Sulfur and chlorine content detection system for 2-ethyl anthraquinone product

Abstract

The utility model relates to the technical field of chemical production, in particular to a sulfur and chlorine content detection system for a 2-ethyl anthraquinone product, which adopts an X-ray fluorescence spectrophotometer for detection, and can measure the proportional relation between the wavelength intensity and concentration of characteristic X-rays of elements according to the characteristic X-rays generated by transition generated by excitation of different elements. And quantitative measurement is facilitated. By utilizing the hydrogen generation device, the discharge of other gases in the detection container can be effectively reduced, the detection interference is reduced, and meanwhile, inflation protection is provided for the detection container. And the waste gas recovery device can reduce waste gas pollution and reduce environmental pollution. Meanwhile, the voltage stabilizer is designed, and the electric energy supplied by the power supply can be stably supplied to the X-ray fluorescence spectrometer, the waste gas recovery device and the hydrogen generation device by utilizing the voltage stabilizer, so that the requirement of the X-ray fluorescence spectrometer on stable voltage is ensured, and the precision requirement of a detection result is ensured.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical production, and particularly relates to a detection system for sulfur and chlorine contents in 2-ethylanthraquinone products. Background Art

[0002] In industrial production, hydrogen peroxide is mainly obtained by separating 2-ethylanthraquinone after the oxidation reaction of 2-ethylhydroanthraquinone dissolved in a solvent. And 2-ethylanthraquinone can generate 2-ethylhydroanthraquinone through a hydrogenation reaction. Therefore, 2-ethylanthraquinone is an important intermediate reaction medium for the production of hydrogen peroxide.

[0003] 2-ethylanthraquinone is synthesized from ethylbenzene and phthalic anhydride as raw materials under the catalysis of chlorobenzene as an organic solvent and anhydrous aluminum trichloride to form 2-benzoylbenzoic acid, and 2-benzoylbenzoic acid is then converted into 2-ethylanthraquinone through fuming sulfuric acid in a closed reaction environment. Since chlorobenzene, anhydrous aluminum trichloride and fuming sulfuric acid are used in the raw materials of 2-ethylanthraquinone, sulfur and chloride ions are inevitably carried in the finished product. Although the finished product has been purified through multiple processes, trace amounts of sulfur and chloride ions are still contained in the finished product. Therefore, the trace amounts of sulfur and chloride ions in 2-ethylanthraquinone will circulate throughout the production process, which will cause the sulfur and chloride ions to deactivate catalysts such as palladium and nickel during the hydrogenation reaction of 2-ethylanthraquinone, seriously affecting the cyclic production of hydrogen peroxide.

[0004] The traditional detection method is to use microcoulometry to determine the sulfur and chlorine residues in 2-ethylanthraquinone. Due to the technical defects of the instrument itself, such as poor reproducibility of analysis data, instability of the instrument, and slow sample analysis speed, it cannot meet the production needs fundamentally. Therefore, a new detection system is needed to solve the above problems. Summary of the Utility Model

[0005] In order to overcome one of the deficiencies of the prior art, the purpose of the utility model is to provide a detection system for sulfur and chlorine contents in 2-ethylanthraquinone products, which has high detection efficiency and accurate detection results.

[0006] To solve the above problems, the technical solutions adopted by the utility model are as follows:

[0007] A detection system for sulfur and chlorine contents in 2-ethylanthraquinone products, comprising

[0008] a detection container for containing a sample to be detected and capable of being opened or closed;

[0009] an X-ray fluorescence spectrometer for detecting the sample in the detection container;

[0010] a hydrogen generation device for providing hydrogen to the detection container;

[0011] An exhaust gas recovery device, which is connected to the detection container;

[0012] A power supply unit for supplying power;

[0013] A voltage regulator, whose input end is connected to the power supply unit, and the output end is connected to an X-ray fluorescence spectrometer, an exhaust gas recovery device, and a hydrogen generation device.

[0014] Further, the hydrogen generation device includes an electrolysis tank and a gas-water separator connected to the electrolysis tank. The gas-water separator is connected to a cooler through an exhaust pipe, the cooler is connected to the detection container through a pipeline, a dryer is provided on the pipeline, and the electrolysis tank is connected to the voltage regulator.

[0015] Further, the hydrogen generation device further includes a hydrogen concentration sensor, which is arranged at the gas outlet end of the dryer.

[0016] Further, an air extraction pump and an intake valve are connected to the exhaust pipe.

[0017] Further, a suction pipe is arranged in parallel on the pipeline. A compression pump is provided on the suction pipe. The compression pump is connected to a gas storage tank. A pressure relief valve is provided on the gas storage tank. A one-way valve is provided at the intake end of the gas storage tank, and a switch valve is provided at the outlet end.

[0018] Further, the X-ray fluorescence spectrometer is connected to a control terminal through a USB data cable.

[0019] Further, a controller is further included. The controller is electrically connected to the voltage regulator, the X-ray fluorescence spectrometer, the exhaust gas recovery device, and the hydrogen generation device.

[0020] Further, an oxygen content sensor and a nitrogen content sensor are arranged in the detection container. Both the oxygen content sensor and the nitrogen content sensor are electrically connected to the controller. The controller can control the working state of the hydrogen generation device according to the detection results of the oxygen content sensor and the nitrogen content sensor.

[0021] Further, the exhaust gas recovery device includes an absorption tank and a purification tank. An organic solution is arranged in the absorption tank. The absorption tank is connected to the detection container through a discharge pipe. The purification tank is connected to the exhaust end of the absorption tank. An exhaust port is provided on the purification tank. A suction pump is arranged between the purification tank and the absorption tank.

[0022] Further, an overload protector is arranged between the power supply unit and the voltage regulator.

[0023] Compared with the prior art, the beneficial effects of the present utility model are as follows:

[0024] A detection system for the sulfur and chlorine content of 2-ethylanthraquinone products of the present utility model uses an X-ray fluorescence spectrometer for detection. According to the characteristic X-rays generated by the excitation and transition of different elements, the proportional relationship between the intensity and concentration of the wavelengths of the characteristic X-rays of the elements can be measured, which is beneficial for quantitative measurement. By using a hydrogen generation device, the discharge of other gases in the detection container can be effectively reduced, the detection interference can be reduced, and at the same time, inflation protection can be provided for the detection container. The waste gas recovery device can reduce waste gas pollution and environmental pollution. At the same time, a voltage regulator is designed. By using the voltage regulator, the electric energy supplied by the power supply can be stably supplied to the X-ray fluorescence spectrometer, the waste gas recovery device, and the hydrogen generation device, so as to ensure the demand of the X-ray fluorescence spectrometer for a stable voltage and the accuracy requirement of the detection result.

[0025] The present utility model will be further described in detail below in conjunction with the accompanying drawings and specific embodiments. Brief Description of the Drawings

[0026] Figure 1 is a schematic structural diagram of an embodiment of the present utility model;

[0027] Figure 2 is a schematic structural diagram of an improved embodiment of the present utility model;

[0028] Figure 3 is a principle block diagram of an embodiment of the present utility model.

[0029] Explanation of the Reference Numerals in the Drawings:

[0030] Detection container 10, oxygen content sensor 11, nitrogen content sensor 12, X-ray fluorescence spectrometer 20, hydrogen generation device 30, electrolysis tank 31, gas-water separator 32, exhaust pipe 33, cooler 34, dryer 35, hydrogen concentration sensor 36, air extraction pump 37, intake valve 38, pipeline 39, suction pipe 3a, compression pump 3b, gas storage tank 3c, pressure relief valve 3d, waste gas recovery device 40, absorption tank 41, purification tank 42, discharge pipe 43, electric suction pump 44, power supply 50, voltage regulator 60, control terminal 70, controller 80, overload protector 90 Specific Embodiments

[0031] In order to make the objectives, technical solutions, and advantages of the present utility model clearer, the present utility model will be further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present utility model and are not used to limit the present utility model.

[0032] Refer to Figures 1 to 3A detection system for sulfur and chlorine content of 2-ethylanthraquinone product shown in the figure includes a detection container 10, an X-ray fluorescence spectrometer 20, a hydrogen generation device 30, an exhaust gas recovery device 40, a power supply 50 and a voltage stabilizer 60. The detection container 10 is used to hold the sample to be detected and can be opened or closed; the X-ray fluorescence spectrometer 20 is used to detect the sample in the detection container 10; the hydrogen generation device 30 is used to supply hydrogen to the detection container 10; the exhaust gas recovery device 40 is connected to the detection container 10; the power supply 50 is used to supply power; the input end of the voltage stabilizer 60 is connected to the power supply 50, and the output end is connected to the X-ray fluorescence spectrometer 20, the exhaust gas recovery device 40 and the hydrogen generation device 30.

[0033] Among them, the detection container 10 is a sealed container. When placing the sample, a protective film needs to be coated on the outside of the sample, which can avoid sample contamination and at the same time reduce the pollution and corrosion of the sample to the detection container 10. In this application, since the power supply required by the X-ray fluorescence spectrometer 20 is relatively stable, it can ensure that the X-rays output by it have sufficient energy and are relatively stable, thereby ensuring the accuracy of the detection results. The power supply 50 and the voltage stabilizer 60 are both conventional electronic components, which will not be elaborated by the applicant here. In an improved embodiment of this application, in order to cope with sudden voltage fluctuations, an overload protector 90 is provided between the power supply 50 and the voltage stabilizer 60. The overload protector 90 can effectively protect the entire circuit, as well as the X-ray fluorescence spectrometer 20, the hydrogen generation device 30, and the exhaust gas recovery device 40, and prevent both from being affected by voltages exceeding the working range of the voltage stabilizer 60.

[0034] When this detection system for sulfur and chlorine content of 2-ethylanthraquinone product uses the X-ray fluorescence spectrometer 20 for detection, according to the characteristic X-rays generated by the excitation and transition of different elements, the proportional relationship between the intensity and concentration of the wavelengths of the characteristic X-rays of the elements can be measured, which is beneficial for quantitative measurement. Among them, the measurement principle is specifically that after being irradiated by X-rays, the inner shell electrons of the atoms of the elements to be detected in the sample are excited, and shell electron transitions occur to emit the characteristic X-rays of the elements. Just collecting and detecting these characteristic X-rays can determine the elements. Using the hydrogen generation device 30 can effectively reduce the discharge of other gases in the detection container 10, reduce detection interference, and at the same time provide inflation protection for the detection container 10. The exhaust gas recovery device 40 can reduce exhaust gas pollution and environmental pollution. At the same time, the voltage stabilizer 60 is designed to make the electric energy supplied by the power supply 50 be able to stably supply the X-ray fluorescence spectrometer 20, the exhaust gas recovery device 40 and the hydrogen generation device 30, so as to ensure the demand of the X-ray fluorescence spectrometer 20 for stable voltage and the accuracy requirements of the detection results.

[0035] In an embodiment of the present application, the hydrogen generation device 30 includes an electrolysis tank 31 and a gas-water separator 32 communicated with the electrolysis tank 31. The gas-water separator 32 is communicated with a cooler 34 through an exhaust pipe 33. The cooler 34 is communicated with a detection container 10 through a pipeline 39. A dryer 35 is arranged on the pipeline 39. The electrolysis tank 31 is communicated with a voltage stabilizer 60. It should be noted that oxygen and hydrogen are generated simultaneously during the electrolysis process. The gas-water separator 32 in the present application is connected to the hydrogen generation end of the electrolysis tank 31. The return water end of the cooler 34 is communicated with the electrolysis tank 31 through a connecting pipe, so that this part of cooling water can be recycled to a certain extent.

[0036] In the above improved embodiment, the hydrogen generation device 30 further includes a hydrogen concentration sensor 36, and the hydrogen concentration sensor 36 is arranged at the gas outlet end of the dryer 35. The purpose of such arrangement is to ensure the normal supply amount of hydrogen and avoid the situation that the hydrogen in the detection container 10 decreases when the hydrogen generated by electrolyzing water decreases.

[0037] In the above improved embodiment, an air extraction pump 37 and an intake valve 38 are communicated with the exhaust pipe 33. The air extraction pump 37 can continuously supply the hydrogen generated in the electrolysis tank 31 outward, and at the same time provide power for the hydrogen so that it can smoothly pass through the cooler 34 and the dryer 35.

[0038] In the improved scheme of the above embodiment, in order to collect and store the excess hydrogen to avoid frequently starting the electrolysis tank 31 under normal circumstances, a suction pipe 3a is arranged in parallel on the pipeline 39. A compression pump 3b is arranged on the suction pipe 3a. The compression pump 3b is communicated with a gas storage tank 3c. A pressure relief valve 3d is arranged on the gas storage tank 3c. A one-way valve is arranged at the intake end of the gas storage tank 3c, and a switch valve is arranged at the outlet end. Under normal circumstances, the gas storage tank 3c can store the excess hydrogen. When it is necessary to detect samples later, the switch valve can be opened at this time, and the hydrogen stored in the gas storage tank 3c can be directly discharged into the dryer 35 through the suction pipe 3a, so that the hydrogen can finally reach the detection container 10.

[0039] See Figure 3 , in some improved embodiments, in order to facilitate the transmission of detection data outward, the X-ray fluorescence spectrometer 20 is communicated with a control terminal 70 through a USB data cable, where the control terminal 70 can be a PC.

[0040] In an embodiment of the present application, the detection system further includes a controller 80, and the controller 80 is electrically connected to a voltage stabilizer 60, an X-ray fluorescence spectrometer 20, an exhaust gas recovery device 40, and a hydrogen generation device 30. Among them, the controller 80 can be a conventional programmable controller. When the voltage stabilizer 60 exceeds its own voltage stabilizing ability, the controller 80 will timely shut down the X-ray fluorescence spectrometer 20, so as to protect the X-ray fluorescence spectrometer 20.

[0041] Further referring to Figure 2 , in order to facilitate the staff to know when the detection can be carried out, that is, whether there are other impurity gases in the detection container 10, such as oxygen, nitrogen, and other gases, etc., in an embodiment of the present application, an oxygen content sensor 11 and a nitrogen content sensor 12 are arranged in the detection container 10, and both the oxygen content sensor 11 and the nitrogen content sensor 12 are electrically connected to the controller 80. The controller 80 can control the working state of the hydrogen generation device 30 according to the detection results of the oxygen content sensor 11 and the nitrogen content sensor 12. Among them, when any one of the detection results of the oxygen content sensor 11 and the nitrogen content sensor 12 does not meet the standard, the controller 80 will control the working efficiency of the hydrogen generation device 30 to supply gas until the detection result is qualified. At the same time, the controller 80 will also control the working state of the hydrogen generation device 30 according to different working stages. For example, in the early exhaust stage, the exhaust volume of the hydrogen generation device 30 can be controlled, so that the miscellaneous gas in the detection container 10 can be quickly cooled and discharged; in the later detection stage, the exhaust volume of the hydrogen generation device 30 can be reduced, so that a protective gas can be continuously provided to the detection container 10.

[0042] In an embodiment of the present application, in order to better reduce the environmental pollution caused by the exhaust gas discharged from the detection container 10, the exhaust gas recovery device 40 includes an absorption tank 41 and a purification tank 42. An organic solution is arranged in the absorption tank 41. The absorption tank 41 is communicated with the detection container 10 through a discharge pipe 43. The purification tank 42 is communicated with the exhaust end of the absorption tank 41. An exhaust port is arranged on the purification tank 42. A suction pump 44 is arranged between the purification tank 42 and the absorption tank 41. Among them, the organic solvent can effectively absorb 2-ethylanthraquinone, and the purification tank 42 has a secondary absorption effect, which is mainly to absorb the organic solution in the gas to avoid environmental pollution when the organic solvent is discharged outward.

[0043] The above embodiments are only the preferred embodiments of the present invention, and the scope of protection of the present invention cannot be limited by this. Any non-substantial changes and substitutions made by those skilled in the art on the basis of the present invention belong to the scope of protection required by the present invention.

Claims

1. A 2-ethylanthraquinone product sulfur and chlorine content detection system, characterized in that: include A detection container, which is used to hold the sample to be detected and can be opened or closed; An X-ray fluorescence spectrometer, which is used to detect the sample in the detection container; A hydrogen generating device, which is used to provide hydrogen to the detection container; An exhaust gas recovery device connected to the detection container; A power supply, used for supplying power; The voltage stabilizer has an input end connected to the power supply, and an output end connected to the X-ray fluorescence spectrometer, the waste gas recovery device and the hydrogen generation device.

2. A 2-ethylanthraquinone product sulfur and chlorine content detection system according to claim 1, characterized in that: The hydrogen generating device comprises an electrolytic box and a gas-water separator connected to the electrolytic box, the gas-water separator is connected to a cooler through an exhaust pipe, the cooler is connected to a detection container through a pipeline, a dryer is provided on the pipeline, and the electrolytic box is connected to the voltage stabilizer.

3. A 2-ethylanthraquinone product sulfur and chlorine content detection system according to claim 2, characterized in that: The hydrogen generating device further comprises a hydrogen concentration sensor, and the hydrogen concentration sensor is arranged at the gas outlet end of the dryer.

4. A 2-ethylanthraquinone product sulfur and chlorine content detection system according to claim 2, characterized in that: The exhaust pipe is connected with an air pump and an air intake valve.

5. A 2-ethylanthraquinone product sulfur and chlorine content detection system according to claim 2, characterized in that: A suction pipe is arranged in parallel on the pipeline, a compression pump is arranged on the suction pipe, the compression pump is connected to an air storage tank, a pressure relief valve is arranged on the air storage tank, a one-way valve is arranged at the air inlet end of the air storage tank, and a switch valve is arranged at the air outlet end.

6. A 2-ethylanthraquinone product sulfur and chlorine content detection system according to claim 1, characterized in that: The X-ray fluorescence spectrometer is connected to the control terminal via a USB data line.

7. A 2-ethylanthraquinone product sulfur and chlorine content detection system according to any one of claims 1 to 6, characterized in that: The device also includes a controller, which is electrically connected to the voltage stabilizer, the X-ray fluorescence spectrometer, the exhaust gas recovery device and the hydrogen generation device.

8. A 2-ethylanthraquinone product sulfur and chlorine content detection system according to claim 7, characterized in that: An oxygen content sensor and a nitrogen content sensor are arranged in the detection container, and both the oxygen content sensor and the nitrogen content sensor are electrically connected to the controller. The controller can control the working state of the hydrogen generating device according to the detection results of the oxygen content sensor and the nitrogen content sensor.

9. A 2-ethylanthraquinone product sulfur and chlorine content detection system according to claim 1, characterized in that: The waste gas recovery device includes an absorption box and a purification box. An organic solution is arranged in the absorption box. The absorption box is connected to the detection container through a discharge pipe. The purification box is connected to the exhaust end of the absorption box. An exhaust port is arranged on the purification box. A suction pump is arranged between the purification box and the absorption box.

10. A 2-ethylanthraquinone product sulfur and chlorine content detection system according to claim 1, characterized in that: An overload protector is arranged between the power supply and the voltage stabilizer.

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