CN113551944A - System and method for monitoring acidity of oxidizing liquid in device for producing hydrogen peroxide by anthraquinone process - Google Patents

System and method for monitoring acidity of oxidizing liquid in device for producing hydrogen peroxide by anthraquinone process Download PDF

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Publication number
CN113551944A
CN113551944A CN202010329100.4A CN202010329100A CN113551944A CN 113551944 A CN113551944 A CN 113551944A CN 202010329100 A CN202010329100 A CN 202010329100A CN 113551944 A CN113551944 A CN 113551944A
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acidity
monitoring
hydrogen peroxide
oxidizing solution
producing hydrogen
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张帆
贾学五
王振刚
刘静如
钱亚男
徐伟
石宁
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/02Devices for withdrawing samples
    • G01N1/10Devices for withdrawing samples in the liquid or fluent state
    • G01N1/14Suction devices, e.g. pumps; Ejector devices
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38Diluting, dispersing or mixing samples
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • G01N31/162Determining the equivalent point by means of a discontinuity
    • G01N31/164Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/02Devices for withdrawing samples
    • G01N1/10Devices for withdrawing samples in the liquid or fluent state
    • G01N2001/1031Sampling from special places

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Abstract

The invention discloses a monitoring system for the acidity of oxidizing liquid in a device for producing hydrogen peroxide by an anthraquinone process, which comprises the following components: a sampling line connected to a sampling port of the oxidizing liquid; and a detection unit including: an analysis pool for stirring and mixing pure water and the oxidation liquid passing through the sampling pipeline and standing and separating into an aqueous phase and an organic phase; and the detection component is used for detecting the acidity value of the water phase obtained by standing separation in the analysis pool. The invention also discloses a method for monitoring the acidity of the oxidizing liquid in the device for producing hydrogen peroxide by the anthraquinone process. The invention realizes the on-line monitoring of the acidity of the oxidizing liquid in the device for producing hydrogen peroxide by the anthraquinone method through on-line sampling, separation and detection, and improves the safety of the device.

Description

System and method for monitoring acidity of oxidizing liquid in device for producing hydrogen peroxide by anthraquinone process
Technical Field
The invention relates to the technical field of hydrogen peroxide production, in particular to a system and a method for monitoring the acidity of an oxidizing solution in a device for producing hydrogen peroxide by an anthraquinone method.
Background
Hydrogen peroxide is one of the main basic chemical products in the world, has oxidation and sterilization effects, can be used as a strong oxidant, a bleaching agent, a disinfectant, a deoxidizer and the like, and is widely applied to the industries of chemical industry, textile industry, papermaking industry, military, electronics industry, medicine industry and the like. However, hydrogen peroxide is a hazardous product, and the safety of the production apparatus is particularly important. The anthraquinone process is the primary method for producing hydrogen peroxide. The anthraquinone process uses anthraquinone compounds as hydrogen carriers to react hydrogen with oxygen to produce aqueous hydrogen peroxide, i.e., hydrogen peroxide. The anthraquinone process has high automation control degree, low product cost and low energy consumption, and is suitable for large-scale production. The main production processes of the hydrogen peroxide comprise a hydrogenation process, an oxidation process, an extraction process and a purification process. Hydrogen peroxide is easily decomposed under the condition of low acidity, which affects the process quality and even causes accidents, so the acidity of the oxidation liquid system needs to be controlled to prevent the acidity from being too low. At present, the operation danger is large, the time consumption is long, the online monitoring cannot be realized, and the safety of the device is influenced mainly by a manual offline sampling and measuring method.
Therefore, there is a need for an automatic on-line analysis technique to improve the analysis efficiency of monitoring the acidity of the oxidation solution, so as to improve the safety of the hydrogen peroxide production equipment.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
An object of the present invention is to provide a system and a method for monitoring the acidity of an oxidizing solution in an apparatus for producing hydrogen peroxide by an anthraquinone method, which can more efficiently monitor the acidity of the oxidizing solution in the apparatus on-line, thereby improving the safety of the apparatus.
In order to achieve the above object, according to a first aspect of the present invention, there is provided a system for monitoring the acidity of an oxidizing solution in an apparatus for producing hydrogen peroxide by an anthraquinone process, comprising: a sampling line connected to a sampling port of the oxidizing liquid; and a detection unit including: an analysis pool for stirring and mixing pure water and the oxidation liquid passing through the sampling pipeline and standing and separating into an aqueous phase and an organic phase; and the detection component is used for detecting the acidity value of the water phase obtained by standing separation in the analysis pool.
Further, in the above technical solution, the detecting component includes: an electrode assembly and a burette, the detection assembly being movable up and down relative to the analysis cell.
Further, in the above technical scheme, the monitoring system for the acidity of the oxidizing solution in the device for producing hydrogen peroxide by the anthraquinone method further comprises: a buffer cell connected between a sampling line and the analysis cell.
Further, in the above technical solution, the buffer tank includes a stirring portion.
Further, in the above technical scheme, the analysis cell extracts the oxidation liquid in the buffer cell through a sample injection metering pump.
Further, in the above technical scheme, a sampling metering pump is arranged on the sampling pipeline, and the analysis pool extracts the pure water through the pure water metering pump.
Further, in the above technical scheme, the pure water is distilled water, deionized water or high-purity water.
Further, in the above technical scheme, the analysis cell adopts mechanical stirring or magnetic stirring.
Further, in the above technical scheme, the monitoring system for the acidity of the oxidizing solution in the device for producing hydrogen peroxide by the anthraquinone method further comprises: a drain line and a flush line.
Further, in the above technical scheme, the monitoring system for the acidity of the oxidizing solution in the device for producing hydrogen peroxide by the anthraquinone method further comprises: a control unit arranged for controlling the sampling line and the detection unit.
According to a second aspect of the present invention, the present invention provides a monitoring method for acidity of an oxidation liquid in a hydrogen peroxide production plant by an anthraquinone process, the monitoring method adopts a monitoring system for acidity of an oxidation liquid in a hydrogen peroxide production plant by an anthraquinone process according to any one of the above technical solutions, the monitoring method at least comprises the following steps: extracting the oxidizing liquid; stirring and mixing the extracted oxidation liquid and pure water in the analysis pool to form a mixed liquid; standing the mixed solution to separate the mixed solution into a water phase and an organic phase; and detecting the acidity value of the water phase obtained by standing separation in the analysis pool.
Further, in the above technical scheme, the acidity value of the water phase obtained by standing separation in the detection and analysis cell is measured by potentiometric titration.
Further, in the above technical solution, before the stirring and mixing step, the oxidizing solution is subjected to a buffering step.
Further, in the above technical solution, the buffering step includes stirring the oxidizing solution.
Further, in the above technical scheme, the method for monitoring the acidity of the oxidizing solution in the device for producing hydrogen peroxide by the anthraquinone process further comprises the steps of: after each detection, emptying the monitoring system; and one or more washing steps.
Further, in the above technical scheme, the method for monitoring the acidity of the oxidizing solution in the device for producing hydrogen peroxide by the anthraquinone process further comprises the steps of: setting an acidity threshold; and issuing an alarm signal when the detected acidity value is lower than the acidity threshold value.
Further, in the above technical solution, the monitoring method is continuous monitoring or timed monitoring.
Compared with the prior art, the invention has the following beneficial effects:
1. the on-line monitoring of the acidity of the oxidizing liquid in the device for producing hydrogen peroxide by the anthraquinone method is realized by on-line sampling, separation and detection, and the safety of the device is improved.
2. The monitoring system does not need to be provided with a stirring and separating device independently, and has simple structure and low manufacturing and maintenance cost.
3. Oxidizing liquid and pure water can be accurately extracted through the metering pump, so that the accuracy of a detection result is higher.
4. Through flowing back pipeline and flushing line, can the automatic evacuation with wash, avoid the residual influence that detects last time, make the result more accurate.
5. And automatic safety control of the acidity of the oxidation liquid is realized by setting of chain alarm and the like, so that production accidents are avoided.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood and to make the technical means implementable in accordance with the contents of the description, and to make the above and other objects, technical features, and advantages of the present invention more comprehensible, one or more preferred embodiments are described below in detail with reference to the accompanying drawings.
Drawings
Fig. 1 is a schematic view of a system for monitoring the acidity of an oxidizing liquid in a hydrogen peroxide production plant by an anthraquinone process according to an embodiment of the present invention.
Fig. 2 is a schematic view of a monitoring system for acidity of an oxidizing liquid in a hydrogen peroxide production plant by an anthraquinone process according to another embodiment of the present invention.
Description of the main reference numerals:
the device comprises a 100-anthraquinone method hydrogen peroxide production device, a 110-sampling pipeline, a 111-sampling metering pump, a 120-pure water source, a 121-pure water metering pump, a 150-detection unit, a 151-analysis pool, a 152-electrode assembly, a 153-burette, a 154-titration pump, a 160-titrant, a 170-liquid discharge pipeline, a 171-liquid discharge pump and a 190-control unit;
the device comprises a 200-anthraquinone method hydrogen peroxide production device, 210-sampling pipelines, 211-sampling metering pumps, 220-pure water sources, 221-pure water metering pumps, 230-buffer tanks, 241-sample feeding metering pumps, 250-detection units, 251-analysis tanks, 252-electrode assemblies, 253-burettes, 254-titration pumps, 260-titrating agents, 270-liquid discharge pipelines, 271-liquid discharge pumps and 290-control units.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
Spatially relative terms, such as "below," "lower," "upper," "above," "upper," and the like, may be used herein for ease of description to describe one element or feature's relationship to another element or feature in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the object in use or operation in addition to the orientation depicted in the figures. For example, if the items in the figures are turned over, elements described as "below" or "beneath" other elements or features would then be oriented "above" the elements or features. Thus, the exemplary term "below" can encompass both an orientation of below and above. The article may be otherwise oriented (rotated 90 degrees or at other orientations) and the spatially relative terms used herein should be interpreted accordingly.
In this document, the terms "first", "second", etc. are used to distinguish two different elements or portions, and are not used to define a particular position or relative relationship. In other words, the terms "first," "second," and the like may also be interchanged with one another in some embodiments.
As shown in FIG. 1, a monitoring system according to an embodiment of the present invention is used for monitoring the acidity of an oxidizing solution in an apparatus 100 for producing hydrogen peroxide by an anthraquinone process, and the monitoring system includes a sampling section, a separating section and a detecting section. The sampling line 110 is connected to a sampling port of the oxidation liquid, which may be an existing manual sampling port (not shown), so as to extract the oxidation liquid. The detection unit 150 includes an analysis cell 151 for stirring and mixing pure water with the oxidation liquid passing through the sampling line 110 and standing to separate into an aqueous phase and an organic phase, and a detection module for detecting an acidity value of the aqueous phase obtained by the standing separation in the analysis cell 151.
Illustratively, in one or more embodiments of the present invention, the detection unit 150 may employ a potentiometric titration method to detect the acidity value of the aqueous phase in the analysis cell 151. The detection assembly may include an electrode assembly 152 and a burette 153, both the electrode assembly 152 and the burette 153 being movable up and down relative to the analysis cell 151. After the oxidizing solution and the pure water in the analyzing cell 151 have been mixed by stirring and allowed to stand to separate into an aqueous phase and an organic phase, the electrode assembly 152 and the burette 153 are immersed below the interface between the aqueous phase and the organic phase of the analyzing cell 151, a titrant 160 such as a sodium hydroxide solution is dropped from the burette 153, the analyzing cell 151 automatically starts stirring, the stirring speed is controlled to ensure that the titrant is rapidly dispersed in the aqueous phase while preventing the aqueous phase and the organic phase from being excessively mixed, and the acidity value is obtained by the potential change of the electrode assembly 152. Illustratively, the detection assembly further includes a titration pump 154 that automatically controls the amount of the titration.
Further, in one or more exemplary embodiments of the present invention, the oxidizing liquid and the pure water are precisely extracted and injected into the analyzing cell 151 by the sampling metering pump 111 and the pure water metering pump 121 provided on the sampling line 110. Illustratively, the pure water metering pump 121 may pump pure water from the pure water source 120. In one or more embodiments of the present invention, the pure water may be, for example, distilled water, deionized water, or high purity water, and it is to be understood that the present invention is not limited thereto.
Further, in one or more exemplary embodiments of the present invention, the analysis cell 151 may employ mechanical stirring or magnetic stirring, and the present invention is not limited thereto.
Preferably, but not by way of limitation, in one or more exemplary embodiments of the invention, the system for monitoring the acidity of the oxidizing solution in the plant for producing hydrogen peroxide by the anthraquinone process further comprises a drain line 170. The analysis cell 151 is illustratively connected to a drain line 170 via a drain valve (not shown) through which the monitoring system can be drained when a test procedure is completed. Illustratively, a drain pump 171 is provided on the drain line 170 to drain the monitoring system as much as possible to avoid affecting the next detection process. Preferably, but not limitatively, the detecting unit 150 may further be provided with a flushing line, and after the detection is completed, the detecting unit may be cleaned with pure water once or more times through the flushing line to ensure the accuracy of the next detection process.
Further, in one or more exemplary embodiments of the present invention, the monitoring system further includes a control unit 190. The control unit 190 can automatically control the monitoring system, for example, the sampling metering pump 111, the pure water metering pump 121, the detection unit 150, the drain pump 171, and the like on the sampling line 110 by a preset program, parameters, and the like.
Referring to fig. 1, the method for monitoring the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process according to the embodiment of the present invention at least comprises the following steps: extracting an oxidizing solution; stirring and mixing the extracted oxidation liquid and pure water in an analysis tank 151 to form a mixed liquid; standing the mixed solution to separate the mixed solution into a water phase and an organic phase; and detecting the acidity value of the aqueous phase obtained by the standing separation in the analysis cell 151.
Further, in one or more exemplary embodiments of the present invention, the acidity value of the aqueous phase obtained by the stationary separation in the detection analysis cell 151 is measured by potentiometric titration.
Further, in one or more exemplary embodiments of the present invention, the method for monitoring the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process further comprises the steps of: after each detection, emptying the monitoring system; and one or more washing steps.
Further, in one or more exemplary embodiments of the present invention, the method for monitoring the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process further comprises the steps of: setting an acidity threshold; and when the detected acidity value is lower than the acidity threshold value, sending an alarm signal to avoid that the acidity value is too low to influence the process quality or cause production accidents. Illustratively, the acidity threshold may be set at 0.01, it being understood that the invention is not so limited. Too high acidity value of the oxidizing liquid may also affect the acidity of the hydrogen peroxide finished product, and for example, a maximum acidity value alarm may be set, for example, when the acidity value of the oxidizing liquid is greater than 2, an alarm signal is sent, and the invention is not limited thereto.
Further, in one or more exemplary embodiments of the present invention, the monitoring method is continuous monitoring or timed monitoring.
Referring to fig. 2, a monitoring system for monitoring the acidity of an oxidizing solution in an apparatus 200 for producing hydrogen peroxide by an anthraquinone process according to another embodiment of the present invention includes a sampling part, a separating part and a detecting part. The sampling line 210 is connected to a sampling port of the oxidation liquid, which may be an existing manual sampling port (not shown), so as to extract the oxidation liquid to be injected into the buffer tank 230 or directly into the detection unit 250. When the process fluctuates or is adjusted, the analysis frequency of single sampling needs to be increased, the pipeline provided with the buffer pool 230 is started, and the oxidation liquid sampled once in the buffer pool 230 can carry out multiple parallel tests, so that the detection accuracy is improved; during the steady operation period of the device, the buffer pool 230 is bypassed, and the oxidizing liquid is directly injected into the detection unit 250, so as to improve the analysis efficiency. The detection unit 250 includes an analysis cell 251 and a detection member. When the buffer pool 230 is started, the sampling pipeline 210 extracts the oxidizing solution and injects the oxidizing solution into the buffer pool 230, the oxidizing solution in the buffer pool 230 is injected into the analysis pool 251 in a plurality of times, and the pure water and the oxidizing solution are stirred and mixed in the analysis pool 251 and are kept stand to separate into an aqueous phase and an organic phase. When the line not including the buffer cell 230 is activated, the sampling line 210 extracts the oxidizing solution and directly injects the oxidizing solution into the analyzing cell 251, and pure water and the oxidizing solution are stirred and mixed in the analyzing cell 251 and are left to stand to separate into an aqueous phase and an organic phase. The detection component is used for detecting the acidity value of the water phase obtained by standing separation in the analysis cell 251. For example, the two detection schemes of switching whether to have the buffer pool 230 may be implemented by providing a valve on the pipeline, and the invention is not limited thereto. Preferably, but not limitatively, the buffer tank 230 includes a stirring part, which can maintain the uniformity of the system, otherwise, the oxidation liquid may contain trace amount of water, and may be layered if left for a long time, which may affect the detection result. Illustratively, the stirring portion of the buffer tank 230 may be mechanically stirred or magnetically stirred, and the invention is not limited thereto.
Illustratively, the volume of the buffer pool 230 may be 100-1000 ml. The volume of the analysis cell 251 may be 10 to 500ml, but the invention is not limited thereto.
Further, in one or more exemplary embodiments of the present invention, the oxidation liquid is precisely extracted and injected into the buffer cell 230 by the sampling metering pump 211 provided on the sampling line 210, the oxidation liquid in the buffer cell 230 is precisely extracted and injected into the analysis cell 251 by the sampling metering pump 241, and pure water is precisely extracted and injected into the analysis cell 251 by the pure water metering pump 221. Illustratively, the pure water metering pump 221 may draw pure water from the pure water source 220. In one or more embodiments of the present invention, the pure water may be, for example, distilled water, deionized water, or high purity water, and it is to be understood that the present invention is not limited thereto.
Further, in one or more exemplary embodiments of the present invention, the analysis cell 251 may employ mechanical stirring or magnetic stirring, and the present invention is not limited thereto.
Preferably, but not limitatively, in one or more exemplary embodiments of the invention, the monitoring system is further provided with a drain line 270. Illustratively, the buffer 230 may be in communication with the drain line 270 through a first drain valve (not shown), and the detection unit 250 may be in communication with the drain line 270 through a second drain valve (not shown), wherein the first drain valve and the second drain valve are opened to drain the monitoring system after the detection process of one sampling is completed. A drain pump 271 is also provided, for example, on the drain line 270 to drain the monitoring system as much as possible to avoid affecting the next detection process. Preferably, but not limitatively, the detection unit 250 may also be provided with a flushing line for flushing the detected detection unit 250. Illustratively, the flush line may be connected to a pure water source 220, with one or more purges with pure water to ensure accuracy of the next testing procedure.
Further, in one or more exemplary embodiments of the present invention, the monitoring system of the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process further includes a control unit 290. The control unit 290 can automatically control the monitoring system, for example, the sampling metering pump 211, the pure water metering pump 221, the buffer pool 230, the sample metering pump 241, the detection unit 250, the drain pump 271, etc., on the sampling pipeline 210 by preset programs and parameters.
Referring to fig. 2, the method for monitoring the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process according to the embodiment of the present invention comprises the following steps: extracting an oxidizing solution; stirring and mixing the extracted oxidizing solution and pure water in the analysis tank 251 to form a mixed solution; standing the mixed solution to separate the mixed solution into a water phase and an organic phase; and detecting the acidity value of the aqueous phase obtained by the standing separation in the analysis cell 251.
Further, in one or more exemplary embodiments of the present invention, the oxidizing liquid is subjected to a buffering step before the agitation mixing step. Illustratively, the extracted oxidizing liquid is buffered in the buffer pool 230, the oxidizing liquid in the buffer pool 230 is extracted, and the extracted buffered oxidizing liquid and pure water are stirred and mixed in the analyzing pool 251 to form a mixed liquid.
Preferably, but not limitatively, in one or more exemplary embodiments of the invention, the buffering step comprises stirring the oxidizing liquid.
Further, in one or more exemplary embodiments of the present invention, the acidity value of the aqueous phase separated by standing in the detection analysis cell 251 is measured by potentiometric titration.
Further, in one or more exemplary embodiments of the present invention, the method for monitoring the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process further comprises the steps of: after each detection, emptying the monitoring system; and one or more washing steps.
Referring to fig. 2, when the buffer tank 230 is used, the operation flow of the system for monitoring the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process according to the present invention is as follows:
1. the sampling metering pump 211 extracts a certain amount of oxidizing liquid from the device for producing hydrogen peroxide by the anthraquinone process to be tested and injects the oxidizing liquid into the buffer pool 230, and after the completion, the buffer pool 230 starts stirring. The amount of the extracted oxidizing solution and the stirring time can be set and adjusted according to the process conditions.
2. After the stirring of the buffer pool 230 is stopped for 10-15 s, the quantitative oxidation liquid is extracted from the buffer pool 230 by the sample injection metering pump 241 and injected into the analysis pool 251.
3. The pure water metering pump 21 pumps a fixed amount of pure water and injects it into the analyzing cell 251 while stirring and mixing are being performed. The amount of the pure water to be extracted can be set and adjusted according to the process condition.
4. After the injection of the oxidizing solution and the pure water is finished, the mixture is continuously stirred for a certain time, which can be set according to the requirement.
5. After the mixed solution is formed by stirring and mixing, standing and layering for a certain time, wherein the time can be set independently according to different systems.
6. And after the standing separation is finished, the detection component detects the acidity of the water phase solution in the analysis pool.
7. When potentiometric titration is adopted for detection, the electrode assembly 252 and the burette 253 of the detection assembly move downwards and are immersed below the interface of the water phase and the organic phase in the analysis cell 251, stirring is automatically started, then the titrant is dripped, the potential change is automatically recorded, and the acidity value is calculated.
8. After the titration detection is completed, the electrode assembly 252 and the burette 253 are lifted, the washing is automatically started by pure water, after the washing is completed, the washing pipeline is closed, and the drain valve of the analysis cell 251 is opened to drain the waste liquid.
9. And repeatedly executing the washing step according to the setting, and finishing a detection process after the washing is finished.
10. And starting the parallel detection of the current sampling or starting the next sampling and the detection process thereof according to the setting.
The following describes the system and method for monitoring the acidity of the oxidation liquid in the apparatus for producing hydrogen peroxide by anthraquinone process in more detail by way of specific examples, which should be understood that the examples are only illustrative and the invention is not limited thereto.
Example 1
Referring to fig. 1, the monitoring system of the present example was used to monitor the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process.
In this example, 2ml of the oxidizing solution and 20ml of pure water were extracted and injected into the analyzing cell 151 for each measurement. After the sample injection is completed, the analytical cell 151 is continuously stirred for 30s, and is kept standing for 30s for layering. The acidity value of the aqueous phase solution separated in the analysis cell 151 is detected by the detection unit. After each test was completed, the cells were washed 8 times. The present embodiment is configured to perform continuous detection, that is, after one detection process is completed, the next detection process is automatically started.
When the device runs for 800h, 9000 times of detection are completed, long-period and high-frequency online monitoring is realized, and the safety of the device is improved.
Example 2
Referring to fig. 1, the monitoring system of the present example was used to monitor the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process.
In this example, 3ml of the oxidizing solution and 15ml of pure water were extracted and injected into the analyzing cell 151 for each measurement. After the sample injection is completed, the analytical cell 151 is continuously stirred for 20s, and is kept standing for layering for 20 s. The acidity value of the aqueous phase solution separated in the analysis cell 151 is detected by the detection unit. After each test was completed, the test was washed three times. In this example, the detection was performed every 1 hour.
The monitoring system of the embodiment realizes the on-line monitoring of the acidity of the oxidizing liquid in the device for producing hydrogen peroxide by the anthraquinone method, and improves the safety of the device.
Example 3
Referring to fig. 2, the monitoring system of the present example was used to monitor the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process.
In this embodiment, 100ml of the oxidation liquid is drawn into the buffer pool 230 for each sampling, and 20ml of the oxidation liquid is drawn from the buffer pool 230 and 20ml of pure water is drawn into the analysis pool 251 for each testing. After the sample injection is completed, the analysis cell 251 continues to stir for 25s, and stands for 25s for layering. The detection unit 250 of the present embodiment employs potentiometric titration detection. After each test, the cell was rinsed three times. Three replicates were run for each sample. The present embodiment is configured as continuous detection, that is, after three detection processes of one sampling are completed, the next sampling and detection processes thereof are automatically started.
When this embodiment runs 800h, accomplish 9000 times sample and detection altogether, realized long period, high-frequency on-line monitoring, improved the security of device to many times parallel detection has improved the degree of accuracy of monitoring.
Example 4
Referring to fig. 2, the monitoring system of the present example was used to monitor the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process.
In this embodiment, when the pipeline provided with the buffer pool 230 is started, 100ml of the oxidation liquid is extracted into the buffer pool 230 every time sampling, 20ml of the oxidation liquid is extracted from the buffer pool 230 and 20ml of pure water is extracted and injected into the analysis pool 251 every time detection is performed, and parallel detection is performed three times every sampling. When the tube without the buffer cell 230 is started, 2ml of the oxidation liquid is directly extracted and 10ml of pure water is extracted and injected into the analysis cell 251 for each test. After each sample injection, the analysis cell 251 continues to stir for 25s, and stands for 25s for layering. The detection unit 250 of the present embodiment employs potentiometric titration detection. After each test, the cell was rinsed three times. In this embodiment, the pipeline with the buffer pool 230 is started at the initial stage of operation, and continuous detection is performed, that is, after three detection processes of one sampling are completed, the next sampling and detection processes are automatically started; after 24 hours of operation or manual setting, the pipeline without the buffer pool 230 is started, and detection is performed every 1 hour.
The embodiment realizes the long-period and high-frequency online monitoring and improves the safety of the device. In the initial running stage, a buffer pool is adopted, and multiple parallel detections are carried out, so that the monitoring accuracy is improved; and a scheme of buffer-pool-free and timing detection is adopted after the device operates stably, so that the detection efficiency is improved, and the monitoring cost is saved.
Example 5
Referring to fig. 1, the monitoring system of the present example was used to monitor the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process.
In this example, 2ml of the oxidizing solution and 20ml of pure water were extracted and injected into the analyzing cell 151 for each measurement. After the sample injection is completed, the analytical cell 151 is continuously stirred for 30s, and is kept standing for 30s for layering. The acidity value of the aqueous phase solution separated in the analysis cell 151 is detected by the detection unit. After each test was completed, the test was washed three times. The embodiment is set as continuous detection in the initial running stage, namely, after one detection process is finished, the next detection process is automatically started; after running for 24h or manually setting, detection is carried out once every 1 hour instead.
The monitoring system of the embodiment realizes the on-line monitoring of the acidity of the oxidizing liquid in the device for producing hydrogen peroxide by the anthraquinone method, and improves the safety of the device; and a timing detection mode is adopted after the device runs stably, so that the device is more energy-saving and environment-friendly.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. Any simple modifications, equivalent changes and modifications made to the above exemplary embodiments shall fall within the scope of the present invention.

Claims (17)

1. A monitoring system for the acidity of an oxidizing liquid in a device for producing hydrogen peroxide by an anthraquinone method is characterized by comprising the following components:
a sampling line connected to a sampling port of the oxidizing liquid; and
a detection unit, comprising:
an analysis cell for stirring and mixing pure water with the oxidation liquid passing through the sampling line and standing to separate into an aqueous phase and an organic phase; and
and the detection component is used for detecting the acidity value of the water phase obtained by standing separation in the analysis pool.
2. The system for monitoring the acidity of an oxidizing solution in an anthraquinone process hydrogen peroxide production plant according to claim 1, wherein the detection assembly comprises: an electrode assembly and a burette, the detection assembly being movable up and down relative to the analysis cell.
3. The system for monitoring the acidity of the oxidizing solution in the apparatus for producing hydrogen peroxide by the anthraquinone process as claimed in claim 2, further comprising:
a buffer cell connected between the sampling line and the analysis cell.
4. The system for monitoring the acidity of an oxidizing solution in an apparatus for producing hydrogen peroxide by an anthraquinone process according to claim 3, wherein the buffer tank comprises a stirring section.
5. The system for monitoring the acidity of the oxidizing solution in the device for producing hydrogen peroxide by an anthraquinone process according to claim 3, wherein the analysis cell is used for extracting the oxidizing solution in the buffer cell by a sample injection metering pump.
6. The system for monitoring the acidity of an oxidizing solution in a device for producing hydrogen peroxide by an anthraquinone process according to claim 1, wherein a sampling metering pump is arranged on the sampling pipeline, and the analysis cell pumps the pure water by the pure water metering pump.
7. The system for monitoring the acidity of an oxidizing solution in an apparatus for producing hydrogen peroxide by an anthraquinone process according to claim 1, wherein the pure water is distilled water, deionized water or high-purity water.
8. The system for monitoring the acidity of the oxidizing solution in the device for producing hydrogen peroxide by the anthraquinone process according to claim 1, wherein the analysis cell adopts mechanical stirring or magnetic stirring.
9. The system for monitoring the acidity of an oxidizing solution in an apparatus for producing hydrogen peroxide by an anthraquinone process according to claim 1, further comprising: a drain line and a flush line.
10. The system for monitoring the acidity of an oxidizing solution in an apparatus for producing hydrogen peroxide by an anthraquinone process according to claim 1, further comprising: a control unit arranged for controlling the sampling line and the detection unit.
11. A monitoring method for the acidity of an oxidizing solution in a device for producing hydrogen peroxide by an anthraquinone process, which is characterized in that the monitoring method adopts a monitoring system for the acidity of the oxidizing solution in the device for producing hydrogen peroxide by the anthraquinone process as claimed in any one of claims 1 to 10, and the monitoring method at least comprises the following steps:
extracting the oxidizing liquid;
stirring and mixing the extracted oxidation liquid and pure water in the analysis pool to form a mixed liquid;
standing the mixed solution to separate the mixed solution into a water phase and an organic phase; and
and detecting the acidity value of the water phase obtained by standing and separating in the analysis pool.
12. The method for monitoring the acidity of an oxidizing solution in an anthraquinone process hydrogen peroxide production plant according to claim 11, wherein the acidity value of an aqueous phase obtained by standing separation in the detection analysis cell is measured by potentiometric titration.
13. The method for monitoring the acidity of an oxidizing solution in an anthraquinone process hydrogen peroxide production plant according to claim 11, wherein before the stirring and mixing step, the oxidizing solution is subjected to a buffering step.
14. A method for monitoring the acidity of an oxidizing solution in an apparatus for producing hydrogen peroxide by an anthraquinone process according to claim 13, wherein the buffering step comprises stirring the oxidizing solution.
15. The method for monitoring the acidity of an oxidizing solution in an anthraquinone process hydrogen peroxide production plant according to claim 11, wherein the monitoring method further comprises the steps of:
emptying the monitoring system after each detection; and
one or more washing steps.
16. The method for monitoring the acidity of an oxidizing solution in an anthraquinone process hydrogen peroxide production plant according to claim 11, wherein the monitoring method further comprises the steps of:
setting an acidity threshold; and
and when the detected acidity value is lower than the acidity threshold value, sending out an alarm signal.
17. The method for monitoring the acidity of an oxidizing solution in a device for producing hydrogen peroxide by an anthraquinone process according to claim 11, wherein the monitoring method is continuous monitoring or timed monitoring.
CN202010329100.4A 2020-04-23 2020-04-23 System and method for monitoring acidity of oxidizing liquid in device for producing hydrogen peroxide by anthraquinone process Pending CN113551944A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114295773A (en) * 2021-12-07 2022-04-08 黎明化工研究设计院有限责任公司 Online testing device and method for acidity of oxidizing liquid or alkalinity of circulating working liquid in process of preparing hydrogen peroxide by anthraquinone method

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102401817A (en) * 2010-09-08 2012-04-04 谭祥明 Online determination method for hydrogen peroxide
CN104317317A (en) * 2014-09-25 2015-01-28 中国石油化工股份有限公司 Method for controlling the content of hydrogen peroxide in working solution for technology of preparing hydrogen peroxide by anthraquinone process
CN204939475U (en) * 2015-09-07 2016-01-06 徐志欣 Coliform online automatic monitor
CN205139153U (en) * 2015-09-07 2016-04-06 徐志欣 Online automatic monitoring system of manganese
CN206223771U (en) * 2016-11-10 2017-06-06 山东省科学院海洋仪器仪表研究所 A kind of seawater total alkalinity on-line monitoring system
CN107037106A (en) * 2017-05-31 2017-08-11 南京霍普斯科技有限公司 Liquid acidity continuous monitor system and monitoring method are aoxidized in hydrogen peroxide process
CN207096197U (en) * 2017-05-31 2018-03-13 南京霍普斯科技有限公司 Liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process
CN108645960A (en) * 2018-07-12 2018-10-12 宣向斌 A kind of automation concentration of hydrogen peroxide on-line detecting system and detection method
CN110131247A (en) * 2019-05-20 2019-08-16 洛阳大工检测技术有限公司 Contamination level of oil liquid control method and control system based on on-line checking

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102401817A (en) * 2010-09-08 2012-04-04 谭祥明 Online determination method for hydrogen peroxide
CN104317317A (en) * 2014-09-25 2015-01-28 中国石油化工股份有限公司 Method for controlling the content of hydrogen peroxide in working solution for technology of preparing hydrogen peroxide by anthraquinone process
CN204939475U (en) * 2015-09-07 2016-01-06 徐志欣 Coliform online automatic monitor
CN205139153U (en) * 2015-09-07 2016-04-06 徐志欣 Online automatic monitoring system of manganese
CN206223771U (en) * 2016-11-10 2017-06-06 山东省科学院海洋仪器仪表研究所 A kind of seawater total alkalinity on-line monitoring system
CN107037106A (en) * 2017-05-31 2017-08-11 南京霍普斯科技有限公司 Liquid acidity continuous monitor system and monitoring method are aoxidized in hydrogen peroxide process
CN207096197U (en) * 2017-05-31 2018-03-13 南京霍普斯科技有限公司 Liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process
CN108645960A (en) * 2018-07-12 2018-10-12 宣向斌 A kind of automation concentration of hydrogen peroxide on-line detecting system and detection method
CN110131247A (en) * 2019-05-20 2019-08-16 洛阳大工检测技术有限公司 Contamination level of oil liquid control method and control system based on on-line checking

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114295773A (en) * 2021-12-07 2022-04-08 黎明化工研究设计院有限责任公司 Online testing device and method for acidity of oxidizing liquid or alkalinity of circulating working liquid in process of preparing hydrogen peroxide by anthraquinone method
CN114295773B (en) * 2021-12-07 2024-02-27 黎明化工研究设计院有限责任公司 On-line testing equipment and method for acidity of oxidation liquid or alkalinity of circulating working liquid in process of preparing hydrogen peroxide by anthraquinone method

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Application publication date: 20211026