A solvent circulation extraction device

Abstract

The invention discloses a solvent circulation extraction device, comprising a layered tube, a first transfer valve, a second transfer valve, a third transfer valve, a collection bottle, a sample bottle, a cleaning bottle, a solvent extraction pump, a spiral tube, a waste liquid barrel and a waste discharge pump. When in use, the extraction solvent and the sample to be extracted are extracted through continuous circulation, which reduces the amount of solvent used, has low cost and is easy to use. The layered tube is used to solve the problem of dehydration of the extraction solvent, and the collection bottle can be directly removed. The extraction solvent in the removed collection bottle can be directly put on liquid chromatography, gas chromatography and other analytical instruments, which saves the time of extracting solvent concentration and reduces the error caused by the extraction solvent transfer process. It has great practical value for extracting small batches of samples.

Description

Technical Field

[0001] The invention relates to the field of extraction, in particular to a solvent circulation extraction device. Background Art

[0002] Extraction is a unit operation that uses the different solubility of components in the system in the solvent to separate the mixture. That is, it is a method of transferring the solute from one solvent to another solvent by using the difference in solubility or distribution coefficient of the substance in two immiscible (or slightly soluble) solvents. At present, the extraction devices for organic matter in water mainly include traditional liquid-liquid extraction and solid phase extraction. The traditional liquid-liquid extraction device has a wide range of applications and mature technology. In addition, the application of fully automatic liquid-liquid extraction devices in recent years has solved the problem of high labor intensity, but this method requires the use of a large amount of solvent, causing environmental pollution; the solid phase extraction device has a high degree of automation, but the steps are relatively complex, expensive, and the operating cost is very high, and a certain amount of solvent is required to activate the extraction column. When extracting small doses of samples, it mainly relies on pure manual operation. There is no special extraction device for extraction operation, and the requirements for operators are high. Summary of the invention

[0003] In order to solve the above problems, the object of the present invention is to provide a solvent circulation extraction device with low cost, convenient extraction, simple steps and less solvent usage.

[0004] The technical solution adopted by the present invention to solve the above problems is: a solvent circulation extraction device, comprising:

[0005] A layered tube, wherein a liquid inlet pipe extending into the layered tube is arranged at the top of the layered tube, a first liquid outlet pipe is arranged at the bottom of the layered tube, and a second liquid outlet pipe is arranged on the side wall of the layered tube;

[0006] a first switching valve, wherein the first switching valve is connected to the first liquid outlet pipe and the second liquid outlet pipe;

[0007] A collecting bottle, wherein the collecting bottle is provided with a first connecting pipe and a second connecting pipe extending into the collecting bottle, wherein the first connecting pipe is connected to the first switching valve;

[0008] a second transfer valve, the second transfer valve being in communication with the second connecting pipe;

[0009] A sample bottle, the sample bottle is connected to the second transfer valve;

[0010] a cleaning bottle, the cleaning bottle being in communication with the second transfer valve;

[0011] a solvent extraction pump, the solvent extraction pump being in communication with the second transfer valve;

[0012] a third transfer valve, the third transfer valve being connected to the solvent extraction pump;

[0013] A spiral tube, one end of which is connected to the third switching valve, and the other end of which is connected to the liquid inlet pipe;

[0014] A waste liquid barrel, the waste liquid barrel is connected to the third transfer valve;

[0015] A waste discharge pump, one end of which is connected to the waste liquid barrel, and the other end of which is connected to the first transfer valve.

[0016] As a further improvement of the above technical solution, the second switching valve includes:

[0017] A tee, the tee is connected to the second connecting pipe and the solvent extraction pump respectively;

[0018] A first four-way valve, wherein the first four-way valve is connected to the three-way valve, the sample bottle and the cleaning bottle respectively, and one port of the first four-way valve is an air port.

[0019] As a further improvement of the above technical solution, the first transfer valve and the third transfer valve are both four-way valves.

[0020] As a further improvement of the above technical solution, an ultrasonic groove is arranged on the outer periphery of the spiral tube, and an ultrasonic generator is arranged in the ultrasonic groove.

[0021] As a further improvement of the above technical solution, the inner diameter of the spiral tube is 0.5-5 mm and the length is 5-30 cm.

[0022] As a further improvement of the above technical solution, the capacity of the collecting bottle is 2-20 ml.

[0023] The beneficial effects of the present invention are as follows: when in use, the sample to be extracted is placed in the sample bottle, and a certain amount of extraction solvent and water are placed in the layered tube; if the specific gravity of the extraction solvent is greater than that of water, the first transfer valve is controlled to connect the first liquid outlet pipe with the first connecting pipe and the second liquid outlet pipe with the waste discharge pump; otherwise, if the specific gravity of the extraction solvent is less than that of water, the first transfer valve is controlled to connect the second liquid outlet pipe with the first connecting pipe and the first liquid outlet pipe with the waste discharge pump; the second transfer valve is controlled to connect the second connecting pipe and the sample bottle with the solvent extraction pump; the third transfer valve is controlled to connect the solvent extraction pump with the spiral tube; the solvent extraction pump will absorb the extraction solvent in the layered tube and the sample to be extracted in the sample bottle together and transfer them into the spiral tube; the spiral length of the spiral tube is increased. The extraction time of the extraction solvent and the sample to be extracted is increased, and the mixing degree of the extraction solvent and the sample to be extracted can be increased. After that, the extraction solvent and the waste liquid after extraction are simultaneously put into the stratification tube and allowed to stand for a period of time to stratify the extraction solvent and the waste liquid. At this time, the extraction solvent with a specific gravity greater than water is located at the bottom of the waste liquid, and the extraction solvent with a specific gravity less than water is located at the top of the waste liquid. Then, the waste liquid is discharged into the waste liquid barrel through the corresponding second liquid outlet pipe or the first liquid outlet pipe through the waste discharge pump. When the amount of the sample to be extracted is large, a second cycle can be performed at this time, and the extraction solvent used once is mixed and extracted with the remaining sample to be extracted for the second time, so as to make full use of the extraction solvent and avoid waste of the extraction solvent. The specific number of cycles is determined according to the amount of the sample to be extracted. When the extraction is completely completed, the extraction solvent is discharged into the collection bottle through the solvent extraction pump, and then the collection bottle is removed, and the extraction solvent in the collection bottle is tested to obtain the concentration of the component to be tested in the extraction solvent in the collection bottle. Then, the concentration of the component to be tested in the sample to be extracted can be obtained by combining the total amount of the extraction solvent and the capacity of the sample to be extracted. When cleaning, add cleaning liquid into the cleaning bottle, connect the cleaning bottle and the second connecting pipe with the solvent extraction pump through the second transfer valve, at this time, first control the third transfer valve to connect the spiral tube with the solvent extraction pump, and drive the cleaning liquid to circulate and flush continuously in the whole set of pipelines through the solvent extraction pump. After flushing for a period of time, control the third transfer valve to connect the waste liquid barrel with the solvent extraction pump, so that the cleaning liquid is directly discharged into the waste liquid barrel along the third transfer valve to complete the cleaning. In actual use, the depth of the liquid inlet pipe inserted into the layered tube, and the depth of the first connecting pipe and the second connecting pipe inserted into the collection bottle can be adjusted according to specific circumstances. Through the whole set of extraction devices, the amount of solvent used is reduced, the cost is low, and it is easy to use. The layered tube solves the problem of dehydration of the extraction solvent. The collection bottle can be directly removed, and the extraction solvent in the removed collection bottle can be directly put on liquid chromatography, gas chromatography and other analytical instruments, which saves the time of extracting solvent concentration and reduces the error caused by the extraction solvent transfer process. It has great practical value for extracting small batches of samples. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] The present invention will be further explained below in conjunction with the accompanying drawings and specific implementation methods.

[0025] Figure 1 It is a schematic structural diagram of a preferred embodiment of the present invention. DETAILED DESCRIPTION

[0026] This section will describe in detail the specific embodiments of the present invention. The preferred embodiments of the present invention are shown in the accompanying drawings. The purpose of the accompanying drawings is to supplement the description of the text part of the specification with graphics, so that people can intuitively and vividly understand each technical feature and the overall technical solution of the present invention, but it cannot be understood as a limitation on the scope of protection of the present invention.

[0027] In the description of the present invention, it should be understood that descriptions involving orientations, such as up, down, front, back, left, right, etc., and orientations or positional relationships indicated are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.

[0028] In the description of the present invention, "several" means one or more, "more" means more than two, "greater than", "less than", "exceed" etc. are understood as not including the number itself, and "above", "below", "within" etc. are understood as including the number itself. If there is a description of "first" or "second", it is only used for the purpose of distinguishing the technical features, and cannot be understood as indicating or implying the relative importance or implicitly indicating the number of the indicated technical features or implicitly indicating the order of the indicated technical features.

[0029] In the description of the present invention, unless otherwise clearly defined, terms such as setting, installing, connecting, etc. should be understood in a broad sense, and technicians in the relevant technical field can reasonably determine the specific meanings of the above terms in the present invention based on the specific content of the technical solution.

[0030] Reference Figure 1 , a solvent circulation extraction device, comprising:

[0031] The layered tube 5 has a liquid inlet pipe extending into the layered tube 5 at the top, a first liquid outlet pipe at the bottom, and a second liquid outlet pipe at the side wall of the layered tube 5;

[0032] a first switching valve 6, wherein the first switching valve 6 is connected to the first liquid outlet pipe and the second liquid outlet pipe;

[0033] A collecting bottle 8, wherein the collecting bottle 8 is provided with a first connecting pipe and a second connecting pipe extending into the collecting bottle 8, and the first connecting pipe is connected to the first switching valve 6;

[0034] a second transfer valve, the second transfer valve being in communication with the second connecting pipe;

[0035] A sample bottle 9, wherein the sample bottle 9 is connected to the second transfer valve;

[0036] a cleaning bottle 13, wherein the cleaning bottle 13 is connected to the second switching valve;

[0037] A solvent extraction pump 1, wherein the solvent extraction pump 1 is connected to the second transfer valve;

[0038] a third transfer valve 7, wherein the third transfer valve 7 is connected to the solvent extraction pump 1;

[0039] A spiral tube 4, one end of which is connected to the third switching valve 7, and the other end of which is connected to the liquid inlet pipe;

[0040] A waste liquid barrel 10, wherein the waste liquid barrel 10 is connected to the third transfer valve 7;

[0041] A waste discharge pump 2 , one end of which is connected to the waste liquid barrel 10 , and the other end of which is connected to the first transfer valve 6 .

[0042] When in use, the sample to be extracted is loaded into the sample bottle 9, and a certain amount of extraction solvent and water are loaded into the delamination tube 5. If the specific gravity of the extraction solvent is greater than that of water, the first transfer valve 6 is controlled to connect the first liquid outlet pipe with the first connecting pipe and connect the second liquid outlet pipe with the waste pump 2 at the same time. On the contrary, if the specific gravity of the extraction solvent is less than that of water, the first transfer valve 6 is controlled to connect the second liquid outlet pipe with the first connecting pipe and connect the first liquid outlet pipe with the waste pump 2 at the same time, the second transfer valve is controlled to connect the second connecting pipe and the sample bottle 9 with the solvent extraction pump 1, and the third transfer valve 7 is controlled to connect the solvent extraction pump 1 with the spiral tube 4. The solvent extraction pump 1 will absorb the extraction solvent in the delamination tube 5 and the sample to be extracted in the sample bottle 9 together and transfer them into the spiral tube 4. Through the spiral length of the spiral tube 4 The extraction time of the extraction solvent and the sample to be extracted is increased, and the mixing degree of the extraction solvent and the sample to be extracted can be increased. After that, the extracted extraction solvent and waste liquid enter the stratification tube 5 at the same time and stand for a period of time to allow the extraction solvent and the waste liquid to be stratified. At this time, the extraction solvent with a specific gravity greater than water is located at the bottom of the waste liquid, and the extraction solvent with a specific gravity less than water is located at the top of the waste liquid. Then, the waste liquid is discharged into the waste liquid barrel 10 through the waste discharge pump 2 through the corresponding second liquid outlet pipe or the first liquid outlet pipe. When the amount of the sample to be extracted is large, a second cycle can be performed at this time, and the extraction solvent used once and the remaining sample to be extracted are mixed and extracted for a second time, so as to make full use of the extraction solvent and avoid wasting the extraction solvent. The specific number of cycles is determined according to the amount of the sample to be extracted. When the extraction is completely completed, the extraction solvent is discharged into the collecting bottle 8 through the solvent extraction pump 1, and then the collecting bottle 8 is removed and the extraction solvent in the collecting bottle 8 is tested. The extraction solvent in the collecting bottle 8 only needs to collect part of the total amount of the extraction solvent, and does not need to collect all of the extraction solvent. The concentration of the component to be tested in the extraction solvent in the collecting bottle 8 is obtained, and then the concentration of the component to be tested in the sample to be extracted is obtained by combining the total amount of the extraction solvent and the volume of the sample to be extracted. During cleaning, cleaning liquid is added into the cleaning bottle 13, and the cleaning bottle 13 and the second connecting pipe are connected to the solvent extraction pump 1 through the second transfer valve. At this time, the third transfer valve 7 is first controlled to connect the spiral tube 4 with the solvent extraction pump 1, and the cleaning liquid is driven by the solvent extraction pump 1 to continuously circulate and flush in the entire pipeline. After flushing for a period of time, the third transfer valve 7 is controlled to connect the waste liquid barrel 10 with the solvent extraction pump 1, so that the cleaning liquid is directly discharged into the waste liquid barrel 10 along the third transfer valve 7 to complete the cleaning. In actual use, the depth of the liquid inlet pipe inserted into the stratification tube 5, and the depth of the first connecting pipe and the second connecting pipe inserted into the collecting bottle 8 can be adjusted according to specific circumstances.The whole set of extraction device can reduce the usage of solvent, and the cost is low and the device is easy to use. The delamination tube 5 can solve the problem of dewatering the extraction solvent. The collecting bottle 8 can be directly removed, and the extraction solvent in the removed collecting bottle 8 can be directly put on liquid chromatography, gas chromatography and other analytical instruments, thereby reducing the error caused by the extraction solvent transfer process, and reducing the time for concentration of the extraction solvent and nitrogen consumption, which has great practical value for extracting small batches of samples.

[0043] Of course, the specific steps during use can be adjusted according to the specific situation. For example, when the extraction solvent is loaded for the first time, there is only the extraction solvent in the layering tube 5. At this time, the first transfer valve 6 is controlled to connect the first connecting tube with the first liquid outlet pipe, so as to facilitate the first extraction solvent circulation. Thereafter, the connectivity state of the first transfer valve 6 is adjusted according to the specific gravity between the extraction solvent and water.

[0044] Further optimization is performed, considering that the solvent extraction pump 1 must be connected to two pipelines regardless of the extraction process or the cleaning process, the second transfer valve preferably includes:

[0045] A tee 11, wherein the tee 11 is connected to the second connecting pipe and the solvent extraction pump 1 respectively;

[0046] The first four-way valve 12 is connected to the three-way valve 11, the sample bottle 9 and the cleaning bottle 13 respectively, and one port of the first four-way valve 12 is an air port.

[0047] When in use, the first four-way valve 12 is used to adjust whether the three-way valve 11 is connected to the sample bottle 9 or the cleaning bottle 13.

[0048] According to further optimization, it is preferred that both the first switching valve 6 and the third switching valve 7 are four-way valves.

[0049] Further optimization is performed, because the extraction time of some extraction solvents and their corresponding extraction components is relatively long in a normal mixed state, it is preferred that an ultrasonic tank 3 is provided on the outer periphery of the spiral tube 4, and an ultrasonic generator is provided in the ultrasonic tank 3. The spiral tube 4 is ultrasonically treated by the ultrasonic generator, thereby accelerating the extraction speed.

[0050] After further optimization, it is preferred that the inner diameter of the spiral tube 4 is 0.5-5 mm and the length is 5-30 cm.

[0051] After further optimization, it is preferred that the capacity of the collecting bottle 8 is 2-20 ml.

[0052] The above are only preferred embodiments of the present invention, and are not intended to limit the patent scope of the present invention. All equivalent structural changes made using the contents of the present invention's specification and drawings under the inventive concept of the present invention, or directly or indirectly applied in other related technical fields, are included in the patent protection scope of the present invention.

Claims

1. A solvent circulation extraction device, characterized in that: include: A layered tube (5), wherein a liquid inlet pipe extending into the layered tube (5) is arranged at the top of the layered tube (5), a first liquid outlet pipe is arranged at the bottom of the layered tube (5), and a second liquid outlet pipe is arranged on the side wall of the layered tube (5); a first switching valve (6), the first switching valve (6) being connected to the first liquid outlet pipe and the second liquid outlet pipe; a collecting bottle (8), wherein the collecting bottle (8) is provided with a first connecting pipe and a second connecting pipe extending into the collecting bottle (8), and the first connecting pipe is connected to the first switching valve (6); a second transfer valve, the second transfer valve being in communication with the second connecting pipe; A sample bottle (9), the sample bottle (9) being connected to the second transfer valve; a cleaning bottle (13), the cleaning bottle (13) being in communication with the second switching valve; A solvent extraction pump (1), the solvent extraction pump (1) being in communication with the second transfer valve; The second switching valve comprises: A tee (11), wherein the tee (11) is connected to the second connecting pipe and the solvent extraction pump (1) respectively; A first four-way valve (12), wherein the first four-way valve (12) is respectively connected to the three-way valve (11), the sample bottle (9) and the cleaning bottle (13), and one port of the first four-way valve (12) is an air port; a third transfer valve (7), the third transfer valve (7) being connected to the solvent extraction pump (1); a spiral tube (4), one end of the spiral tube (4) being connected to the third switching valve (7), and the other end of the spiral tube (4) being connected to the liquid inlet pipe; A waste liquid barrel (10), the waste liquid barrel (10) being in communication with the third switching valve (7); A waste discharge pump (2), one end of the waste discharge pump (2) is connected to the waste liquid barrel (10), and the other end of the waste discharge pump (2) is connected to the first transfer valve (6).

2. A solvent circulation extraction device as claimed in claim 1, characterized in that: The first transfer valve (6) and the third transfer valve (7) are both four-way valves.

3. A solvent circulation extraction device as claimed in claim 1, characterized in that: An ultrasonic groove (3) is arranged on the outer periphery of the spiral tube (4), and an ultrasonic generator is arranged in the ultrasonic groove (3).

4. A solvent circulation extraction device as claimed in claim 1, characterized in that: The inner diameter of the spiral tube (4) is 0.5-5 mm, and the length is 5-30 cm.

5. A solvent circulation extraction device as claimed in claim 1, characterized in that: The capacity of the collecting bottle (8) is 2-20 ml.

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