessarily prevent the upward gushing of the solvent during boiling, because the single-channel condenser does not have a one-way valve to prevent backflow. If a one-way valve is added, the upward solvent vapor cannot pass; At the same time, the condenser tube (such as the serpentine condenser tube) that achieves good condensation effect by increasing the length of the condensation channel and increasing the degree of tortuosity of the condensation channel also has a problem: the temperature of the steam in the inner tube of the condenser tube decreases from the boiling point to the temperature of the condensing agent. If the raw material with a boiling point lower than the boiling point of the reflux solvent in the reaction system is directly added during the use of the serpentine condenser tube, then the longer inner tube channel will transfer part of the heat of the steam to the input raw material, causing part of the input raw material to vaporize and be driven up by the solvent vapor until it condenses and repeats the process of heat exchange and vaporization to form a "vaporization-condensation cycle", resulting in part of the input raw material remaining in the condenser tube and unable to reach the reaction system. The smaller the feed equivalent, the more obvious this phenomenon is.

[0051] Although the double-channel condenser of Comparative Example 3 can solve the problem of inaccurate feeding amount due to the formation of a "vaporization-condensation cycle" caused by the excessively long condensation channel during feeding in the condenser, a straight glass tube is used in the feeding process, and there is still a possibility that boiling solvent or splashes will be easily sprayed out from the top of the straight glass tube. The poor condensation effect during the feeding process will also cause a part of the reflux solvent to be lost.

[0052] The downstream direction of the condenser of Example 1 is from the air outlet to the air inlet. The reflux solvent and feed raw materials from top to bottom mainly flow through the main pipeline to the reaction system below. The distance is similar to that of the straight condenser. The heat exchange time is very short, and it is difficult to form a "gasification-condensation cycle"; and the reflux solvent condensed in the branch channel will converge in the main channel, resulting in a larger flow and flow rate of the reflux solvent in the main channel. Even if there is residual feed, the residual feed can be flushed to the reaction system very quickly. The steam below rises upward, which is a countercurrent direction for the Tesla valve. The steam path is the main channel plus the branch channel. At the same time, the reverse Tesla valve plays a role of a flow disturbance, which can make the steam stay in the Tesla valve for a longer time, and has a better condensation effect for the straight condenser and the spherical condenser; the sputtering liquid / gushing liquid during the violent reaction is a countercurrent direction for the Tesla valve. At this time, the Tesla valve can directly prevent backflow. Therefore, the present invention proposes a condenser that can simultaneously solve the three problems existing in the background technology: it can ensure the condensation effect during the condensation and reflux process, prevent liquid splashing after feeding or gushing of reflux solvent, and solve the problem of inaccurate feeding caused by the "gasification-condensation cycle" in which part of the raw materials are vaporized in the condenser due to heat exchange during the feeding process, especially the serpentine condenser.

[0053] In previous technologies, Tesla valves are mostly used in throttle valves or one-way valves. There has never been a related technology that uses Tesla valves to solve the problem of "the heat exchange of condensers during the feeding process, especially serpentine condensers and other condensers with good condensation effect, which causes part of the raw materials to be vaporized in the condenser "vaporization-condensation cycle" leading to inaccurate feeding"; there has never been a related technology that simultaneously solves the three problems existing in the background technology: ensuring the condensation effect during the condensation and reflux process, preventing liquid splashing after feeding or reflux solvent gushing, and solving the problem of the heat exchange of the condenser during the feeding process, which causes part of the raw materials to be vaporized in the condenser "vaporization-condensation cycle" leading to inaccurate feeding.

[0054] The condenser tube of the present invention can simplify the feeding operation in the reflux experiment, and ensure both safety and accuracy when feeding above the condenser tube.

[0055] Although the embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the claims and their equivalents.

Claims

1. A condenser, characterized in that: Including outer tube and inner tube; The inner tube passes through the outer tube, the inner tube is a Tesla valve tube, and the downstream direction of the Tesla valve tube is opposite to the steam flow direction of the condenser tube; The outer tube has a liquid inlet and a liquid outlet, and the space between the outer tube and the inner tube forms a condensing agent channel.

2. A condenser according to claim 1, characterized in that: Both ends of the outer tube penetrated by the inner tube are respectively provided with air inlets and / or air outlets.

3. A condenser according to claim 2, characterized in that: The downstream direction of the Tesla valve pipeline is from the air outlet to the air inlet.

4. A condenser according to claim 1, characterized in that: The diameter of the inner tube is 0.3-10 cm.

5. The condenser according to claim 1, characterized in that: The Tesla valve pipeline is composed of 5-30 single-stage Tesla valve pipelines, and the single-stage Tesla valve pipeline includes a main channel and a branch channel.

6. A condenser according to claim 5, characterized in that: The included angle between the main channel and the branch channel is 30° to 60°.

7. The condenser according to claim 5, characterized in that: The ratio of the length of the main channel to the length of the branch channel is 1:1.2-3.

8. The condenser according to claim 5, characterized in that: The main channel is a straight channel, and the branch channel is an arc channel.

9. A condensation reflux reaction device, characterized in that: The condensation reflux reaction device comprises the condenser tube according to any one of claims 1 to 8.

10. A method for feeding above a condenser, characterized in that: The method uses the condenser described in any one of claims 1 to 8.

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