A device and method for on-line detection of the degree of splitting in the chemical exchange method for separating boron isotopes

Abstract

The application provides a cracking degree on-line detection device and method for separating boron isotopes by chemical exchange method, and the device comprises a sample on-line introduction pipeline, an absorbance detection module and a sample on-line reflux pipeline connected in sequence, and the inlet of the sample on-line introduction pipeline and the outlet of the sample on-line reflux pipeline are connected with a process main pipeline, so as to form on-line internal circulation. The application mainly utilizes the spectrophotometry to on-line detect the cracking degree of the boron isotopes separated by the chemical exchange method, the sample liquid can realize internal circulation, the detection of the cracking degree of the boron trifluoride anisole complex can be completed without generating waste liquid, and therefore the operation parameters of the cracking process can be accurately controlled.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical exchange method for separating boron isotopes, and particularly relates to a cracking degree online detection device for chemical exchange method for separating boron isotopes and a method thereof. BACKGROUND

[0002] There are two natural isotopes of boron, namely boron-10 and boron-11. Boron-10 can be used as a good neutron absorber to control the chain reaction speed of a nuclear reactor, 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 been concerned.

[0003] The chemical exchange rectification method for separating boron isotopes is the most commonly used method at present. In this method, the benzyl ether boron trifluoride complex needs to be heated to separate the boron trifluoride gas for internal circulation or extraction, and the separated benzyl ether is purified and recycled. During the heating and separation process, the temperature, pressure, time and other conditions will affect the cracking degree of the complex and the concentration of the by-products. If the cracking degree is low, not only the utilization rate of boron trifluoride will be greatly reduced, but also the benzyl ether boron trifluoride complex in the benzyl ether will affect the subsequent process, and a large amount of by-products and toxic and corrosive gases will be produced. Therefore, a high cracking degree needs to be maintained in this process.

[0004] At present, the methods of increasing temperature or prolonging time are usually used to increase the cracking degree, but these two methods will increase the speed of the side reaction, which is not conducive to the subsequent process. Therefore, it is necessary to develop a device and method for online detection of the cracking degree of benzyl ether boron trifluoride complex, which can reduce the cracking temperature and cracking time as much as possible under the premise of achieving the purpose of cracking, and reduce the occurrence of side reactions. SUMMARY

[0005] In view of the problems in the prior art, the present application provides a cracking degree online detection device for chemical exchange method for separating boron isotopes and a method thereof, which mainly uses spectrophotometry to online detect the cracking degree of chemical exchange method for separating boron isotopes, such as the online detection device and method for the low-concentration benzyl ether boron trifluoride complex content remaining in benzyl ether as a complexing agent. The sample liquid can realize internal circulation, and the detection of the cracking degree of benzyl ether boron trifluoride complex can be completed without generating waste liquid, so as to accurately control the operation parameters of the cracking process.

[0006] To achieve this purpose, the present application adopts the following technical solutions:

[0007] One of the purposes of the present application is to provide a cracking degree online detection device for chemical exchange method separation of boron isotopes, which comprises a sample online introduction pipeline, an absorbance detection module and a sample online reflux pipeline connected in sequence; the inlet of the sample online introduction pipeline and the outlet of the sample online reflux pipeline are connected with a process main pipeline, thereby forming an online internal circulation.

[0008] A multi-channel selection valve is arranged on the sample online introduction pipeline, and other inlets of the multi-channel selection valve are connected with standard liquid storage tanks, so as to provide standard liquids with different complexing degrees for the absorbance detection module, and establish a standard working curve of absorbance and complexing degree.

[0009] The absorbance detection module is electrically connected with a cracking process flow control module corresponding to the process main pipeline, so that the cracking process flow control module finely controls the cracking process flow based on online detection data.

[0010] As a preferred technical solution of the present application, a cooler is arranged on the sample online introduction pipeline, and the cooler is arranged between the process main pipeline and the multi-channel selection valve.

[0011] As a preferred technical solution of the present application, a flow control valve is arranged on the sample online introduction pipeline, and the flow control valve is arranged between the process main pipeline and the cooler.

[0012] As a preferred technical solution of the present application, the absorbance detection module comprises a sample flow cell for containing a sample solution; the outlet of the sample online introduction pipeline is in communication with the bottom of the sample flow cell; and the inlet of the sample online reflux pipeline is in communication with the top of the sample flow cell.

[0013] As a preferred technical solution of the present application, the cracking degree online detection device further comprises a waste liquid collector connected with the absorbance detection module through a waste liquid collection pipeline.

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

[0015] Another purpose of the present application is to provide a cracking degree online detection method of the cracking degree online detection device for chemical exchange method separation of boron isotopes according to the first purpose, which comprises the following contents.

[0016] By adjusting the multi-channel selection valve, the standard liquid with known complex degree in a certain standard liquid storage tank is introduced into the absorbance detection module, and flushing and absorbance detection are sequentially performed to obtain a group of detection data of absorbance and complex degree; the multi-channel selection valve is adjusted again, another standard liquid storage tank is replaced, the above operation is repeated, and a standard working curve of absorbance and complex degree is established.

[0017] By adjusting the multi-channel selection valve, the sample liquid in the process main line is introduced into the absorbance detection module, and flushing and absorbance detection are sequentially performed; based on the standard working curve of absorbance and complex degree, the complex degree of the sample liquid is determined, and then the online detection data of the cleavage degree is obtained according to the relationship of cleavage degree = 100%-complex degree; the cleavage process control module performs fine control on the cleavage process based on the obtained online detection data of the cleavage degree.

[0018] As a preferred technical solution of the present application, the number of the standard liquid with known complex degree is greater than or equal to 2, and the corresponding complex degree includes at least two of 0%, 1%, 2%, 3%, 4% and 5%.

[0019] As a preferred technical solution of the present application, the flushing is repeated at least 3 times.

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

[0021] Compared with the prior art, the present application has at least the following beneficial effects:

[0022] (1) The present application mainly uses spectrophotometry to detect the cleavage degree of boron isotope separated by chemical exchange method online, for example, an online detection device and method for the content of low-concentration boron trifluoride complex remaining in anisole as a complexing agent, and the sample liquid can realize internal circulation, so that the detection of the cleavage degree of boron trifluoride anisole complex can be completed without generating waste liquid, thereby accurately controlling the operation parameters of the cleavage process.

[0023] (2) Based on the online detection results of the cleavage degree, the cleavage process can reduce the cleavage temperature and cleavage time as much as possible under the premise of achieving the cleavage purpose, and reduce the occurrence of side reactions; in addition, this online detection method avoids the release of toxic gas caused by offline sampling detection, and can also simplify the process. BRIEF DESCRIPTION OF DRAWINGS

[0024] Figure 1 is a structural schematic diagram of the online detection device for the cleavage degree of boron isotope separated by chemical exchange method according to Embodiment 1 of the present application.

[0025] In the figure: 1-process main line; 2-standard liquid storage tank; 3-flow control valve; 4-cooler; 5-multichannel selection valve; 6-sample online introduction pipeline; 7-absorbance detection module; 8-sample flow cell; 9-sample online backflow pipeline; 10-one-way valve. DETAILED DESCRIPTION

[0026] The technical solutions of the present application are further illustrated below by specific embodiments in combination with the accompanying drawings.

[0027] The present application provides a cracking degree online detection device for separating boron isotopes by chemical exchange method, which comprises a sample online introduction pipeline, an absorbance detection module and a sample online backflow pipeline connected in sequence; the inlet of the sample online introduction pipeline and the outlet of the sample online backflow pipeline are connected with the process main line, thereby forming an online internal circulation.

[0028] A multichannel selection valve is arranged on the sample online introduction pipeline, and the other inlets of the multichannel selection valve are connected with standard liquid storage tanks for providing the absorbance detection module with standard liquids of different complexing degrees to establish a standard working curve of absorbance and complexing degree.

[0029] The absorbance detection module is electrically connected with a cracking process flow control module corresponding to the process main line, so that the cracking process flow control module performs fine control on the cracking process flow based on the online detection data.

[0030] The present application mainly utilizes spectrophotometry to online detect the cracking degree of boron isotopes separated by chemical exchange method, such as an online detection device and method for the low-concentration boron trifluoride complex content of anisole remaining in anisole as a complexing agent, and sample liquid can realize internal circulation, and the detection of the cracking degree of boron trifluoride anisole complex can be completed without generating waste liquid, so as to accurately control the operation parameters of the cracking process.

[0031] It should be noted that a plurality of standard liquid storage tanks are arranged, which respectively store anisole standard liquids of different complexing degrees and are respectively connected with different inlets of the multichannel selection valve; in order to avoid moisture in the air from entering the standard liquid storage tank, dry nitrogen gas of a slight positive pressure can be filled in the tank; the standard liquid storage tank at least includes one standard liquid storage tank with a complexing degree of 0, i.e. a dry anisole storage tank, and one standard liquid storage tank with a known complexing degree which is relatively large (generally less than 10%).

[0032] In some specific embodiments, a cooler is arranged on the sample online introduction pipeline, and the cooler is arranged between the process main line and the multichannel selection valve.

[0033] It should be noted that the sample introduction system is to introduce the sample to be measured through the side pipe of the process main line, and since the sample temperature is generally about 100 DEG C, in order to improve the accuracy of the detection result, the sample needs to be cooled to room temperature, and then introduced into the sample flow cell of the absorbance detection module through the valve.

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

[0035] In some embodiments, the absorbance detection module comprises a sample flow cell for containing a sample solution, the outlet of the sample online introduction pipeline is communicated with the bottom of the sample flow cell, and the inlet of the sample online return pipeline is communicated with the top of the sample flow cell.

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

[0037] In some embodiments, the degree of cracking online detection device further comprises a waste liquid collector connected with the absorbance detection module through a waste liquid collection pipeline.

[0038] It should be noted that although the anisole used for flushing and used for standard curve determination has a difference in complex degree from the anisole in the process main line, the amount is small, and even if it is directly returned to the process main line, it will not cause an impact; however, in order to be rigorous in the process, the waste liquid collector can be optionally added.

[0039] In some embodiments, a one-way valve is arranged on the sample online return pipeline.

[0040] The application also provides a degree of cracking online detection method of the degree of cracking online detection device for separating boron isotopes by chemical exchange method, and the degree of cracking online detection method comprises the following contents:

[0041] By adjusting the multi-channel selection valve, the standard liquid with known complex degree in a certain standard liquid storage tank is introduced into the absorbance detection module, and flushing and absorbance detection are sequentially performed to obtain a group of detection data of absorbance and complex degree; the multi-channel selection valve is adjusted again, another standard liquid storage tank is replaced, the above operation is repeated, and a standard working curve of absorbance and complex degree is established.

[0042] The sample liquid in the process main line is guided into the absorbance detection module by adjusting the multi-channel selection valve, and flushing and absorbance detection are sequentially performed; based on the standard working curve of the absorbance and the complex degree, the complex degree of the sample liquid is determined, and then the online cracking degree detection data is obtained according to the relationship formula of cracking degree = 100%-complex degree; the cracking process control module performs fine control on the cracking process based on the obtained online cracking degree detection data.

[0043] It should be noted that before starting detection, the entire pipeline is filled and flushed with dry anisole, the absorbance of anisole is read, and then other standard liquids with known complex degrees are introduced to fill the flow cell, and the corresponding absorbance is read to establish the absorbance standard working curve corresponding to different complex degrees; the absorbance detection module can be calibrated at intervals (usually 8 hours), and then the absorbance standard working curve is redrawn to ensure the accuracy of online detection. After the absorbance standard working curve is established, online detection can be started, and the absorbance of anisole in the process main line can be obtained by opening the valve to introduce the sample to be measured, reading the complex degree according to the standard curve, and calculating the corresponding cracking degree (cracking degree = 100%-complex degree). The data processing system is mainly used to calculate the relationship between absorbance and complex degree, and transmit the calculation result to the cracking process control module and fine-tune the operation parameters to realize fine control; after detection is completed, anisole can be used to clean and fill the pipeline.

[0044] In some specific embodiments, the number of standard liquids with known complex degrees is ≥2, and the corresponding complex degrees include at least two of 0%, 1%, 2%, 3%, 4%, and 5%.

[0045] In some specific embodiments, the flushing is repeated at least 3 times.

[0046] In some specific embodiments, during the establishment of the absorbance and complex degree standard working curve, the absorbance detection is repeated at least 3 times until the error of the complex degree is ±0.1%.

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

[0048] Embodiment 1

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

[0050] A multi-channel selection valve 5 is arranged on the sample online introduction pipeline 6, other inlets of the multi-channel selection valve 5 are connected with standard liquid storage tanks 2, for providing different complex degree standard liquids to the absorbance detection module 7, and establishing the standard working curve of absorbance and complex degree;

[0051] The absorbance detection module 7 is electrically connected with a cracking process flow control module (not shown in the figure) corresponding to the process main pipeline 1, so that the cracking process flow control module finely controls the cracking process flow based on the online detection data;

[0052] Wherein, a cooler 4 is arranged on the sample online introduction pipeline 6, the cooler 4 is arranged between the process main pipeline 1 and the multi-channel selection valve 5; a flow control valve 3 is arranged on the sample online introduction pipeline 6, the flow control valve 3 is arranged between the process main pipeline 1 and the cooler 4; the absorbance detection module 7 includes a sample flow cell 8 for containing sample solution; the outlet of the sample online introduction pipeline 6 is communicated with the bottom of the sample flow cell 8; the inlet of the sample online return pipeline 9 is communicated with the top of the sample flow cell 8; a one-way valve 10 is arranged on the sample online return pipeline 9.

[0053] The embodiment also provides a cracking degree online detection method of the cracking degree online detection device for separating boron isotopes by chemical exchange method, and the method includes the following contents:

[0054] (1) According to the above-mentioned cracking degree online detection device for separating boron isotopes by chemical exchange method, the following steps are performed: Figure 1 After the detection device is assembled, dry and dehydrated anisole standard liquid (water content is less than 30 ppm) is stored in one of the standard liquid storage tanks 2, and 5% complex degree standard liquid (the molar ratio of boron trifluoride to anisole in the standard liquid is 5:100, the standard liquid is calibrated by weighing method, 3.14 grams of boron trifluoride is absorbed by 100 grams of dry anisole solution under absolute water condition, and the standard liquid with 5% complex degree is obtained) is stored in another standard storage tank 2;

[0055] (2) By adjusting the multi-channel selection valve 5, first select the dry and dehydrated anisole standard solution to flush the detection pipeline for about 1 minute, close the multi-channel selection valve 5; set the absorbance detection module 7 to the concentration mode, read the absorbance of the sample flow cell 8 and set its concentration value to 0, repeat the flushing for three times until the concentration display value is within ±0.001 each time, if it exceeds the range, repeat the flushing process; by adjusting the multi-channel selection valve 5, select to 5% complex degree standard solution, until the concentration value displayed by the absorbance detection module 7 is stable, set its value to 0.05, repeat the determination for three times, until the concentration display value is between 0.0490~0.0510 (error ±0.001), if it exceeds the range, flush the pipeline with 5% complex degree standard solution; further establish the standard working curve of absorbance and complex degree;

[0056] (3) By adjusting the multi-channel selection valve 5, guide the sample liquid in the process main pipeline 1 into the sample online introduction pipeline 6, the sample liquid first passes through the flow control valve 3, control the flow to make the liquid flow in the test pipeline smooth, then passes through the cooler 4 to cool the sample liquid to room temperature, then guide the sample liquid into the absorbance detection module 7, read the absorbance value of the sample flow cell 8, based on the standard working curve of absorbance and complex degree, determine the complex degree of the sample liquid, then according to the relationship of cracking degree = 100%-complex degree, obtain the online detection data of cracking degree; the cracking process flow control module controls the cracking process flow based on the obtained online detection data of cracking degree. For example, if the cracking degree is higher than 0.98, the main valve of the process main pipeline 1 can be controlled to be opened, if the cracking degree is lower than 0.98, the main valve is closed to make it backflow.

[0057] It should be noted that if the online detection is stopped, the multi-channel selection valve 5 can be selected to anisole standard solution to flush the test pipeline, after complete cleaning, close the multi-channel selection valve 5 and the one-way valve 10, keep the test pipeline full of anisole to avoid air entering.

[0058] In summary, the present application mainly uses spectrophotometry to detect the cracking degree of the chemical exchange method for separating boron isotopes, for example, the online detection device and method of the low-concentration boron trifluoride complex content remaining in anisole as a complexing agent, the sample liquid can realize internal circulation, and the detection of the cracking degree of the boron trifluoride anisole complex can be completed without generating waste liquid, so as to accurately control the operation parameters of the cracking process; based on the online detection result of the cracking degree, the cracking process can reduce the cracking temperature and cracking time as much as possible under the premise of achieving the cracking purpose, and reduce the occurrence of side reactions; in addition, this online detection method avoids the release of toxic gas caused by offline sampling detection, and can also simplify the process.

[0059] The application is described above by the above-mentioned embodiments to illustrate the detailed structural features of the application, but the application is not limited to the above-mentioned detailed structural features, i.e. it does not mean that the application must rely on the above-mentioned detailed structural features to be implemented. It should be understood by those skilled in the art that any improvement of the application, equivalent replacement of the components selected by the application, addition of auxiliary components, selection of specific modes, etc. all fall within the protection scope and disclosure scope of the application.

[0060] The preferred embodiments of the application are described in detail above, but the application is not limited to the specific details in the above-mentioned embodiments, and within the technical concept scope of the application, various simple modifications can be made to the technical solutions of the application, and these simple modifications all belong to the protection scope of the application.

[0061] In addition, it should be noted that each specific technical feature described in the above-mentioned specific embodiments can be combined by any suitable method without contradiction, and in order to avoid unnecessary repetition, the application will not further describe various possible combination methods.

[0062] In addition, various different embodiments of the application can also be combined arbitrarily, as long as it does not deviate from the idea of the application, and it should also be considered as disclosed by the application.

Claims

1. A method for on-line detection of the degree of cleavage of a device for on-line detection of the degree of cleavage for the separation of boron isotopes by chemical exchange, characterized in that, The cracking degree online detection device comprises a sample online introduction pipeline, an absorbance detection module and a sample online reflux pipeline connected in sequence. The inlet of the sample online introduction pipeline and the outlet of the sample online reflux pipeline are connected with the process main pipeline, thereby forming online internal circulation. A multi-channel selection valve is arranged on the sample online introduction pipeline, and other inlets of the multi-channel selection valve are connected with standard liquid storage tanks, so as to provide different standard liquids with different complexing degrees for the absorbance detection module, and establish a standard working curve of absorbance and complexing degree. The absorbance detection module is electrically connected with a cracking process flow control module corresponding to the process main pipeline, so that the cracking process flow control module finely controls the cracking process flow based on online detection data. The cracking degree online detection method comprises the following contents: By adjusting the multi-channel selection valve, the standard liquid with a known complexing degree in a certain standard liquid storage tank is introduced into the absorbance detection module, and flushing and absorbance detection are sequentially performed to obtain a group of detection data of absorbance and complexing degree; the multi-channel selection valve is adjusted again, another standard liquid storage tank is replaced, and the above operation is repeated to establish a standard working curve of absorbance and complexing degree. By adjusting the multi-channel selection valve, the sample liquid in the process main pipeline is introduced into the absorbance detection module, and flushing and absorbance detection are sequentially performed; based on the standard working curve of absorbance and complexing degree, the complexing degree of the sample liquid is determined, and then the cracking degree online detection data is obtained according to the relationship of cracking degree = 100%-complexing degree. The cracking process flow control module finely controls the cracking process flow based on the obtained cracking degree online detection data.

2. The method according to claim 1, wherein A cooler is arranged on the sample online introduction pipeline, and the cooler is arranged between the process main pipeline and the multi-channel selection valve.

3. The method according to claim 2, wherein A flow control valve is arranged on the sample online introduction pipeline, and the flow control valve is arranged between the process main pipeline and the cooler.

4. The online splitting degree detection method according to claim 1, characterized in that, The absorbance detection module comprises a sample flow cell for containing a sample solution; the outlet of the sample online introduction pipeline is in communication with the bottom of the sample flow cell; and the inlet of the sample online reflux pipeline is in communication with the top of the sample flow cell.

5. The online splitting degree detection method according to claim 1, characterized in that, The cracking degree online detection device further comprises a waste liquid collector connected with the absorbance detection module through a waste liquid collection pipeline.

6. The online splitting degree detection method according to claim 1, characterized in that, A one-way valve is arranged on the sample online reflux pipeline.

7. The online splitting degree detection method according to claim 1, characterized in that, The number of standard liquids with known complexing degrees is greater than or equal to 2, and the corresponding complexing degrees include at least two of 0%, 1%, 2%, 3%, 4% and 5%.

8. The online splitting degree detection method according to claim 1, characterized in that, The flushing is repeated at least 3 times.

9. The online splitting degree detection method according to claim 1, characterized in that, During the establishment of the standard working curve of absorbance and complexing degree, the absorbance detection is repeated at least 3 times until the error of the complexing degree is ±0.1%.

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