A continuous production control system and method for ultrapure hydrogen peroxide

Abstract

The present invention discloses a continuous production control system and method for ultrapure hydrogen peroxide, belonging to the field of ultrapure hydrogen peroxide production. The continuous production control system includes an ion exchange column, a first flow sensor, a first delivery pump, a first two-way valve, an organic matter concentration detection module, an intermediate storage tank, a second delivery pump, a multi-stage electrodialysis system, an ion concentration detection module, a second two-way valve, a filter, and an ultrapure hydrogen peroxide finished product tank. The control system also includes a data processing module, a data acquisition module, and a control execution module. The control method of the continuous production control system includes: setting the power of the first delivery pump, detecting the organic matter concentration in real time, reversely regulating and correcting the flow rate; setting the operating parameters of the multi-stage electrodialysis system; detecting the ion concentration in the primary pure hydrogen peroxide, correcting the operating parameters of the multi-stage electrodialysis system, and obtaining ultrapure hydrogen peroxide. This solution realizes dynamic regulation of the production process and long-term stable high-quality continuous production.

Description

Technical Field

[0001] The present invention relates to the field of ultrapure hydrogen peroxide production, and in particular to a continuous production control system and method for ultrapure hydrogen peroxide. Background Art

[0002] Ultrapure hydrogen peroxide is also called "electronic grade hydrogen peroxide". Ultrapure hydrogen peroxide is a blue viscous liquid. Its aqueous solution is called hydrogen peroxide. It is mainly used as a cleaning agent, etchant and photoresist remover for semiconductor silicon wafers. It can also be used for the preparation of advanced insulating layers, removal of inorganic impurities in electroplating solutions, processing of copper, copper alloys, gallium and germanium in the electronics industry, and etching and cleaning of solar silicon wafers.

[0003] Traditional hydrogen peroxide production processes often struggle to achieve continuous and stable production of ultrapure hydrogen peroxide, and suffer from deficiencies in purity control and impurity removal efficiency. During the impurity separation process, there is a lack of effective real-time monitoring and feedback control mechanisms. Therefore, a new control system and method for the continuous production of ultrapure hydrogen peroxide is urgently needed. Summary of the Invention

[0004] In view of the above-mentioned deficiencies in the prior art, the present invention provides a continuous production control system and method for ultrapure hydrogen peroxide, which promotes the continuous production of ultrapure hydrogen peroxide and ensures the quality and production efficiency of ultrapure hydrogen peroxide.

[0005] In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention is:

[0006] Provided is a continuous production control system for ultrapure hydrogen peroxide, comprising a first flow sensor installed at the liquid outlet of an ion exchange column, a first delivery pump provided between the ion exchange column and an industrial hydrogen peroxide storage tank, the first flow sensor connected to a first two-way valve, an organic matter concentration detection module provided between the flow sensor and the first two-way valve for detecting organic matter concentration data in the hydrogen peroxide, one end of the first two-way valve connected to the industrial hydrogen peroxide storage tank via a reflux pump, the other end of the first two-way valve connected to an intermediate storage tank, the intermediate storage tank connected to a multi-stage electrodialysis system via a second delivery pump, a multi-stage control valve provided at the liquid inlet of the multi-stage electrodialysis system, an ion concentration detection module and a second two-way valve provided in sequence at the liquid outlet of the multi-stage electrodialysis system, the second two-way valve being connected in sequence to a filter and an ultrapure hydrogen peroxide finished product tank, and the multi-stage control valve being used to control the passage of each stage of the electrodialysis system.

[0007] It also includes a control system, which includes a data processing module, a data acquisition module and a control execution module. The multi-stage electrodialysis system, the first flow sensor, the second flow sensor, the first delivery pump, the second delivery pump, the multi-stage control valve, the second two-way valve, the ion monitoring module, and the organic matter concentration detection module are all electrically connected to the data acquisition module; the data processing module is used to process and analyze the data collected by the data acquisition module, generate control instructions and send them to the control execution module, and the control execution module is used to control the continuous production control system to operate.

[0008] A control method for the continuous production control system of the ultrapure hydrogen peroxide is provided, comprising:

[0009] Step S1: setting the power of a first delivery pump according to the product size parameters of the ion exchange column used in the continuous production control system. The first delivery pump delivers industrial hydrogen peroxide to the ion exchange column to remove organic matter, thereby obtaining ordinary hydrogen peroxide.

[0010] Step S2: The organic matter concentration detection module detects the organic matter concentration in the ordinary hydrogen peroxide discharged from the liquid outlet of the ion exchange column in real time, evaluates whether the ordinary hydrogen peroxide is qualified, and reversely adjusts and corrects the power of the first delivery pump, adjusts the flow rate of the industrial hydrogen peroxide in the ion exchange column, and discharges qualified ordinary hydrogen peroxide into the intermediate storage tank;

[0011] Step S3: The second delivery pump extracts qualified ordinary hydrogen peroxide in the intermediate storage tank into the multi-stage electrodialysis system, and sets the operating parameters of the multi-stage electrodialysis system according to the ion concentration in the ordinary hydrogen peroxide;

[0012] Step S4: The ion detection module detects the ion concentration in the primary pure hydrogen peroxide output by the multi-stage electrodialysis system in real time, evaluates whether the primary pure hydrogen peroxide is qualified, and reversely corrects the operating parameters of the multi-stage electrodialysis system so that the qualified primary pure hydrogen peroxide is filtered through the filter to obtain ultrapure hydrogen peroxide, which is stored in the ultrapure hydrogen peroxide finished product tank.

[0013] Furthermore, it also includes:

[0014] Step S21: evaluating the quality level of ultrapure hydrogen peroxide produced in different continuous production periods based on the organic matter concentration in the ordinary hydrogen peroxide detected by the organic matter concentration detection module and the ion concentration in the primary pure hydrogen peroxide detected by the ion detection module;

[0015]

[0016] Among them, C u The organic matter concentration data of ordinary hydrogen peroxide flowing into the intermediate storage tank detected by the organic matter concentration detection module, u is the data number, U is the data quantity, c uis the ion concentration data of the ultrapure hydrogen peroxide flowing into the ultrapure hydrogen peroxide finished product tank detected by the ion detection module, γ1 and γ2 are the weights of the influence of organic matter concentration and ion concentration on the quality of ultrapure hydrogen peroxide, and Q is the quality coefficient of ultrapure hydrogen peroxide production;

[0017] Step S22: Setting the threshold Q for quality level evaluation 阈值 ;

[0018] If Q≤Q 阈值 , then the quality level of ultrapure hydrogen peroxide produced during the corresponding continuous production period is judged to be excellent;

[0019] If Q>Q 阈值 , then the quality level of the ultrapure hydrogen peroxide produced during the corresponding continuous production period is determined to be medium.

[0020] Furthermore, step S1 includes:

[0021] Step S11: Calculating the ideal flow rate l1 of industrial hydrogen peroxide entering the ion exchange column for cleaning organic matter based on the product size parameters of the ion exchange column used in the continuous production control system;

[0022]

[0023] Wherein, V is the designed resin volume in the ion exchange column, E is the exchange capacity of the resin, T is the resin regeneration cycle, C1 is the organic matter concentration when the industrial hydrogen peroxide enters the ion exchange column, and C2 is the target organic matter concentration when the industrial hydrogen peroxide leaves the ion exchange column;

[0024] Step S12: setting the power P1 of the first delivery pump according to the ideal flow rate l1;

[0025]

[0026] Wherein, ρ is the density of industrial hydrogen peroxide, g is the acceleration due to gravity, η is the efficiency of the first delivery pump, z2 and z1 are the heights of the inlet end of the ion exchange column and the outlet of the first delivery pump relative to the installation surface, p2 and p1 are the theoretical pressures of the inlet end of the ion exchange column and the outlet of the first delivery pump, s2 and s1 are the cross-sectional areas of the inlet end of the ion exchange column and the outlet of the first delivery pump, h1 is the head loss along the flow between the first delivery pump and the ion exchange column, and h2 is the local head loss of the first delivery pump.

[0027] Step S13: The control execution module controls the first delivery pump to deliver the industrial hydrogen peroxide to the ion exchange column at a power of P1. The ion exchange column removes organic matter from the industrial hydrogen peroxide and discharges it from the liquid outlet of the ion exchange column to obtain ordinary hydrogen peroxide.

[0028] Furthermore, step S2 includes:

[0029] Step S21: The organic matter concentration detection module detects the organic matter concentration C in the ordinary hydrogen peroxide discharged from the liquid outlet of the ion exchange column in real time. t , calculate the organic matter concentration C t The difference between the target organic matter concentration C2 and ΔC = C2-C t , t is the organic matter concentration C t The moment of detection;

[0030] Step S22: Setting the permissible value ΔC of the organic matter concentration error in ordinary hydrogen peroxide during the production process 误差 ;

[0031] If ΔC>ΔC 误差 , then it is determined that the ordinary hydrogen peroxide discharged from the ion exchange column is unqualified, and steps S23-S25 are executed;

[0032] If ΔC≤ΔC 误差 , then it is determined that the ordinary hydrogen peroxide discharged from the ion exchange column is qualified, and step S26 is executed;

[0033] Step S23: Calculate the flow rate v1 of ordinary hydrogen peroxide flowing in the pipeline between the liquid outlet of the ion exchange column and the first two-way valve under the ideal flow rate l1: s3 is the cross-sectional area of ​​the pipe;

[0034] Calculate the time it takes for ordinary hydrogen peroxide to flow in the pipe between the organic matter concentration detection module and the first two-way valve based on the flow rate v1 L1 is the length of the pipeline between the organic matter concentration detection module and the first two-way valve;

[0035] At time t1+t, the first two-way valve opens the passage connected to the reflux pump and closes the passage connected to the intermediate storage tank. At the same time, the reflux pump starts working and discharges unqualified ordinary hydrogen peroxide back to the industrial hydrogen peroxide storage tank.

[0036] Step S24: Calculate the organic matter concentration C t The difference between the organic matter target concentration C2 and ΔC = C t -C2, and correct the target organic matter concentration to C2-ΔC, return to step S11, and correct the power P1 of the first delivery pump;

[0037] Step S25: until the organic matter concentration detection module detects that the ion exchange column discharges qualified ordinary hydrogen peroxide, and after the interval t1, the passage connected to the reflux pump is closed, the passage connected to the intermediate storage tank is opened, and the qualified ordinary hydrogen peroxide is discharged into the intermediate storage tank;

[0038] Step S26: The first two-way valve continuously opens the passage connected to the intermediate storage tank and closes the passage connected to the reflux pump, so that the qualified ordinary hydrogen peroxide is discharged into the intermediate storage tank.

[0039] Furthermore, step S3 includes:

[0040] Step S31: The second delivery pump draws qualified ordinary hydrogen peroxide from the intermediate storage tank into the multi-stage electrodialysis system. At this time, the multi-stage electrodialysis system is powered off, and the second two-way valve opens the passage to the intermediate storage tank and closes the passage to the filter. The ion detection module detects the ion concentration in the current ordinary hydrogen peroxide.

[0041] Step S32: calculating the rated flow rate v of ordinary hydrogen peroxide in the multi-stage electrodialysis system according to the ion concentration;

[0042]

[0043] Where i is the type of ion in ordinary hydrogen peroxide, J i is the rated ion flow rate set in the multi-stage electrodialysis system, D i is the diffusion coefficient of the i-th ion, c i is the concentration of the i-th ion, x is the width of the liquid channel in the multi-stage electrodialysis system, z i is the charge of the i-th ion, F is the Faraday constant, R is the ideal gas constant, T' is the temperature of the electroosmotic environment in the multi-stage electrodialysis system, is the rated potential of the multi-stage electrodialysis system;

[0044] Step S33: Calculating the rated current I of the multi-stage electrodialysis system;

[0045]

[0046] Step S34: Adjust the power P2 of the second delivery pump so that the flow rate monitored by the second flow sensor reaches v·s4, where s4 is the cross-sectional area of ​​the pipeline between the second delivery pump and the multi-stage electrodialysis system. At the same time, the multi-stage electrodialysis system is powered on and the operating current is set to the rated current I. The second two-way valve closes the passage to the intermediate storage tank and opens the passage to the filter.

[0047] Furthermore, step S4 includes:

[0048] Step S41: After ordinary hydrogen peroxide is deionized in a multi-stage electrodialysis system, initially pure hydrogen peroxide is obtained. The ion detection module detects the ion concentration c in the initially pure hydrogen peroxide in real time. t′ , t′ is the detection ion concentration c t′ moment;

[0049] Step S42: Set the target concentration c2 of ions in the primary pure hydrogen peroxide, and calculate the target concentration c2 and the ion concentration c t′ The difference between Δc=c t′ -c2; the difference Δc and the error allowable value Δc 误差 Make comparisons;

[0050] If Δc>Δc 误差 , then it is determined that the primary pure hydrogen peroxide discharged from the multi-stage electrodialysis system is unqualified, and steps S43-S45 are executed;

[0051] If Δc≤Δc 误差 , then it is determined that the primary pure hydrogen peroxide discharged from the multi-stage electrodialysis system is qualified, and step S46 is executed;

[0052] Step S43: Second two-way valve delay Open the passage to the intermediate storage tank and close the passage to the filter to allow unqualified primary pure hydrogen peroxide to flow back to the intermediate storage tank;

[0053] Step S44: Calculating a corrected ion concentration c+Δc in the ordinary hydrogen peroxide solution based on the difference Δc. Returning to step S32, the corrected ion concentration c+Δc is used to calculate the rated flow rate v1 of the ordinary hydrogen peroxide solution in the multi-stage electrodialysis system and the rated current I1 of the multi-stage electrodialysis system, and correcting the electrodialysis process of the multi-stage electrodialysis system. s5 is the cross-sectional area of ​​the pipe between the second two-way valve and the ion detection module, and l3 is the length of the pipe between the second two-way valve and the ion detection module.

[0054] Step S45: The second two-way valve is delayed until the ion detection module detects that the primary pure hydrogen peroxide is qualified in real time. Close the passage to the intermediate storage tank and open the passage to the filter;

[0055] Step S46: The second two-way valve closes the passage to the intermediate storage tank and keeps the passage to the filter open; the initially pure hydrogen peroxide is filtered through the filter to obtain ultrapure hydrogen peroxide, which is stored in an ultrapure hydrogen peroxide finished product tank.

[0056] The beneficial effects of the present invention are as follows: this solution constructs a continuous production control system for ultrapure hydrogen peroxide and a control method suitable for continuous production. By introducing real-time organic matter and ion detection modules in the organic matter removal stage and the ion removal stage of the production system, the production quality and qualification of each production stage are evaluated in real time. The production parameters of each link of the production system can be reversely adjusted and corrected in real time based on the detection data, thereby preventing unqualified intermediate products from entering the next production stage. The production quality of ultrapure hydrogen peroxide is effectively improved in each link, dynamic regulation of the production process is achieved, and the uncertainty factors of the production system are prevented from affecting the purity of ultrapure hydrogen peroxide, thereby achieving long-term stable high-quality production. BRIEF DESCRIPTION OF THE DRAWINGS

[0057] Figure 1 This is the principle block diagram of the continuous production control system for ultrapure hydrogen peroxide. DETAILED DESCRIPTION

[0058] The specific embodiments of the present invention are described below to facilitate understanding of the present invention by those skilled in the art. However, it should be clear that the present invention is not limited to the scope of the specific embodiments. For those skilled in the art, as long as various changes are within the spirit and scope of the present invention as defined and determined by the appended claims, these changes are obvious, and all inventions and creations utilizing the concepts of the present invention are protected.

[0059] like Figure 1 As shown, a continuous production control system for ultrapure hydrogen peroxide includes a first flow sensor installed at the liquid outlet of an ion exchange column, the first flow sensor being used to monitor the flow rate of ordinary hydrogen peroxide at the liquid outlet of the ion exchange column. A first delivery pump is provided between the ion exchange column and an industrial hydrogen peroxide storage tank, the first delivery pump being used to pump industrial hydrogen peroxide into the ion exchange column. The first flow sensor is connected to a first two-way valve, and an organic matter concentration detection module is provided between the flow sensor and the first two-way valve to detect the concentration of organic matter in the hydrogen peroxide. One end of the first two-way valve is connected to the industrial hydrogen peroxide storage tank via a reflux pump. When it is detected that the organic matter concentration in the ordinary hydrogen peroxide does not meet the standard, the ordinary hydrogen peroxide is directly refluxed to the industrial hydrogen peroxide storage tank via the reflux pump for re-removal of organic matter.

[0060] The other end of the first two-way valve is connected to the intermediate storage tank, which is connected to the multi-stage electrodialysis system through a second delivery pump. The second delivery pump pumps ordinary hydrogen peroxide in the intermediate storage tank into the multi-stage electrodialysis system for electrodialysis to remove charged ions in the multi-stage electrodialysis system. The liquid inlet of the multi-stage electrodialysis system is provided with a multi-stage control valve, and the liquid outlet of the multi-stage electrodialysis system is sequentially provided with an ion concentration detection module and a second two-way valve. The second two-way valve is sequentially connected to the filter and the ultra-pure hydrogen peroxide product tank. The multi-stage control valve is used to control the path of each stage of the electrodialysis system.

[0061] It also includes a control system, which includes a data processing module, a data acquisition module and a control execution module. The multi-stage electrodialysis system, the first flow sensor, the second flow sensor, the first delivery pump, the second delivery pump, the multi-stage control valve, the second two-way valve, the ion monitoring module, and the organic matter concentration detection module are all electrically connected to the data acquisition module; the data processing module is used to process and analyze the data collected by the data acquisition module, generate control instructions and send them to the control execution module, and the control execution module is used to control the continuous production control system to operate.

[0062] The control method of the continuous production control system of the ultrapure hydrogen peroxide includes:

[0063] Step S1: The power of the first delivery pump is set according to the product size parameters of the ion exchange column used in the continuous production control system. The first delivery pump delivers industrial hydrogen peroxide to the ion exchange column to remove organic matter and obtain ordinary hydrogen peroxide. Step S1 specifically includes:

[0064] Step S11: Calculating the ideal flow rate l1 of industrial hydrogen peroxide entering the ion exchange column for cleaning organic matter based on the product size parameters of the ion exchange column used in the continuous production control system;

[0065]

[0066] Wherein, V is the designed resin volume in the ion exchange column, E is the exchange capacity of the resin, T is the resin regeneration cycle, C1 is the organic matter concentration when the industrial hydrogen peroxide enters the ion exchange column, and C2 is the target organic matter concentration when the industrial hydrogen peroxide leaves the ion exchange column;

[0067] Step S12: setting the power P1 of the first delivery pump according to the ideal flow rate l1;

[0068]

[0069] Wherein, ρ is the density of industrial hydrogen peroxide, g is the acceleration due to gravity, η is the efficiency of the first delivery pump, z2 and z1 are the heights of the inlet end of the ion exchange column and the outlet of the first delivery pump relative to the installation surface, p2 and p1 are the theoretical pressures of the inlet end of the ion exchange column and the outlet of the first delivery pump, s2 and s1 are the cross-sectional areas of the inlet end of the ion exchange column and the outlet of the first delivery pump, h1 is the head loss along the flow between the first delivery pump and the ion exchange column, and h2 is the local head loss of the first delivery pump.

[0070] Step S13: The control execution module controls the first delivery pump to deliver the industrial hydrogen peroxide to the ion exchange column at a power of P1. The ion exchange column removes organic matter from the industrial hydrogen peroxide and discharges it from the liquid outlet of the ion exchange column to obtain ordinary hydrogen peroxide.

[0071] Step S2: The organic matter concentration detection module detects the organic matter concentration in the ordinary hydrogen peroxide discharged from the liquid outlet of the ion exchange column in real time, evaluates whether the ordinary hydrogen peroxide is qualified, and reversely adjusts and corrects the power of the first delivery pump, adjusts the flow rate of the industrial hydrogen peroxide in the ion exchange column, and discharges qualified ordinary hydrogen peroxide into the intermediate storage tank. Step S2 specifically includes:

[0072] Step S21: The organic matter concentration detection module detects the organic matter concentration C in the ordinary hydrogen peroxide discharged from the liquid outlet of the ion exchange column in real time. t, calculate the organic matter concentration C t The difference between the target organic matter concentration C2 and ΔC = C2-C t , t is the organic matter concentration C t The moment of detection;

[0073] Step S22: Setting the permissible value ΔC of the organic matter concentration error in ordinary hydrogen peroxide during the production process 误差 , allowable value ΔC 误差 Indicates that the organic matter concentration in ordinary hydrogen peroxide exceeds the allowable value of the organic matter target concentration C2;

[0074] If ΔC>ΔC 误差 , then it is determined that the ordinary hydrogen peroxide discharged from the ion exchange column is unqualified, and steps S23-S25 are executed;

[0075] If ΔC≤ΔC 误差 , then it is determined that the ordinary hydrogen peroxide discharged from the ion exchange column is qualified, and step S26 is executed;

[0076] Step S23: Calculate the flow rate v1 of ordinary hydrogen peroxide flowing in the pipeline between the liquid outlet of the ion exchange column and the first two-way valve under the ideal flow rate l1: s3 is the cross-sectional area of ​​the pipe;

[0077] Calculate the time it takes for ordinary hydrogen peroxide to flow in the pipe between the organic matter concentration detection module and the first two-way valve based on the flow rate v1 L1 is the length of the pipeline between the organic matter concentration detection module and the first two-way valve;

[0078] At time t1+t, the first two-way valve opens the passage connected to the reflux pump and closes the passage connected to the intermediate storage tank. At the same time, the reflux pump starts working and discharges unqualified ordinary hydrogen peroxide back to the industrial hydrogen peroxide storage tank.

[0079] Step S24: Calculate the organic matter concentration C t The difference between the organic matter target concentration C2 and ΔC = C t -C2, and correct the target organic matter concentration to C2-ΔC, return to step S11, and correct the power P1 of the first delivery pump;

[0080] Step S25: until the organic matter concentration detection module detects that the ion exchange column discharges qualified ordinary hydrogen peroxide, and after the interval t1, the passage connected to the reflux pump is closed, the passage connected to the intermediate storage tank is opened, and the qualified ordinary hydrogen peroxide is discharged into the intermediate storage tank;

[0081] Step S26: The first two-way valve continuously opens the passage connected to the intermediate storage tank and closes the passage connected to the reflux pump, so that the qualified ordinary hydrogen peroxide is discharged into the intermediate storage tank.

[0082] Step S3: The second delivery pump extracts qualified ordinary hydrogen peroxide in the intermediate storage tank into the multi-stage electrodialysis system, and sets the operating parameters of the multi-stage electrodialysis system according to the ion concentration in the ordinary hydrogen peroxide. Step S3 specifically includes:

[0083] Step S31: The second delivery pump draws qualified ordinary hydrogen peroxide from the intermediate storage tank into the multi-stage electrodialysis system. At this time, the multi-stage electrodialysis system is powered off, and the second two-way valve opens the passage to the intermediate storage tank and closes the passage to the filter. The ion detection module detects the ion concentration in the current ordinary hydrogen peroxide.

[0084] Step S32: calculating the rated flow rate v of ordinary hydrogen peroxide in the multi-stage electrodialysis system according to the ion concentration;

[0085]

[0086] Where i is the type of ion in ordinary hydrogen peroxide, J i is the rated ion flow rate set in the multi-stage electrodialysis system, D i is the diffusion coefficient of the i-th ion, c i is the concentration of the i-th ion, x is the width of the liquid channel in the multi-stage electrodialysis system, z i is the charge of the i-th ion, F is the Faraday constant, R is the ideal gas constant, T' is the temperature of the electroosmotic environment in the multi-stage electrodialysis system, is the rated potential of the multi-stage electrodialysis system;

[0087] Step S33: Calculating the rated current I of the multi-stage electrodialysis system;

[0088]

[0089] Step S34: Adjust the power P2 of the second delivery pump so that the flow rate monitored by the second flow sensor reaches v·s4, where s4 is the cross-sectional area of ​​the pipeline between the second delivery pump and the multi-stage electrodialysis system. At the same time, the multi-stage electrodialysis system is powered on and the operating current is set to the rated current I. The second two-way valve closes the passage to the intermediate storage tank and opens the passage to the filter.

[0090] Step S4: The ion detection module detects the ion concentration of the initially pure hydrogen peroxide output by the multi-stage electrodialysis system in real time, evaluates whether the initially pure hydrogen peroxide is qualified, and reversely corrects the operating parameters of the multi-stage electrodialysis system so that the qualified initially pure hydrogen peroxide is filtered through the filter to obtain ultrapure hydrogen peroxide, which is stored in the ultrapure hydrogen peroxide finished product tank. Step S4 specifically includes:

[0091] Step S41: After ordinary hydrogen peroxide is deionized in a multi-stage electrodialysis system, initially pure hydrogen peroxide is obtained. The ion detection module detects the ion concentration c in the initially pure hydrogen peroxide in real time.t′ , t′ is the detection ion concentration c t′ moment;

[0092] Step S42: Set the target concentration c2 of ions in the primary pure hydrogen peroxide, and calculate the target concentration c2 and the ion concentration c t′ The difference between Δc=c t′ -c2; the difference Δc and the error allowable value Δc 误差 Make comparisons;

[0093] If Δc>Δc 误差 , then it is determined that the primary pure hydrogen peroxide discharged from the multi-stage electrodialysis system is unqualified, and steps S43-S45 are executed;

[0094] If Δc≤Δc 误差 , then it is determined that the primary pure hydrogen peroxide discharged from the multi-stage electrodialysis system is qualified, and step S46 is executed;

[0095] Step S43: Second two-way valve delay Open the passage to the intermediate storage tank and close the passage to the filter to allow unqualified primary pure hydrogen peroxide to flow back to the intermediate storage tank;

[0096] Step S44: Calculating a corrected ion concentration c+Δc in the ordinary hydrogen peroxide solution based on the difference Δc. Returning to step S32, the corrected ion concentration c+Δc is used to calculate the rated flow rate v1 of the ordinary hydrogen peroxide solution in the multi-stage electrodialysis system and the rated current I1 of the multi-stage electrodialysis system, and correcting the electrodialysis process of the multi-stage electrodialysis system. s5 is the cross-sectional area of ​​the pipe between the second two-way valve and the ion detection module, and l3 is the length of the pipe between the second two-way valve and the ion detection module.

[0097] Step S45: The second two-way valve is delayed until the ion detection module detects that the primary pure hydrogen peroxide is qualified in real time. Close the passage to the intermediate storage tank and open the passage to the filter;

[0098] Step S46: The second two-way valve closes the passage to the intermediate storage tank and keeps the passage to the filter open; the initially pure hydrogen peroxide is filtered through the filter to obtain ultrapure hydrogen peroxide, which is stored in an ultrapure hydrogen peroxide finished product tank.

[0099] Also includes:

[0100] Step S21: evaluating the quality level of ultrapure hydrogen peroxide produced in different continuous production periods based on the organic matter concentration in the ordinary hydrogen peroxide detected by the organic matter concentration detection module and the ion concentration in the primary pure hydrogen peroxide detected by the ion detection module;

[0101]

[0102] Among them, C u The organic matter concentration data of ordinary hydrogen peroxide flowing into the intermediate storage tank detected by the organic matter concentration detection module, u is the data number, U is the data quantity, c u is the ion concentration data of the ultrapure hydrogen peroxide flowing into the ultrapure hydrogen peroxide finished product tank detected by the ion detection module, γ1 and γ2 are the weights of the influence of organic matter concentration and ion concentration on the quality of ultrapure hydrogen peroxide, and Q is the quality coefficient of ultrapure hydrogen peroxide production;

[0103] Step S22: Setting the threshold Q for quality level evaluation 阈值 , threshold Q 阈值 Indicates the minimum reference value for the quality assessment of the ultrapure hydrogen peroxide production process, only when the quality coefficient Q exceeds the threshold Q 阈值 Can be rated as excellent.

[0104] If Q≤Q 阈值 , then the quality level of ultrapure hydrogen peroxide produced during the corresponding continuous production period is judged to be excellent;

[0105] If Q>Q 阈值 , then the quality level of the ultrapure hydrogen peroxide produced during the corresponding continuous production period is determined to be medium.

[0106] The present invention constructs a continuous production control system for ultrapure hydrogen peroxide and a control method suitable for continuous production. By introducing real-time organic matter and ion detection modules in the organic matter removal stage and the ion removal stage of the production system, the production quality and qualification of each production stage are evaluated in real time. The production parameters of each link of the production system can be reversely adjusted and corrected in real time based on the detection data, thereby preventing unqualified intermediate products from entering the next production stage. The production quality of ultrapure hydrogen peroxide is effectively improved in each link, dynamic regulation of the production process is achieved, and the purity of the ultrapure hydrogen peroxide is prevented from being affected by uncertain factors in the production system, thereby achieving long-term stable high-quality production.

Claims

1. A control method for a continuous production control system for ultrapure hydrogen peroxide, the control system comprising: a first flow sensor mounted at a liquid outlet of an ion exchange column; a first delivery pump disposed between the ion exchange column and an industrial hydrogen peroxide storage tank; the first flow sensor connected to a first two-way valve; an organic matter concentration detection module disposed between the flow sensor and the first two-way valve for detecting organic matter concentration data in the hydrogen peroxide; one end of the first two-way valve connected to the industrial hydrogen peroxide storage tank via a reflux pump; the other end of the first two-way valve connected to an intermediate storage tank; the intermediate storage tank connected to a multi-stage electrodialysis system via a second delivery pump; a multi-stage control valve disposed at a liquid inlet of the multi-stage electrodialysis system; an ion concentration detection module and a second two-way valve disposed sequentially at a liquid outlet of the multi-stage electrodialysis system; the second two-way valve connected sequentially to a filter and an ultrapure hydrogen peroxide finished product tank; the multi-stage control valve for controlling the passage of each stage of the electrodialysis system; The system further includes a control system, which includes a data processing module, a data acquisition module, and a control execution module. The multi-stage electrodialysis system, the first flow sensor, the second flow sensor, the first delivery pump, the second delivery pump, the multi-stage control valve, the second two-way valve, the ion monitoring module, and the organic matter concentration detection module are all electrically connected to the data acquisition module. The data processing module is used to process and analyze the data collected by the data acquisition module, generate control instructions, and send them to the control execution module. The control execution module is used to control the continuous production control system to operate. It is characterized by: include: Step S1: setting the power of a first delivery pump according to the product size parameters of the ion exchange column used in the continuous production control system. The first delivery pump delivers industrial hydrogen peroxide to the ion exchange column to remove organic matter, thereby obtaining ordinary hydrogen peroxide. Step S2: The organic matter concentration detection module detects the organic matter concentration in the ordinary hydrogen peroxide discharged from the liquid outlet of the ion exchange column in real time, evaluates whether the ordinary hydrogen peroxide is qualified, and reversely adjusts and corrects the power of the first delivery pump, adjusts the flow rate of the industrial hydrogen peroxide in the ion exchange column, and discharges qualified ordinary hydrogen peroxide into the intermediate storage tank; Step S3: The second delivery pump extracts qualified ordinary hydrogen peroxide in the intermediate storage tank into the multi-stage electrodialysis system, and sets the operating parameters of the multi-stage electrodialysis system according to the ion concentration in the ordinary hydrogen peroxide; Step S4: The ion detection module detects the ion concentration of the initially pure hydrogen peroxide output by the multi-stage electrodialysis system in real time, evaluates whether the initially pure hydrogen peroxide is qualified, and reversely corrects the operating parameters of the multi-stage electrodialysis system so that the qualified initially pure hydrogen peroxide is filtered through the filter to obtain ultrapure hydrogen peroxide, which is stored in an ultrapure hydrogen peroxide finished product tank; The step S1 comprises: Step S11: Calculate the ideal flow rate of industrial hydrogen peroxide entering the ion exchange column for cleaning organic matter based on the product size parameters of the ion exchange column used in the continuous production control system. l 1; ； in, V is the designed resin volume in the ion exchange column, E is the exchange capacity of the resin, T is the resin regeneration cycle, C 1 is the organic matter concentration when industrial hydrogen peroxide enters the ion exchange column, C 2 is the target concentration of organic matter when industrial hydrogen peroxide leaves the ion exchange column; Step S12: According to the ideal flow l 1. Set the power of the first delivery pump P 1; ； in, ρ is the density of industrial hydrogen peroxide, g is the acceleration due to gravity, is the efficiency of the first delivery pump, are the heights of the liquid inlet end of the ion exchange column and the outlet of the first delivery pump relative to the installation surface, are the theoretical pressures at the inlet end of the ion exchange column and the outlet of the first delivery pump, respectively. are the cross-sectional areas of the liquid inlet end of the ion exchange column and the outlet of the first delivery pump, is the head loss along the path between the first delivery pump and the ion exchange column, is the local head loss of the first delivery pump; Step S13: The control execution module controls the first delivery pump to P 1. The industrial hydrogen peroxide is transported to the ion exchange column, which removes organic matter from the industrial hydrogen peroxide and discharges it from the liquid outlet of the ion exchange column to obtain ordinary hydrogen peroxide.

2. The control method of the continuous production control system of ultrapure hydrogen peroxide according to claim 1, characterized in that, Also includes: Step S21: evaluating the quality level of ultrapure hydrogen peroxide produced in different continuous production periods based on the organic matter concentration in the ordinary hydrogen peroxide detected by the organic matter concentration detection module and the ion concentration in the primary pure hydrogen peroxide detected by the ion detection module; ； in, This is the organic matter concentration data of ordinary hydrogen peroxide flowing into the intermediate storage tank detected by the organic matter concentration detection module. u is the data number, U is the number of data, This is the ion concentration data of the ultrapure hydrogen peroxide flowing into the ultrapure hydrogen peroxide finished product tank detected by the ion detection module. are the weights of influence of organic matter concentration and ion concentration on the quality of ultrapure hydrogen peroxide, Q Quality factor for the production of ultrapure hydrogen peroxide; Step S22: Setting the threshold for quality level evaluation ; like , then the quality level of ultrapure hydrogen peroxide produced during the corresponding continuous production period is judged to be excellent; like , then the quality level of the ultrapure hydrogen peroxide produced during the corresponding continuous production period is determined to be medium.

3. The control method of the continuous production control system of ultrapure hydrogen peroxide according to claim 2, characterized in that, The step S2 comprises: Step S21: The organic matter concentration detection module detects the organic matter concentration in the ordinary hydrogen peroxide discharged from the liquid outlet of the ion exchange column in real time. C t , calculate the organic matter concentration C t Target concentration of organic matter C Difference of 2 , t Organic matter concentration C t The moment of detection; Step S22: Setting the allowable value of organic matter concentration error in ordinary hydrogen peroxide during the production process ; like , then it is determined that the ordinary hydrogen peroxide discharged from the ion exchange column is unqualified, and steps S23-S25 are executed; like , then it is determined that the ordinary hydrogen peroxide discharged from the ion exchange column is qualified, and step S26 is executed; Step S23: Calculate the ideal flow rate l 1. The flow rate of ordinary hydrogen peroxide in the pipe between the outlet of the ion exchange column and the first two-way valve under the following conditions: v 1: , s 3 is the cross-sectional area of ​​the pipe; According to flow rate v 1 Calculate the time that ordinary hydrogen peroxide flows in the pipeline between the organic matter concentration detection module and the first two-way valve , L 1 is the length of the pipeline between the organic matter concentration detection module and the first two-way valve; The first two-way valve at time Open the passage connected to the reflux pump, close the passage connected to the intermediate storage tank, and at the same time start the reflux pump to discharge the unqualified ordinary hydrogen peroxide back to the industrial hydrogen peroxide storage tank; Step S24: Calculate organic matter concentration C t Target concentration of organic matter C The difference between 2 , and correct the target concentration of organic matter to , return to step S11, correct the power of the first delivery pump P 1; Step S25: until the organic matter concentration detection module detects that the ion exchange column discharges qualified ordinary hydrogen peroxide, and within the interval time Then close the passage connected to the reflux pump, open the passage connected to the intermediate storage tank, and discharge the qualified ordinary hydrogen peroxide into the intermediate storage tank; Step S26: The first two-way valve continuously opens the passage connected to the intermediate storage tank and closes the passage connected to the reflux pump, so that the qualified ordinary hydrogen peroxide is discharged into the intermediate storage tank.

4. The control method of the continuous production control system of ultrapure hydrogen peroxide according to claim 1, characterized in that: The step S3 comprises: Step S31: The second delivery pump draws qualified ordinary hydrogen peroxide from the intermediate storage tank into the multi-stage electrodialysis system. At this time, the multi-stage electrodialysis system is powered off, and the second two-way valve opens the passage to the intermediate storage tank and closes the passage to the filter. The ion detection module detects the ion concentration in the current ordinary hydrogen peroxide. Step S32: Calculate the rated flow rate of ordinary hydrogen peroxide in the multi-stage electrodialysis system based on the ion concentration v ; ； in, i It is the type of ions in ordinary hydrogen peroxide. is the rated ion flow rate set in the multi-stage electrodialysis system, D i For the i The diffusion coefficient of the ions, c i For the i The concentration of the ions, x is the width of the liquid channel in the multi-stage electrodialysis system, z i For the i The charge of the ion, F is the Faraday constant, R is the ideal gas constant, is the temperature of the electroosmotic environment in the multi-stage electrodialysis system, is the rated potential of the multi-stage electrodialysis system; Step S33: Calculate the rated current of the multi-stage electrodialysis system I ; ； Step S34: Adjust the power of the second delivery pump P 2. Make the flow rate monitored by the second flow sensor reach , s 4 is the cross-sectional area of ​​the pipeline between the second delivery pump and the multi-stage electrodialysis system. At the same time, the multi-stage electrodialysis system is powered on and the working current is set to the rated current. I The second two-way valve closes the passage between the intermediate storage tank and opens the passage between the filter.

5. The control method of the continuous production control system of ultrapure hydrogen peroxide according to claim 4, characterized in that, The step S4 comprises: Step S41: After ordinary hydrogen peroxide is deionized in a multi-stage electrodialysis system, initially pure hydrogen peroxide is obtained. The ion detection module detects the ion concentration in the initially pure hydrogen peroxide in real time. , To detect ion concentration moment; Step S42: Setting the target concentration of ions in the primary pure hydrogen peroxide , calculate the target concentration and ion concentration The difference between ; The difference and error tolerance Make comparisons; like , then it is determined that the primary pure hydrogen peroxide discharged from the multi-stage electrodialysis system is unqualified, and steps S43-S45 are executed; like , then it is determined that the primary pure hydrogen peroxide discharged from the multi-stage electrodialysis system is qualified, and step S46 is executed; Step S43: Second two-way valve delay Open the passage to the intermediate storage tank and close the passage to the filter to allow unqualified primary pure hydrogen peroxide to flow back to the intermediate storage tank; Step S44: According to the difference Calculating the ion-corrected concentration in ordinary hydrogen peroxide , return to step S32, use ion correction concentration Calculating the Rated Flow Rate of Ordinary Hydrogen Peroxide in a Multistage Electrodialysis System v 1. Rated current of multi-stage electrodialysis system I 1. Correct the electrodialysis process of the multi-stage electrodialysis system, s 5 is the cross-sectional area of ​​the pipeline between the second two-way valve and the ion detection module, l 3 is the length of the pipeline between the second two-way valve and the ion detection module; Step S45: The second two-way valve is delayed until the ion detection module detects that the primary pure hydrogen peroxide is qualified in real time. Close the passage to the intermediate storage tank and open the passage to the filter; Step S46: The second two-way valve closes the passage to the intermediate storage tank and keeps the passage to the filter open; the initially pure hydrogen peroxide is filtered through the filter to obtain ultrapure hydrogen peroxide, which is stored in an ultrapure hydrogen peroxide finished product tank.

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