Cracking degree online detection device and method for separating boron isotope by chemical exchange method

Abstract

The invention provides a cracking degree on-line detection device and method for separating boron isotopes by a chemical exchange method, and the device comprises a sample on-line introduction pipeline, an absorbance detection module and a sample on-line return pipeline which are connected in sequence, an inlet of the on-line sample lead-in pipeline and an outlet of the on-line sample return pipeline are respectively connected with a process main line, so that on-line internal circulation is formed. The spectrophotometric method is mainly used for detecting the cracking degree of the boron isotope separated by the chemical exchange method on line, the sample liquid can realize internal circulation, and the detection of the cracking degree of the boron trifluoride anisole complex can be completed under the condition of not generating waste liquid, so that the operation parameters of the cracking process are accurately controlled.

Description

Technical Field

[0001] This invention relates to the field of chemical exchange separation of boron isotopes, specifically to an online detection device and method for the degree of fragmentation of boron isotopes separated by chemical exchange. Background Technology

[0002] Boron has two natural isotopes, boron-10 and boron-11. Boron-10 is a good neutron absorber that can control the chain reaction rate of nuclear reactors and can also be used to destroy the growth of tumor cells. Boron-11 can endow materials with special physical and chemical properties. Therefore, the separation technology of boron isotopes has always attracted much attention.

[0003] Chemical exchange distillation is currently the most commonly used method for separating boron isotopes. In this method, the boron trifluoride complex of anisole is heated to separate boron trifluoride gas for internal circulation or extraction. Simultaneously, the separated anisole is purified and recycled. During the heating separation process, conditions such as temperature, pressure, and time all affect the degree of complex decomposition and the concentration of byproducts. A low degree of decomposition not only significantly reduces the utilization rate of boron trifluoride, but the high concentration of boron trifluoride complex in anisole can also affect subsequent processes, easily generating large amounts of byproducts and releasing toxic and corrosive gases. Therefore, a high degree of decomposition needs to be maintained during this process.

[0004] Currently, increasing the temperature or extending the time is commonly used to improve the degree of cracking, but both methods increase the rate of side reactions, which is detrimental to subsequent processes. Therefore, there is a need to develop an online device and method for detecting the degree of cracking of anisole boron trifluoride complexes, which can minimize the cracking temperature and time while achieving the cracking objective, thereby reducing the occurrence of side reactions. Summary of the Invention

[0005] In view of the problems existing in the prior art, the present invention provides an online detection device and method for the degree of cracking of boron isotopes separated by chemical exchange. It mainly utilizes spectrophotometry to detect the degree of cracking of boron isotopes separated by chemical exchange, such as the online detection device and method for the content of low concentration of boron trifluoride complex in anisole with anisole as a complexing agent. The sample liquid can be internally circulated, and the degree of cracking of boron trifluoride anisole complex can be detected without generating waste liquid, thereby accurately controlling the operating parameters of the cracking process.

[0006] To achieve this objective, the present invention adopts the following technical solution:

[0007] One objective of this invention is to provide an online detection device for the fission degree of boron isotope separation by chemical exchange method. The online detection device includes an online sample introduction pipeline, an absorbance detection module, and an online sample reflux pipeline connected in sequence. The inlet of the online sample introduction pipeline and the outlet of the online sample reflux pipeline are respectively connected to the main process line, thereby forming an online internal circulation.

[0008] A multi-channel selection valve is installed on the online sample introduction pipeline. The other inlets of the multi-channel selection valve are connected to the standard solution storage tank to provide standard solutions with different complexation degrees to the absorbance detection module and establish a standard working curve of absorbance and complexation.

[0009] The absorbance detection module is electrically connected to the pyrolysis process control module corresponding to the main process circuit, enabling the pyrolysis process control module to perform fine control of the pyrolysis process based on online detection data.

[0010] As a preferred embodiment of the present invention, a cooler is provided on the online sample introduction pipeline, and the cooler is located between the main process line and the multi-channel selection valve.

[0011] As a preferred embodiment of the present invention, a flow control valve is provided on the online sample introduction pipeline, and the flow control valve is located between the main process line and the cooler.

[0012] As a preferred embodiment of the present invention, the absorbance detection module includes a sample flow cell for holding a sample solution; the outlet of the online sample inlet tube is connected to the bottom of the sample flow cell; and the inlet of the online sample return tube is connected to the top of the sample flow cell.

[0013] As a preferred technical solution of the present invention, the online cracking degree detection device further includes a waste liquid collector, which is connected to the absorbance detection module through a waste liquid collection pipeline.

[0014] As a preferred technical solution of the present invention, a one-way valve is installed on the online reflux pipeline of the sample.

[0015] The second objective of this invention is to provide an online detection method for the fragmentation degree of the chemical exchange method for separating boron isotopes, as described in the first objective. The online detection method for fragmentation degree includes the following:

[0016] By adjusting the multi-channel selection valve, a standard solution with known complexation in a standard solution storage tank is introduced into the absorbance detection module. The solution is then rinsed and the absorbance is detected sequentially to obtain a set of absorbance and complexation detection data. The multi-channel selection valve is adjusted again, another standard solution storage tank is replaced, and the above operation is repeated to establish a standard working curve of absorbance and complexation.

[0017] By adjusting the multi-channel selection valve, the sample liquid in the main process circuit is introduced into the absorbance detection module for sequential rinsing and absorbance detection. Based on the standard working curve of absorbance and complexation degree, the complexation degree of the sample liquid is determined, and then the online detection data of pyrolysis degree is obtained according to the relationship of pyrolysis degree = 100% - complexation degree. The pyrolysis process control module performs fine control of the pyrolysis process based on the obtained online detection data of pyrolysis degree.

[0018] As a preferred technical solution of the present invention, the number of standard solutions with known complexation degree is ≥2, and the corresponding complexation degree includes at least two of 0%, 1%, 2%, 3%, 4%, and 5%.

[0019] As a preferred embodiment of the present invention, the rinsing is repeated at least 3 times.

[0020] As a preferred technical solution of the present invention, in the process of establishing the standard working curve of absorbance and complexation degree, the absorbance detection is repeated at least 3 times until the error of complexation degree is ±0.1%.

[0021] Compared with existing technical solutions, the present invention has at least the following beneficial effects:

[0022] (1) This invention mainly utilizes spectrophotometry to detect the degree of cracking of boron isotopes separated by chemical exchange, such as an online detection device and method for the content of low concentration boron trifluoride complex in anisole with anisole as a complexing agent. The sample liquid can be internally circulated, and the cracking degree of boron trifluoride anisole complex can be detected without generating waste liquid, thereby accurately controlling the operating parameters of the cracking process.

[0023] (2) Based on the online detection results of the cracking degree of the present invention, the cracking process can reduce the cracking temperature and cracking time as much as possible while achieving the cracking purpose, and reduce the occurrence of side reactions. In addition, this online detection method avoids the release of toxic gases that may be caused by offline sampling and detection, and can also simplify the process. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the online detection device for the degree of fragmentation of boron isotopes separated by chemical exchange method as described in Embodiment 1 of the present invention.

[0025] In the diagram: 1-Main process line; 2-Standard solution storage tank; 3-Flow control valve; 4-Cooler; 5-Multi-channel selector valve; 6-Online sample introduction pipeline; 7-Absorbance detection module; 8-Sample flow cell; 9-Online sample reflux pipeline; 10-Check valve. Detailed Implementation

[0026] The technical solution of the present invention will be further described below with reference to the accompanying drawings and specific embodiments.

[0027] This invention provides an online detection device for the fission degree of boron isotope separation by chemical exchange method. The online detection device includes an online sample introduction pipeline, an absorbance detection module, and an online sample reflux pipeline connected in sequence. The inlet of the online sample introduction pipeline and the outlet of the online sample reflux pipeline are respectively connected to the main process line, thereby forming an online internal circulation.

[0028] A multi-channel selection valve is installed on the online sample introduction pipeline. The other inlets of the multi-channel selection valve are connected to the standard solution storage tank to provide standard solutions with different complexation degrees to the absorbance detection module and establish a standard working curve of absorbance and complexation.

[0029] The absorbance detection module is electrically connected to the pyrolysis process control module corresponding to the main process circuit, enabling the pyrolysis process control module to perform fine control of the pyrolysis process based on online detection data.

[0030] This invention mainly utilizes spectrophotometry for online detection of the degree of cracking of boron isotopes separated by chemical exchange, such as an online detection device and method for the content of low concentration boron trifluoride complexes remaining in anisole using anisole as a complexing agent. The sample solution can be internally circulated, and the degree of cracking of boron trifluoride anisole complexes can be detected without generating waste liquid, thereby accurately controlling the operating parameters of the cracking process.

[0031] It should be noted that there are multiple standard solution storage tanks, each storing anisole standard solutions with different complexation degrees, and each connected to a different inlet of a multi-channel selector valve. To prevent moisture from the air from entering the standard solution storage tanks, dry nitrogen gas with a slight positive pressure can be filled into the tanks. The standard solution storage tanks include at least one standard solution storage tank with a complexation degree of 0, i.e., a dry anisole storage tank, and one standard solution storage tank with a known complexation degree of relatively high (generally less than 10%).

[0032] In some specific embodiments, a cooler is provided on the online sample introduction pipeline, and the cooler is located between the main process line and the multi-channel selection valve.

[0033] It should be noted that the sample introduction system draws out the sample to be tested through the side pipe flowing on the main process line. Since the sample temperature is generally around 100℃, in order to improve the accuracy of the detection results, the sample needs to be cooled to room temperature before entering the sample flow cell of the absorbance detection module through the valve.

[0034] In some specific embodiments, a flow control valve is provided on the online sample introduction pipeline, and the flow control valve is located between the main process line and the cooler.

[0035] In some specific embodiments, the absorbance detection module includes a sample flow cell for holding a sample solution; the outlet of the online sample introduction line is connected to the bottom of the sample flow cell; and the inlet of the online sample return line is connected to the top of the sample flow cell.

[0036] It should be noted that the sample flow cell is generally made of quartz, and its length can be determined according to the model of the absorbance detection equipment. The absorbance detection module can use a common commercially available spectrophotometer.

[0037] In some specific embodiments, the online splitting degree detection device further includes a waste liquid collector, which is connected to the absorbance detection module through a waste liquid collection pipeline.

[0038] It should be noted that although the anisole used for rinsing and standard curve determination has a different degree of complexation than the anisole in the main process, the amount is small and will not have an impact even if it is directly refluxed to the main process. However, for the sake of process rigor, a waste liquid collector may be added.

[0039] In some specific embodiments, a one-way valve is installed on the online reflux line of the sample.

[0040] This invention also provides an online detection method for the online detection of the fragmentation degree of a chemical exchange method for separating boron isotopes, the online detection method comprising the following:

[0041] By adjusting the multi-channel selection valve, a standard solution with known complexation in a standard solution storage tank is introduced into the absorbance detection module. The solution is then rinsed and the absorbance is detected sequentially to obtain a set of absorbance and complexation detection data. The multi-channel selection valve is adjusted again, another standard solution storage tank is replaced, and the above operation is repeated to establish a standard working curve of absorbance and complexation.

[0042] By adjusting the multi-channel selection valve, the sample liquid in the main process circuit is introduced into the absorbance detection module for sequential rinsing and absorbance detection. Based on the standard working curve of absorbance and complexation degree, the complexation degree of the sample liquid is determined, and then the online detection data of pyrolysis degree is obtained according to the relationship of pyrolysis degree = 100% - complexation degree. The pyrolysis process control module performs fine control of the pyrolysis process based on the obtained online detection data of pyrolysis degree.

[0043] It should be noted that before starting the test, the entire pipeline should be filled and flushed with dried anisole, and the absorbance of the anisole should be read. Then, other standard solutions with known complexation degrees should be introduced to fill the flow cell, and the corresponding absorbance should be read to establish absorbance standard working curves for different complexation degrees. The absorbance detection module can be calibrated at certain intervals (usually 8 hours), and then the absorbance standard working curve should be redrawn to ensure the accuracy of online detection. After the absorbance standard working curve is established, online detection can begin. Open the valve to introduce the sample to obtain the absorbance of anisole in the main process circuit. Read the complexation degree according to the standard curve and calculate the corresponding degree of pyrolysis (pyrolysis degree = 100% - complexation degree). The data processing system is mainly used to calculate the relationship between absorbance and complexation degree, and transmit the calculation results to the pyrolysis process control module to fine-tune the operating parameters to achieve precise control. After the test is completed, anisole can be used to clean and fill the pipeline.

[0044] In some specific embodiments, the number of standard solutions with known complexation degree is ≥2, and the corresponding complexation degree includes at least two of 0%, 1%, 2%, 3%, 4%, and 5%.

[0045] In some specific embodiments, the rinsing is repeated at least three times.

[0046] In some specific implementations, during the process of establishing a standard working curve for absorbance and complexation, the absorbance detection is repeated at least 3 times until the error of complexation is ±0.1%.

[0047] To better illustrate the present invention and facilitate understanding of its technical solutions, typical but non-limiting embodiments of the present invention are as follows:

[0048] Example 1

[0049] This embodiment provides an online detection device for the degree of fragmentation of boron isotopes separated by chemical exchange, such as... Figure 1 As shown, the online pyrolysis detection device includes an online sample introduction pipeline 6, an absorbance detection module 7, and an online sample reflux pipeline 9 connected in sequence; the inlet of the online sample introduction pipeline 6 and the outlet of the online sample reflux pipeline 9 are respectively connected to the main process line 1, thereby forming an online internal circulation;

[0050] A multi-channel selection valve 5 is installed on the online sample introduction pipeline 6. The other inlets of the multi-channel selection valve 5 are connected to the standard solution storage tank 2 to provide standard solutions with different complexation degrees to the absorbance detection module 7 and establish a standard working curve of absorbance and complexation.

[0051] The absorbance detection module 7 is electrically connected to the pyrolysis process control module (not shown in the figure) corresponding to the main process circuit 1, so that the pyrolysis process control module can perform fine control of the pyrolysis process based on online detection data.

[0052] The sample online inlet pipeline 6 is equipped with a cooler 4, which is located between the main process line 1 and the multi-channel selection valve 5; a flow control valve 3 is also installed on the sample online inlet pipeline 6, located between the main process line 1 and the cooler 4; the absorbance detection module 7 includes a sample flow cell 8 for holding the sample solution; the outlet of the sample online inlet pipeline 6 is connected to the bottom of the sample flow cell 8; the inlet of the sample online reflux pipeline 9 is connected to the top of the sample flow cell 8; and a one-way valve 10 is installed on the sample online reflux pipeline 9.

[0053] This embodiment also provides an online detection method for the fragmentation degree of a chemical exchange method for separating boron isotopes, including the following:

[0054] (1) According to Figure 1 After assembling the detection device, store the dried and dehydrated anisole standard solution (water content less than 30 ppm) in one standard solution storage tank 2, and store the 5% complexation standard solution in another standard storage tank 2 (the molar ratio of boron trifluoride to anisole in this standard solution is 5:100; the standard solution is calibrated by weighing; 100 grams of dried anisole solution absorbs 3.14 grams of boron trifluoride under anhydrous conditions to obtain a standard solution with a complexation degree of 5%).

[0055] (2) By adjusting the multi-channel selection valve 5, first use the dried and dehydrated anisole standard solution to rinse the detection pipeline for about 1 minute, and then close the multi-channel selection valve 5; set the absorbance detection module 7 to concentration mode, read the absorbance of the sample flow cell 8 and set its concentration value to 0, repeat the rinsing three times until the concentration display value is within ±0.001 each time. If it exceeds this range, repeat the rinsing process; by adjusting the multi-channel selection valve 5, select to 5% complexation standard solution until the concentration value displayed by the absorbance detection module 7 is stable, then set its value to 0.05, repeat the measurement three times until the concentration display value is between 0.0490 and 0.0510 (error ±0.001). If it exceeds the range, clean the pipeline with 5% complexation standard solution; then establish a standard working curve of absorbance and complexation.

[0056] (3) By adjusting the multi-channel selection valve 5, the sample liquid in the main process line 1 is introduced into the online sample introduction pipeline 6. The sample liquid first passes through the flow control valve 3 to control the flow rate so that the liquid flow in the test pipeline is stable. Then, it passes through the cooler 4 to cool the sample liquid to room temperature. The sample liquid is then introduced into the absorbance detection module 7 to read the absorbance value of the sample flow cell 8. Based on the standard working curve of absorbance and complexation degree, the complexation degree of the sample liquid is determined. Then, according to the relationship of pyrolysis degree = 100% - complexation degree, the online detection data of pyrolysis degree is obtained. The pyrolysis process flow control module performs fine control of the pyrolysis process flow based on the obtained online detection data of pyrolysis degree. For example, if the pyrolysis degree is higher than 0.98, the main valve of the main process line 1 can be controlled to collect the sample. If the pyrolysis degree is lower than 0.98, the main valve is closed to allow it to flow back.

[0057] It should be noted that if online testing is stopped, the multi-channel selector valve 5 can be switched to the anisole standard solution and the test line can be flushed. After the flushing is complete, the multi-channel selector valve 5 and the one-way valve 10 should be closed to keep the test line full of anisole and prevent air from entering.

[0058] In summary, this invention primarily utilizes spectrophotometry for online detection of the degree of fragmentation of boron isotopes separated by chemical exchange, such as an online detection device and method for the content of low-concentration boron trifluoride complexes remaining in anisole using anisole as a complexing agent. The sample solution can be internally circulated, allowing for the detection of the degree of fragmentation of boron trifluoride anisole complexes without generating waste liquid, thereby precisely controlling the operating parameters of the fragmentation process. Based on the online detection results of the degree of fragmentation of this invention, the fragmentation process can be optimized to minimize the fragmentation temperature and time while achieving the desired fragmentation objective, reducing the occurrence of side reactions. Furthermore, this online detection method avoids the release of toxic gases that may occur with offline sampling and detection, and also simplifies the process.

[0059] The present invention has been illustrated with the above embodiments to illustrate its detailed structural features. However, the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must rely on the above detailed structural features to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent substitutions for the components used in the present invention, additions of auxiliary components, and selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0060] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0061] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.

[0062] Furthermore, various different embodiments of the present invention can be combined in any way, as long as they do not violate the spirit of the present invention, they should also be regarded as the content disclosed by the present invention.

Claims

1. An online detection device for the degree of fragmentation of boron isotopes separated by chemical exchange, characterized in that, The online splitting degree detection device includes an online sample inlet pipeline, an absorbance detection module, and an online sample reflux pipeline connected in sequence. The inlet of the online sample introduction pipeline and the outlet of the online sample return pipeline are respectively connected to the main process line, thereby forming an online internal circulation; A multi-channel selection valve is installed on the online sample introduction pipeline. The other inlets of the multi-channel selection valve are connected to the standard solution storage tank to provide standard solutions with different complexation degrees to the absorbance detection module and establish a standard working curve of absorbance and complexation. The absorbance detection module is electrically connected to the pyrolysis process control module corresponding to the main process circuit, enabling the pyrolysis process control module to perform fine control of the pyrolysis process based on online detection data.

2. The online splitting degree detection device according to claim 1, characterized in that, A cooler is installed on the online sample introduction pipeline, and the cooler is located between the main process line and the multi-channel selection valve.

3. The online splitting degree detection device according to claim 2, characterized in that, A flow control valve is installed on the online sample introduction pipeline, and the flow control valve is located between the main process line and the cooler.

4. The online splitting degree detection device according to claim 1, characterized in that, The absorbance detection module includes a sample flow cell for holding a sample solution; the outlet of the online sample inlet tube is connected to the bottom of the sample flow cell; and the inlet of the online sample return tube is connected to the top of the sample flow cell.

5. The online splitting degree detection device according to claim 1, characterized in that, The online splitting degree detection device also includes a waste liquid collector, which is connected to the absorbance detection module through a waste liquid collection pipeline.

6. The online splitting degree detection device according to claim 1, characterized in that, A one-way valve is installed on the online reflux line of the sample.

7. A method for online detection of the fragmentation degree of an online detection device for separating boron isotopes by chemical exchange according to any one of claims 1-6, characterized in that, The online splitting degree detection method includes the following: By adjusting the multi-channel selection valve, a standard solution with known complexation in a standard solution storage tank is introduced into the absorbance detection module. The solution is then rinsed and the absorbance is detected sequentially to obtain a set of absorbance and complexation detection data. The multi-channel selection valve is adjusted again, another standard solution storage tank is replaced, and the above operation is repeated to establish a standard working curve of absorbance and complexation. By adjusting the multi-channel selection valve, the sample liquid in the main process line is introduced into the absorbance detection module, and rinsing and absorbance detection are performed in sequence. Based on the standard working curve of absorbance and complexation degree, the complexation degree of the sample liquid is determined, and then the online detection data of pyrolysis degree is obtained according to the relationship of pyrolysis degree = 100% - complexation degree. The pyrolysis process control module performs fine control over the pyrolysis process based on the obtained online pyrolysis degree detection data.

8. The online splitting degree detection method according to claim 7, characterized in that, The number of standard solutions with known complexation degree is ≥2, and the corresponding complexation degree includes at least two of the following: 0%, 1%, 2%, 3%, 4%, and 5%.

9. The online splitting degree detection method according to claim 7, characterized in that, The rinsing process should be repeated at least three times.

10. The online splitting degree detection method according to claim 7, characterized in that, In establishing the standard working curve for absorbance and complexation, the absorbance detection is repeated at least 3 times until the error of complexation is ±0.1%.

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