Low-temperature vacuum distillation equipment for synthesizing tertiary butyl ester compounds

Abstract

This invention discloses a low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds, comprising: a distillate tank, made of transparent borosilicate glass, for holding the tert-butyl ester compound solution to be distilled. Its transparency allows operators to easily observe the state and level of the internal solution and monitor the distillation process. The invention also includes a vacuum pump that precisely adjusts the system pressure according to distillation requirements, achieving vacuum distillation. At lower pressures, the boiling point of the tert-butyl ester compounds decreases, allowing distillation at lower temperatures and avoiding the degradation of compound activity by high temperatures. This is particularly suitable for purifying heat-sensitive tert-butyl ester compounds, ensuring product quality and performance. A temperature sensor is installed in the water bath heating tank to monitor the water bath temperature in real time and feed the signal back to the control system of the heating panel for precise temperature control.

Description

Technical Field

[0001] This utility model relates to the field of chemical synthesis technology, and in particular to a low-temperature vacuum distillation apparatus for the synthesis of tert-butyl ester compounds. Background Technology

[0002] In the field of chemical synthesis, tert-butyl esters have wide applications in numerous fields such as pharmaceuticals, fragrances, and polymer materials due to their unique chemical properties. Therefore, the efficient and high-quality synthesis and purification of tert-butyl esters are particularly important. Distillation is one of the key steps in the purification of tert-butyl esters.

[0003] Traditional distillation equipment has several limitations in the purification of tert-butyl esters. For heat-sensitive tert-butyl esters, traditional distillation often requires high temperatures, which can easily damage the compound's activity, leading to a decline in product quality and performance, failing to meet the demand for high-quality tert-butyl esters. In terms of distillation efficiency, traditional equipment struggles to achieve uniform boiling of the liquid, resulting in incomplete volatilization of the compound in the solution, low distillation efficiency, prolonged distillation time, and increased production time and costs. Furthermore, inaccurate temperature control is a major drawback of traditional distillation equipment. Temperature fluctuations affect the stability of the distillation process, leading to poor distillation results and difficulty in guaranteeing product quality and consistency. In the condensation stage, traditional distillation equipment has low condensation efficiency. Incomplete condensation of vapor into liquid results in vapor loss, reducing product collection rate. Moreover, the condensation temperature adjustment of traditional equipment is not flexible enough to adapt to the condensation requirements of tert-butyl esters with different boiling points, limiting the equipment's versatility and failing to meet diverse production needs. Utility Model Content

[0004] Therefore, it is necessary to provide a low-temperature vacuum distillation apparatus for the synthesis of tert-butyl ester compounds, which can precisely control the low-temperature vacuum conditions and has good sealing performance and high condensation efficiency, in order to address the above-mentioned technical problems.

[0005] To achieve the above objectives, the present invention adopts the following technical solution: A low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds includes: a distillate tank, which is made of transparent borosilicate glass and is used to hold the tert-butyl ester compound solution to be distilled. Its transparency allows operators to easily observe the state and level of the internal solution and monitor the distillation process. A Kirschner distillation head, mounted above the distillate tank, has an interface for inserting a capillary tube and a thermometer. The capillary tube is used to introduce an inert gas into the distillation system or to act as a bubble generation point to promote uniform boiling of the liquid. The thermometer is used to monitor the distillation temperature in real time. The capillary tube can be used to introduce an inert gas (such as nitrogen) into the distillation system to protect the compound from oxidation, or it can act as a bubble generation point to promote uniform boiling of the liquid. The thermometer provides accurate temperature information for operation by monitoring the distillation temperature in real time. The capillary tube and thermometer are fixed with a sealing plug to ensure a seal at the interface and prevent outside air from entering.

[0006] The inclined tube, connected at one end to the Kirschner distillation head and at the other end to a flow tube, is used to guide the distilled vapor. The flow tube is made of corrosion-resistant polytetrafluoroethylene with a smooth inner wall to reduce the flow resistance of the condensate and allow the condensate to flow smoothly into the condensate tank. The condenser is connected to three spiral condenser tubes via an inlet and outlet pipe. The spiral condenser tubes are made of copper, a high-efficiency heat-conducting material. The spiral structure increases the contact time and area between the steam and the cooling medium, thereby improving condensation efficiency.

[0007] A condensate tank, connected to the flow pipe, is used to collect the condensed liquid; A vacuum pump, connected to the system via a vacuum pipe, is used to reduce the pressure within the system and achieve vacuum distillation. A water bath heating tank is located outside the distillate tank, with a heating panel below it for water bath heating of the distillate tank.

[0008] In a preferred embodiment of the low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds provided by this utility model, sealing rings are provided between the Krirk distillation head, the distillate tank, and the inclined tube to ensure the sealing of the connection and prevent steam leakage.

[0009] In a preferred embodiment of the low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds provided by this utility model, the capillary and thermometer are fixed to the Kreutz distillation head by a sealing plug, which ensures the seal at the interface and prevents outside air from entering the system.

[0010] As a preferred embodiment of the low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds provided by this utility model, the spiral condenser is made of a high-efficiency thermally conductive material, and its spiral structure can increase the contact time and area between steam and cooling medium, thereby improving condensation efficiency.

[0011] As a preferred embodiment of the low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds provided by this utility model, the condenser is equipped with a temperature control system that can precisely adjust the temperature of the cooling medium to meet the condensation requirements of different tert-butyl ester compounds.

[0012] As a preferred embodiment of the low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds provided by this utility model, the water bath heating tank is equipped with a temperature sensor, which can monitor the water bath temperature in real time and feed the signal back to the control system of the heating panel to achieve precise temperature control.

[0013] As a preferred embodiment of the low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds provided by this utility model, the vacuum pump is equipped with a pressure regulating device, which can adjust the pressure in the system according to the distillation requirements.

[0014] In a preferred embodiment of the low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds provided by this utility model, the liquid flow tube is made of corrosion-resistant material and has a smooth inner wall to reduce the resistance of the condensate during the flow process.

[0015] As a preferred embodiment of the low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds provided by this utility model, the distillate tank, condensate tank and water bath heating tank are all made of transparent or semi-transparent materials, which facilitates observation of the state and level of the internal liquid.

[0016] In a preferred embodiment of the low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds provided by this utility model, the various components of the apparatus are connected by a quick-connect device, which facilitates the assembly, disassembly and maintenance of the apparatus.

[0017] Compared with the prior art, the present invention has the following beneficial effects: This invention provides a low-temperature vacuum distillation apparatus for the synthesis of tert-butyl ester compounds. The vacuum pump can precisely adjust the system pressure according to distillation requirements, achieving vacuum distillation. At lower pressures, the boiling points of tert-butyl ester compounds decrease, allowing distillation at lower temperatures and avoiding the degradation of compound activity by high temperatures. This is particularly suitable for the purification of heat-sensitive tert-butyl ester compounds, ensuring product quality and performance. The capillary tube can introduce inert gas into the distillation system to protect the compounds from oxidation and also serves as a bubble generation point, promoting uniform boiling. Uniform boiling allows for more complete volatilization of the compounds in the solution, improving distillation efficiency, shortening distillation time, and also contributing to higher product purity. A temperature sensor inside the water bath heating tank monitors the water bath temperature in real time and feeds the signal back to the control system on the heating panel for precise temperature control. Precise temperature control ensures that the distillation process is conducted under stable temperature conditions, avoiding the impact of temperature fluctuations on the distillation effect, making the distillation process more stable and reliable, and improving product quality and consistency.

[0018] This invention provides a low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds. The condenser is connected to three spiral condenser tubes via inlet and outlet pipes. These spiral condenser tubes are made of copper, a highly efficient heat-conducting material, and their spiral structure increases the contact time and area between the steam and the cooling medium, improving condensation efficiency and allowing for more complete condensation of the steam into liquid. This reduces steam loss and increases product collection rate. The condenser is equipped with an internal temperature control system that can precisely adjust the temperature of the cooling medium according to the condensation requirements of different tert-butyl ester compounds. For tert-butyl ester compounds with different boiling points, the cooling temperature can be flexibly adjusted to ensure that the steam condenses under optimal conditions, expanding the applicability and versatility of the equipment. Attached Figure Description

[0019] To more clearly illustrate the technical solutions in the embodiments of this utility model, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0020] Figure 1 A schematic diagram of the overall structure of this utility model; Figure 2 A schematic diagram showing the disassembled structure of the Kirschner distillation head, capillary tube, and thermometer provided by this utility model; Figure 3 A schematic diagram of the connection structure of the Kirschner distillation head, inclined tube, and flow tube provided by this utility model; Figure 4A schematic diagram showing the disassembled structure of the condenser and spiral condenser provided by this utility model; Figure 5 A schematic diagram showing the disassembled structure of the distillation tank and water bath heating tank provided by this utility model; Figure 6 This is a schematic diagram showing the disassembled structure of the air extraction pipe and air extraction pump provided by this utility model.

[0021] The markings in the diagram are explained as follows: 1. Distillate tank; 2. Condensate tank; 3. Kirschner distillation head; 4. Sealing ring; 5. Inclined tube; 6. Flow tube; 7. Vacuum tube; 8. Vacuum pump; 9. Water bath heating tank; 10. Heating panel; 11. Capillary tube; 12. Thermometer; 13. Sealing plug; 14. Condenser; 15. Discharge tube; 16. Inlet tube; 17. Spiral condenser. Detailed Implementation

[0022] To enable those skilled in the art to better understand the present invention, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort should fall within the protection scope of the present invention. Example

[0023] Please refer to Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 and Figure 6 A low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds includes components such as a distillate tank 1, a Kirschner head 3, an inclined tube 5, a condenser 14, a condensate tank 2, a vacuum pump 8, and a water bath heating tank 9.

[0024] The distillation tank 1 is used to hold the tert-butyl ester compound solution to be distilled. It is made of transparent borosilicate glass, allowing for easy observation of the internal solution's state and level. The Kirschner head 3 is mounted above the distillation tank 1, with a sealing ring 4 between them. The sealing ring 4 is made of high-temperature resistant and corrosion-resistant rubber material, effectively ensuring a tight seal and preventing vapor leakage during distillation. The Kirschner head 3 has interfaces for inserting a capillary tube 11 and a thermometer 12. The capillary tube 11 and thermometer 12 are fixed to the Kirschner head 3 by a sealing plug 13, which also provides excellent sealing performance, preventing outside air from entering the system. The capillary tube 11 can be used to introduce an inert gas, such as nitrogen, into the distillation system to protect the tert-butyl ester compound from oxidation during distillation; it can also serve as a bubble generation point, promoting uniform boiling of the liquid. The thermometer 12 is used to monitor the distillation temperature in real time, providing accurate temperature information to the operator. An inclined tube 5 is connected at one end to the Kirschner head 3 and at the other end to a flow tube 6, its function being to guide the distilled vapor. The flow tube 6 is made of polytetrafluoroethylene (PTFE), a material with excellent corrosion resistance. Its smooth inner wall reduces resistance during flow, allowing the condensate to flow smoothly into the condensate tank 2. The condensate tank 2, connected to the flow tube 6, is used to collect the condensed liquid and is also made of transparent borosilicate glass.

[0025] It is worth mentioning that the condenser 14 is connected to three spiral condenser tubes 17 via the inlet pipe 16 and the outlet pipe 15. The spiral condenser tubes 17 are made of copper, which has excellent thermal conductivity and is a highly efficient heat-conducting material. Furthermore, the spiral structure increases the contact time and area between the steam and the cooling medium, thereby improving condensation efficiency. The condenser 14 is equipped with a temperature control system that can precisely adjust the temperature of the cooling medium according to the condensation requirements of different tert-butyl ester compounds. For example, for some tert-butyl ester compounds with low boiling points, the temperature of the cooling medium can be lowered to ensure sufficient steam condensation. The vacuum pump 8 is connected to the system via the vacuum pipe 7 and is equipped with a pressure regulating device that can adjust the pressure within the system according to distillation requirements. During distillation, the vacuum pump 8 reduces the pressure within the system, allowing the tert-butyl ester compounds to boil at a lower temperature, achieving vacuum distillation and preventing high temperatures from damaging the compounds. The water bath heating tank 9 is located outside the distillate tank 1, with a heating panel 10 below it. The water bath heating tank 9 is equipped with a temperature sensor that can monitor the water bath temperature in real time and feed the signal back to the control system of the heating panel 10 for precise temperature control. For example, when the water bath temperature is lower than the set value, the heating panel 10 will automatically heat up; when the temperature reaches the set value, the heating panel 10 will stop heating, thereby ensuring the stability and accuracy of the distillation process.

[0026] Furthermore, the various components of the equipment are connected via quick-connect devices, facilitating assembly, disassembly, and maintenance. This benefits factory maintenance and improves the equipment's efficiency and lifespan.

[0027] The low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds provided by this utility model operates as follows: First, the tert-butyl ester compound solution to be distilled is introduced into the distillate tank 1. Then, the Kirschner head 3, inclined tube 5, and flow tube 6 are installed sequentially, and the sealing is checked. Next, the vacuum pump 8 is started to reduce the pressure in the system to the required value, and simultaneously, the heating panel 10 of the water bath heating tank 9 is activated to heat the distillate tank 1. During the distillation process, the temperature is monitored in real time by the thermometer 12, and the temperature of the cooling medium is adjusted by the temperature control system of the condenser 14 to ensure that the steam can be fully condensed and flow into the condensate tank 2. After distillation, the vacuum pump 8 and the heating panel 10 are turned off.

[0028] In this utility model, unless otherwise explicitly specified and limited, the terms "installation," "connection," "joining," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection, an electrical connection, or a connection that allows communication between them; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this utility model according to the specific circumstances.

[0029] Obviously, the embodiments described above are only some embodiments of this utility model, not all embodiments. The accompanying drawings show preferred embodiments of this utility model, but do not limit the patent scope of this utility model. This utility model can be implemented in many different forms; rather, the purpose of providing these embodiments is to provide a more thorough and comprehensive understanding of the disclosure of this utility model. Although this utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing specific embodiments, or make equivalent substitutions for some of the technical features. Any equivalent structures made using the content of this utility model specification and drawings, directly or indirectly applied to other related technical fields, are similarly within the patent protection scope of this utility model.

Claims

1. A low-temperature vacuum distillation apparatus for the synthesis of tert-butyl ester compounds, comprising a distillate tank (1), characterized in that: The distillation tank (1) is used to hold the tert-butyl ester compound solution to be distilled; The Kirschner distillation head (3) is installed above the distillate tank (1) and has an interface for inserting a capillary tube (11) and a thermometer (12). The capillary tube (11) is used to introduce inert gas into the distillation system or as a bubble generation point to promote uniform boiling of the liquid. The thermometer (12) is used to monitor the distillation temperature in real time. An inclined tube (5) is connected at one end to the Kreutz distillation head (3) and at the other end to a flow tube (6) to guide the distilled steam. The condenser (14) is connected to three spiral condenser tubes (17) through the liquid inlet pipe (16) and the liquid outlet pipe (15); A condensate tank (2) is connected to the liquid flow pipe (6) and is used to collect the condensed liquid; A vacuum pump (8) is connected to the system via a vacuum pipe (7) to reduce the pressure inside the system and achieve vacuum distillation. A water bath heating tank (9) is located outside the distillate tank (1) and a heating panel (10) is provided below it for water bath heating of the distillate tank (1).

2. The low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds according to claim 1, characterized in that, The Kreutz distillation head (3) is provided with sealing rings (4) between the distillate tank (1) and the inclined tube (5) to ensure the sealing of the connection and prevent steam leakage.

3. The low-temperature reduced-pressure distillation apparatus for synthesizing a tertiary butyl ester compound according to claim 1, characterized by, The capillary tube (11) and thermometer (12) are fixed to the Kreutz distillation head (3) by a sealing plug (13), which can ensure the seal at the interface and prevent outside air from entering the system.

4. The low-temperature reduced-pressure distillation apparatus for synthesizing a tertiary butyl ester compound according to claim 1, characterized by, The spiral condenser tube (17) is made of a high-efficiency heat-conducting material, and its spiral structure can increase the contact time and area between steam and cooling medium, thereby improving condensation efficiency.

5. The low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds according to claim 1, characterized in that, The condenser (14) is equipped with a temperature control system that can precisely adjust the temperature of the cooling medium to meet the condensation requirements of different tert-butyl ester compounds.

6. The low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds according to claim 1, characterized in that, The water bath heating tank (9) is equipped with a temperature sensor, which can monitor the water bath temperature in real time and feed the signal back to the control system of the heating panel (10) to achieve precise temperature control.

7. The low-temperature vacuum distillation apparatus for synthesizing tert-butyl ester compounds according to claim 1, characterized in that, The air pump (8) is equipped with a pressure regulating device, which can adjust the pressure in the system according to the distillation requirements.

8. A low-temperature reduced-pressure distillation apparatus for synthesizing tert-butyl ester compounds according to claim 1, characterized in that, The flow tube (6) is made of corrosion-resistant material and has a smooth inner wall to reduce the resistance of the condensate during the flow process.

9. The low-temperature reduced-pressure distillation apparatus for synthesizing a tertiary butyl ester compound according to claim 1, characterized by, The distillate tank (1), condensate tank (2) and water bath heating tank (9) are all made of transparent or semi-transparent materials, which makes it easy to observe the state and level of the internal liquid.

10. The low-temperature reduced-pressure distillation apparatus for synthesizing a tertiary butyl ester compound according to claim 1, characterized by, The various components of the device are connected by quick-connect devices, which facilitates the assembly, disassembly and maintenance of the device.

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