A heating reflux device for high temperature derivatization, saponification reaction

Abstract

The application relates to the field of experimental equipment, and particularly discloses a heating reflux device for high-temperature derivation and saponification reaction, which comprises a base and a fixing frame fixedly arranged on the base, at least two heating cavities with independent temperature control are arranged on the base and used for heating reaction containers; a plurality of composite condensing device groups are detachably arranged on the fixing frame, the plurality of composite condensing device groups correspond to the plurality of heating cavities in a one-to-one manner; each composite condensing device group comprises a plurality of condensing units, each condensing unit comprises a lower air condensing section and an upper medium condensing section, and the lower end of the lower air condensing section is detachably connected to the mouth of the reaction container. The application can simultaneously meet the requirements of sufficient condensation reflux in high-temperature experiments and reduction of water resource consumption.

Description

Technical Field

[0001] This application relates to the field of experimental equipment, and in particular to a heating reflux device for high-temperature derivatization and saponification reactions. Background Technology

[0002] In analytical testing in fields such as food, the pretreatment of target substances such as imazalil, fatty acids, and fat-soluble vitamins typically involves derivatization, saponification, or hydrolysis reactions under high-temperature heating. These reactions generally require reflux condensation at specific temperatures to prevent solvent and reactant evaporation losses, ensure complete reaction, and reduce the release of toxic and harmful gases.

[0003] The traditional condenser tubes (single-medium cooling, such as water cooling) commonly used in current detection procedures have the following shortcomings under high-throughput, high-temperature, or complex reaction conditions: In high-temperature (>200℃) experiments such as imazalil derivatization, the large volume of steam and high temperature necessitate a continuous flow of large amounts of cooling water to achieve the desired condensation effect, resulting in significant water consumption. Furthermore, traditional water condenser tubes may experience a sharp drop in condensation efficiency due to severe thermal shock at high temperatures, and there is a risk of tube bursting. Although air condensation (relying on natural convection for heat dissipation) can replace water cooling in some reactions to reduce water consumption, its cooling capacity is limited. In high-temperature derivatization reactions such as imazalil derivatization, air condensation alone cannot promptly and adequately condense and reflux the large amount of high-temperature steam; this may lead to significant volatilization losses of valuable reactants, intermediates, products, and harmful gases (such as pyridine hydrochloride decomposition products), directly affecting the accuracy and precision of the detection results and impacting the experimental environment and personnel health. Therefore, a single condensation method cannot simultaneously meet the requirements of adequate condensation and reflux in high-temperature experiments and reduced water consumption. Utility Model Content

[0004] To address the problem that traditional single condensation methods cannot simultaneously achieve efficient condensation reflux and reduce water consumption, this application provides a heating reflux device for high-temperature derivatization and saponification reactions.

[0005] The heating reflux device for high-temperature derivatization and saponification reactions provided in this application adopts the following technical solution:

[0006] A heating reflux device for high-temperature derivatization and saponification reactions includes a base and a fixed frame fixedly mounted on the base. The base has at least two independently temperature-controlled heating chambers for heating a reaction vessel. Multiple composite condensation device groups are detachably mounted on the fixed frame, each group corresponding to one of the heating chambers. Each composite condensation device group includes multiple condensation units, each unit comprising a lower air condensation section and an upper medium condensation section. The lower end of the lower air condensation section is detachably connected to the inlet of the reaction vessel.

[0007] Furthermore, the lower air condensation section is a spike-shaped condenser tube exposed to the air.

[0008] Furthermore, the upper medium condensation section is a serpentine condenser or a spherical condenser with a medium inlet and a medium outlet.

[0009] Furthermore, the medium inlet is connected to a condensing medium supply system, wherein the condensing medium is water or ethanol.

[0010] This application employs a segmented condensation design. The lower air condensation section serves as a pre-cooling zone, utilizing natural airflow for initial cooling of the high-temperature steam. This effectively reduces the steam temperature and slows its ascent, allowing the steam to enter the upper medium condensation section in a gentler state. The upper medium condensation section is the main cooling zone, using water or ethanol as the condensing medium for further condensation of the steam. This segmented condensation design helps to address the problems of drastic drops in condensation efficiency and high risk of glass breakage caused by severe thermal shock in traditional water-cooled condenser tubes at high temperatures. Furthermore, the lower air condensation section requires no cooling medium, and the upper medium condensation section, due to the pre-cooling of the steam, significantly reduces the consumption of cooling water or ethanol and improves condensation reflux efficiency.

[0011] Furthermore, the height of the lower air condensation section accounts for 30%-50% of the total height of the condensation unit.

[0012] An appropriate height ratio between the lower air condensation section and the upper medium condensation section is beneficial for improving condensation reflux efficiency.

[0013] Furthermore, the lower air condensation section and the upper medium condensation section are fixedly connected by a connecting structure.

[0014] Furthermore, the connection structure is a ground joint, and the lower air condensation section is detachably connected to the upper medium condensation section.

[0015] The lower air condensation section and the upper medium condensation section are connected by a ground joint for easy connection and disassembly.

[0016] Furthermore, the mounting bracket has multiple mounting holes for the condensing unit to pass through, and the diameter of the mounting holes is adapted to the outer diameter of the condensing unit.

[0017] The mounting bracket provides support and stability to the condenser unit.

[0018] Furthermore, a graphite heat-conducting block is provided in the heating chamber, and the graphite heat-conducting block has holes for accommodating the reaction vessel; multiple heating rods are uniformly embedded in the graphite heat-conducting block.

[0019] During the experiment, the reaction vessel was placed in the hole on the graphite heat-conducting block, and the graphite heat-conducting block was heated by a heating rod. The high thermal conductivity of graphite helps to conduct heat quickly and avoid local overheating, thereby heating the reaction vessel evenly.

[0020] Furthermore, an insulation layer is provided between the inner wall of the heating chamber and the graphite heat-conducting block.

[0021] The insulation layer helps reduce heat loss from the graphite heat-conducting block.

[0022] In summary, this application includes at least one of the following beneficial technical effects:

[0023] 1. This application uses the lower air condensation section (pre-cooling zone) to pre-cool the high-temperature steam, effectively reducing the steam temperature and slowing down the steam rise rate, so that the steam enters the upper medium condensation section (main cooling zone) in a gentler state. The segmented condensation design helps to improve the problem of the sudden drop in condensation efficiency and high risk of glass breakage caused by severe thermal shock at high temperatures in traditional water condenser tubes. At the same time, the lower air condensation section uses natural air flow for heat dissipation without any cooling medium. Since the steam in the upper medium condensation section has been pre-cooled, the consumption of cooling water or ethanol is significantly reduced, and the condensation reflux efficiency is improved.

[0024] 2. This application combines a zoned independent temperature control system with a composite condensation design, enabling simultaneous high-temperature reactions (such as 240℃ imazalil derivatization) and medium-temperature reactions (such as 80℃ fatty acid derivatization and 80℃ fat-soluble vitamin saponification). Each zone operates independently according to different temperature requirements, which helps to improve experimental efficiency. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of the overall structure of an embodiment of this application.

[0026] Reference numerals: 1. Base; 11. Heating chamber; 12. Graphite heat-conducting block; 121. Hole; 2. Fixing frame; 21. Fixing hole; 3. Composite condensation device assembly; 31. Condensation unit; 311. Lower air condensation section; 312. Upper medium condensation section. Detailed Implementation

[0027] The following is in conjunction with the appendix Figure 1 This application will be described in further detail.

[0028] This application discloses a heating reflux apparatus for high-temperature derivatization and saponification reactions. (Refer to...) Figure 1The heating reflux device for high-temperature derivatization and saponification reactions includes a base 1 and a fixed frame 2 fixedly mounted on the base 1; the base 1 is provided with at least two independently temperature-controlled heating chambers 11 for heating the reaction vessel; the fixed frame 2 is detachably provided with multiple composite condensation device groups 3, and the multiple composite condensation device groups 3 correspond one-to-one with the multiple heating chambers 11.

[0029] Reference Figure 1 Each composite condensing unit group 3 comprises multiple condensing units 31, each condensing unit 31 including a lower air condensing section 311 and an upper medium condensing section 312. The lower air condensing section 311 is a spike-shaped condenser tube exposed to air; the upper medium condensing section 312 is a serpentine or spherical condenser tube with a medium inlet and a medium outlet. Typically, the medium inlet is located at the lower part of the serpentine or spherical condenser tube, and the medium outlet is located at the upper part. The medium inlet is connected to a condensing medium supply system, and the condensing medium is water or ethanol. The height of the lower air condensing section 311 accounts for 30%-50% of the total height of the condensing unit 31.

[0030] Furthermore, the lower air condensation section 311 and the upper medium condensation section 312 are fixedly connected by a connecting structure, specifically a ground glass joint. The upper end of the lower air condensation section 311 and the lower end of the upper medium condensation section 312 are detachably connected by a plug-in joint, facilitating connection and disassembly. The lower end of the lower air condensation section 311 is also detachably connected to the reaction vessel inlet by a ground glass joint plug-in joint.

[0031] Reference Figure 1 The mounting bracket 2 has multiple mounting holes 21 for the condensing unit 31 to pass through, and the diameter of the mounting holes 21 is adapted to the outer diameter of the condensing unit 31. The mounting bracket 2 can provide support and stability for the condensing unit 31. To improve the stability of the condensing unit 31, an elastic fixing ring can be fixed in the mounting hole 21. The fixing ring is fitted onto the upper medium condensing section 312, so that the upper medium condensing section 312 is stably placed on the mounting bracket 2. Furthermore, one side of the mounting hole 21 is connected to a strip hole. When installing the upper medium condensing section 312, the connecting pipe on the serpentine condensing tube or the spherical condensing tube used to connect to the condensing medium supply system can pass through the strip hole on the mounting bracket 2, which facilitates the installation of the condensing tube.

[0032] This application employs a segmented condensation design. The lower air condensation section 311 serves as a pre-cooling zone, utilizing natural airflow for heat dissipation. This pre-cools the high-temperature vapor escaping from the reaction vessel opening, effectively reducing the vapor temperature and slowing its ascent, allowing the vapor to enter the upper medium condensation section 312 in a gentler state. The upper medium condensation section 312 is the main cooling zone, using water or ethanol as the condensing medium for further condensation of the vapor. This segmented condensation design helps to address the problems of drastic drop in condensation efficiency and high risk of glass breakage caused by severe thermal shock in traditional water-cooled condenser tubes at high temperatures. Furthermore, the lower air condensation section 311 requires no cooling medium, and the upper medium condensation section 312, due to the pre-cooling of the vapor, significantly reduces the consumption of cooling water or ethanol and improves condensation reflux efficiency.

[0033] To heat the reaction vessel (reaction tube, reaction flask, etc.), refer to... Figure 1 A graphite heat-conducting block 12 is provided inside the heating chamber 11, and multiple heating rods (not shown in the figure) are uniformly embedded in the graphite heat-conducting block 12. Each graphite heat-conducting block 12 has multiple holes 121 for accommodating the reaction vessel; the holes 121 are usually round holes, and the size of the holes 121 is adapted to the size of the reaction vessel, so that the outer wall of the reaction vessel can fully contact the inner wall of the holes 121 to achieve uniform heat transfer.

[0034] During the experiment, the reaction vessel was placed in the hole 121 on the graphite heat-conducting block 12. The graphite heat-conducting block 12 was heated by heating rods. The high thermal conductivity of graphite facilitates rapid heat conduction, avoiding localized overheating and thus ensuring uniform heating of the reaction vessel. The heating rods are symmetrically distributed to reduce edge effects and ensure temperature consistency within the same heating chamber 11. To reduce heat loss from the graphite heat-conducting block 12, an insulation layer can be provided between the inner wall of the heating chamber 11 and the graphite heat-conducting block 12. The insulation layer is made of a material with low thermal conductivity, such as multilayer composite ceramic fiberboard.

[0035] To enable independent temperature control of each graphite heat-conducting block 12, each block is equipped with an independent thermocouple (not shown in the figure). Specifically, the temperature-sensing end of the thermocouple is embedded inside the graphite heat-conducting block 12 of each heating chamber 11. Based on the Seebeck effect, the thermocouple converts the temperature difference at the detection point into a micro-voltage signal. This signal is transmitted to the central control unit via an analog-to-digital converter. Based on the feedback data from the thermocouples in each heating chamber 11, the output power of the corresponding heating rod is dynamically adjusted using a PID (proportional-integral-derivative) algorithm to accurately compensate for heat loss and suppress temperature fluctuations. Each heating chamber 11 operates independently according to different temperature requirements, enabling multiple experiments at different temperatures to be conducted simultaneously on a single heating reflux device, thus improving experimental efficiency.

[0036] To reduce the impact of harmful gas emissions on the environment and personnel, an exhaust and harmful gas absorption device can be installed on the fixed frame 2 to absorb the harmful gases escaping from the upper opening of the condensation unit 31; alternatively, the heating reflux device provided in this embodiment can be placed in a fume hood for use.

[0037] For reactions that require continuous stirring, an ultrasonic device or a magnetic stirrer can be installed in the base 1 to achieve homogenization of the reactants, thereby ultrasonically mixing the reactants in the reaction flask or using a magnetic stirrer in the reaction flask to stir and mix the reactants.

[0038] The heating reflux apparatus provided in this application is suitable for various experiments in the field of food testing, such as imazalil derivatization, fatty acid derivatization, and saponification of fat-soluble vitamins, as detailed below:

[0039] Example 1: Derivatization reaction of prochloraz

[0040] The reaction flask containing the extract residue of imazalil and pyridine hydrochloride was placed in the graphite heat-conducting block 121 of heating zone A. The condensation unit 31 was installed on the fixing frame 2 and connected to the mouth of the reaction flask. The temperature of heating zone A was set to 230±0.5℃. During the reaction, the lower air condensation section 311 used air condensation and the upper medium condensation section 312 used water cooling. Heating was stopped after 60 minutes of reaction.

[0041] Example 2: Fatty acid derivatization reaction

[0042] The reaction flask containing fatty acid extract (oil droplets) and sodium hydroxide methanol solution is placed in the graphite heat-conducting block 121 of heating zone B. The condensation unit 31 is installed on the fixing frame 2 and connected to the mouth of the reaction flask. The temperature of heating zone B is set to 80±0.2℃. During the reaction, the lower air condensation section 311 uses air condensation and the upper medium condensation section 312 uses water cooling. After the oil droplets in the reaction flask disappear, boron trifluoride methanol solution is injected from the top of the condenser tube (without disassembling the device). The reaction is maintained at 80℃ for 10 minutes and then heating is stopped.

[0043] Example 3: Saponification reaction of fat-soluble vitamins

[0044] The vitamin-containing sample, anhydrous ethanol, and potassium hydroxide solution were placed in a reaction flask and placed in the graphite heat-conducting block 121 of the heating zone C. The condensation unit 31 was installed on the fixing frame 2 and connected to the mouth of the reaction flask. The temperature of the heating zone C was set to 80±0.2℃. During the reaction, the lower air condensation section 311 used air condensation, and the upper medium condensation section 312 used ethanol cooling. Heating was stopped after 30 minutes of reaction.

[0045] The above are all preferred embodiments of this application and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. A heating reflux apparatus for high-temperature derivatization and saponification reactions, characterized in that: The device includes a base and a mounting bracket fixedly mounted on the base. The base has at least two independently temperature-controlled heating chambers for heating a reaction vessel. The mounting bracket has multiple composite condensation device groups detachably mounted on it, with each composite condensation device group corresponding to one of the heating chambers. Each composite condensation device group includes multiple condensation units, and each condensation unit includes a lower air condensation section and an upper medium condensation section. The lower end of the lower air condensation section is detachably connected to the inlet of the reaction vessel.

2. The heating reflux apparatus for high-temperature derivatization and saponification reactions according to claim 1, characterized in that: The lower air condensation section is a spike-shaped condenser tube exposed to the air.

3. The heating reflux apparatus for high-temperature derivatization and saponification reactions according to claim 2, characterized in that: The upper medium condensation section is a serpentine condenser or a spherical condenser with a medium inlet and a medium outlet.

4. The heating reflux apparatus for high-temperature derivatization and saponification reactions according to claim 3, characterized in that: The lower air condensation section and the upper medium condensation section are fixedly connected by a connecting structure.

5. A heating reflux apparatus for high-temperature derivatization and saponification reactions according to claim 4, characterized in that: The connection structure is a ground joint, and the lower air condensation section is detachably connected to the upper medium condensation section.

6. A heating reflux apparatus for high-temperature derivatization and saponification reactions according to claim 3, characterized in that: The medium inlet is connected to a condensing medium supply system, and the condensing medium is water or ethanol.

7. The heating reflux apparatus for high-temperature derivatization and saponification reactions according to claim 1, characterized in that: The height of the lower air condensation section accounts for 30%-50% of the total height of the condensation unit.

8. A heating reflux apparatus for high-temperature derivatization and saponification reactions according to claim 1, characterized in that: The mounting bracket has multiple mounting holes for the condensing unit to pass through, and the diameter of the mounting holes is adapted to the outer diameter of the condensing unit.

9. A heating reflux apparatus for high-temperature derivatization and saponification reactions according to claim 1, characterized in that: The heating chamber is provided with a graphite heat-conducting block, and the graphite heat-conducting block has holes for accommodating the reaction vessel; multiple heating rods are uniformly embedded in the graphite heat-conducting block.

10. A heating reflux apparatus for high-temperature derivatization and saponification reactions according to claim 9, characterized in that: An insulation layer is provided between the inner wall of the heating chamber and the graphite heat-conducting block.

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