Purification system and purification method of 4-aminoantipyrine

Abstract

The invention relates to the technical field of substance purification, in particular to a purification system and a purification method of 4-aminoantipyrine, the purification system comprises a first container for storing 4-aminoantipyrine, a purification assembly for purifying 4-aminoantipyrine and a second container for storing purified 4-aminoantipyrine; the first container is communicated with the purification assembly through a first pipeline, and a first pump used for extracting 4-aminoantipyrine from the first container and conveying the 4-aminoantipyrine into the purification assembly is arranged on the first pipeline; the second container is communicated with the first container through a second pipeline, and a second pump for extracting 4-aminoantipyrine from the second container and conveying the 4-aminoantipyrine into the first container is arranged on the second pipeline; according to the method, an automatic purification system is constructed, so that the purification efficiency and the purification safety are improved, and the purified 4-aminoantipyrine can meet the purification requirements of volatile phenol tests through multiple purification.

Description

Technical Field

[0001] The invention relates to the technical field of substance purification, and in particular to a purification system and a purification method for 4-aminoantipyrine. Background Art

[0002] Volatile phenol in water refers to whether phenols can be evaporated with water vapor. It can be divided into volatile phenol and non-volatile phenol. It is very harmful to crops, aquatic fish and human body. Natural water generally does not contain phenols, but due to the pollution of certain industrial wastewater, natural water may contain phenolic compounds. Volatile phenol in daily water has become one of the must-measure items for water quality monitoring. At present, there are many analytical methods for volatile phenol, and the most commonly used method is 4-aminoantipyrine spectrophotometry.

[0003] Since 4-aminoantipyrine is easily deliquescent and oxidized to produce 4-aminoantipyrine red, the blank value of the determination is high, affecting the detection limit of the method, as well as the accuracy and precision of the measurement. Therefore, 4-aminoantipyrine needs to be purified before testing.

[0004] At present, commonly used methods for purifying 4-aminoantipyrine include chloroform extraction purification method, ethanol purification method, benzene purification method, activated carbon purification method, and floral silica purification method. For example, the invention patent with publication number CN106243041A discloses a method for purifying 4-aminoantipyrine, in which floral silica is replaced by bleaching earth, and the bleaching earth is added to a 4-aminoantipyrine solution, and the solution is stirred evenly, allowed to stand, separated, and the filtrate is collected to obtain purified 4-aminoantipyrine. For another example, the invention patent with publication number CN113200917A discloses another method for purifying 4-aminoantipyrine, in which colloidal impurities are adsorbed by activated carbon, and then the activated carbon adsorbed with impurities is filtered out to completely remove the impurities from the system to obtain a purified solution.

[0005] The above purification methods all adopt manual operation, which is time-consuming, labor-intensive, and some reagents are harmful to the human body in actual production. In addition, 4-aminoantipyrine purified only once may still have the defect of not being able to meet the requirements of spectrophotometric testing. Summary of the invention

[0006] In order to solve the problems existing in the prior art, the purpose of the first aspect of the present invention is to provide a purification system for 4-aminoantipyrine, which improves the purification efficiency and purification safety by constructing an automated purification system, and ensures that the purified 4-aminoantipyrine can meet the purification requirements of volatile phenol testing through multiple purifications.

[0007] The purpose of the second aspect of the present invention is to provide a method for purifying 4-aminoantipyrine.

[0008] According to the purpose of the first aspect of the present invention, a purification system for 4-aminoantipyrine is provided, comprising a first container for storing 4-aminoantipyrine, a purification component for purifying 4-aminoantipyrine and a second container for storing purified 4-aminoantipyrine; the first container is connected to the purification component through a first pipeline, and a first pump for extracting 4-aminoantipyrine from the first container and transporting it to the purification component is provided on the first pipeline; the second container is connected to the first container through a second pipeline, and a second pump for extracting 4-aminoantipyrine from the second container and transporting it to the first container is provided on the second pipeline.

[0009] Furthermore, the purification system of 4-aminoantipyrine provided by the present invention may also have the following feature: the pumping speed of the first pump is lower than the pumping speed of the second pump.

[0010] Furthermore, the purification system of 4-aminoantipyrine provided by the present invention may also have the following characteristics: the purification component includes a vertically movable cover body and a shell body arranged below the cover body; the cover body is provided with an interface for connecting to the first pipeline, the shell body is provided with a liquid outlet, and the second container is arranged below the liquid outlet.

[0011] Furthermore, the purification system of 4-aminoantipyrine provided by the present invention may also have the following characteristics: a purification section is provided inside the shell, and the purification section includes an adsorption layer for adsorbing impurities in 4-aminoantipyrine and a filtration layer provided below the adsorption layer.

[0012] Furthermore, the purification system of 4-aminoantipyrine provided by the present invention may also have the following characteristics: the adsorption layer includes an activated carbon adsorption layer and / or a floral silica adsorption layer.

[0013] Furthermore, the purification system of 4-aminoantipyrine provided by the present invention may also have the following characteristics: it also includes a photometric sensor for collecting the photometric value of 4-aminoantipyrine in the first container and the photometric value of 4-aminoantipyrine in the second container, and the photometric sensor is connected to the second pump signal.

[0014] Furthermore, the purification system of 4-aminoantipyrine provided by the present invention may also have the following characteristics: it also includes a rotating base arranged between the first container and the second container, and the photometric sensor is arranged on the rotating base; when the photometric sensor rotates to a first position with the rotating base, the photometric sensor collects the photometric value of the first container, and when the photometric sensor rotates to a second position with the rotating base, the photometric sensor collects the photometric value of the second container.

[0015] Furthermore, the purification system of 4-aminoantipyrine provided by the present invention may also have the following characteristics: a side of the first container away from the photometric sensor and a side of the second container away from the photometric sensor are both provided with a reflective plate for enhancing the light signal collection of the photometric sensor.

[0016] According to the purpose of the second aspect of the present invention, a method for purifying 4-aminoantipyrine is provided, which is applicable to the purification system of 4-aminoantipyrine as described above, comprising the following steps: S1. A first pump extracts 4-aminoantipyrine from a first container and delivers it to a purification component, and the purification component purifies 4-aminoantipyrine and outputs it to a second container; S2. Detect whether the 4-aminoantipyrine in the second container meets the purification requirements. If the purification requirements are met, the purification is completed. If the purification requirements are not met, step S3 is performed; S3. The second pump extracts 4-aminoantipyrine from the second container and transports it to the first container, and returns to step S1, and the above steps are repeated until the purification requirements are met.

[0017] Furthermore, the method for purifying 4-aminoantipyrine provided by the present invention may also have the following characteristics: in step S2, the process of detecting whether the 4-aminoantipyrine in the second container meets the purification requirements comprises: The photometric value of 4-aminoantipyrine in the first container is collected by a photometric sensor, which is recorded as the first photometric value; the photometric value of 4-aminoantipyrine in the second container is collected by a photometric sensor, which is recorded as the second photometric value; the comparison value between the first photometric value and the second photometric value is solved by the following formula: Wherein, ω represents the contrast value, C0 is the first photometric value, and C is the second photometric value; the relationship between the contrast value and the preset value is judged, if the contrast value is greater than or equal to the preset value, the purification requirement is met, if the contrast value is less than the preset value, the purification requirement is not met.

[0018] The beneficial effects of the present invention are: 1. In the present application, the 4-aminoantipyrine solution in the first container is extracted by the first pump for primary purification. When the 4-aminoantipyrine solution in the second container still does not meet the purification requirements for the volatile phenol test, the 4-aminoantipyrine solution in the second container is extracted by the second pump and transported back to the first container for secondary purification, and the purification is repeated multiple times by circulating this process until the 4-aminoantipyrine solution in the second container meets the purification requirements for the volatile phenol test. Such an automated purification system greatly improves the purification efficiency, and the entire process does not require manual intervention, thereby improving the purification safety.

[0019] 2. In the present application, a purification component is formed by cooperating a vertically movable cover and a fixed shell. When purification is not performed, the cover and the shell can be separated to facilitate their replacement. When purification is performed, the cover and the shell are combined to form a purification component for solution purification.

[0020] 3. In the present application, a photometric sensor is provided to collect the photometric values ​​of the 4-aminoantipyrine solution in the first container and the second container, and an intelligent comparison is performed between the two to quantitatively evaluate the purification process, automatically determine whether purification is required again, and issue a work instruction to the second pump, thereby further improving the automation level and purification efficiency of the entire purification system. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] The accompanying drawings, which are incorporated into the specification and constitute a part of the specification, illustrate embodiments of the present invention and are used together with the description to explain the principles of the present invention. In these drawings, similar reference numerals are used to represent similar elements. The drawings described below are some embodiments of the present invention, but not all embodiments. For those of ordinary skill in the art, other drawings can be obtained from these drawings without paying creative work.

[0022] Figure 1 It is a structural schematic diagram of the present invention; Figure 2 It is a schematic structural diagram of the shell of the present invention.

[0023] In the figure: 1. First container; 2. Purification component; 201. Cover; 202. Shell; 203. Activated carbon adsorption layer; 204. Florisil adsorption layer; 205. Filter layer; 206. Liquid outlet; 3. Second container; 4. First pipeline; 5. First pump; 6. Second pipeline; 7. Second pump; 801. Lifting bracket; 802. Fixed bracket; 9. Photometric sensor; 10. Rotating base; 11. First limit block; 12. Second limit block; 13. Reflector. DETAILED DESCRIPTION

[0024] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0025] The present invention provides a purification system for 4-aminoantipyrine, the specific structure of which is as follows: like Figure 1As shown, the purification system includes a first container 1 for storing 4-aminoantipyrine, a purification component 2 for purifying 4-aminoantipyrine, and a second container 3 for storing purified 4-aminoantipyrine; the first container 1 is connected to the purification component 2 through a first pipeline 4, and a first pump 5 is provided on the first pipeline 4 for extracting 4-aminoantipyrine from the first container 1 and transporting it to the purification component 2; the second container 3 is connected to the first container 1 through a second pipeline 6, and a second pump 7 is provided on the second pipeline 6 for extracting 4-aminoantipyrine from the second container 3 and transporting it to the first container 1. When in use, the first pump 5 extracts the 4-aminoantipyrine solution in the first container 1 for primary purification. When the 4-aminoantipyrine solution in the second container 3 still does not meet the purification requirements, the second pump 7 extracts the 4-aminoantipyrine solution in the second container 3 and transports it back to the first container 1 for secondary purification. This process is circulated for multiple purifications until the 4-aminoantipyrine solution in the second container 3 meets the purification degree required by the volatile phenol test. Such an automated purification system greatly improves the purification efficiency, and the entire process does not require human intervention, which improves the safety of purification.

[0026] In order to ensure the normal operation of the first pipeline 4 and the second pipeline 6, the first container 1 is provided with a liquid outlet for connecting to the first pipeline 4, a liquid inlet for connecting to the second pipeline 6, and an air port for connecting to the atmosphere. In addition, in order to facilitate secondary and multiple purifications, the bottom of the second container 3 is designed to be funnel-shaped and connected to the second pump 7 through a quick-connect connector.

[0027] When the pumping speed of the second pump 7 is lower than that of the first pump 5, the liquid in the second container 3 may be slowly updated, resulting in a problem of low purity in a local area. Therefore, the pumping speed of the second pump 7 is preferably higher than that of the first pump 5, which helps to break the laminar flow structure that may be formed in the second container 3. Further, considering the homogenization requirements of the solution and the economic requirements of the equipment, the pumping speed of the second pump 7 is preferably five times that of the first pump 5. In this embodiment, the pumping speed of the first pump 5 is 10 ml / min, and the pumping speed of the second pump 7 is 50 ml / min.

[0028] The purification component 2 includes a vertically movable cover 201 and a shell 202 disposed below the cover 201. The purification system also includes a lifting bracket 801 and a fixed bracket 802. The cover 201 is mounted on the lifting bracket 801, and the shell 202 is mounted on the fixed bracket 802. The cover 201 is provided with an interface for connecting the first pipeline 4, the shell 202 is provided with a liquid outlet 206, and the second container 3 is disposed below the liquid outlet 206. In order to prevent the additives in the shell 202 from affecting the test results of volatile phenols, the shell 202 is preferably made of high borosilicate glass material, and plastic material is avoided. When purification is not performed, the lifting bracket 801 is at a higher height to keep the cover 201 away from the shell 202, so that the cover 201 or the shell 202 can be replaced as needed. When purification is performed, the lifting bracket 801 drives the cover 201 to descend, so that the cover 201 and the shell 202 abut to form a complete purification component 2 to purify the 4-aminoantipyrine solution.

[0029] like Figure 2 As shown, a purification part is provided in the shell 202, and the purification part includes an adsorption layer for adsorbing impurities in 4-aminoantipyrine and a filter layer 205 arranged below the adsorption layer. When the shell 202 is replaced, according to the needs, the shell 202 can be disassembled from the fixed bracket 802 to replace the entire shell 202, or only the adsorption layer or the filter layer 205 can be replaced. Among them, the adsorption layer includes an activated carbon adsorption layer 203 and / or a Florisil adsorption layer 204. In a specific embodiment, the adsorption layer includes an activated carbon adsorption layer 203, which is used for the first purification of the 4-aminoantipyrine solution, and the Florisil adsorption layer 204 arranged below the activated carbon adsorption layer 203 is used for the second purification of the 4-aminoantipyrine solution. The filter layer 205 includes a quantitative filter paper layer, which is used to filter the 4-aminoantipyrine solution that has undergone two purification processes, and the filtered 4-aminoantipyrine solution enters the second container 3 through the liquid outlet 206. Compared with the single-layer setting of the activated carbon adsorption layer 203 or the floral silica adsorption layer 204 , the present invention effectively improves the purification efficiency of the solution by designing a double adsorption layer and a quantitative filtration layer 205 .

[0030] like Figure 1 As shown, in order to achieve quantitative evaluation of the purification process and improve the automated working efficiency of the purification system, the purification system also includes a photometric sensor 9 for collecting the photometric value of the 4-aminoantipyrine solution in the first container 1 and the photometric value of the 4-aminoantipyrine solution in the second container 3, and the photometric sensor 9 is signal-connected to the second pump 7. The photometric sensor 9 can judge whether the 4-aminoantipyrine solution in the second container 3 meets the purification requirements by comparing the two photometric values. If the purification requirements are not met, the photometric sensor 9 automatically issues instructions through the software workstation, and the second pump 7 starts to work.

[0031] The purification system also includes a rotating base 10 arranged between the first container 1 and the second container 3, and a photometric sensor 9 is arranged on the rotating base 10, and the rotating base 10 has a first position and a second position; when the photometric sensor 9 rotates to the first position with the rotating base 10, the photometric sensor 9 collects the photometric value of the first container 1; when the photometric sensor 9 rotates to the second position with the rotating base 10, the photometric sensor 9 collects the photometric value of the second container 3.

[0032] A reflective plate 13 for enhancing light signal collection by the light sensor 9 is disposed on one side of the first container 1 and one side of the second container 3 away from the light sensor 9 . The reflective plate 13 is used to reflect the light signal passing through the 4-aminoantipyrine solution to the light sensor 9 .

[0033] like Figure 1 As shown, since the operation of the first pump 5 or the second pump 7 may cause the first container 1 or the second container 3 to be displaced, in order to prevent such displacement from affecting the stability of the system, a first limit block 11 for limiting the displacement of the first container 1 is provided between the first container 1 and the photometric sensor 9, and a second limit block 12 for limiting the displacement of the second container 3 is provided between the second container 3 and the photometric sensor 9.

[0034] The present invention also provides a method for purifying 4-aminoantipyrine, which is applicable to the purification system of 4-aminoantipyrine as described above, and comprises the following steps: S1. The first pump 5 extracts 4-aminoantipyrine from the first container 1 and delivers it to the purification component 2, and the purification component 2 purifies the 4-aminoantipyrine and outputs it to the second container 3; S2. Detect whether the 4-aminoantipyrine in the second container 3 meets the purification requirements. If the purification requirements are met, the purification is completed. If the purification requirements are not met, step S3 is performed; S3. The second pump 7 extracts 4-aminoantipyrine from the second container 3 and transports it to the first container 1, and returns to step S1, and the above steps are repeated until the purification requirements are met.

[0035] In step S2, in order to automatically determine whether the 4-aminoantipyrine solution meets the purification requirements, the process of detecting whether the 4-aminoantipyrine in the second container 3 meets the purification requirements includes: The photometric value of the 4-aminoantipyrine solution in the first container 1 is collected by the photometric sensor 9 and recorded as the first photometric value. The photometric value of the 4-aminoantipyrine solution in the second container 3 is collected by the photometric sensor 9 and recorded as the second photometric value. The comparison value between the first photometric value and the second photometric value is solved by the following formula: Wherein, ω represents the contrast value, C0 is the first photometric value, and C is the second photometric value; the relationship between the contrast value and the preset value is judged, if the contrast value is greater than or equal to the preset value, the purification requirement is met, if the contrast value is less than the preset value, the purification requirement is not met.

[0036] In this embodiment, the preset value is 35%. When ω≥35%, the 4-aminoantipyrine solution in the second container 3 meets the purification requirements, and the purification ends; when ω<35%, the 4-aminoantipyrine solution in the second container 3 does not meet the purification requirements, and step S3 is continued.

[0037] Furthermore, in order to conduct a more detailed quantitative evaluation of the purification process, when ω < 35%, the following standards can also be set: When 10%≤ω≤20%, the 4-aminoantipyrine solution needs to be purified twice more; When 20%<ω<30%, the 4-aminoantipyrine solution needs to be purified again.

[0038] The contents described above may be implemented individually or in combination in various ways, and these variations are all within the protection scope of the present invention.

[0039] In the description of the invention, it should be noted that relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "comprise", "include" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device comprising a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the statement "comprise a ..." do not exclude the presence of other identical elements in the process, method, article or device comprising the elements.

[0040] In the description of the invention, it is also necessary to explain that the terms "center", "upper", "lower", "front", "back", "top", "bottom", "inside", "outside", etc. indicate positions or positional relationships based on the positions or positional relationships shown in the drawings, and are only for the convenience of describing the invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific position, be constructed and operated in a specific position, and therefore cannot be understood as a limitation on the invention. In the description of the invention, unless otherwise specified, "several" means two or more.

[0041] The above contents are further detailed descriptions of the present invention in combination with specific preferred implementation modes, and it cannot be determined that the specific embodiments of the present invention are limited to these descriptions. For ordinary technicians in the technical field to which the present invention belongs, several simple deductions or substitutions can be made without departing from the concept of the present invention, which should be regarded as belonging to the protection scope of the present invention.

Claims

1. A purification system for 4-aminoantipyrine, characterized in that: The invention comprises a first container (1) for storing 4-aminoantipyrine, a purification component (2) for purifying 4-aminoantipyrine, and a second container (3) for storing the purified 4-aminoantipyrine; the first container (1) is connected to the purification component (2) via a first pipeline (4); the first pipeline (4) is provided with a first pump (5) for extracting 4-aminoantipyrine from the first container (1) and transporting it to the purification component (2); the second container (3) is connected to the first container (1) via a second pipeline (6); the second pipeline (6) is provided with a second pump (7) for extracting 4-aminoantipyrine from the second container (3) and transporting it to the first container (1).

2. The purification system of 4-aminoantipyrine according to claim 1, characterized in that: The pumping speed of the first pump (5) is lower than the pumping speed of the second pump (7).

3. The purification system of 4-aminoantipyrine according to claim 1, characterized in that: The purification component (2) comprises a vertically movable cover (201) and a shell (202) disposed below the cover (201); the cover (201) is provided with an interface for connecting to the first pipeline (4), the shell (202) is provided with a liquid outlet (206), and the second container (3) is disposed below the liquid outlet (206).

4. The purification system of 4-aminoantipyrine according to claim 3, characterized in that: A purification section is provided inside the housing (202), and the purification section comprises an adsorption layer for adsorbing impurities in 4-aminoantipyrine and a filtration layer (205) provided below the adsorption layer.

5. The purification system of 4-aminoantipyrine according to claim 4, characterized in that: The adsorption layer includes an activated carbon adsorption layer (203) and / or a Florisil adsorption layer (204).

6. The purification system of 4-aminoantipyrine according to claim 1, characterized in that: It also includes a photometric sensor (9) for collecting the photometric value of 4-aminoantipyrine in the first container (1) and the photometric value of 4-aminoantipyrine in the second container (3), and the photometric sensor (9) is connected to the second pump (7) by a signal.

7. The purification system of 4-aminoantipyrine according to claim 6, characterized in that: The invention also comprises a rotating base (10) arranged between the first container (1) and the second container (3), and the photometric sensor (9) is arranged on the rotating base (10); when the photometric sensor (9) rotates to a first position along with the rotating base (10), the photometric sensor (9) collects the photometric value of the first container (1); and when the photometric sensor (9) rotates to a second position along with the rotating base (10), the photometric sensor (9) collects the photometric value of the second container (3).

8. The purification system of 4-aminoantipyrine according to claim 7, characterized in that: A side of the first container (1) away from the photometric sensor (9) and a side of the second container (3) away from the photometric sensor (9) are both provided with a reflection plate (13) for enhancing the light signal collection of the photometric sensor (9).

9. A method for purifying 4-aminoantipyrine, characterized in that: A purification system for 4-aminoantipyrine according to any one of claims 1 to 8, comprising the following steps: S1. The first pump (5) extracts 4-aminoantipyrine from the first container (1) and delivers it to the purification component (2). The purification component (2) purifies the 4-aminoantipyrine and then outputs it to the second container (3); S2. Detecting whether the 4-aminoantipyrine in the second container (3) meets the purification requirements. If the purification requirements are met, the purification is terminated. If the purification requirements are not met, step S3 is performed; S3. The second pump (7) extracts 4-aminoantipyrine from the second container (3) and transfers it to the first container (1), and returns to step S1, and the above steps are repeated until the purification requirements are met.

10. The method for purifying 4-aminoantipyrine according to claim 9, characterized in that: In step S2, the process of detecting whether the 4-aminoantipyrine in the second container (3) meets the purification requirements includes: The photometric value of 4-aminoantipyrine in the first container (1) is collected by the photometric sensor (9) and recorded as the first photometric value. The photometric value of 4-aminoantipyrine in the second container (3) is collected by the photometric sensor (9) and recorded as the second photometric value. The comparison value between the first photometric value and the second photometric value is solved by the following formula: Wherein, ω represents the contrast value, C0 is the first photometric value, and C is the second photometric value; the relationship between the contrast value and the preset value is judged, if the contrast value is greater than or equal to the preset value, the purification requirement is met, if the contrast value is less than the preset value, the purification requirement is not met.

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