Process and apparatus for purifying electronic grade sulfur dioxide

Abstract

The application relates to the technical field of sulfur dioxide purification, in particular to a purification process and equipment for electronic-grade sulfur dioxide, which comprises the following steps: vaporizing and adsorbing industrial-grade sulfur dioxide, and obtaining the pressure, temperature and carbon dioxide concentration in the adsorption environment during the adsorption process; obtaining the adsorption effectiveness at each collection time, obtaining the detrended fluctuation sequence of each time period, and obtaining the adsorption action duration in the adsorption process of each time period; extracting the persistence loss degree of the adsorption action of the adsorber at the current collection time, which is used for judging whether the adsorption capacity of the current adsorber reaches a saturation state, so as to perform switching operation on the adsorber; filtering and rectifying the sulfur dioxide gas after adsorption by the adsorber, and obtaining electronic-grade sulfur dioxide gas products. The application can improve the adsorption purification effect of the sulfur dioxide adsorption process.

Description

Technical Field

[0001] The present application relates to the technical field of sulfur dioxide purification, and in particular to a purification process and equipment for electronic-grade sulfur dioxide. Background Art

[0002] Electronic-grade sulfur dioxide plays an important role in the manufacture of fine chemicals in the electronics industry. However, during the preparation of sulfur dioxide, industrial-grade sulfur dioxide may contain a variety of impurities, and it is often necessary to purify industrial-grade sulfur dioxide to meet the demand for high-purity sulfur dioxide in the electronics and semiconductor industries.

[0003] Chinese invention patent 202110979509.5 proposes a method for purifying high-purity electronic-grade sulfur dioxide, which includes subjecting the sulfur dioxide to three-stage water washing, deep dehydration, high-efficiency filtration, and two-stage distillation in sequence to finally produce high-purity electronic-grade sulfur dioxide. However, this method involves a relatively complicated process flow and the process operation is difficult to control, and it is unable to effectively remove various impurity components in industrial-grade sulfur dioxide.

[0004] At present, the purification process of electronic-grade sulfur dioxide can effectively remove light components such as carbon dioxide, nitrogen, and water, as well as heavy components and impurity particles through four steps: vaporization, adsorption, filtration, and distillation. At the same time, the existing process often sets up two adsorbers for the sulfur dioxide adsorption process. If the adsorption capacity of the current adsorber reaches saturation, the adsorption operation is switched to the backup adsorber to continue, ensuring the continuity of the sulfur dioxide adsorption process and the effect of adsorption purification. However, because the adsorption capacity of the adsorber can be affected by environmental factors, it is impossible to fully consider whether the adsorption capacity of the adsorber has reached saturation under the complex interference of adsorption environmental factors. As a result, it is impossible to effectively and accurately switch the adsorbers, which affects the adsorption and purification effect of the impurity components in the sulfur dioxide. Summary of the Invention

[0005] In order to solve the above technical problems, the purpose of this application is to provide a purification process and equipment for electronic grade sulfur dioxide. The technical solutions adopted are as follows:

[0006] The present invention provides a purification process for electronic-grade sulfur dioxide, comprising the following steps:

[0007] Vaporize and adsorb industrial-grade sulfur dioxide, and obtain the pressure, temperature and carbon dioxide concentration in the adsorption environment during the adsorption process;

[0008] Analyze the correlation between the change in carbon dioxide concentration within the preset time period before each collection moment and the pressure and temperature, and combine the average level of carbon dioxide concentration change to obtain the adsorption effectiveness at each collection moment;

[0009] The adsorption effectiveness at all acquisition moments is divided into adsorption effectiveness subsequences for each time period. Detrended fluctuation analysis is performed to obtain the detrended fluctuation sequence for each time period. Based on the similarity between the detrended fluctuation sequence and the adsorption effectiveness subsequence, as well as the data difference within the detrended fluctuation sequence, the adsorption duration during the adsorption process in each time period is obtained.

[0010] The adsorption duration corresponding to all time periods before the current collection moment is divided into a set of continuity losses at the current collection moment. The average level of adsorption continuity within the continuity loss set and the differences in different adsorption durations are analyzed to obtain the adsorber adsorption continuity loss at the current collection moment. This is used to determine whether the adsorption capacity of the current adsorber has reached saturation, so that the adsorber can be switched.

[0011] The sulfur dioxide gas adsorbed by the adsorber is filtered and distilled to obtain electronic grade sulfur dioxide gas product.

[0012] Preferably, the calculation method of the adsorption effectiveness at each collection moment is:

[0013] ;

[0014] Where, is the adsorption effectiveness at the tth collection moment, is the element mean in the carbon dioxide change sequence corresponding to the t-th acquisition moment, is an exponential function with a natural constant as its base, 、 are the covariances between the local pressure sequence and the local temperature sequence at the t-th acquisition moment and the carbon dioxide change sequence, respectively. The pressure, temperature, and carbon dioxide concentration at all acquisition moments are normalized, and the normalized data of pressure, temperature, and carbon dioxide concentration within a preset time period before each acquisition moment are arranged in chronological order to obtain the local pressure sequence, local temperature sequence, and local carbon dioxide concentration sequence at each acquisition moment.

[0015] Preferably, the method for obtaining the carbon dioxide change sequence is further as follows: each element in the first-order difference sequence of the local carbon dioxide concentration sequence is replaced by the absolute value of each element, and the sequence obtained after the replacement is used as the carbon dioxide change sequence.

[0016] Preferably, the method for obtaining the adsorption effectiveness subsequence of each time period is:

[0017] The adsorption effectiveness sequence at the current collection moment is extracted and evenly divided into K subsequences, corresponding to K time periods of adsorption effectiveness subsequences, where K is a preset number.

[0018] Preferably, the method for extracting the adsorption effectiveness sequence is further as follows:

[0019] The adsorption effectiveness at all collection moments before the current collection moment is arranged in chronological order to form an adsorption effectiveness sequence at the current collection moment.

[0020] Preferably, the method for obtaining the duration of the adsorption during the adsorption process in each time period is:

[0021] ;

[0022] Where, is the duration of adsorption during the k-th time period, is the number of elements in the detrended fluctuation sequence of the kth time period, is the Jaccard similarity between the adsorption effectiveness subsequence and the detrended fluctuation sequence in the kth time period, and are the jth and j-1th elements in the detrended fluctuation sequence of the kth time period, To avoid a constant with a zero denominator.

[0023] Preferably, the method for obtaining the continuity loss set at the current collection moment is:

[0024] Threshold segmentation is performed on the adsorption durations of all time periods before the current acquisition moment to obtain a segmentation threshold, and all adsorption durations below the segmentation threshold are combined into a continuity loss set at the current acquisition moment.

[0025] Preferably, the calculation method of the degree of loss of the adsorber adsorption continuity at the current collection moment is:

[0026] ;

[0027] Where, is the degree of continuous loss of adsorber adsorption at the current collection moment, is the mean value of the elements in the persistence loss set at the current acquisition moment, is the number of adsorption durations in the duration loss set at the current collection moment, and are the gth and g-1th adsorption durations in the duration loss set at the current collection moment, is an exponential function with a natural constant as its base.

[0028] Preferably, the determining whether the adsorption capacity of the current adsorber has reached a saturated state so as to switch the adsorber further includes:

[0029] If the persistence loss degree of the current collection time is greater than or equal to the preset persistence loss threshold, the adsorption capacity of the adsorber reaches a saturation state, and the adsorber is switched, otherwise, the adsorption capacity of the adsorber does not reach the saturation state, and the adsorber is not switched.

[0030] The embodiment of the present application also provides a kind of electronic grade sulfur dioxide purification equipment, including memory, processor and computer program stored in the memory and running on the processor, when the processor executes the computer program, the steps of the electronic grade sulfur dioxide purification process of any one described above are realized.

[0031] From the above, the electronic grade sulfur dioxide purification process and equipment provided by the present application at least have the following beneficial effects:

[0032] The present application analyzes the effectiveness of the adsorption of the adsorber itself, avoids the complex interference of the adsorption environment factors, and more accurately evaluates the adsorption state of the adsorber itself, which is conducive to more effectively and accurately switching the adsorber subsequently, and avoids affecting the effect of adsorption purification;

[0033] The present application fully considers the interference of adsorption environment factors on the adsorption capacity of the adsorber, and according to the change of the effectiveness of the adsorption of the adsorber itself, the trend fluctuation analysis algorithm is used to analyze the characteristics of the adsorption of the adsorber itself in different time periods, which can effectively exclude the interference of the adsorption of the adsorber itself by the adsorption environment factors, so as to more accurately judge whether the adsorption capacity of the adsorber reaches the saturation state;

[0034] The present application extracts the persistence loss set to represent the loss characteristics of the persistence of the adsorption of the adsorber, more accurately measures the persistence loss degree of the adsorption of the adsorber, and then accurately judges whether the adsorption capacity of the adsorber reaches the saturation state by using the persistence loss degree, so as to effectively and accurately switch the adsorber, and ensure the continuity of the sulfur dioxide adsorption process and the adsorption purification effect. BRIEF DESCRIPTION OF DRAWINGS

[0035] In order to more clearly illustrate the technical solutions and advantages of the embodiments of the present application or prior art, the following will briefly introduce the drawings needed in the embodiment or prior art description. Obviously, the drawings in the following description are only some embodiments of the present application, and those skilled in the art can obtain other drawings according to these drawings without creating any creative labor.

[0036] Figure 1 A step flow chart of the electronic grade sulfur dioxide purification process provided by the present application. DETAILED DESCRIPTION

[0037] To further illustrate the technical means and effectiveness of this application to achieve its intended purpose, the following, in conjunction with the accompanying drawings and preferred embodiments, details the specific implementation, structure, features, and effectiveness of an electronic-grade sulfur dioxide purification process and apparatus proposed in this application. In the following description, references to different "one embodiment" or "another embodiment" do not necessarily refer to the same embodiment. Furthermore, specific features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.

[0038] Unless otherwise specified and limited, terms such as "comprises", "includes" or any other variants thereof are intended to cover non-exclusive inclusion, so that a circuit structure, article or device comprising a series of elements includes not only those elements, but also includes other elements not explicitly listed, or also includes elements inherent to such article or device. In the absence of further restrictions, an element defined by the sentence "comprises a ..." does not exclude the presence of other identical elements in the article or device comprising the element. In addition, the term "and\or" used herein includes any and all combinations of one or more related listed items. All technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art to which this application belongs.

[0039] The specific scheme of the purification process and equipment of electronic-grade sulfur dioxide provided by the present application is described in detail below with reference to the accompanying drawings.

[0040] See also Figure 1 , which shows a flow chart of a process for purifying electronic-grade sulfur dioxide provided by one embodiment of the present application, comprising the following steps:

[0041] Step 1: Vaporize and adsorb industrial-grade sulfur dioxide, and obtain the pressure, temperature, and carbon dioxide concentration in the adsorption environment during the adsorption process.

[0042] The sulfur dioxide purification process in this embodiment involves four steps: vaporization, adsorption, filtration, and distillation. By accurately switching the adsorber during the adsorption process, light components and heavy components such as carbon dioxide, nitrogen, and water, as well as impurity particles, can be effectively removed, so that industrial-grade sulfur dioxide can be purified to 5N electronic-grade sulfur dioxide.

[0043] In this embodiment, industrial-grade sulfur dioxide is purified by vaporization, adsorption, filtration, and distillation to obtain an electronic-grade sulfur dioxide product. Preferably, the specific process in this embodiment is as follows:

[0044] S1. Vaporization: In this embodiment, the sulfur dioxide in the industrial-grade sulfur dioxide cylinder is vaporized by an electric heating blanket. The vaporization temperature of the vaporization treatment is 10-100°C, and the vaporization pressure is 0.2-1.0 MPa. In this embodiment, the preferred vaporization temperature is 40°C and the vaporization pressure is 0.5 MPa. In actual application scenarios, the implementer can set the vaporization temperature and vaporization pressure according to actual conditions.

[0045] S2, adsorption: The sulfur dioxide gas after vaporization treatment enters the adsorber, and the adsorber adsorbs impurities such as carbon dioxide and moisture contained in the sulfur dioxide gas. There are two adsorbers, namely the main adsorber and the backup adsorber. The main adsorber and the backup adsorber are equipped with pressure sensors, temperature sensors, and carbon dioxide gas detectors, which can collect the pressure, temperature, and carbon dioxide concentration in the adsorption environment in real time.

[0046] During the adsorption of vaporized sulfur dioxide, the pressure, temperature, and carbon dioxide concentration in the adsorption environment of the adsorber currently in use are collected by a data acquisition device. In this embodiment, the data collection time interval is 10 seconds. The implementer can adaptively set the collection time interval according to actual conditions to obtain the pressure, temperature, and carbon dioxide concentration at each collection moment during the adsorption process.

[0047] Step 2: Analyze the correlation between the change in carbon dioxide concentration within the preset time period before each collection moment and the pressure and temperature, and combine the average level of carbon dioxide concentration change to obtain the adsorption effectiveness at each collection moment.

[0048] Generally speaking, the adsorption capacity of an adsorber is subject to complex interference from adsorption environmental factors. For example, fluctuations in pressure and temperature in the adsorption environment can affect the thermal motion of impurity molecules in the sulfur dioxide gas, thereby affecting the adsorber's ability to adsorb impurities in the sulfur dioxide. However, this does not mean that the adsorber's adsorption capacity has reached saturation, but rather that it is subject to complex interference from adsorption environmental factors, affecting the adsorber's own adsorption capacity. Therefore, it is necessary to more accurately determine whether the adsorber's adsorption capacity has reached saturation in order to effectively and accurately switch the adsorber.

[0049] In order to avoid the influence of data dimensions between different indicators, the different indicators at all collection moments, namely pressure, temperature, and carbon dioxide concentration, are exponentially normalized. In this embodiment, the normalized data of different indicators obtained within 10 minutes before each collection moment are arranged in chronological order to obtain the local pressure sequence, local temperature sequence, and local carbon dioxide concentration sequence at each collection moment. In this embodiment, the preset time length is 10 minutes.

[0050] Furthermore, the first-order difference sequence of the local carbon dioxide concentration sequence is calculated, all elements in the first-order difference sequence are replaced by the absolute values ​​of the elements, and the result after replacement is recorded as the carbon dioxide change sequence. The data changes in the carbon dioxide change sequence reflect the level of changes in carbon dioxide impurities in the adsorber. If the correlation between the carbon dioxide change sequence and the local pressure sequence and the local temperature sequence is smaller, and if the concentration change of carbon dioxide in the adsorption environment is greater at this time, it indicates that the carbon dioxide impurities are less affected by the complex interference of the adsorption environment factors at this time, and are more affected by the adsorption effect of the adsorber itself, indicating that the adsorber can better exert its own adsorption effect at this time.

[0051] Through the above analysis, this embodiment calculates the adsorption effectiveness at each collection moment during the adsorption process:

[0052] ;

[0053] Where, is the adsorption effectiveness at the tth collection moment, is the element mean in the carbon dioxide change sequence corresponding to the t-th acquisition moment, is an exponential function with a natural constant as its base, 、 are the covariances between the local pressure sequence and the local temperature sequence at the t-th acquisition moment and the carbon dioxide change sequence, respectively. The covariance is used to reflect the degree of correlation between sequences. This embodiment uses the covariance to measure the degree of correlation. The implementer can adopt other existing correlation degree measurement methods in actual application scenarios. The covariance calculation is an existing technology and will not be described in detail in this embodiment.

[0054] Adsorption effectiveness reflects the effectiveness of the adsorption effect of the adsorber itself during the adsorption process, and to a certain extent eliminates the complex interference of adsorption environmental factors, thereby more accurately evaluating the adsorption state of the adsorber itself, which is conducive to more effective and accurate switching operations of the adsorber in the subsequent process, avoiding affecting the effect of adsorption purification.

[0055] Step 3: The adsorption effectiveness at all acquisition moments is divided into adsorption effectiveness subsequences for each time period. The detrended fluctuation sequence for each time period is obtained through detrended fluctuation analysis. Based on the similarity between the detrended fluctuation sequence and the adsorption effectiveness subsequence, as well as the data difference within the detrended fluctuation sequence, the duration of the adsorption effect during the adsorption process in each time period is obtained.

[0056] Generally speaking, the adsorption effect of the adsorber itself is characterized by continuity, while the changes in the adsorption effect under the influence of adsorption environmental factors are often characterized by transience. If the adsorption effect is more persistent during the historical adsorption process using the current adsorber, it can be clearly shown that the current adsorber still has a strong adsorption capacity, and there is no need to switch the adsorber at this time.

[0057] Furthermore, the adsorption effectiveness at all collection moments is divided into adsorption effectiveness subsequences of each time period. In this embodiment, preferably, for the current adsorber, the adsorption effectiveness at all collection moments before the current collection moment is sequenced in chronological order and recorded as the adsorption effectiveness sequence at the current collection moment. The adsorption effectiveness sequence reflects the change in adsorption effectiveness during the adsorption process using the current adsorber.

[0058] At the same time, in order to analyze the persistence characteristics of the adsorption effect in different time periods during the historical process of using the current adsorber, the adsorption effectiveness sequence at the current collection moment is evenly divided into K subsequences. If the elements in a subsequence are incomplete, the mean interpolation method is used to complete the missing elements to obtain the adsorption effectiveness subsequences of K time periods. The adsorption effectiveness subsequences reflect the persistence characteristics of the adsorption effect in different time periods, where K is a preset number. The value of K in the embodiment is 50, and the implementer can adaptively select the value according to the actual situation.

[0059] In order to more accurately extract the persistence characteristics of the adsorption effect in each time period, the adsorption effectiveness subsequence of each time period is used as the input of the DFA detrended fluctuation analysis algorithm. The DFA detrended fluctuation analysis algorithm is used to obtain the detrended fluctuation sequence corresponding to the adsorption effectiveness subsequence of each time period. In this embodiment, it is recorded as the detrended fluctuation sequence of each time period. The detrended fluctuation sequence of each time period reflects the fluctuation of the adsorption effectiveness in the adsorption process corresponding to each time period. If the fluctuation degree of the adsorption effectiveness is smaller and the similarity between the detrended fluctuation sequence and its corresponding adsorption effectiveness subsequence is greater, it indicates that the effectiveness of the adsorption effect in the adsorption process lasts longer, and the persistence of the adsorption effect played by the adsorber itself in this time period is higher, and the adsorption capacity of the adsorber is far from reaching saturation.

[0060] Through the above analysis, in this embodiment, the duration of adsorption during the adsorption process in each time period is calculated:

[0061] ;

[0062] Where, is the duration of adsorption during the k-th time period, is the number of elements in the detrended fluctuation sequence of the kth time period, is the Jaccard similarity between the adsorption effectiveness subsequence and the detrended fluctuation sequence in the kth time period. The Jaccard similarity is used to measure the similarity between sequences. In actual application, the implementer may select other existing sequence similarity measurement methods. This embodiment does not specifically limit this. This embodiment uses the Jaccard similarity to measure the similarity. The larger the Jaccard similarity, the higher the similarity between the adsorption effectiveness subsequence and the detrended fluctuation sequence in each time period. and are the jth and j-1th elements in the detrended fluctuation sequence of the kth time period, To avoid a constant with a denominator of zero, the value range is (0.001, 0.005). The value within this range has a small impact on the calculation result and can be ignored. In this embodiment, the value is 0.03.

[0063] The duration of adsorption reflects the continuous characteristics of the adsorption effect played by the adsorber itself. The greater the duration of adsorption, the higher the continuity of the adsorption effect played by the adsorber itself during this time period, and the smaller the transient characteristics of the adsorption effect played during the adsorption process. It can effectively eliminate the interference of adsorption environmental factors on the adsorption effect, thereby more accurately judging whether the adsorption capacity of the adsorber has reached saturation.

[0064] Step 4: Divide the adsorption duration corresponding to all time periods before the current collection moment to obtain the continuity loss set at the current collection moment, analyze the average level of adsorption continuity within the continuity loss set and the difference in different adsorption continuities, and obtain the continuity loss of the adsorber adsorption at the current collection moment. This is used to determine whether the adsorption capacity of the current adsorber has reached saturation so as to switch the adsorber.

[0065] If the characteristics of adsorption continuity loss appear in the historical process of using the current adsorber, it means that the adsorption capacity of the adsorber currently in use is about to reach saturation, and the greater the characteristics of adsorption continuity loss, the worse the adsorption capacity of the adsorber itself is at this time, and the adsorber should be switched to ensure the continuity of the sulfur dioxide adsorption process and the effect of adsorption purification.

[0066] Furthermore, the adsorption durations corresponding to all time periods before the current acquisition moment are input into the maximum inter-class variance algorithm, and the segmentation threshold is obtained using the maximum inter-class variance algorithm. The set consisting of all adsorption durations below the segmentation threshold is taken as the continuity loss set at the current acquisition moment. The adsorption duration represented in the continuity loss set is low, which is conducive to more accurately measuring the characteristics of the adsorption continuity loss, thereby more accurately judging whether the adsorption capacity of the adsorber has reached saturation.

[0067] Through the above analysis, this embodiment calculates the degree of loss of continuity of the adsorber adsorption at the current collection moment:

[0068] ;

[0069] Where, is the degree of continuous loss of adsorber adsorption at the current collection moment, is the mean value of the elements in the persistence loss set at the current acquisition moment, is the number of adsorption durations in the duration loss set at the current collection moment, and are the gth and g-1th adsorption durations in the duration loss set at the current collection moment, is an exponential function with a natural constant as its base.

[0070] The continuity loss degree reflects the loss characteristics of adsorption continuity during the adsorber adsorption process. The greater the continuity loss degree, the poorer the continuity of the adsorption effect of the adsorber and the more the change in the continuity of the adsorption effect tends to be stable. It also indicates that the adsorption capacity of the adsorber has reached saturation. It is necessary to switch the adsorber in a timely and accurate manner to effectively ensure the continuity of the sulfur dioxide adsorption process and the effect of adsorption purification.

[0071] Furthermore, to accurately switch adsorbers during the adsorption process, the degree of persistence loss during adsorption using the current adsorber is monitored in real time. If the persistence loss at the current acquisition moment is greater than or equal to a persistence loss threshold, the adsorber's adsorption capacity has reached saturation, and the adsorber is switched, thereby ensuring the effectiveness of the adsorption purification process. If the persistence loss at the current acquisition moment is less than the persistence loss threshold, the adsorber's adsorption capacity has not reached saturation, and the adsorber is not switched, thereby ensuring stability during the adsorption purification process. In this embodiment, the persistence loss threshold is set to 0.64.

[0072] Step 5: Filter and distill the sulfur dioxide gas after adsorption by the adsorber to obtain electronic grade sulfur dioxide gas product.

[0073] Furthermore, the following process steps are performed on the sulfur dioxide gas after adsorption by the adsorber to obtain an electronic-grade sulfur dioxide product. It should be noted that the process of filtering and distilling the adsorbed sulfur dioxide gas can be implemented through existing process flows, and implementers can choose the process they want in actual application. Preferably, the specific process of filtration and distillation in this embodiment is:

[0074] S3, Filtration: In a filter with a filter element diameter less than 0.04um and a filter element retention area greater than 2000m², the sulfur dioxide gas after adsorption by the adsorber is efficiently filtered to remove particulate matter in the sulfur dioxide gas.

[0075] S4, distillation: the filtered sulfur dioxide is successively fed into a heavy component removal tower and a light component removal tower to remove heavy components and light components in turn to obtain an electronic grade sulfur dioxide gas product. Condensers are provided on the top of the heavy component removal tower and the light component removal tower, wherein the pressure of the heavy component removal tower is stabilized at 4.3-4.5 bar. In this embodiment, the pressure of the heavy component removal tower is stabilized at 4.5 bar, and the pressure of the light component removal tower is stabilized at 4.8-5.0 bar. In this embodiment, the pressure of the light component removal tower is stabilized at 5.0 bar. The refrigerant temperature range of the condensers on the top of the heavy component removal tower and the light component removal tower is -10°C to 0°C, and -7°C in this embodiment.

[0076] Based on the same inventive concept as the above method, an embodiment of the present application also provides an electronic-grade sulfur dioxide purification device, including a memory, a processor, and a computer program stored in the memory and running on the processor. When the processor executes the computer program, the steps of any one of the above-mentioned electronic-grade sulfur dioxide purification processes are implemented.

[0077] Preferably, the electronic grade sulfur dioxide purification equipment in this embodiment further includes an electric heating blanket, a main adsorber, a spare adsorber, a pressure sensor, a temperature sensor, a carbon dioxide gas detector, a filter, a heavy component removal tower, a light component removal tower, and a condenser.

[0078] Among them, electric heating blankets are used for industrial grade The sulfur dioxide in the cylinder is vaporized; the main adsorber and the standby adsorber are used to adsorb the vaporized sulfur dioxide gas; the pressure sensor, temperature sensor, and carbon dioxide gas detector are used to collect the pressure, temperature, and carbon dioxide concentration in the adsorption environment during the adsorption process; the filter is used to filter the sulfur dioxide gas after adsorption by the adsorber; the heavy component removal tower, light component removal tower, and condenser are used to remove the heavy components and light components of the filtered sulfur dioxide in turn to obtain electronic-grade sulfur dioxide gas products.

[0079] It should be understood that the order in which the embodiments of the present application are presented is for illustrative purposes only and does not necessarily represent the superiority or inferiority of the embodiments. Furthermore, the foregoing descriptions of specific embodiments of this specification are provided. Furthermore, the processes depicted in the accompanying drawings do not necessarily require the specific order or sequential sequence shown to achieve the desired results. In certain embodiments, multitasking and parallel processing are also possible or may be advantageous.

[0080] The various embodiments in this specification are described in a progressive manner, and the same or similar parts between the various embodiments can be referred to each other. Each embodiment focuses on the differences from other embodiments.

[0081] The above content is only an implementation method of the present application and is not intended to limit the scope of the present application. Any equivalent structure or equivalent process transformation made using the contents of the present application specification and drawings, or directly or indirectly applied in other related technical fields, are also included in the scope of protection of the present application.

Claims

1. A process for purifying electronic grade sulfur dioxide, characterized in that: The following steps are involved: Vaporize and adsorb industrial-grade sulfur dioxide, and obtain the pressure, temperature and carbon dioxide concentration in the adsorption environment during the adsorption process; Analyze the correlation between the change in carbon dioxide concentration within the preset time period before each collection moment and the pressure and temperature, and combine the average level of carbon dioxide concentration change to obtain the adsorption effectiveness at each collection moment; The adsorption effectiveness at all acquisition moments is divided into adsorption effectiveness subsequences for each time period. Detrended fluctuation analysis is performed to obtain the detrended fluctuation sequence for each time period. Based on the similarity between the detrended fluctuation sequence and the adsorption effectiveness subsequence, as well as the data difference within the detrended fluctuation sequence, the adsorption duration during the adsorption process in each time period is obtained. The adsorption duration corresponding to all time periods before the current collection moment is divided into a set of continuity losses at the current collection moment. The average level of adsorption continuity within the continuity loss set and the differences in different adsorption durations are analyzed to obtain the adsorber adsorption continuity loss at the current collection moment. This is used to determine whether the adsorption capacity of the current adsorber has reached saturation, so that the adsorber can be switched. The sulfur dioxide gas after adsorption by the adsorber is filtered and distilled to obtain electronic grade sulfur dioxide gas product; The calculation method of the adsorption effectiveness at each collection moment is: ； Where, is the adsorption effectiveness at the tth collection moment, is the element mean in the carbon dioxide change sequence corresponding to the t-th acquisition moment, is an exponential function with a natural constant as its base, 、 are the covariances between the local pressure sequence and the local temperature sequence at the t-th acquisition moment and the carbon dioxide change sequence, respectively. The pressure, temperature, and carbon dioxide concentration at all acquisition moments are normalized, and the normalized data of pressure, temperature, and carbon dioxide concentration within a preset time period before each acquisition moment are arranged in chronological order to obtain the local pressure sequence, local temperature sequence, and local carbon dioxide concentration sequence at each acquisition moment. The method for obtaining the duration of the adsorption during the adsorption process in each time period is as follows: ； Where, is the duration of adsorption during the k-th time period, is the number of elements in the detrended fluctuation sequence of the kth time period, is the Jaccard similarity between the adsorption effectiveness subsequence and the detrended fluctuation sequence in the kth time period, and are the jth and j-1th elements in the detrended fluctuation sequence of the kth time period, To avoid constants with zero denominators; The calculation method of the degree of loss of the adsorber adsorption continuity at the current collection moment is: ； Where, is the degree of continuous loss of adsorber adsorption at the current collection moment, is the mean value of the elements in the persistence loss set at the current acquisition moment, is the number of adsorption durations in the duration loss set at the current collection moment, and are the gth and g-1th adsorption durations in the duration loss set at the current collection moment, is an exponential function with a natural constant as its base.

2. The process for purifying electronic grade sulfur dioxide according to claim 1, wherein: The method for obtaining the carbon dioxide change sequence further comprises: replacing each element in the first-order difference sequence of the local carbon dioxide concentration sequence with the absolute value of each element, and using the sequence obtained after the replacement as the carbon dioxide change sequence.

3. The process for purifying electronic grade sulfur dioxide according to claim 1, wherein: The method for obtaining the adsorption effectiveness subsequence of each time period is as follows: The adsorption effectiveness sequence at the current collection moment is extracted and evenly divided into K subsequences, corresponding to K time periods of adsorption effectiveness subsequences, where K is a preset number.

4. The process for purifying electronic grade sulfur dioxide according to claim 3, wherein: The method for extracting the adsorption effectiveness sequence is further as follows: The adsorption effectiveness at all collection moments before the current collection moment is arranged in chronological order to form an adsorption effectiveness sequence at the current collection moment.

5. The process for purifying electronic grade sulfur dioxide according to claim 1, wherein: The method for obtaining the continuity loss set at the current collection moment is: Threshold segmentation is performed on the adsorption durations of all time periods before the current acquisition moment to obtain a segmentation threshold, and all adsorption durations below the segmentation threshold are combined into a continuity loss set at the current acquisition moment.

6. The process for purifying electronic grade sulfur dioxide according to claim 1, wherein: The determining whether the adsorption capacity of the current adsorber has reached a saturated state so as to switch the adsorber further includes: If the persistence loss degree at the current collection moment is greater than or equal to the preset persistence loss threshold, the adsorber's adsorption capacity reaches saturation and the adsorber is switched; otherwise, the adsorber's adsorption capacity does not reach saturation and the adsorber is not switched.

7. An electronic grade sulfur dioxide purification device, comprising a memory, a processor, and a computer program stored in the memory and running on the processor, characterized in that: When the processor executes the computer program, the steps of the electronic-grade sulfur dioxide purification process as described in any one of claims 1 to 6 are implemented.

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