Multifunctional partition temperature control continuous extraction instrument

Abstract

The application discloses a multifunctional partition temperature control continuous extraction instrument, which comprises a flask, an extraction tube and a reflux condenser, and the top end of the flask is connected with the reflux condenser through the extraction tube; a first interval partition plate and a second interval partition plate are sequentially arranged in the extraction tube from top to bottom, the extraction tube is divided into an upper extraction area, a lower extraction area and a bottom avoiding area from top to bottom through the first interval partition plate and the second interval partition plate, the bottom avoiding area is connected with the top end of the flask, and the top end of the upper extraction area is connected with the reflux condenser; a bypass pipe is arranged on one side of the extraction tube, the top end of the bypass pipe is connected with the upper extraction area, the middle part of the bypass pipe is connected with the lower extraction area, the bottom end of the bypass pipe is connected with the bottom avoiding area, an upper siphon pipe is arranged between the bottom end of the upper extraction area and the lower extraction area, and a lower flow pipe is arranged between the bottom end of the lower extraction area and the inside of the flask; heating equipment is arranged on the outer periphery of the upper extraction area and the lower extraction area.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of chemical sample processing, in particular to a multifunctional partition temperature control continuous extraction instrument. BACKGROUND

[0002] The extraction instrument is a kind of glass instrument for extracting required substances from solid substances by using organic solvents. The Soxhlet extractor, which is commonly used at present, is divided into three parts from bottom to top, namely flask, extraction tube and condenser tube, and is a commonly used extraction device. When the Soxhlet extractor is used for extraction, the solvent in the lower flask is continuously vaporized, the vaporized solvent reaches the upper condenser tube through the bypass pipe of the extraction tube, and is cooled into liquid and dropped into the extraction tube to soak the extracted material to achieve the extraction purpose. However, since the extraction temperature of each substance is different, the existing extraction instrument can only extract one kind of substance, and cannot simultaneously extract different substances under different temperature conditions, so its functionality is relatively single, and it is necessary to improve it. SUMMARY

[0003] The present application aims at the above problems, and provides a multifunctional partition temperature control continuous extraction instrument with simple structure and partition temperature control extraction operation.

[0004] In order to achieve the above purpose, the technical scheme of the present application is as follows:

[0005] A multifunctional partition temperature control continuous extraction instrument, comprising a flask, an extraction tube and a reflux condenser tube, the top end of the flask is connected with the reflux condenser tube through the extraction tube; a first interval partition plate and a second interval partition plate are arranged in the extraction tube from top to bottom, and the interior of the extraction tube is divided into an upper extraction zone, a lower extraction zone and a bottom avoiding zone from top to bottom by the first interval partition plate and the second interval partition plate, the bottom avoiding zone is connected with the top end of the flask, and the top end of the upper extraction zone is connected with the bottom end of the reflux condenser tube; a bypass pipe is arranged on one side of the extraction tube, the top end of the bypass pipe is connected with the top of the upper extraction zone, the middle of the bypass pipe is connected with the top of the lower extraction zone, the bottom end of the bypass pipe is connected with the bottom avoiding zone, an upper siphon pipe is arranged between the bottom end of the upper extraction zone and the lower extraction zone, and a lower flow pipe is arranged between the bottom end of the lower extraction zone and the interior of the flask; heating devices are arranged on the outer periphery of the upper extraction zone and the lower extraction zone respectively.

[0006] Further, the heating devices comprise an upper infrared heating jacket and a lower infrared heating jacket, the upper infrared heating jacket and the lower infrared heating jacket are fixedly sleeved on the outer side of the extraction tube, the upper infrared heating jacket is located on the outer side of the upper extraction zone and performs heating operation on the upper extraction zone, and the lower infrared heating jacket is located on the outer side of the lower extraction zone and performs heating operation on the lower extraction zone.

[0007] Further, the upper siphon pipe is provided with an upper siphon pipe backflow control valve for controlling the flow state of the upper siphon pipe; and the lower flow pipe is provided with a lower flow pipe backflow control valve for controlling the flow state of the lower flow pipe.

[0008] Further, one side of the lower extraction zone is provided with a lower extraction zone feed inlet for feeding into the lower extraction zone, and the lower extraction zone feed inlet is a closable feed inlet.

[0009] Further, the flask is provided with an electric heating jacket outside the flask for heating the interior of the flask; the bottom end of the flask is provided with a bottom liquid outlet connected with a liquid outlet conduit, and the bottom liquid outlet is provided with a liquid outlet control valve.

[0010] Further, the top end of the flask is provided with a liquid inlet on one side and connected with a liquid inlet assembly; the liquid inlet assembly comprises a plurality of liquid storage bottles, the top end of each of the liquid storage bottles is provided with a liquid storage bottle feed inlet, the bottom end of each of the liquid storage bottles is provided with a liquid storage bottle discharge outlet provided with a liquid storage bottle control valve, and the liquid storage bottle discharge outlets are in communication with one end of a flow guide pipe, and the other end of the flow guide pipe is in communication with the liquid inlet at the top end of the flask.

[0011] Further, each of the liquid storage bottles is fixedly connected to a liquid storage bottle support.

[0012] Further, the multifunctional partition temperature control continuous extraction instrument further comprises an extraction instrument controller connected with the upper infrared heating jacket, the lower infrared heating jacket and the electric heating jacket in circuit and respectively controlling the heating temperature thereof; and the extraction instrument controller is connected with the upper siphon pipe backflow control valve, the lower flow pipe backflow control valve, the liquid outlet control valve and the plurality of liquid storage bottle control valves in circuit and respectively controls the opening and closing state thereof.

[0013] Compared with the prior art, the present application has the advantages and positive effects that:

[0014] 1. The present application can simultaneously extract two different extracted substances at different temperatures by dividing the extraction pipe into an upper extraction zone and a lower extraction zone and arranging infrared heating jackets outside the zones, thereby improving the extraction efficiency and precision.

[0015] 2. The present application can extract a single extracted substance or two extracted substances simultaneously by arranging the upper siphon pipe and the lower flow pipe and arranging control valves, thereby diversifying the functions of the extraction instrument.

[0016] 3. The present invention, by setting up a number of storage bottles, allows different types of solvents to be contained in different storage bottles. Under the control of the extraction instrument controller, the alternating and continuous automatic extraction operation of different solvents on the extracted material can be realized.

[0017] 4. This invention can place different solid-phase adsorbents and extraction solvents in several storage bottles, and different solid-phase adsorbents and extraction solvents can be selected according to the properties of the target substance, which has a wide range of applicability and application scope.

[0018] 5. During the extraction process, the present invention allows for sampling and testing of different types of solvents or extracts at different reaction times in the flask without stopping the reaction, making the operation more convenient.

[0019] 6. After extraction, the present invention allows the extract to be directly concentrated and injected into the sample without the need for filtration, centrifugation and other steps, which facilitates automation.

[0020] 7. This invention can achieve extraction and purification simultaneously, simplifying the operation steps, reducing sample loss and error, and improving the precision and accuracy of the experimental operation. Attached Figure Description

[0021] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0022] Figure 1 This is a schematic diagram of the structure of the present invention. Detailed Implementation

[0023] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, any modifications, equivalent substitutions, improvements, etc., made by those skilled in the art to all other embodiments obtained without creative effort should be included within the protection scope of the present invention.

[0024] like Figure 1As shown, the embodiment discloses a multifunctional partition temperature control continuous extraction instrument, which mainly comprises an extraction tube 2, a round-bottom flask 17, a No. 1 liquid storage bottle 23, a No. 2 liquid storage bottle 24, an electric heating jacket 30, an upper infrared heating jacket 3, a lower infrared heating jacket 4, an extraction instrument controller 31, a first interval baffle 7 and a second interval baffle 11 arranged in the extraction tube 2 from top to bottom, and the extraction tube 2 is divided into an upper extraction zone 6, a lower extraction zone 10 and a bottom avoiding zone 15 from top to bottom by the first interval baffle 7 and the second interval baffle 11, the top end of the upper extraction zone 6 is connected with a reflux condenser tube 1 for condensation and reflux of gas, the inner diameter of the upper port of the extraction tube 2 is 4-5 cm, the inner diameter of the lower port is 3-4 cm, and the inner diameter of the extraction tube 2 is 8-10 cm, a lower extraction zone feed inlet 9 is arranged on the side wall of the lower extraction zone 10, the diameter of the lower extraction zone feed inlet is 3-5 cm, an upper siphon tube 12 is arranged on the right side of the upper extraction zone 6 and has a height of 8-10 cm, one end of the upper siphon tube 12 is communicated with the upper end of the first interval baffle 7, and the other end forms a pipeline downward and has an outlet close to the top of the lower extraction zone 10, an upper siphon tube reflux control valve 13 is arranged in the pipeline of the upper siphon tube 12 and has an inner diameter of 0.5-1 cm, a lower flow-through tube 14 is arranged on the right side of the lower extraction zone 10, one end of the lower flow-through tube 14 is communicated with the upper end of the second interval baffle 11, the other end forms a pipeline downward and has an outlet communicated with a round-bottom flask port 18, a lower flow-through tube reflux control valve 16 is arranged in the pipeline of the lower flow-through tube 14 and has an inner diameter of 0.5-1 cm, a bypass tube 5 is arranged on the left side of the extraction tube 2, the top end of the bypass tube 5 is connected with the upper extraction zone 6, a communication interface 8 is arranged in the middle of the bypass tube 5 and connects the lower extraction zone 10 through the communication interface 8, and the bottom end of the bypass tube 5 is connected with the bottom avoiding zone 15, the bottom avoiding zone 15 is communicated with the round-bottom flask port 18, a liquid inlet 19 of the round-bottom flask 17 is communicated with the No. 1 liquid storage bottle 23 and the No. 2 liquid storage bottle 24, a liquid outlet 20 at the bottom of the round-bottom flask 17 is communicated with a liquid outlet pipe 22, a liquid outlet control valve 21 is arranged and used for controlling the opening and closing state of the liquid outlet 20 and discharging liquid in the round-bottom flask, the liquid inlet 19 of the round-bottom flask 17 is connected with the No. 1 liquid storage bottle 23 and the No. 2 liquid storage bottle 24 through a flow guide pipe 28, the No. 1 liquid storage bottle 23 and the No. 2 liquid storage bottle 24 are arranged on a liquid storage bottle support 29, liquid storage bottle feed inlets 25 are arranged at the top ends of the two liquid storage bottles, the liquid storage bottle feed inlets 25 are used for adding different solvents into the bottles, liquid storage bottle discharge outlets 26 are arranged at the bottom ends of the two liquid storage bottles and are connected with liquid storage bottle control valves 27, the liquid storage bottle control valves 27 control the flow of the solvents in the liquid storage bottles into the round-bottom flask 17, and the inner diameter of the liquid storage bottle control valves is 0.5~1cm; the electric heating jacket 30 is used for heating the round bottom flask 17, the upper infrared heating jacket 3 and the lower infrared heating jacket 4 are respectively used for heating the upper extraction zone 6 and the lower extraction zone 10, and the temperature of the upper and lower extraction zones can be independently adjusted and controlled; the extraction instrument controller 31 can respectively set the temperature, time and switch of the electric heating jacket 30, the upper infrared heating jacket 3 and the lower infrared heating jacket 4, and can also set and switch the opening and closing time of the upper siphon reflux control valve 13, the lower flow tube reflux control valve 16, the liquid outlet control valve 21 and the storage bottle control valve 27.

[0025] In the partition temperature control continuous extraction process, the upper extraction zone 6 and the lower extraction zone 10 are respectively put into different solid samples wrapped with filter paper, the solid sample for low temperature extraction is placed in the upper extraction zone 6, and the solid sample for high temperature extraction is placed in the lower extraction zone 10; different kinds of solvents are added in the round bottom flask 17, the No. 1 liquid storage bottle 23 and the No. 2 liquid storage bottle 24, the reflux condenser 1, the extraction tube 2, the round bottom flask 17, the liquid outlet conduit 22, the flow conduit 28, the No. 1 liquid storage bottle 23 and the No. 2 liquid storage bottle 24 are connected from top to bottom and then placed in the electric heating jacket 30, the upper infrared heating jacket 3, the lower infrared heating jacket 4, the upper siphon tube reflux control valve 13, the lower flow tube reflux control valve 16, the liquid outlet control valve 21 and the liquid storage bottle control valve 27 are connected to the extraction instrument controller 31 through the round hole plug line, the display screen and the key of the extraction instrument controller 31 are opened, the upper infrared heating jacket 3 and the lower infrared heating jacket 4 are opened, the temperature of the upper infrared heating jacket 3 is set to be lower than that of the lower infrared heating jacket 4, the lower flow tube reflux control valve 16 is set to be opened 10 seconds before the siphon reflux of the upper extraction zone 6, and is closed after 10 seconds (for example, the siphon reflux period of the upper extraction zone 6 is 200 seconds, the lower flow tube reflux control valve 16 is set to be closed for 190 seconds and opened for 10 seconds, and the action period of the two extraction zones is synchronized for 200 seconds), the opening time of the liquid storage bottle control valve 27 of the No. 1 liquid storage bottle 23 and the No. 2 liquid storage bottle 24 is set, the heating time, the heating temperature and the extraction liquid discharge time of the electric heating jacket 30 to the round bottom flask 17 are set, and after the setting, the automatic control sequence of the extraction instrument is as follows: the upper siphon tube reflux control valve 13, the lower flow tube reflux control valve 16, the liquid storage bottle control valve 27 and the liquid outlet control valve 21 are closed, the round bottom flask 17 is heated, the solvent in the round bottom flask 17 enters the upper extraction zone 6 through the bypass tube 5 and enters the reflux condenser 1 for condensation, the condensed solvent is refluxed into the upper extraction zone 6, and under the action of the upper infrared heating jacket 3, the solid sample in the upper extraction zone 6 is extracted, when the solvent in the upper extraction zone 6 reaches a certain height, it is siphoned back to the lower extraction zone 10, 10 seconds before the siphon reflux of the condensate, the lower flow tube reflux control valve 16 is opened, the liquid in the lower extraction zone 10 is first refluxed into the round bottom flask 17 through the lower flow tube 14, 10 seconds later, the lower flow tube reflux control valve 16 is closed, the upper siphon tube reflux control valve 13 is opened, the condensate in the upper extraction zone 6 enters the lower extraction zone 10 through the upper siphon tube 12 and under the action of the lower infrared heating jacket 4, the solid sample in the lower extraction zone 10 is extracted, after the reflux of the condensate in the upper extraction zone 6 is completed, the upper siphon tube reflux control valve 13 is closed, and the next reflux operation is waited.After 60-120 minutes, the round bottom flask 17 stops heating, the upper siphon reflux control valve 13, the lower flow tube reflux control valve 16 and the liquid outlet control valve 21 are opened, the liquid in the extraction tube 2 is refluxed into the round bottom flask 17, and then is discharged through the bottom liquid outlet 20 of the round bottom flask 17 for collection; after 5-10 minutes, the upper siphon reflux control valve 13, the lower flow tube reflux control valve 16 and the liquid outlet control valve 21 are closed, and the liquid storage bottle control valve 27 is opened, so that the solvent in the No. 1 liquid storage bottle 23 enters the round bottom flask 17 through the flow guide tube 28, and the above steps are repeated to extract the solid sample in the upper extraction zone 6 and the lower extraction zone 10 again with the solvent in the No. 1 liquid storage bottle 23; the above sequence is repeated, and finally the solid sample in the upper extraction zone 6 and the lower extraction zone 10 is extracted again with the solvent in the No. 2 liquid storage bottle 24, so that the solid sample is finally extracted with three kinds of extraction solvents automatically and alternately.

[0026] During the extraction process, the solvent in the round bottom flask 17 is boiled under the heating of the electric heating jacket 30, the generated steam is condensed into the reflux condenser 1 through the bypass tube 5, the refluxed solvent passes through the sample and extracts the related substances, and during the extraction process, the liquid outlet control valve 21 can be opened at any time to take samples through the liquid outlet guide tube 22; after each extraction is completed, the lower flow tube reflux control valve 16 is closed, and the round bottom flask 17 is heated for distillation, so that the extraction and distillation are realized without transferring the liquid.

[0027] The extraction instrument in the embodiment is used to analyze the extraction rates of acetone, tetrahydrofuran and carbon disulfide on the anthracite and coking coal and the composition of the extraction liquid, and the specific operation is as follows:

[0028] Put the coking coal sample into the upper extraction zone and the anthracite coal sample into the lower extraction zone through the extraction tube top end port, add the acetone solvent into the round bottom flask, add the tetrahydrofuran solvent into the No.1 liquid storage bottle, and add the carbon disulfide solvent into the No.2 liquid storage bottle, place the round bottom flask in the electric heating jacket connected with the extraction instrument controller, connect the upper end of the extraction tube with the reflux condenser, close the upper siphon tube reflux control valve, the lower flow tube reflux control valve, the liquid storage bottle control valve and the liquid outlet control valve, set the lower flow tube reflux control valve to be closed for 300s and then opened for 10s when the round bottom flask starts to heat through the extraction instrument controller, and cycle in this order, set the heating temperature of the round bottom flask containing the acetone solution to be 55 DEG C, the heating temperature of the upper infrared heating jacket to be 45 DEG C, the heating temperature of the lower infrared heating jacket to be 55 DEG C, and the heating time to be 60 min; when the tetrahydrofuran solution is used as the solvent, the heating temperature of the round bottom flask is 65 DEG C, the heating temperature of the upper infrared heating jacket is 55 DEG C, the heating temperature of the lower infrared heating jacket is 65 DEG C, and the heating time is 60 min; when the carbon disulfide solution is used as the solvent, the heating temperature of the round bottom flask is 45 DEG C, the heating temperature of the upper infrared heating jacket is 35 DEG C, the heating temperature of the lower infrared heating jacket is 45 DEG C, and the heating time is 60 min; the reflux liquid replacement time of the extraction liquid extracted by each kind of solvent is 10 min; after the setting is completed, the automatic alternating extraction operation of the three kinds of extraction solvents on the sample is started for 200 min, and after the extraction is completed, the three kinds of extraction liquids are evaporated and concentrated to 1 ml at the set temperature, and then the GC / MS instrument is used for determination.

[0029] The multifunctional partition temperature control continuous extraction instrument in the application combines the universality and high efficiency of the partition temperature control heating extraction and the high selectivity of the solid phase extraction, has a simple structure and is convenient to operate, can realize one machine with multiple functions, can continuously extract two different samples through the partition temperature control, can continuously extract the samples using different kinds of solvents, and can take samples, concentrate and distill the extraction liquid without transferring the sample, thereby reducing the loss of effective substances and improving the extraction efficiency and extraction precision of the extraction instrument.

Claims

1. A multifunctional zone-controlled temperature continuous extraction apparatus, comprising a flask, an extraction tube, and a reflux condenser, wherein the top of the flask is connected to the reflux condenser via the extraction tube; characterized in that: The extraction tube is provided with a first partition and a second partition from top to bottom, which divide the interior of the extraction tube into an upper extraction zone, a lower extraction zone, and a bottom clearance zone. The bottom clearance zone is connected to the top of the flask, and the top of the upper extraction zone is connected to the bottom of the reflux condenser. A bypass tube is provided on one side of the extraction tube. The top of the bypass tube is connected to the top of the upper extraction zone, the middle of the bypass tube is connected to the top of the lower extraction zone, and the bottom of the bypass tube is connected to the bottom clearance zone. An upper siphon tube is provided between the bottom of the upper extraction zone and the lower extraction zone, and a lower flow tube is provided between the bottom of the lower extraction zone and the interior of the flask. Heating devices are provided on the outer periphery of the upper and lower extraction zones, respectively.

2. The multifunctional zone-controlled temperature continuous extraction instrument as described in claim 1, characterized in that: The heating device includes an upper infrared heating sleeve and a lower infrared heating sleeve. Both the upper and lower infrared heating sleeves are fixedly sleeved on the outside of the extraction tube. The upper infrared heating sleeve is located outside the upper extraction area and heats the upper extraction area. The lower infrared heating sleeve is located outside the lower extraction area and heats the lower extraction area.

3. The multifunctional zone-controlled temperature continuous extraction instrument as described in claim 2, characterized in that: The upper siphon pipe is equipped with an upper siphon pipe reflux control valve to control the flow state of the upper siphon pipe; the lower flow pipe is equipped with a lower flow pipe reflux control valve to control the flow state of the lower flow pipe.

4. The multifunctional zone-controlled temperature continuous extraction instrument as described in claim 3, characterized in that: The lower extraction zone is provided with a lower extraction zone inlet on one side, which is a closable inlet.

5. The multifunctional zone-controlled temperature continuous extraction instrument as described in claim 4, characterized in that: The flask is equipped with an electric heating jacket on the outside, which heats the inside of the flask. The bottom of the flask is equipped with a bottom outlet and a liquid outlet tube connected to the bottom outlet. The bottom outlet is equipped with a liquid outlet control valve.

6. The multifunctional zone-controlled temperature continuous extraction instrument as described in claim 5, characterized in that: The flask has a liquid inlet on one side of its top and is connected to a liquid inlet assembly. The liquid inlet assembly includes several liquid storage bottles, each with a liquid inlet at its top and a liquid outlet at its bottom. Each liquid outlet is equipped with a liquid control valve. Each liquid outlet is connected to one end of a guide tube, and the other end of the guide tube is connected to the liquid inlet at the top of the flask.

7. The multifunctional zone-controlled temperature continuous extraction instrument as described in claim 6, characterized in that: The various liquid storage bottles are all fixedly connected to the liquid storage bottle support.

8. The multifunctional zone-controlled temperature continuous extraction instrument as described in claim 7, characterized in that: The multifunctional zone-controlled temperature continuous extraction instrument also includes an extraction instrument controller. The extraction instrument controller is connected to the upper infrared heating jacket, the lower infrared heating jacket, and the electric heating jacket respectively, and controls their heating temperatures. The extraction instrument controller is also connected to the upper siphon tube reflux control valve, the lower flow pipe reflux control valve, the liquid outlet control valve, and several liquid storage bottle control valves respectively, and controls their opening and closing states.

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