A device and method for determining 1,3-propane sultone content

Abstract

The present invention discloses a kind of 1,3-propane sultone content determination device and method, relate to the field of lithium battery material detection technology, including sampling device, solid-state sampling device, spectrometry device, free acid determination device and chip-based detection controller, the sampling device is arranged on one side of a negative pressure stainless steel packaging barrel, and the sampling port of the sampling device is communicated with the internal space of the negative pressure stainless steel packaging barrel, and the finished product 1,3-propane sultone crystalline powder is sampled using the method of negative pressure adsorption, and powder is sent to solid-state sampling device. The present invention completes finished product 1,3-propane sultone powder and takes out by closed sampling device, avoids sampling the contamination risk of finished product, uses solid-state sampling device to carry out secondary grinding to 1,3-propane sultone powder, to improve subsequent detection accuracy, so as to achieve more accurate 1,3-propane sultone content determination and the intelligent analysis of measurement result.

Description

Technical Field

[0001] The present invention relates to the technical field of lithium battery material detection, and in particular to a device and method for determining the content of 1,3-propane sultone. Background Art

[0002] 1,3-Propane sultone is an organic compound with the chemical formula C3H6O3S. It is slightly soluble in water and is mainly used as a surfactant. It is also used in the formulation of cosmetics and as a pharmaceutical intermediate in the pharmaceutical industry. It is also used in leather making, inks and sensitizing dyes to synthesize sulfonating agents. It is widely used in pharmaceutical chemicals, photosensitive materials, lithium batteries, biochemistry, textiles, lubrication, wastewater treatment, surface treatment and other industries.

[0003] High-end lithium-ion battery electrolytes have increasingly higher quality requirements for 1,3-propane sultone, especially higher requirements for purity (≥99.9%), moisture (<50ppm) and acid value (<50ppm).

[0004] Currently, the primary method for determining 1,3-propane sultone concentration is gas chromatography / tandem mass spectrometry (GC / MS-MS). This method employs extraction technology to extract 1,3-propane sultone. The extract is then concentrated and fixed to volume before being directly tested by gas chromatography / tandem mass spectrometry, using an external standard method for quantification. This method is simple, highly sensitive, and provides accurate quantification, fully meeting the needs of routine testing for 1,3-propane sultone in lithium-ion batteries and their electrolytes.

[0005] Chinese invention patent publication number CN109485631A discloses a method for preparing electronic-grade 1,3-propane sultone, comprising the following steps: recrystallizing industrial-grade 1,3-propane sultone from an anhydrous organic solvent, separating the crystals, and fractionating the crystals to separate water and impurities under total reflux to obtain electronic-grade 1,3-propane sultone. This method combines recrystallization and fractionation to produce electronic-grade 1,3-propane sultone. The recrystallization from an anhydrous organic solvent removes free acid and impurities from the industrial-grade 1,3-propane sultone. Compared to traditional methods, this method reduces waste, waste products, and energy consumption, while also improving production capacity and product yield.

[0006] In order to produce electronic-grade 1,3-propane sultone, this technical solution adopts a preparation method combining recrystallization and distillation for further purification, with a purity of ≥99.90%. However, it is still inevitably doped with some impurities, mainly water and trace amounts of hydrofluoric acid.

[0007] Although the above-mentioned patent discloses the use of an Agilent gas chromatograph to detect product purity and a Swiss Metrohm 905 fully automatic potentiometric titrator to detect acid value and calculate moisture, it does not disclose a specific sampling device to match the extremely high precision requirements of electronic-grade 1,3-propane sultone determination, nor does it design a method for processing the measurement data. Therefore, how to achieve high-precision 1,3-propane sultone content sampling and process the test data are technical problems that need to be solved urgently. Summary of the Invention

[0008] In order to solve the above technical problems, the present invention provides a device and method for determining the content of 1,3-propane sultone. The following technical solutions are adopted:

[0009] A 1,3-propane sultone content determination device comprises a sampling device, a solid-state sampling device, a spectrophotometric device, a free acid determination device, and a chip-based detection controller. The sampling device is arranged on one side of a negative pressure stainless steel packaging barrel, and a sampling port of the sampling device is connected to the internal space of the negative pressure stainless steel packaging barrel. The finished product 1,3-propane sultone crystalline powder is sampled by negative pressure adsorption and the powder is fed into the solid-state sampling device. The solid-state sampling device grinds the finished product 1,3-propane sultone crystalline powder twice before detection. The solid-state sampling device is provided with a spectrophotometric sampling port and a titration sampling port. The spectrophotometric sampling port is connected to the sampling port of the spectrophotometric device. The spectrophotometric device determines the 1,3-propane sultone content. The titration sampling port is connected to the sampling port of the free acid determination device. The free acid determination device determines the free acid. The detection controller is connected to the data output ports of the spectrophotometric device and the free acid determination device, respectively, and is used to integrate detection data, determine whether the detection data is qualified, and display the data.

[0010] By adopting the above technical solution, the finished 1,3-propane sultone powder is taken out from the negative pressure stainless steel packaging barrel through a sampling device, and the 1,3-propane sultone powder is secondary ground using a solid-state sampling device to improve the detection accuracy of subsequent spectroscopic measurement devices and free acid measurement devices. The spectroscopic measurement device and the free acid measurement device respectively perform detection based on the secondary ground 1,3-propane sultone powder and transmit the detection results to a chip-based detection controller. The detection controller can determine whether the 1,3-propane sultone content meets the standard and whether the acidity is qualified based on the setting of the threshold, thereby achieving more accurate 1,3-propane sultone content determination and intelligent analysis of the measurement results.

[0011] Optionally, the sampling device includes an electric linear slide, an integrated block, a sampling tube, a conveying hose, a sampling tube and a vacuum sampling pump. The bottom of the track of the electric linear slide is fixedly installed on the bottom of the inner wall of the negative pressure stainless steel packaging barrel. An inlet is provided on one side of the integrated block, an outlet is provided on the top, and a sampling channel is provided inside. The sampling channel connects the inlet and the outlet. The bottom of the integrated block is installed on the slider of the electric linear slide and moves left and right with the slider. One end of the sampling tube is connected to the inlet of the integrated block. When the slider of the electric linear slide moves, the other end of the sampling tube is driven to insert into the finished 1,3-propane sultone crystal powder in the negative pressure stainless steel packaging barrel and press against the side wall of the negative pressure stainless steel packaging barrel. One end of the sampling tube is connected to the other end of the sampling tube, the inlet of the vacuum sampling pump is connected to the other end of the sampling tube, and the outlet is connected to the inlet of the solid-state sampling device.

[0012] Optionally, the sampling device further includes a vacuum suction cup, which is arranged at the end of the sampling tube.

[0013] By adopting the above technical solution, the sampling device adopts the concept of negative pressure extraction. Generally, negative pressure extraction is achieved by directly burying the sample to be tested. This direct sampling method will disturb other nearby samples and affect the quality of the finished product. Here, during sampling, the electric linear slide moves, and the slider of the electric linear slide drives the sampling tube and vacuum suction cup to press against the inner wall of the negative pressure stainless steel packaging barrel. During this movement, the finished 1,3-propane sultone crystalline powder is collected in the sampling tube. The vacuum sampling pump is activated to extract the powder from the sampling tube, completing the sampling action. The sampling volume is small at a time, and the action can be repeated multiple times to meet the sampling volume requirements. During sampling, the vacuum suction action is confined to the sampling tube, delivery hose, and sample outlet tube, avoiding uncontrollable interference with the finished 1,3-propane sultone in the negative pressure stainless steel packaging barrel.

[0014] Optionally, all components of the sampling device are made of hydrofluoric acid-resistant materials.

[0015] By adopting the above technical solution, the components of the sampling device made of hydrofluoric acid-resistant materials can avoid corrosion caused by hydrofluoric acid hydrolyzed from the finished product 1,3-propane sultone.

[0016] Optionally, the solid-state sampling device includes a feed solenoid valve, an air shutoff, a temporary storage box, a discharge funnel, a discharge solenoid valve, a sealed grinding device and a sample discharge control device, wherein the feed solenoid valve is arranged at the outlet end of the sample discharge tube, the top inlet of the temporary storage box is connected to the outlet of the feed solenoid valve through the air shutoff, a discharge funnel is arranged at the bottom outlet of the temporary storage box, a discharge solenoid valve is arranged at the bottom outlet of the discharge funnel, the outlet of the discharge solenoid valve is connected to the feed port at the top of the sealed grinding device through a pipeline, the inlet of the sample discharge control device is connected to the outlet of the sealed grinding device, and the sample discharge control device is provided with a spectral sample outlet and a titration sample outlet.

[0017] Optionally, the sample discharge control device includes a blanking solenoid valve, a discharge auger, a spectral sample discharge solenoid valve and a titration sample discharge solenoid valve. The inlet of the discharge auger is connected to the outlet at the bottom of the sealed grinding device through the blanking solenoid valve. The discharge auger is provided with two outlets, and the spectral sample discharge solenoid valve and the titration sample discharge solenoid valve are respectively provided at the two outlets.

[0018] Optionally, the discharge auger is a small weighing auger.

[0019] By adopting the above technical solution, the solid-state sampling device uses an air lock, a temporary storage box and a discharge funnel to collect the sampled finished product 1,3-propane sultone and put it into a sealed grinding device. The sealed grinding device completes the secondary grinding of the finished product 1,3-propane sultone. The finished product 1,3-propane sultone powder after the secondary grinding is finer, which can improve the accuracy of subsequent detection. Through the control of the discharge auger, the spectral sampling solenoid valve and the titration sampling solenoid valve, the set weight of the finished product 1,3-propane sultone powder can be added to the spectral measurement device and the free acid measurement device respectively, realizing automated sampling and detection feeding.

[0020] Optionally, the spectrometric determination device is an Agilent gas chromatograph, and the free acid determination device is a fully automatic potentiometric titrator.

[0021] Optionally, the detection controller includes a chip-based main control circuit board, an industrial touch display, a USB data interface and a memory. The main control circuit board is communicatively connected to the data interfaces of the spectral measurement device and the free acid measurement device through the USB data interface. The industrial touch display, USB data interface and memory are communicatively connected to the main control circuit board respectively. The main control circuit board is also controlled and connected to various electrical components of the sampling device and the solid-state sampling device, and is used to control the sampling action of the sampling device, and control the injection volume and injection action of the solid-state sampling device.

[0022] By adopting the above technical solution, the chip-based main control circuit board can realize intelligent judgment of detection data, and can also control various electrical components of the sampling device and solid-state injection device to realize automated sampling, injection control and detection data processing.

[0023] A method for determining the content of 1,3-propane sultone, the specific method being:

[0024] Step 1: The detection controller controls the movement of the electric linear slide, driving the sampling tube and the vacuum suction cup to press against the inner wall of the negative pressure stainless steel packaging barrel. During the movement, the finished 1,3-propane sultone crystal powder is collected into the sampling tube, and the vacuum sampling pump is started to extract the powder from the sampling tube, completing the sampling action;

[0025] Step 2: The detection controller controls the feed solenoid valve to open. After the sampled powder enters the temporary storage box, the feed solenoid valve is closed and the air shutoff is opened. The powder settles in the temporary storage box. The discharge solenoid valve is then controlled to open. The powder enters the sealed grinding device from the discharge funnel. The sealed grinding device is started to grind the powder twice to 3000 mesh and then stops. The discharge solenoid valve is opened and the powder falls into the discharge auger.

[0026] Step 3: The detection controller controls the spectral sampling solenoid valve to open and the titration sampling solenoid valve to close, and controls the discharging auger to convey a specified weight of powder into the spectral measurement device. The spectral measurement device detects the powder and outputs 1,3-propane sultone content data to the detection controller via the USB interface. The detection controller controls the spectral sampling solenoid valve to close and the titration sampling solenoid valve to open, conveying a specified weight of powder into the free acid measurement device. The free acid measurement device detects the acid value of the powder and calculates the moisture content, and transmits the test results to the detection controller via the USB interface.

[0027] Step 4: The detection controller determines whether the detection value is qualified based on the threshold value and displays it on the industrial touch screen.

[0028] In summary, the present invention includes at least one of the following beneficial technical effects:

[0029] The present invention provides a 1,3-propane sultone content determination device and method. Finished product 1,3-propane sultone powder is taken out through a closed sampling device to avoid the risk of contamination of the finished product by sampling. A solid-state sampling device is used to perform secondary grinding on the 1,3-propane sultone powder to improve subsequent detection accuracy. A detection controller determines whether the 1,3-propane sultone content meets the standard and whether the acidity is qualified based on the setting of a threshold value, thereby achieving more accurate 1,3-propane sultone content determination and intelligent analysis of the determination results. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 This is a schematic structural diagram of a 1,3-propane sultone content determination device of the present invention in a non-sampling state;

[0031] Figure 2 This is a schematic diagram of the sampling state structure of a 1,3-propane sultone content determination device of the present invention;

[0032] Figure 3 This is a schematic structural diagram of a 1,3-propane sultone content determination device of the present invention, with the sampling device removed;

[0033] Figure 4 The present invention is a schematic diagram of the connection principle of electrical components of a device for determining the content of 1,3-propane sultone.

[0034] Explanation of the accompanying symbols: 11. Electric linear slide; 12. Integrated block; 13. Sampling tube; 14. Delivery hose; 15. Sample discharge tube; 16. Vacuum sampling pump; 17. Vacuum suction cup; 21. Feed solenoid valve; 26. Air shutoff; 22. Temporary storage box; 23. Discharge funnel; 24. Discharge solenoid valve; 25. Sealed grinding device; 31. Blanking solenoid valve; 32. Discharge auger; 33. Spectral sample discharge solenoid valve; 34. Titration sample discharge solenoid valve; 100. Negative pressure stainless steel packaging barrel; 101. Spectral measurement device; 102. Free acid measurement device; 103. Detection controller; 104. Main control circuit board; 105. Industrial touch screen; 106. USB data interface; 107. Memory. DETAILED DESCRIPTION

[0035] The present invention will be further described in detail below with reference to the accompanying drawings.

[0036] The embodiments of the present invention disclose a device and method for determining the content of 1,3-propane sultone.

[0037] Reference Figures 1-4A 1,3-propane sultone content determination device includes a sampling device, a solid-state sampling device, a spectrum determination device 101, a free acid determination device 102, and a chip-based detection controller 103. The sampling device is arranged on one side of a negative pressure stainless steel packaging barrel 100, and the sampling port of the sampling device is connected to the internal space of the negative pressure stainless steel packaging barrel 100. The finished product 1,3-propane sultone crystal powder is sampled by negative pressure adsorption and the powder is fed into the solid-state sampling device. The solid-state sampling device feeds the finished product 1,3-propane sultone crystal powder into the solid-state sampling device. A second grinding is performed before testing. The solid-state sampling device is provided with a spectral sampling port and a titration sampling port. The spectral sampling port is connected to the sampling port of the spectral measurement device 101, and the spectral measurement device 101 performs the measurement of the 1,3-propane sultone content. The titration sampling port is connected to the sampling port of the free acid measurement device, and the free acid measurement device performs the measurement of the free acid. The detection controller 103 is connected to the data output ports of the spectral measurement device 101 and the free acid measurement device 102 respectively, and is used to integrate the detection data, make a qualified judgment on the detection data, and display it.

[0038] By adopting the above technical solution, the finished 1,3-propane sultone powder is removed from the negative pressure stainless steel packaging barrel 100 using a sampling device, and the 1,3-propane sultone powder is secondary ground using a solid-state sampling device to improve the detection accuracy of the subsequent spectrophotometric device 101 and the free acid determination device 102. The spectrophotometric device 101 and the free acid determination device 102 respectively perform tests based on the secondary ground 1,3-propane sultone powder and transmit the test results to the chip-based detection controller 103. The detection controller 103 can determine whether the 1,3-propane sultone content meets the standard and whether the acidity is qualified based on the set threshold value, thereby achieving more accurate 1,3-propane sultone content determination and intelligent analysis of the measurement results.

[0039] The sampling device includes an electric linear slide 11, an integrated block 12, a sampling tube 13, a conveying hose 14, a sampling tube 15 and a vacuum sampling pump 16. The bottom of the track of the electric linear slide 11 is fixedly installed on the bottom of the inner wall of the negative pressure stainless steel packaging barrel 100. An inlet is provided on one side of the integrated block 12, an outlet is provided on the top, and a sampling channel is provided inside. The sampling channel connects the inlet and outlet. The bottom of the integrated block 12 is installed on the slider of the electric linear slide 11 and moves left and right with the slider. One end of the sampling tube 13 is connected to the inlet of the integrated block 12. When the slider of the electric linear slide 11 moves, the other end of the sampling tube 13 is driven to insert into the finished 1,3-propane sultone crystal powder in the negative pressure stainless steel packaging barrel 100 and press against the side wall of the negative pressure stainless steel packaging barrel 100. One end of the sampling tube 15 is connected to the other end of the sampling tube 13, the inlet of the vacuum sampling pump 16 is connected to the other end of the sampling tube 15, and the outlet is connected to the inlet of the solid-state sampling device.

[0040] The sampling device further includes a vacuum suction cup 17 , which is disposed at the end of the sampling tube 13 .

[0041] The sampling device adopts the concept of negative pressure extraction. Generally, negative pressure extraction is achieved by directly burying the sample to be tested. This direct sampling method will disturb other nearby samples and affect the quality of the finished product. When sampling, the electric linear slide 11 moves, and the slider of the electric linear slide 11 drives the sampling tube 13 and the vacuum suction cup 17 to press against the inner wall of the negative pressure stainless steel packaging barrel 100. During the movement, the finished product 1,3-propane sultone crystal powder is collected into the sampling tube 13, and the vacuum sampling pump 16 is started to extract the powder in the sampling tube 13 to complete the sampling action. The sampling volume is small at a time, and the action can be repeated multiple times to meet the sampling volume requirements. During sampling, the vacuum suction action is limited to the sampling tube 13, the conveying hose 14 and the sample outlet tube 15 to avoid uncontrollable interference with the finished product 1,3-propane sultone in the negative pressure stainless steel packaging barrel 100.

[0042] All components of the sampling device are made of materials resistant to hydrofluoric acid.

[0043] The components of the sampling device are made of hydrofluoric acid-resistant materials to avoid corrosion caused by hydrofluoric acid hydrolyzed from the finished product 1,3-propane sultone.

[0044] The solid-state sampling device includes a feed solenoid valve 21, an air lock 26, a temporary storage box 22, a discharge funnel 23, a discharge solenoid valve 24, a sealed grinding device 25 and a sample discharge control device. The feed solenoid valve 21 is arranged at the outlet end of the sample discharge tube 15, and the top inlet of the temporary storage box 22 is connected to the outlet of the feed solenoid valve 21 through the air lock 26. The discharge funnel 23 is arranged at the bottom outlet of the temporary storage box 22, and the discharge solenoid valve 24 is arranged at the bottom outlet of the discharge funnel 23. The outlet of the discharge solenoid valve 24 is connected to the feed port at the top of the sealed grinding device 25 through a pipeline. The inlet of the sample discharge control device is connected to the outlet of the sealed grinding device 25. The sample discharge control device is provided with a spectral sample outlet and a titration sample outlet.

[0045] The sample discharge control device includes a blanking solenoid valve 31, a discharge auger 32, a spectral sample discharge solenoid valve 33 and a titration sample discharge solenoid valve 34. The inlet of the discharge auger 32 is connected to the outlet at the bottom of the sealed grinding device 25 through the blanking solenoid valve 31. The discharge auger 32 is provided with two outlets, and the spectral sample discharge solenoid valve 33 and the titration sample discharge solenoid valve 34 are respectively provided at the two outlets.

[0046] The discharge auger 32 is a small weighing auger.

[0047] The solid-state sampling device uses an air lock 26, a temporary storage box 22 and a discharge funnel 23 to collect the sampled finished product 1,3-propane sultone and place it into a sealed grinding device 25. The sealed grinding device 25 completes the secondary grinding of the finished product 1,3-propane sultone. After the secondary grinding, the finished product 1,3-propane sultone powder is finer, which can improve the accuracy of subsequent testing. Through the control of the discharge auger 32, the spectral sampling solenoid valve 33 and the titration sampling solenoid valve 34, a set weight of the finished product 1,3-propane sultone powder can be added to the spectral measurement device 101 and the free acid measurement device 102 respectively, realizing automated sampling and detection feeding.

[0048] The spectrum measuring device 101 is an Agilent gas chromatograph, and the free acid measuring device 102 is a fully automatic potentiometric titrator.

[0049] The detection controller 103 includes a chip-based main control circuit board 104, an industrial touch screen display 105, a USB data interface 106 and a memory 107. The main control circuit board 104 is communicatively connected to the data interfaces of the spectral measurement device 101 and the free acid measurement device 102 via the USB data interface 106. The industrial touch screen display 105, the USB data interface 106 and the memory 107 are communicatively connected to the main control circuit board 104 respectively. The main control circuit board 104 is also controllably connected to the electrical components of the sampling device and the solid-state sampling device to control the sampling action of the sampling device and the injection volume and injection action of the solid-state sampling device.

[0050] The chip-based main control circuit board 104 can realize intelligent judgment of detection data, and can also control various electrical components of the sampling device and the solid-state injection device to realize automatic sampling, injection control and detection data processing.

[0051] A method for determining the content of 1,3-propane sultone, the specific method being:

[0052] Step 1: The detection controller 103 controls the electric linear slide 11 to move, driving the sampling tube 13 and the vacuum suction cup 17 against the inner wall of the negative pressure stainless steel packaging barrel 100. During the movement, the finished 1,3-propane sultone crystal powder is collected into the sampling tube 13, and the vacuum sampling pump 16 is started to extract the powder from the sampling tube 13, completing the sampling operation;

[0053] Step 2: The detection controller 103 controls the feed solenoid valve 21 to open. After the sampled powder enters the temporary storage box 22, the feed solenoid valve 21 is closed and the air shutoff 26 is opened. The powder is allowed to settle in the temporary storage box 22. The discharge solenoid valve 24 is then controlled to open. The powder enters the sealed grinding device 25 from the discharge funnel 23. The sealed grinding device 25 is started to grind the powder to 3000 mesh for the second time and then stops. The discharge solenoid valve 31 is opened and the powder falls into the discharge auger 32.

[0054] Step 3: The detection controller 103 controls the spectral sampling solenoid valve 33 to open and the titration sampling solenoid valve 34 to close, and controls the discharging auger 32 to convey a specified weight of powder into the spectral measurement device 101. The spectral measurement device 101 detects the powder and outputs 1,3-propane sultone content data to the detection controller 103 via the USB interface. The detection controller 103 controls the spectral sampling solenoid valve 33 to close and the titration sampling solenoid valve 34 to open, conveying a specified weight of powder into the free acid measurement device 102. The free acid measurement device 102 detects the acid value of the powder and calculates the moisture content, and transmits the test results to the detection controller 103 via the USB interface.

[0055] In step 4, the detection controller 103 determines whether the detection value is qualified based on the threshold value and displays it through the industrial touch screen 105.

[0056] The implementation principle of a device and method for determining the content of 1,3-propane sultone in an embodiment of the present invention is as follows:

[0057] Now, it is necessary to determine the content of a batch of finished 1,3-propane sultone. First, the detection controller 103 controls the movement of the electric linear slide 11, driving the sampling tube 13 and the vacuum suction cup 17 to press against the inner wall of the negative pressure stainless steel packaging barrel 100. During the movement, the finished 1,3-propane sultone crystal powder is collected into the sampling tube 13. The vacuum sampling pump 16 is started to extract the powder from the sampling tube 13, completing the sampling operation.

[0058] The detection controller 103 controls the feed solenoid valve 21 to open. After the sampled powder enters the temporary storage box 22, the feed solenoid valve 21 is closed and the air shutoff 26 is opened. The powder settles in the temporary storage box 22. The discharge solenoid valve 24 is then controlled to open. The powder enters the sealed grinding device 25 from the discharge funnel 23. The sealed grinding device 25 is started to grind the powder to 3000 mesh for the second time and then stops. The discharge solenoid valve 31 is opened and the powder falls into the discharge auger 32.

[0059] The detection controller 103 controls the spectral sampling solenoid valve 33 to open and the titration sampling solenoid valve 34 to close. It also controls the discharging auger 32 to convey 20 g of powder into the spectral measurement device 101. The spectral measurement device 101 detects the powder and outputs the 1,3-propane sultone content data of 99.938% to the detection controller 103 via the USB interface. The spectral sampling solenoid valve 33 is closed and the titration sampling solenoid valve 34 is opened to convey 20 g of powder into the free acid measurement device 102. The free acid measurement device 102 detects the acid value of the powder and calculates the moisture content. The acidity source is hydrofluoric acid, the content is 6.8 ppm, and the moisture content is 31.5 ppm. The test results are transmitted to the detection controller 103 via the USB interface.

[0060] The detection controller 103 determines whether the detection value is qualified based on the threshold value. The threshold value of 1,3-propane sultone content is 99.90%, the hydrofluoric acid content is 10ppm, and the moisture content is 40ppm. After analysis, the finished product 1,3-propane sultone of this batch is qualified. The qualified product is displayed on the industrial touch screen 105 and the detection data is displayed.

[0061] The above are all preferred embodiments of the present invention, and are not intended to limit the scope of protection of the present invention. Therefore, any equivalent changes made based on the structure, shape, and principle of the present invention should be included in the scope of protection of the present invention.

Claims

1. A device for measuring the content of 1,3-propane sultone, characterized in that: The invention comprises a sampling device, a solid-state sampling device, a spectrum measuring device (101), a free acid measuring device (102) and a chip-based detection controller (103). The sampling device is arranged on one side of a negative pressure stainless steel packaging barrel (100). The sampling port of the sampling device is connected to the internal space of the negative pressure stainless steel packaging barrel (100). The finished product 1,3-propane sultone crystal powder is sampled by negative pressure adsorption and the powder is fed into the solid-state sampling device. The solid-state sampling device grinds the finished product 1,3-propane sultone crystal powder twice before detection. The solid-state sampling device is provided with a spectrum sampling port and a titration sampling port, the spectrum sampling port is connected to the sampling port of the spectrum measuring device (101), the spectrum measuring device (101) realizes the determination of the content of 1,3-propane sultone, the titration sampling port is connected to the sampling port of the free acid measuring device, the free acid measuring device realizes the determination of the free acid, and the detection controller (103) is respectively connected to the data output ports of the spectrum measuring device (101) and the free acid measuring device (102), and is used to integrate the detection data, make a judgment on whether the detection data is qualified, and display it; The sampling device comprises an electric linear slide (11), an integrated block (12), a sampling tube (13), a delivery hose (14), a sample outlet tube (15) and a vacuum sampling pump (16). The bottom of the track of the electric linear slide (11) is fixedly mounted on the bottom of the inner wall of a negative pressure stainless steel packaging barrel (100). An inlet is provided on one side of the integrated block (12), an outlet is provided on the top, and a sampling channel is provided inside. The sampling channel connects the inlet and the outlet. The bottom of the integrated block (12) is mounted on the slider of the electric linear slide (11) and moves left and right with the slider. The electric linear slide (11) is driven to move, one end of the sampling tube (13) is connected to the inlet of the integrated block (12), and when the slider of the electric linear slide (11) moves, the other end of the sampling tube (13) is driven to insert into the finished 1,3-propane sultone crystal powder in the negative pressure stainless steel packaging barrel (100) and press against the side wall of the negative pressure stainless steel packaging barrel (100), one end of the sampling tube (15) is connected to the other end of the sampling tube (13), the inlet of the vacuum sampling pump (16) is connected to the other end of the sampling tube (15), and the outlet is connected to the inlet of the solid-state sampling device.

2. A 1,3-propane sultone content measuring device according to claim 1, characterized in that: The sampling device further comprises a vacuum suction cup (17), and the vacuum suction cup (17) is arranged at the end of the sampling tube (13).

3. A 1,3-propane sultone content measuring device according to claim 2, characterized in that: All components of the sampling device are made of materials resistant to hydrofluoric acid.

4. A 1,3-propane sultone content measuring device according to claim 2, characterized in that: The solid-state sampling device comprises a feeding solenoid valve (21), an air lock (26), a temporary storage box (22), a discharge funnel (23), a discharge solenoid valve (24), a sealed grinding device (25) and a sample discharge control device, wherein the feeding solenoid valve (21) is arranged at the outlet end of the sample discharge tube (15), the top inlet of the temporary storage box (22) is communicated with the outlet of the feeding solenoid valve (21) through the air lock (26), the discharge funnel (23) is arranged at the bottom outlet of the temporary storage box (22), the discharge solenoid valve (24) is arranged at the bottom outlet of the discharge funnel (23), the outlet of the discharge solenoid valve (24) is communicated with the feeding port at the top of the sealed grinding device (25) through a pipeline, the inlet of the sample discharge control device is communicated with the outlet of the sealed grinding device (25), and the sample discharge control device is provided with a spectral sample outlet and a titration sample outlet.

5. A 1,3-propane sultone content measuring device according to claim 4, characterized in that: The sample discharging control device comprises a blanking solenoid valve (31), a discharging auger (32), a spectral sample discharging solenoid valve (33) and a titration sample discharging solenoid valve (34). The inlet of the discharging auger (32) is connected to the outlet at the bottom of the sealing grinding device (25) through the blanking solenoid valve (31). The discharging auger (32) is provided with two outlets, and the spectral sample discharging solenoid valve (33) and the titration sample discharging solenoid valve (34) are respectively provided at the two outlets.

6. A 1,3-propane sultone content measuring device according to claim 5, characterized in that: The discharging auger (32) is a small weighing auger.

7. A 1,3-propane sultone content measuring device according to claim 1, characterized in that: The spectrum measuring device (101) is an Agilent gas chromatograph, and the free acid measuring device (102) is a fully automatic potentiometric titrator.

8. A 1,3-propane sultone content measuring device according to claim 5, characterized in that: The detection controller (103) includes a chip-based main control circuit board (104), an industrial touch display screen (105), a USB data interface (106) and a memory (107). The main control circuit board (104) is respectively connected to the data interfaces of the spectrum measurement device (101) and the free acid measurement device (102) via the USB data interface (106). The industrial touch display screen (105), the USB data interface (106) and the memory (107) are respectively connected to the main control circuit board (104). The main control circuit board (104) is also connected to various electrical components of the sampling device and the solid-state sampling device for controlling the sampling action of the sampling device and controlling the injection amount and injection action of the solid-state sampling device.

9. A method for determining the content of 1,3-propane sultone, characterized in that: The 1,3-propane sultone content determination device according to claim 8 is used to determine the content of the finished product 1,3-propane sultone in the negative pressure stainless steel packaging barrel (100), and the specific method is: Step 1: The detection controller (103) controls the electric linear slide (11) to move, drives the sampling tube (13) and the vacuum suction cup (17) to press against the inner wall of the negative pressure stainless steel packaging barrel (100), collects the finished product 1,3-propane sultone crystal powder into the sampling tube (13) during the movement, starts the vacuum sampling pump (16) to extract the powder in the sampling tube (13), and completes the sampling action; Step 2: The detection controller (103) controls the feed solenoid valve (21) to open. After the sampled powder enters the temporary storage box (22), the feed solenoid valve (21) is closed and the air shutoff device (26) is opened. The powder is precipitated in the temporary storage box (22). The discharge solenoid valve (24) is then controlled to open. The powder enters the sealed grinding device (25) from the discharge funnel (23). The sealed grinding device (25) is started to grind the powder for the second time to 3000 mesh and then stops. The discharge solenoid valve (31) is opened and the powder falls into the discharge auger (32). Step 3: The detection controller (103) controls the spectrum sample discharging solenoid valve (33) to open and the titration sample discharging solenoid valve (34) to close, and controls the discharging auger (32) to convey a specified weight of powder into the spectrum measuring device (101). The spectrum measuring device (101) detects the powder and outputs 1,3-propane sultone content data to the detection controller (103) through the USB interface. The spectrum sample discharging solenoid valve (33) is controlled to close and the titration sample discharging solenoid valve (34) is controlled to open, conveying a specified weight of powder into the free acid measuring device (102). The free acid measuring device (102) detects the acid value of the powder and calculates the moisture content, and transmits the detection result to the detection controller (103) through the USB interface. In step 4, the detection controller (103) determines whether the detection value is qualified based on the threshold value and displays it through the industrial touch screen (105).

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