CN214680162U - Extraction device - Google Patents

Extraction device Download PDF

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Publication number
CN214680162U
CN214680162U CN202120717898.XU CN202120717898U CN214680162U CN 214680162 U CN214680162 U CN 214680162U CN 202120717898 U CN202120717898 U CN 202120717898U CN 214680162 U CN214680162 U CN 214680162U
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extraction
bottle
liquid
flask
recovery liquid
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纪爱亮
张洁
王光辉
董栋
张宁
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Beijing Red Avenue Innova Co ltd
Red Avenue New Materials Group Co Ltd
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Beijing Red Avenue Innova Co ltd
Red Avenue New Materials Group Co Ltd
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Abstract

The application relates to the technical field of extraction equipment, in particular to an extraction device, which comprises a first extraction bottle, a dryer, a second extraction bottle and a third recovery liquid bottle which are sequentially connected in series from high to low, wherein the first recovery liquid bottle is arranged below the first extraction bottle, the second recovery liquid bottle is arranged below the second extraction bottle, the first extraction bottle is respectively connected with the first recovery liquid bottle and the dryer through a first tee, and the second extraction bottle is respectively communicated with the second recovery liquid bottle and the third recovery liquid bottle through a second tee; the extraction device also comprises a first circulating pump used for conveying the fluid in the first recovery liquid bottle to the first extraction bottle and a second circulating pump used for conveying the fluid in the second recovery liquid bottle to the second extraction bottle. The utility model provides a practice thrift cost, extraction efficient, extract effectual to reduce staff's intensity of labour, guarantee staff operational environment's extraction device.

Description

Extraction device
Technical Field
The application relates to the technical field of extraction equipment generally, and particularly relates to an extraction device.
Background
The extraction is widely applied to the industries of chemistry, pharmacy, metallurgy, food and the like. In the past, in a simple extraction process, people often shake, stand and separate by adding two or more different solvents into a separating funnel.
In the fields of rubber products, chemical pharmacy and mineral dressing medicaments, analysis, purification and extraction of specific components of rubber materials and medicaments are frequently required, for example, in the extraction analysis experiments of various types of products such as natural rubber, styrene-butadiene rubber, chloroprene rubber, xanthate medicaments, ammonium sulfate medicaments and the like, because the components are complex, the requirement on extraction is high, multiple extractions are required, and a large amount of volatile and high-toxicity reagents such as diethyl ether, trichloromethane, toluene and the like are used. When adopting conventional extraction mode to extract, need the experimenter to carry out continuous oscillation, a large amount of repetitive work such as minute liquid, conventional separating funnel need regularly gassing in rocking simultaneously to divide liquid in open environment, so can make the experimenter be in the environment of high toxicity for a long time, cause great injury to staff's physical and mental health.
SUMMERY OF THE UTILITY MODEL
In order to solve among the prior art at extraction in-process working strength big, during volatile high toxic reagent was discharged to the air, influences staff's physical and mental health's technical problem, this application provides an extraction device.
In order to realize the purpose of the utility model, the following technical scheme is adopted in the application:
according to one aspect of the application, an extraction device is provided, which comprises a first extraction bottle, a dryer, a second extraction bottle and a third recovery liquid bottle which are sequentially connected in series from high to low;
the extraction device also comprises a first recovery liquid bottle arranged below the first extraction bottle and a second recovery liquid bottle arranged below the second extraction bottle, the first extraction bottle is respectively connected with the first recovery liquid bottle and the dryer through a first tee joint, and the second extraction bottle is respectively communicated with the second recovery liquid bottle and the third recovery liquid bottle through a second tee joint;
the extraction device also comprises a first circulating pump used for conveying the fluid in the first recovery liquid bottle to the first extraction bottle and a second circulating pump used for conveying the fluid in the second recovery liquid bottle to the second extraction bottle.
According to an embodiment of the present application, a vibration stirring device is disposed on each of the first extraction flask and the second extraction flask, and the vibration stirring device comprises a magnetic stirrer and an ultrasonic oscillator.
According to an embodiment of the present application, the first extraction flask is provided with a first highest liquid level line, and the second extraction flask is provided with a second highest liquid level line.
According to an embodiment of the present application, wherein the liquid outlet of the first circulating pump is higher than the first highest liquid level line, and the liquid outlet of the second circulating pump is higher than the second highest liquid level line.
According to an embodiment of the present application, a filter screen and a drying agent are disposed in the dryer, and the drying agent is disposed on the filter screen.
According to an embodiment of the present application, wherein the drying agent is anhydrous sodium sulfate or activated carbon.
According to an embodiment of the present application, wherein the first extraction flask and the second extraction flask each comprise an inner chamber and an outer chamber, the outer chamber of the first extraction flask and/or the outer chamber of the second extraction flask is provided with a circulating liquid device.
According to an embodiment of the application, the lumen is tapered in cross-section in its depth direction.
According to an embodiment of the present application, wherein the circulating liquid device comprises a circulating liquid inlet and a circulating liquid outlet provided on the outer chamber, the height of the circulating liquid outlet on the outer chamber is higher than the height of the circulating liquid inlet on the outer chamber.
According to an embodiment of the present application, wherein the first extraction flask and/or the second extraction flask is provided with a distillation apparatus.
According to the technical scheme, the extraction device has the advantages and positive effects that: adding an extraction liquid into a first extraction bottle, vibrating and stirring the first extraction bottle by a vibrating and stirring device, after standing, introducing a water phase or an organic phase in the first extraction bottle into a first recovery liquid bottle, then adding saturated sodium chloride into the first extraction bottle, vibrating and stirring the first extraction bottle by the vibrating and stirring device, introducing the water phase or the organic phase in the first extraction bottle into the first recovery liquid bottle, introducing the organic phase or the water phase in the first extraction bottle into a drier, drying, introducing into a second extraction bottle, introducing a fluid in the first recovery liquid bottle into the first extraction bottle by a first circulating pump, and repeating the operations. And vibrating and stirring the second extraction bottle by using a vibrating and stirring device, adding a solvent into the second extraction bottle for vibrating and stirring, introducing the water phase or the organic phase in the second extraction bottle into a second recovery liquid bottle, introducing the organic phase or the water phase in the second extraction bottle into a third recovery liquid bottle, introducing the fluid in the second recovery liquid bottle into the second extraction bottle by using a second circulating pump, repeating the operation, and taking the water phase or the organic phase in the third recovery liquid bottle for detection. Through this kind of mode, improve extraction efficiency and extraction effect, reduce staff's intensity of labour, guarantee staff operational environment.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic diagram (a) showing the overall structure of an extraction apparatus according to an exemplary embodiment.
Fig. 2 is a schematic diagram (ii) showing the overall structure of an extraction apparatus according to an exemplary embodiment.
Wherein the reference numerals are as follows:
1. a first extraction flask; 2. a first recovery liquid bottle; 3. a dryer; 4. a second extraction flask; 5. a third recovery liquid bottle; 6. a second recovery liquid bottle; 7. a first circulation pump; 8. a vibrating and stirring device; 9. a sample inlet; 10. a circulating liquid inlet; 11. a circulating liquid outlet; 12. a distillation apparatus; 13. a second circulation pump; 14. a first tee joint; 15. a second tee joint; 16. a first branch; 17. a second branch circuit; 18. and a third branch.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It is noted that in the description and claims of the present application and in the above-mentioned drawings, relational terms such as "first" and "second", and the like, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those illustrated or otherwise described herein.
Also, the terms "comprises," "comprising," and "having," as well as any variations thereof or any other variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. For example, a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements explicitly listed, but may include other steps or elements not explicitly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Spatially relative terms, such as "above … …," "above … …," "above … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial relationship to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is turned over, devices described as "above" or "on" other devices or configurations would then be oriented "below" or "under" the other devices or configurations. Thus, the exemplary term "above … …" can include both an orientation of "above … …" and "below … …". The device may be otherwise variously oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
The inventors of the present application have found that, in the case of extraction experiments, when the experiments were carried out in accordance with the standard of GB/T13646-1992, the following steps were generally carried out. (1) Accurately weighing a certain amount of dried sample, placing the dried sample in a microwave digestion tank, adding a certain amount of concentrated nitric acid for microwave digestion, and naturally cooling the solution to room temperature (25 ℃) after the digestion is finished to obtain a reaction solution; (2) transferring the reaction solution into a beaker, adjusting the pH value of the reaction solution to be more than 1 by using 5mol/L aqueous solution of sodium hydroxide, then dropwise adding nitric acid to adjust the pH value of the reaction solution to be 1, and naturally cooling to room temperature; (3) transferring the solution obtained in the step 2 to a separating funnel 1, adding 40mL-70mL of ether for extraction, pouring the water layer into the original beaker, and extracting the ether layer with 25mL of saturated sodium chloride solution; the extracted water layer was poured into the original beaker, and the ether layer was poured into the beaker containing 5g to 10g of anhydrous sodium sulfate, dried and transferred to a separatory funnel 2. Repeating the above operations for 3 times, and drying the diethyl ether extractive solution with anhydrous sodium sulfate; (4) adding 50mL-80mL of 0.1mol/L sodium hydroxide solution into a separating funnel 2 for extraction, and pouring the sodium hydroxide solution layer obtained after extraction into a 250mL volumetric flask P; extracting with 0.1mol/L sodium hydroxide solution for three times; (5) combining the sodium hydroxide extract obtained after the four-time extraction in the step 4 in a 250mL volumetric flask P, using 0.1mol/L sodium hydroxide solution to fix the volume to a scale, and shaking up; if necessary, the solution is diluted with 0.1mol/L sodium hydroxide solution so that the absorbance of the test solution at the test wavelength is 0.2 to 0.8. Therefore, a large amount of volatile and highly toxic reagents such as diethyl ether, chloroform, toluene and the like can be used in the experimental process, the conventional separating funnel needs to be deflated regularly during shaking and is used for separating liquid in an open environment, so that experimenters can be in the highly toxic environment for a long time, and the physical and mental health of workers is greatly injured.
Based on the above thought, the embodiment of the present disclosure provides an extraction apparatus, the structure of which is shown in fig. 1, and the extraction apparatus includes a first extraction flask 1, a dryer 3, a second extraction flask 4, and a third recovery flask 5, which are sequentially connected in series from high to low. The extraction device further comprises a first recovery liquid bottle 2 arranged below the first extraction bottle 1 and a second recovery liquid bottle 6 arranged below the second extraction bottle 4, the first extraction bottle 1 is respectively connected with the first recovery liquid bottle 2 and the dryer 3 through a first tee 14, and the second extraction bottle 4 is respectively communicated with the second recovery liquid bottle 6 and the third recovery liquid bottle 5 through a second tee; the extraction device also comprises a first circulating pump 7 for conveying the fluid in the first recovery liquid bottle 2 to the first extraction bottle 1 and a second circulating pump 13 for conveying the fluid in the second recovery liquid bottle 6 to the second extraction bottle 4.
Further, a first extraction liquid is arranged in the first extraction bottle 1, and a second extraction liquid is arranged in the second extraction bottle 4; the first extraction flask 1 and the second extraction flask 4 are both provided with sample inlets 9.
Specifically, the first tee 14 has a liquid inlet and two liquid outlets, the liquid inlet of the first tee 14 is communicated with the first extraction bottle 1, and the two liquid outlets of the first tee 14 are respectively communicated with the dryer 3 and the first recovery liquid bottle 2. The second tee 15 also has a liquid inlet and two liquid outlets, the liquid inlet of the second tee 15 is communicated with the second extraction bottle 4, and the two liquid outlets of the second tee 15 are respectively communicated with the second liquid recovery bottle 6 and the third liquid recovery bottle 5.
Specifically, a first branch 16 is communicated between the first recovery liquid bottle 2 and the first circulating pump 7, a second branch 17 is communicated between the dryer 3 and the second extraction bottle 4, and a third branch 18 is communicated between the second recovery liquid bottle 6 and the second circulating pump 13.
In the experiment, a worker adds a first extraction liquid into a first extraction bottle 1 through a sample inlet 9, a vibration stirring device 8 vibrates and stirs the first extraction bottle 1 and then stands still, after standing, a water phase and an organic phase are respectively led into a first recovery liquid bottle 2 and a dryer 3 through a first tee 14, a dried organic phase or a dried water phase is led into a second extraction bottle 4 through a second branch 17, a first circulating pump 7 conveys the water phase or the organic phase in the first recovery liquid bottle 2 into the first extraction bottle 1 through a first branch 16, and the operation is repeated for 1-3 times. Then, a worker adds a second extraction liquid into the second extraction bottle 4 through the sample inlet 9, the vibration stirring device 8 performs vibration stirring on the second extraction bottle 4 and then stands still, a water phase and an organic phase in the second extraction bottle 4 are respectively led into the second recovery liquid bottle 6 and the third recovery liquid bottle 5 through the second tee 15, the second circulating pump 13 conveys the water phase or the organic phase in the second recovery liquid bottle 6 into the second extraction bottle 4 through the third branch 18, and the operation is repeated for 1-3 times; the fluid in the second recovery liquid bottle 5 is taken for detection.
Through the above-mentioned mode of setting up, extract through inclosed device, in extracting volatile, toxic reagent such as in-process ether, toluene can not volatilize the air, protection staff's operational environment vibrates the stirring through vibration agitating unit 8, need not vibrate by the manual work, alleviates staff's working strength, reduces operation error, improves extraction efficiency and extraction effect.
Further, a first switch is arranged at the liquid outlet of the first extraction bottle 1, a second switch is arranged at the liquid inlet of the first recovery liquid bottle 2, a third switch is arranged at the liquid outlet of the first recovery liquid bottle 2, a fourth switch is arranged at the liquid inlet of the dryer 3, a fifth switch is arranged at the liquid outlet of the dryer 3, a sixth switch is arranged at the liquid outlet of the second extraction bottle 4, a seventh switch is arranged at the liquid inlet of the second recovery liquid bottle 6, and an eighth switch is arranged at the liquid inlet of the third recovery liquid bottle 5. Through the setting of above-mentioned switch, guarantee the stability of device working process, the extraction effect is guaranteed to the flow direction of the control liquid of being convenient for simultaneously.
Optionally, the first switch, the second switch, the third switch, the fourth switch, the fifth switch, the sixth switch, the seventh switch, and the eighth switch are all valves. The opening and closing of each branch are adjusted through the valve, circulation and sealing of each branch are convenient to control, liquid backflow and other conditions in the experiment process can be effectively prevented, and the experiment effect is guaranteed.
Further, the volume of the first extraction flask 1 and the volume of the second extraction flask 4 are the same or different. In the course of the experiment, it is generally the case that the liquid in the second extraction flask 4 is less than the liquid in the first extraction flask 1. Therefore, in order to save cost and reduce the occupied space of the experimental device, the volume of the first extraction bottle 1 is optionally larger than that of the second extraction bottle 4.
Further, the first extraction liquid comprises a reagent and a solvent, and specifically, the reagent can be selected from different reagents according to different experimental operations of an experimenter. For example, when it is desired to extract styrene from rubber articles, the agent is selected to be a rubber digest. Similarly, the rubber particles can be directly put into the first extraction flask 1 through the injection port 9 of the first extraction flask 1, and then strong acid is added into the first extraction flask 1 and heated to dissolve the rubber particle solid into liquid.
Further, the solvent is diethyl ether, chloroform, toluene, ethyl acetate, acetone, cyclohexane or tetrahydrofuran, etc. Specifically, the solvent may be any one of the above solvents, or a mixture of a plurality of solvents, and the specific choice of the solvent may be selected according to the use of a skilled person.
Further, the mass ratio of the solution to the solvent is 1:1-1: 5. By adding a large amount of solvent, the action effect of the solvent on the solution is improved, and the vibration and stirring effects are ensured.
Optionally, the mass ratio of the solution to the solvent is 1:2-1:4, so that the addition of the solvent is reduced while the extraction effect is ensured, and the cost is saved.
Further, the first extraction flask 1 is provided with a first highest liquid level line, and the second extraction flask 4 is provided with a second highest liquid level line. Through the setting of the highest liquid level line of first highest liquid level line and the highest liquid level line of second, can make things convenient for the staff to look over the maximum of the extraction liquid in first extraction flask 1 and the second extraction flask 4, make things convenient for the operation of vibration agitating unit 8, avoid adding too much first extraction liquid or second extraction liquid and influence the extraction effect.
Optionally, the first highest liquid level line is two thirds of the volume of the first extraction flask 1, and the second highest liquid level line is two thirds of the volume of the second extraction flask 4. It should be noted that, in the actual experiment process, the first highest liquid level line and the second highest liquid level line may be selected at different positions according to different experiment requirements and the like.
Further, the liquid outlet of the first circulation pump 7 is higher than the first highest liquid level line, and the liquid outlet of the second circulation pump 13 is higher than the second highest liquid level line. Make the liquid of first circulating pump 7 can stably flow into in first extraction flask 1 for the liquid of second circulating pump 13 can stably flow into effectively avoid the refluence phenomenon in second extraction flask 4.
Further, in order to guarantee the safety of experimental effect, experimentation and the reliability of device, first circulating pump 7 and second circulating pump 13 are acid and alkali-resistance, resistant oily device. The first extraction bottle 1, the second extraction bottle 4, the first recovery liquid bottle 2, the second recovery liquid bottle 6, the third recovery liquid bottle 5 and the dryer 3 are all acid-base and high-temperature resistant glass.
Optionally, first circulating pump 7 and second circulating pump 13 are the peristaltic pump, and the peristaltic pump can effectually prevent liquid refluence, effectively prevents through the setting of peristaltic pump that partial solvent such as chloroform from melting the hose, avoids the phenomenon of weeping to appear in the working process.
Further, a filter screen and a drying agent are arranged in the dryer 3, and the drying agent is arranged on the filter screen. The setting through the filter screen plays the effect of support to the drier for liquid can flow from the liquid outlet of desicator 3 after passing through the drier, avoids the condition that the drier stops up 3 liquid outlets of desicator.
Optionally, the filter screen is not smaller than 50 meshes.
Further, the dryer 3 is a closed container, and volatile toxic reagents can be effectively prevented from volatilizing into the air through the arrangement of the closed container. The drier 3 is provided with a cover body, and the drier is convenient for workers to add or take out or replace the drier through opening and closing of the cover body.
Optionally, the desiccant is anhydrous sodium sulfate or activated carbon. The utility model discloses do not inject the kind of drier, at specific experimentation, thereby the staff can select different driers according to reagent or different experimental requirement of difference.
Further, the first extraction flask 1 and the second extraction flask 4 both comprise an inner cavity and an outer cavity, the first extraction liquid is disposed in the inner cavity of the first extraction flask 1, and the second extraction liquid is disposed in the inner cavity of the second extraction flask 4. The vibration stirring devices 8 are arranged in the outer cavity, the first recovery liquid bottle 2 is connected with the inner cavity of the first extraction bottle 1 through the liquid inlet of the first tee joint 14, and the second recovery liquid bottle 6 is connected with the inner cavity of the second extraction bottle 4 through the liquid inlet of the second tee joint 15. The liquid outlet of the first circulating pump 7 is communicated with the inner cavity of the first extraction bottle 1, and the liquid outlet of the second circulating pump 13 is communicated with the inner cavity of the second extraction bottle 4; the dryer 3 is communicated with the inner cavity of the second extraction bottle 4 through a second branch 17.
Specifically, vibration agitating unit 8 includes magnetic stirrers and ultrasonic oscillator, carries out magnetic stirring through magnetic stirrers to first extraction liquid or the second extraction liquid in the inner chamber, carries out ultrasonic oscillation through ultrasonic oscillator to first extraction liquid or the second extraction liquid in the inner chamber for liquid stirring oscillation in the inner chamber is more even, and the effect is better, efficiency is higher.
Optionally, magnetic stirrers and ultrasonic oscillator adopt and parallel independent two switches to connect the setting for magnetic stirrers and ultrasonic oscillator can carry out work alone, thereby satisfy different experimental demands. Similarly, the magnetic stirrer and the ultrasonic vibrator can work simultaneously, and the working efficiency is ensured.
Optionally, the double switch can be a timing switch, and the staff can set the time of vibration stirring according to different experimental operations, so that the vibration stirring device 8 can automatically stop working after reaching the time without the real-time monitoring of the staff.
Further, the inner cavity is tapered in cross section in the depth direction thereof. The opening at the top of the inner cavity is larger through the conical arrangement, so that the arrangement of the sample inlet 9 is convenient, and the extraction liquid is also convenient to be put into the inner cavity. The opening at the bottom of the inner cavity is small due to the conical arrangement, so that the inner cavity can discharge fluid outwards relatively slowly, experimenters can observe the discharge condition of the fluid in the inner cavity, organic phases and water phases in the inner cavity can be effectively discharged into different bottles respectively, and the operation is convenient.
Optionally, the shape of the inner cavity may be selected from other shapes in the prior art to meet the experimental requirements. Specifically, the cross section of the inner cavity in the depth direction thereof may also be an inverted triangle or the like.
Further, a liquid circulating device is arranged on the first extraction bottle 1 and/or the second extraction bottle 4. The circulating liquid in the circulating liquid device can be high-temperature liquid or low-temperature liquid, and specifically, the high-temperature liquid and the low-temperature liquid are compared with the indoor room temperature.
Further, the outer cavity comprises a first cavity and a second cavity, the vibration stirring device 8 is arranged in the first cavity, and the liquid circulating device is arranged in the second cavity. In order to ensure that the circulating liquid in the circulating liquid device can have an effect on the fluid in the inner cavity, optionally, the inner cavity is made of a heat-conducting material.
Specifically, the second cavity is provided with a circulating liquid inlet 10 and a circulating liquid outlet 11. The circulating liquid inlet 10 is arranged at the bottom of the second cavity, and the circulating liquid outlet 11 is arranged at the top of the second cavity. Through setting up circulation liquid outlet 11 in the top of second cavity, guarantee the effect of circulation liquid to liquid in the inner chamber. The circulating liquid inlet 10 on the first extraction flask 1 should be lower than the first highest liquid level line, and the circulating liquid inlet 10 on the second extraction flask 4 should be lower than the second highest liquid level line, so as to further ensure the effect of the circulating liquid.
Optionally, the circulating liquid inlet 10 and the circulating liquid outlet 11 may be respectively provided with a switch, and the opening or closing of the circulating liquid inlet 10 or the circulating liquid outlet 11 is realized through the switch, so as to meet different requirements of different experiments.
Alternatively, the circulating liquid may be water or oil, or the like. Specifically, according to different experimental requirements or requirements of experimenters, the circulating liquid can adopt water or oil with different temperatures. For example, when the liquid in the inner cavity needs to be heated or insulated, the circulating liquid can be water at 40 ℃ or water at 60 ℃; when experimenters need to heat or keep warm to higher temperature with the liquid in the inner chamber, the circulation liquid can adopt 70 degrees centigrade oil or 150 degrees centigrade oil etc to realize heating the inner chamber. Similarly, ice water or the like may be used as the circulating liquid.
Further, when the first extraction flask 1 and the second extraction flask 4 are both provided with a circulating liquid device, the circulating liquid outlet 11 on the first extraction flask 1 can be communicated with the circulating liquid inlet 10 on the second extraction flask 4, so that the operation is convenient. Similarly, the circulating liquid inlet 10 of the first extraction flask 1 may be connected to the circulating liquid outlet 11 of the second extraction flask 4. The utility model discloses do not do the restriction to concrete connection mode.
Referring to fig. 1 and 2, the first extraction flask 1 and/or the second extraction flask 4 is provided with a distillation apparatus 12. Specifically, the experimenter can set according to different requirements. When the liquid in the first extraction flask 1 needs to be purified, a distillation device 12 is arranged on the first extraction flask 1; when the liquid in the second extraction bottle 4 needs to be purified, a distillation device 12 is arranged on the second extraction bottle 4; when the liquids in the first extraction flask 1 and the second extraction flask 4 need to be purified, the first extraction flask 1 and the second extraction flask 4 are both provided with a distillation device 12.
Specifically, the distillation apparatus 12 may be any one of the prior arts, for example, the distillation apparatus 12 may be an RE-201D evaporator or other conventional distillation means.
It should be noted that the number of the extraction bottles in the extraction apparatus provided by the present invention includes, but is not limited to, two, i.e., the first extraction bottle 1 and the second extraction bottle 4 in the above description. In the process of specific experimental operation, a third extraction bottle, a fourth extraction bottle and the like can be arranged. When a third extraction bottle needs to be arranged, namely the second recovery liquid bottle 6 needs to be communicated with the dryer 3, and the liquid outlet of the dryer 3 is communicated with the third extraction bottle. Other means for connecting the third extraction flask to the second extraction flask 4 may be provided, so that the connection of different numbers of extraction flasks can be achieved without inventive work by those skilled in the art, and fall within the scope of the present application.
The present invention will be further described with reference to the following specific examples. However, the present invention is not limited to these examples.
Example 1
The experimental process for extracting styrene from rubber products comprises the steps of adding 30ml of rubber digestion solution into a first extraction bottle 1, adding 50ml of ether solvent for vibration stirring at a stirring speed of 300r/min for 20min, guiding an aqueous phase into a first recovery liquid bottle 2 after standing, adding 50ml of saturated sodium chloride into the first extraction bottle 1 for vibration stirring at a stirring speed of 300r/min for 10min, guiding the aqueous phase into the first recovery liquid bottle 2, guiding an organic phase into a dryer 3, drying anhydrous sodium sulfite serving as a drying agent in the dryer 3, and guiding the dried aqueous phase into a second extraction bottle 4. The aqueous phase in the first recovery liquid bottle 2 is led into a first extraction bottle 1 through a first circulating pump 7, the extraction is repeated for 3 times, the organic phase is led into a second extraction bottle 4 for 3 times respectively, 50ml of a 0.1mol/L sodium hydroxide solution is added into the second extraction bottle 4 for vibration stirring, the stirring speed is 300r/min, the stirring time is 10min, the aqueous phase is led into a second recovery liquid bottle 5, the organic phase is led into a third recovery liquid bottle 6, the organic phase in the second recovery liquid bottle 6 is led into the second extraction bottle 4 through a second circulating pump 13, the extraction is repeated for 3 times, and the aqueous phase in the third recovery liquid bottle 5 is taken for styrene detection.
The extraction rate of the extraction apparatus in this example after the experiment was 95.6%, and the extraction rate of the above experiment was 81.5% according to GB/T13646-1992.
Example 2
In the experimental process of extracting the by-product sodium thioglycolate from the mining chemical reagent ethionamide, 30ml of ethionamide is added into a first extraction bottle 1, 50ml of pure water is added for vibration stirring at the same time, the stirring speed is 300r/min, the stirring time is 10min, after standing, an organic phase is led into a first recovery bottle 2, an aqueous phase is led into a dryer 3, a drying agent in the dryer 3 is activated carbon, and the aqueous phase in the dryer 3 is degreased through the activated carbon and then led into a second extraction bottle 4. And (3) introducing the organic phase in the first recovery liquid bottle 2 into the first extraction bottle 1 through a first circulating pump 7, repeating the extraction for three times, respectively introducing the three aqueous phases into the second extraction bottle 4, adding 50ml of ethyl acetate solution into the second extraction bottle 4, carrying out vibration stirring at the stirring speed of 300r/min for 10min, introducing the aqueous phase into the second recovery liquid bottle 6, introducing the organic phase into the third recovery liquid bottle 5, and taking the aqueous phase in the second recovery liquid bottle 6 for sodium thioglycolate detection.
The extraction ratio of the extraction apparatus in this example after the experiment was 98.5%, and the extraction ratio when the above experiment was carried out in accordance with the standard of GB/T13646-1992 was 72.8%.
Example 3
In the experimental process of extraction of styrene in oil-containing rubber material, 10ml of oil-extended styrene-butadiene rubber digestion solution is taken and added into a first extraction bottle 1, 30ml of ether solvent is added at the same time for vibration stirring, the stirring speed is 100r/min, the stirring time is 10min, and after standing, the water phase is led into a first recovery liquid bottle 2. And then 30ml of saturated sodium chloride is added into the first extraction bottle 1, vibration stirring is carried out, the stirring speed is 100r/min, the stirring time is 10min, the water phase is introduced into the first recovery bottle 2, the organic phase is introduced into the dryer 3, the drying agent in the dryer 3 is anhydrous sodium sulfite, and the dried product is introduced into the second extraction bottle 4. The water phase in the first recovery liquid bottle 2 is led into the first extraction bottle 1 through a first circulating pump 7, the extraction is repeated for 3 times, the organic phase in three times is led into the second extraction bottle 4 respectively, 50ml of 0.1mol/L sodium hydroxide solution is added into the second extraction bottle 4 for vibration stirring, the stirring speed is 100r/min, the stirring time is 10min, the water phase is led into a third recovery liquid bottle 5, the organic phase is led into a second recovery liquid bottle 6, the organic phase in the second recovery liquid bottle 6 is led into the second extraction bottle 4 through a second circulating pump 13, the extraction is repeated for 3 times, and the water phase in the third recovery liquid bottle 6 is taken for styrene detection.
The extraction rate of the extraction apparatus in this example after the experiment was 97.2%, and the extraction rate of the above experiment was 84.2% according to GB/T13646-1992.
Through the experiment in each embodiment above-mentioned and the conventional extraction mode among the prior art contrast, the utility model provides an extraction device extracts in-process solvent volume consumption less, and the experimental time is short, vibrates the stirring through vibration agitating unit 8 and makes extraction effectual, efficient, alleviates experimenter's work load. And simultaneously, the utility model provides an extraction device need not regularly deflate at the extraction in-process to need not divide the liquid in open environment, ensure experimenter's operational environment, protection experimenter's health.
It should be noted that the utility model provides an extraction device provides the device that can carry out the extraction experiment in airtight container, because the airtight container so can appear in the experimentation because the problem of pressure leads to the unable condition that flows of liquid. In a specific experimental operation process, because the first extraction flask 1 and the second extraction flask 4 need to be vibrated and stirred or a chemical reaction occurs in the flasks, the pressure in the first extraction flask 1 and the second extraction flask 4 is relatively high during the experimental operation process, and the fluid in the first extraction flask 1 and the fluid in the second extraction flask 4 flow into other flasks under the action of the pressure and the gravity. If the fluid in the first extraction flask 1 or the second extraction flask 4 does not flow due to the pressure problem, the peristaltic pump connected with the first extraction flask 1 or the second extraction flask 4 can be opened to perform air pressure balance. Alternatively, the air above the first extraction bottle 1, the second extraction bottle 4, the first recovery liquid bottle 2, the third recovery liquid bottle 5 and the second recovery liquid bottle 6 can be communicated with each other through pipelines, so that the internal air pressures are balanced.
The above description is merely exemplary of the present application and is presented to enable those skilled in the art to understand and practice the present application. Various modifications and changes to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. An extraction device is characterized by comprising a first extraction bottle (1), a dryer (3), a second extraction bottle (4) and a third recovery liquid bottle (5) which are sequentially connected in series from high to low;
the extraction device further comprises a first recovery liquid bottle (2) arranged below the first extraction bottle (1) and a second recovery liquid bottle (6) arranged below the second extraction bottle (4), the first extraction bottle (1) is respectively connected with the first recovery liquid bottle (2) and the dryer (3) through a first tee joint (14), and the second extraction bottle (4) is respectively communicated with the second recovery liquid bottle (6) and the third recovery liquid bottle (5) through a second tee joint (15);
the extraction device also comprises a first circulating pump (7) used for conveying the fluid in the first recovery liquid bottle (2) to the first extraction bottle (1) and a second circulating pump (13) used for conveying the fluid in the second recovery liquid bottle (6) to the second extraction bottle (4).
2. The extraction apparatus according to claim 1, wherein the first extraction flask (1) and the second extraction flask (4) are provided with a vibration stirring device (8), and the vibration stirring device (8) comprises a magnetic stirrer and an ultrasonic oscillator.
3. The extraction apparatus according to claim 1, wherein the first extraction flask (1) is provided with a first highest liquid level line, and the second extraction flask (4) is provided with a second highest liquid level line.
4. Extraction plant according to claim 3, characterized in that the outlet of the first circulation pump (7) is higher than the first highest liquid level line and the outlet of the second circulation pump (13) is higher than the second highest liquid level line.
5. Extraction device according to claim 1, characterized in that a sieve and a drying agent are arranged in the dryer (3), which drying agent is arranged on the sieve.
6. The extraction apparatus of claim 5, wherein the drying agent is anhydrous sodium sulfate or activated carbon.
7. The extraction apparatus according to claim 1, wherein the first extraction flask (1) and the second extraction flask (4) each comprise an inner chamber and an outer chamber, the outer chamber of the first extraction flask (1) and/or the outer chamber of the second extraction flask (4) being provided with means for circulating liquid.
8. The extraction apparatus as claimed in claim 7, wherein the inner chamber is tapered in cross-section in the direction of its depth.
9. Extraction device according to claim 7, characterized in that the circulating liquid means comprise a circulating liquid inlet (10) and a circulating liquid outlet (11) arranged in the outer chamber, the level of the circulating liquid outlet (11) in the outer chamber being higher than the level of the circulating liquid inlet (10) in the outer chamber.
10. The extraction apparatus according to claim 1, characterized in that the first extraction flask (1) and/or the second extraction flask (4) is provided with a distillation apparatus (12).
CN202120717898.XU 2021-04-08 2021-04-08 Extraction device Active CN214680162U (en)

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