CN113551943A - System and method for monitoring hydrogen peroxide concentration in raffinate - Google Patents
System and method for monitoring hydrogen peroxide concentration in raffinate Download PDFInfo
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- CN113551943A CN113551943A CN202010328217.0A CN202010328217A CN113551943A CN 113551943 A CN113551943 A CN 113551943A CN 202010328217 A CN202010328217 A CN 202010328217A CN 113551943 A CN113551943 A CN 113551943A
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 167
- 238000012544 monitoring process Methods 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 47
- 238000001514 detection method Methods 0.000 claims abstract description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000000926 separation method Methods 0.000 claims abstract description 46
- 238000003756 stirring Methods 0.000 claims abstract description 36
- 238000005070 sampling Methods 0.000 claims abstract description 27
- 239000008346 aqueous phase Substances 0.000 claims abstract description 21
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 150000004056 anthraquinones Chemical class 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000012074 organic phase Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 25
- 238000013019 agitation Methods 0.000 claims description 14
- 239000012071 phase Substances 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 10
- 238000003918 potentiometric titration Methods 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000000835 electrochemical detection Methods 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims 1
- 229960002163 hydrogen peroxide Drugs 0.000 description 63
- 239000007788 liquid Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000011010 flushing procedure Methods 0.000 description 7
- 238000002347 injection Methods 0.000 description 6
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- -1 anthraquinone compounds Chemical class 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
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- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
- G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N2001/1031—Sampling from special places
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Abstract
The invention discloses a system for monitoring the concentration of hydrogen peroxide in raffinate, which is the raffinate in a device for producing hydrogen peroxide by an anthraquinone process, and comprises: a sampling line connected to a sampling port of the raffinate; a stirring separation tank for stirring and mixing pure water and the raffinate passing through the sampling line and standing and separating into an aqueous phase and an organic phase; and a detection unit for detecting the hydrogen peroxide concentration in the aqueous phase obtained by the standing separation. The invention also discloses a method for monitoring the concentration of hydrogen peroxide in the raffinate. The invention realizes the on-line monitoring of the hydrogen peroxide concentration of the raffinate in the device for producing hydrogen peroxide by the anthraquinone method through on-line sampling, separation and detection, and improves the production safety.
Description
Technical Field
The invention relates to the technical field of hydrogen peroxide production, in particular to a system and a method for monitoring the concentration of hydrogen peroxide in raffinate.
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. Wherein, the oxydol is obtained after the oxidation liquid is extracted, but partial hydrogen peroxide still remains in the raffinate, and the concentration of the hydrogen peroxide is important index data for the safety control of the device. At present, hydrogen peroxide in raffinate is mainly analyzed manually, so that the operation risk is high, the time is long, the online monitoring cannot be realized, and the safety of the device is influenced.
Therefore, there is a need for an automatic on-line analysis technique to improve the analysis efficiency of the residual concentration of hydrogen peroxide in the raffinate, 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 concentration of hydrogen peroxide in a raffinate, which can more efficiently perform on-line monitoring of the concentration of hydrogen peroxide in a raffinate during the production of hydrogen peroxide by an anthraquinone process, thereby improving the safety of the device.
Another objective of the present invention is to provide a system and a method for monitoring the concentration of hydrogen peroxide in raffinate, so as to avoid the injury of the operator caused by manual analysis of the hydrogen peroxide concentration.
In order to achieve the above object, according to a first aspect of the present invention, there is provided a system for monitoring a hydrogen peroxide concentration in a raffinate from a hydrogen peroxide production plant using an anthraquinone process, the system comprising: a sampling line connected to a sampling port of the raffinate; a stirring separation tank for stirring and mixing pure water and the raffinate passing through the sampling line and standing and separating into an aqueous phase and an organic phase; and a detection unit for detecting the hydrogen peroxide concentration in the aqueous phase obtained by the standing separation.
Further, in the above technical scheme, be equipped with the sample measuring pump on the sampling pipeline, the stirring separation pond passes through the pure water measuring pump and extracts the pure water.
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 stirring separation tank adopts mechanical stirring or magnetic stirring.
Further, in the above technical scheme, the detection unit extracts the water phase obtained by standing separation through a water phase metering pump.
Further, in the above technical solution, the monitoring system for the concentration of hydrogen peroxide in the raffinate further includes: a drain line and a flush line.
Further, in the above technical solution, the monitoring system for the concentration of hydrogen peroxide in the raffinate further includes: a control unit configured to control the sampling line, the agitation separation tank, and the detection unit.
Further, in the above technical solution, the detection unit adopts optical detection or electrochemical detection.
Further, in the above technical solution, the detection unit adopts potentiometric titration for detection, and the detection unit includes an analysis cell and an electrode assembly.
According to a second aspect of the present invention, there is provided a method for monitoring the concentration of hydrogen peroxide in a raffinate, the method using a system for monitoring the concentration of hydrogen peroxide in a raffinate as described in any one of the above technical solutions, the method at least comprising the following steps: extracting the raffinate; stirring and mixing the extracted raffinate and pure water in the stirring and separating tank 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 concentration of the hydrogen peroxide in the water phase obtained by standing separation.
Further, in the above technical solution, the method for monitoring the concentration of hydrogen peroxide in raffinate further comprises the steps of: after the detection is finished, emptying the stirring separation pool and the detection unit; and one or more washing steps.
Further, in the above technical solution, the method for monitoring the concentration of hydrogen peroxide in raffinate further comprises the steps of: setting a concentration threshold value; and sending out an alarm signal when the hydrogen peroxide concentration value detected by the detection unit exceeds the concentration 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 hydrogen peroxide concentration of the raffinate in the device for producing hydrogen peroxide by the anthraquinone method is realized through on-line sampling, separation and detection, and the safety of the device is improved.
2. The raffinate, the pure water and/or the separated aqueous phase solution can be accurately extracted through the metering pump, so that the detection result accuracy is higher.
3. 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.
4. And the automatic safety control of the concentration of the hydrogen peroxide in the raffinate is realized through the settings of chain alarm and the like.
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 diagram of a system for monitoring hydrogen peroxide concentration in raffinate according to one or more embodiments of the present invention.
Description of the main reference numerals:
the method comprises the steps of 1-anthraquinone-method hydrogen peroxide production device, 10-sampling pipeline, 11-sampling metering pump, 20-pure water source, 21-pure water metering pump, 30-stirring separation tank, 41-aqueous phase metering pump, 50-detection unit, 51-analysis tank, 52-electrode assembly, 60-control unit, 70-liquid discharge pipeline, 71-liquid discharge pump and 80-flushing pipeline.
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, the system for monitoring the hydrogen peroxide concentration in the raffinate according to the embodiment of the present invention is used for monitoring the hydrogen peroxide concentration in the raffinate in the apparatus 1 for producing hydrogen peroxide by the anthraquinone process. The monitoring system of the present invention includes a sampling portion, a separation portion, and a detection portion. The sampling line 10 is connected to an existing manual sampling port of the apparatus for producing hydrogen peroxide by the anthraquinone process 1, thereby extracting raffinate. The agitation separation tank 30 is used to agitate and mix pure water with the raffinate solution passing through the sampling line 10 and to stand to separate into an aqueous phase and an organic phase. The separated aqueous phase liquid enters a detection unit 50 to detect the hydrogen peroxide concentration.
Further, in one or more exemplary embodiments of the present invention, the raffinate and pure water are precisely extracted and injected into the agitation separation tank 30 by the sampling metering pump 11 and the pure water metering pump 21 provided on the sampling line 10. Illustratively, the pure water metering pump 21 may pump pure water from the pure water source 20. 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 stirring separation tank 30 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 present invention, the aqueous phase solution obtained by the still separation in the agitation separation tank 30 may be drawn by the aqueous phase metering pump 41 as the liquid to be measured.
Preferably, but not by way of limitation, in one or more exemplary embodiments of the invention, the system for monitoring the concentration of hydrogen peroxide in the raffinate may further comprise a drain line 70. For example, the agitation separation tank 30 may be provided with a first drain valve (not shown) connected to the drain line 70, and the detection unit 50 may be provided with a second drain valve (not shown) connected to the drain line 70, so that the monitoring system may be drained through the first drain valve and the second drain valve when a detection process is completed. Illustratively, a drain pump 71 is provided on the drain line 70 to drain the monitoring system as much as possible to avoid affecting the next detection process. Preferably, but not limitatively, the detection unit 50 may also be provided with a flushing line 80 for flushing the detected detection unit 50. Illustratively, the flush line 80 may be connected to the pure water source 20, with one or more purges of pure water to ensure accuracy of the next testing procedure.
Further, in one or more exemplary embodiments of the present invention, the system for monitoring the concentration of hydrogen peroxide in the raffinate may further include a control unit 60. The control unit 60 can automatically control the monitoring system, for example, the sampling metering pump 11, the pure water metering pump 21, the agitation separation tank 30, the aqueous phase metering pump 41, the detection unit 50, the flush line 80, and the like on the sampling line 10 by a preset program.
Further, in one or more exemplary embodiments of the present invention, the detecting unit 50 may employ optical detection or electrochemical detection, and the present invention is not limited thereto, and a person skilled in the art may select a detection method according to actual needs.
Illustratively, as shown in FIG. 1, in one or more embodiments of the invention, the detection unit 50 employs potentiometric titration detection. The detection unit 50 includes an analysis cell 51 and an electrode assembly 52. After the liquid to be measured (aqueous phase obtained by standing separation) is injected into the detection unit 50, the electrode assembly 52 moves down and is immersed into the liquid to be measured, the analysis cell 51 automatically starts stirring, and then the titrant is dripped according to the titration sequence, and the hydrogen peroxide concentration is obtained through potential change.
The method for monitoring the concentration of hydrogen peroxide in raffinate according to the embodiment of the invention at least comprises the following steps: extracting raffinate in a device for producing hydrogen peroxide by an anthraquinone method; stirring and mixing the extracted raffinate and pure water in a stirring and separating tank 30 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 concentration of the hydrogen peroxide in the water phase obtained by standing separation.
Further, in one or more exemplary embodiments of the present invention, the method for monitoring the concentration of hydrogen peroxide in raffinate further comprises the steps of: after the detection is finished, emptying the stirring separation pool 30 and the detection unit 50; and one or more washing steps.
Further, in one or more exemplary embodiments of the present invention, the method for monitoring the concentration of hydrogen peroxide in raffinate further comprises the steps of: setting a concentration threshold value; and when the hydrogen peroxide concentration value detected by the detection unit 50 exceeds the concentration threshold value, sending out an alarm signal.
Further, in one or more exemplary embodiments of the present invention, the monitoring method may employ continuous monitoring or timed monitoring.
Referring to fig. 1, the operation of the system for monitoring the concentration of hydrogen peroxide in raffinate according to the present invention is as follows:
1. the sampling metering pump 11 extracts quantitative raffinate from the device for producing hydrogen peroxide by the anthraquinone method to be tested and injects the quantitative raffinate into the stirring separation tank 30. The amount of raffinate withdrawn can be set and adjusted according to the process conditions.
2. The pure water metering pump 21 pumps a fixed amount of pure water and injects it into the agitation separation tank 30 while stirring and mixing are performed. The amount of the pure water to be extracted can be set and adjusted according to the process condition.
3. After the injection of the raffinate and the pure water is finished, the mixture is continuously stirred for a certain time, which can be set according to the requirement.
4. 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.
5. The aqueous phase solution at the bottom of the agitation separation tank 30 is pumped by the aqueous phase metering pump 41 and injected into the detection unit 50. Illustratively, the amount of aqueous phase solution drawn is no more than 90% of the amount of pure water drawn.
6. The detection unit 50 detects the hydrogen peroxide concentration of the liquid to be measured.
7. When potentiometric titration is adopted for detection, the electrode assembly 52 of the detection unit 50 is moved downwards and immersed into the solution, stirring is automatically started, then the titrant is dripped, and the potential change is automatically recorded, so that the concentration of the hydrogen peroxide is obtained.
8. After the titration detection is completed, the electrode assembly 52 of the detection unit 50 is lifted, the flushing is automatically started, after the flushing is completed, the flushing pipeline 80 is closed, the first drain valve of the stirring separation tank 30 and the second drain valve of the detection unit 50 are opened, and the drain pipeline 70 empties the monitoring system.
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 next detection process continuously or at regular time according to the setting.
The following describes the system and method for monitoring the concentration of hydrogen peroxide in raffinate according to the present invention in more detail by way of specific examples, which should be understood as illustrative only and not limiting.
Example 1
Referring to FIG. 1, in the system for monitoring the concentration of hydrogen peroxide in raffinate of this example, 5ml of raffinate and 20ml of pure water were extracted and injected into the agitation separation tank 30 for each measurement. And after the sample injection is finished, continuously stirring for 30s in the stirring separation pool 30, and standing for 30s for layering. 2ml of aqueous phase solution is withdrawn each time and injected into the test unit 50. The detection unit 50 of the present embodiment employs potentiometric titration detection. After completion of the assay, three rinses were performed. 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, in the system for monitoring the concentration of hydrogen peroxide in raffinate of this example, 5ml of raffinate and 20ml of pure water were extracted and injected into the agitation separation tank 30 for each measurement. And after the sample injection is finished, continuously stirring for 30s in the stirring separation pool 30, and standing for 30s for layering. 2ml of aqueous phase solution is withdrawn each time and injected into the test unit 50. The detection unit 50 of the present embodiment employs potentiometric titration detection. After completion of the assay, three rinses were performed. This example is set up to perform the test every 1 hour.
The embodiment realizes the on-line monitoring of the concentration of the hydrogen peroxide in the raffinate, and improves the safety of the device.
Example 3
Referring to FIG. 1, in the system for monitoring the concentration of hydrogen peroxide in raffinate of this example, 3ml of raffinate and 15ml of pure water were extracted and injected into the agitation separation tank 30 for each measurement. After the sample injection is completed, the stirring separation pool 30 continues to stir for 20s, and the mixture is kept standing for layering for 20 s. 1ml of aqueous phase solution is withdrawn each time and injected into the test unit 50. The detection unit 50 of the present embodiment employs potentiometric titration detection. After completion of the assay, three rinses were performed. 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 4
Referring to FIG. 1, in the system for monitoring the concentration of hydrogen peroxide in raffinate of this example, 3ml of raffinate and 15ml of pure water were extracted and injected into the agitation separation tank 30 for each measurement. After the sample injection is completed, the stirring separation pool 30 continues to stir for 20s, and the mixture is kept standing for layering for 20 s. 1ml of aqueous phase solution is withdrawn each time and injected into the test unit 50. The detection unit 50 of the present embodiment employs potentiometric titration detection. After completion of the assay, three rinses were performed. This example is set up to perform the test every 1 hour.
The embodiment realizes the on-line monitoring of the concentration of the hydrogen peroxide in the raffinate, and improves the safety of the device.
Example 5
Referring to FIG. 1, in the system for monitoring the concentration of hydrogen peroxide in raffinate of this example, 3ml of raffinate and 15ml of pure water were extracted and injected into the agitation separation tank 30 for each measurement. After the sample injection is completed, the stirring separation pool 30 continues to stir for 20s, and the mixture is kept standing for layering for 20 s. 1ml of aqueous phase solution is withdrawn each time and injected into the test unit 50. The detection unit 50 of the present embodiment employs potentiometric titration detection. After completion of the assay, three rinses were performed. This example is set up to perform the test every 0.5 hours.
The embodiment realizes the on-line monitoring of the concentration of the hydrogen peroxide in the raffinate, and improves the safety of the device.
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 (13)
1. A system for monitoring the concentration of hydrogen peroxide in a raffinate from a hydrogen peroxide production plant using an anthraquinone process, the system comprising:
a sampling line connected to a sampling port of the raffinate;
a stirring separation tank for stirring and mixing pure water and the raffinate passing through the sampling line and standing and separating into an aqueous phase and an organic phase; and
and the detection unit is used for detecting the concentration of the hydrogen peroxide in the water phase obtained by standing separation.
2. The system for monitoring the concentration of hydrogen peroxide in raffinate according to claim 1, wherein a sampling metering pump is disposed on the sampling pipeline, and the stirring separation tank is used for pumping the pure water through the pure water metering pump.
3. The system for monitoring the concentration of hydrogen peroxide in a raffinate according to claim 1, wherein said pure water is distilled water, deionized water or high purity water.
4. The system for monitoring the concentration of hydrogen peroxide in raffinate according to claim 1, wherein the stirred separation cell is mechanically or magnetically stirred.
5. The system for monitoring the concentration of hydrogen peroxide in raffinate solution according to claim 1, wherein the detection unit is used for extracting the water phase obtained by standing separation through a water phase metering pump.
6. The system for monitoring the concentration of hydrogen peroxide in a raffinate solution according to claim 1, further comprising: a drain line and a flush line.
7. The system for monitoring the concentration of hydrogen peroxide in a raffinate solution according to claim 1, further comprising: a control unit configured to control the sampling line, the agitation separation tank, and the detection unit.
8. The system for monitoring the concentration of hydrogen peroxide in raffinate solution according to claim 1, wherein the detection unit employs optical detection or electrochemical detection.
9. The system for monitoring the concentration of hydrogen peroxide in raffinate solution as claimed in claim 1, wherein said detection unit comprises an analysis cell and an electrode assembly, and is used for potentiometric titration.
10. A method for monitoring the concentration of hydrogen peroxide in a raffinate, which comprises the following steps:
extracting the raffinate;
stirring and mixing the extracted raffinate and pure water in the stirring and separating tank to form a mixed solution;
standing the mixed solution to separate the mixed solution into a water phase and an organic phase; and
and detecting the concentration of the hydrogen peroxide in the water phase obtained by standing separation.
11. The method of claim 10, further comprising the steps of:
after the detection is finished, emptying the stirring separation pool and the detection unit; and
one or more washing steps.
12. The method of claim 10, further comprising the steps of:
setting a concentration threshold value; and
and when the concentration value of the hydrogen peroxide detected by the detection unit exceeds the concentration threshold value, sending out an alarm signal.
13. The method of claim 10, wherein the monitoring is continuous or timed.
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Cited By (1)
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| CN114441517A (en) * | 2021-12-31 | 2022-05-06 | 南京菘大仪表有限公司 | A analytical equipment that is arranged in hydrogen peroxide solution raffinate |
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