CN114813616A - Device and method for detecting carbon content in lithium iron phosphate - Google Patents
Device and method for detecting carbon content in lithium iron phosphate Download PDFInfo
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- CN114813616A CN114813616A CN202210746636.5A CN202210746636A CN114813616A CN 114813616 A CN114813616 A CN 114813616A CN 202210746636 A CN202210746636 A CN 202210746636A CN 114813616 A CN114813616 A CN 114813616A
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- Prior art keywords
- pipe
- iron phosphate
- lithium iron
- heating tank
- tank body
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 78
- 239000007789 gas Substances 0.000 claims abstract description 58
- 239000000463 material Substances 0.000 claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- 230000007246 mechanism Effects 0.000 claims abstract description 27
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 claims abstract description 23
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007773 negative electrode material Substances 0.000 claims abstract description 15
- 239000001301 oxygen Substances 0.000 claims abstract description 15
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 15
- 238000012216 screening Methods 0.000 claims abstract description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000007789 sealing Methods 0.000 claims abstract description 13
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 11
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 11
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims abstract description 8
- 238000002347 injection Methods 0.000 claims abstract description 8
- 239000007924 injection Substances 0.000 claims abstract description 8
- 238000004458 analytical method Methods 0.000 claims abstract description 7
- 238000005086 pumping Methods 0.000 claims description 38
- 238000003860 storage Methods 0.000 claims description 32
- 239000004744 fabric Substances 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 15
- 238000011084 recovery Methods 0.000 claims description 15
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 14
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 12
- 239000000920 calcium hydroxide Substances 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 12
- 239000000945 filler Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 10
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000010406 cathode material Substances 0.000 claims description 2
- 125000003003 spiro group Chemical group 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 238000004804 winding Methods 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims 1
- 239000002893 slag Substances 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 235000011116 calcium hydroxide Nutrition 0.000 description 9
- 239000013078 crystal Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000004891 communication Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 ferrous iron ion Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Images
Classifications
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
-
- 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
-
- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses equipment and a method for detecting the carbon content in lithium iron phosphate, and relates to the technical field of lithium iron phosphate battery material detection. The device comprises a carbon-sulfur analyzer, wherein a screening mechanism is arranged at the acquisition end of the carbon-sulfur analyzer; the screening mechanism comprises a heating tank body, a sealing upper cover with a gas discharge pipe is installed at the top end of the heating tank body, and an oxygen injection pipe is fixedly connected to one side of the outer portion of the heating tank body. According to the invention, the terminal negative electrode material of the lithium iron phosphate battery is firstly introduced into the reaction tank with the stirring function, then the sulfuric acid solution is filled into the reaction tank, so that substances in the negative electrode material, which react with the acid solution, are removed in advance, then the reacted solution slag is dried and put into the heating tank, and the carbon element in the negative electrode material of the lithium iron phosphate battery reacts with oxygen to produce carbon dioxide by filling pure oxygen to react with the solution slag, and finally the carbon element and the oxygen are introduced into the carbon-sulfur analyzer for analysis, so that the accuracy of actual detection data is improved.
Description
Technical Field
The invention relates to the technical field of lithium iron phosphate battery material detection, in particular to equipment and a method for detecting the carbon content in lithium iron phosphate.
Background
In the preparation process of lithium iron phosphate battery, when carbon content is low in the lithium iron phosphate battery negative pole, the proportion of oxidation of ferrous iron ion in the material is big, thereby can cause sample purity to reduce, in addition when carbon content is too high in the lithium iron phosphate material, can influence the tap density of material, cause the gram capacity of material low, also can bring a lot of adverse effects for the processability when carbon content is too high, need detect carbon content in the lithium iron phosphate battery negative pole for this when preparing the lithium iron phosphate battery.
When the lithium iron phosphate battery is charged, positive lithium ions migrate to the surface of the crystal from the positive lithium iron phosphate crystal, enter the electrolyte under the action of an electric field force, then pass through the diaphragm, migrate to the surface of the negative graphite crystal through the electrolyte, and finally are embedded into the graphite lattice, so that when the carbon content in the lithium iron phosphate battery is actually detected, ions embedded into the surface of the graphite crystal need to be removed, and the carbon content in the lithium iron phosphate is detected in the current stage, most of the ways of the acidic solvent reacting with the graphite crystal are adopted, after the ions are removed, the ions are filtered, and finally the undissolved parts are dried and weighed, so that the numerical value of the carbon content is obtained, but when the way is actually detected, carbon-containing gas is generated during the actual reaction, and can be taken away by the carbon-containing gas, so that the data obtained by the traditional way is inaccurate, therefore, the present application provides a method for detecting the carbon content in lithium iron phosphate and a device used in the method to solve the above problems.
Disclosure of Invention
The invention aims to provide equipment and a method for detecting the carbon content in lithium iron phosphate so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the device for detecting the carbon content in the lithium iron phosphate comprises a carbon-sulfur analyzer, wherein a screening mechanism is installed at the acquisition end of the carbon-sulfur analyzer;
the screening mechanism comprises a heating tank body, a sealing upper cover with a gas discharge pipe is mounted at the top end of the heating tank body, an oxygen injection pipe is fixedly connected to one side of the outer part of the heating tank body, one end of the gas discharge pipe is fixedly communicated with a collecting end of the carbon-sulfur analyzer, and a material distribution assembly, an adjusting assembly and a gas collection assembly are sequentially mounted inside the heating tank body from outside to inside;
the gas collecting assembly comprises a gas collecting pipe, one end of the outside of the gas collecting pipe is fixed and communicated with one end of the oxygen injection pipe, the bottom of the gas collecting pipe is fixed with the bottom end of the inside of the heating tank body, and a flow guide pipe is arranged at the top of the gas collecting pipe;
the adjusting assembly comprises an adjusting cover, through holes are fully distributed in the adjusting cover, the top end of the adjusting cover is fixed with the bottom end in the flow guide pipe, and the bottom end of the adjusting cover is fixedly connected with an adjusting turning plate;
the cloth subassembly includes the cloth motor, and the cloth motor is fixed the bottom of the heating jar body, the output fixedly connected with screw thread post of cloth motor, the top of screw thread post is run through the bottom of the heating jar body, cloth screw and screwed pipe are installed from bottom to top to the outside of screw thread post, and the top of screwed pipe is fixed with the inside storage basin that is covered with the through-hole, the inside of storage basin with the one end of board is turned over in the regulation contacts.
Furthermore, the outer wall of the material storage basin and the outer wall of the adjusting cover are respectively attached to two ends of the inner wall of the gas collecting pipe.
Furthermore, the cloth screw includes the fitting ring, the inner wall of fitting ring with the outer wall looks spiro union of screw thread post, the outer wall fixedly connected with screw of fitting ring, the bottom fixedly connected with cloth of screw is protruding, the bellied bottom of cloth with the bottom of the internal portion of heating tank contacts.
Furthermore, the honeycomb duct is integrally of an inverted funnel structure, one end of the outside of the honeycomb duct is fixedly connected with an adding pipe, a through hole is formed in one end of the outside of the adjusting cover, one end of the adding pipe penetrates through the upper sealing cover to be communicated with the outside of the heating tank body, and the other end of the adding pipe penetrates through the through hole to be communicated with the inside of the material storage basin.
Furthermore, a particle catcher is screwed at one end inside the guide pipe, a supporting handle is fixedly connected to the top of the particle catcher, and a stainless steel filter screen is installed inside the particle catcher.
Furthermore, the two sides of one end outside the flow guide pipe are respectively and fixedly connected with a stressed handle, the stressed handle is made of glass, and the overall appearance structure of the stressed handle is an annular structure.
Furthermore, one end of the top of the sealing upper cover is provided with a communicating valve pipe which is matched with the adding pipe.
Furthermore, the output of the internal portion of the heating tank is a heating resistor, the heating resistor is integrally fixed on the inner wall of the heating tank in a spiral winding manner, one side of the external portion of the heating tank is fixedly connected with an inlet pipe, the heating tank and the gas collecting pipe are communicated through the inlet pipe, the pumping pump is installed at the other end of the inlet pipe, and the pumping end of the pumping pump is provided with a pretreatment mechanism.
Furthermore, the pretreatment mechanism comprises a dissolving component and a baking component, the dissolving component comprises a recovery tank, one end of the outer part of the recovery tank is provided with a liquid outlet pipe, the top of the recovery tank is provided with a liquid pump, the output end of the liquid pump is provided with a communicating pipe, and one end of the communicating pipe is fixedly provided with a storage component;
the baking assembly comprises a baking box, a material pumping pipe is fixedly connected between one end of the outside of the baking box and the bottom of the storage assembly, a belt pipe air collecting cover is installed on one side of the outside of the baking box, one end of the belt pipe air collecting cover is fixedly communicated with the material pumping end of the material pumping pump, the other end of the outside of the baking box is provided with the material pumping pipe, and the material pumping air pump is installed at one end of the material pumping pipe.
Furthermore, the storage component comprises a reaction cylinder, a sealing cover is screwed on the top of the reaction cylinder, a filler pipe is fixedly connected to one side of the outside of the reaction cylinder, a funnel is placed on one end of the outside of the filler pipe, a micro motor is fixedly connected to the bottom of the reaction cylinder, a stirring paddle is rotatably connected to the bottom of the inside of the reaction cylinder, and the output end of the micro motor penetrates through the bottom of the reaction cylinder and is fixed to the bottom of the stirring paddle.
In order to achieve the purpose, the invention also provides the following technical scheme: the method for detecting the carbon content in the lithium iron phosphate comprises the following detection steps:
step one, pouring a negative electrode material in a lithium iron phosphate battery into the reaction cylinder through a filler pipe, and pouring a sulfuric acid solution into the reaction cylinder from the filler pipe;
step two, driving a stirring paddle to rotate for 10 mm to 15min by a micro motor through an external controller, and pumping reaction liquid into a recovery tank for recovery through a liquid pump after stirring treatment;
thirdly, a material pumping air pump works to pump the reacted raw materials into a baking box, the temperature of the baking box is 200 +/-20 ℃, the raw materials are dried for 3-5 hours, and then the dried raw materials are conveyed into a heating tank body by the material pumping air pump;
filling pure oxygen into the heating tank body, then heating the heating tank body to keep the internal temperature at 260 +/-20 ℃ for 2-2.5 hours, and adding calcium hydroxide slurry to a storage basin in the heating tank body before heating, wherein the ratio of the calcium hydroxide slurry to the cathode material is 2: 1;
and fifthly, reacting the raw materials in the heating tank body with pure oxygen to generate carbon dioxide gas and sulfur dioxide gas, reacting and eliminating the sulfur dioxide gas and the calcium hydroxide slurry, and allowing the carbon dioxide gas to enter a carbon-sulfur analyzer along a gas discharge pipe for analysis.
Compared with the prior art, the invention has the beneficial effects that:
this detect equipment and method of carbon content in lithium iron phosphate, through leading-in the retort that has stirring function earlier with lithium iron phosphate battery terminal negative electrode material, fill sulphuric acid solution in the retort again, make the material of reacting with the acid solution in the negative electrode material rejected in advance, solution sediment stoving processing after through reacting, and put into the heating jar and react rather than through filling pure oxygen, make carbon element and oxygen reaction production carbon dioxide in the lithium iron phosphate battery negative electrode material, and finally lead to the setting of carrying out the analysis in the carbon sulfur analysis appearance, the precision of actual detection data has been improved.
In addition, through the arranged material distribution assembly, the contact area between the detection raw material and the reaction additive material and oxygen can be increased during actual reaction, the actual reaction rate is increased, and the time required for measuring the lithium iron phosphate is indirectly shortened.
Drawings
FIG. 1 is an isometric view of the present invention;
FIG. 2 is a structural composition diagram of a pretreatment mechanism in the rack of the present invention;
FIG. 3 is a structural assembly view of the dissolution unit of the present invention;
FIG. 4 is an isometric view of a toasting assembly in accordance with the present invention;
FIG. 5 is an internal structural view of the bake assembly of the present invention;
FIG. 6 is a structural component view of the storage assembly of the present invention;
FIG. 7 is a front cross-sectional view of the sifting mechanism of the present invention;
FIG. 8 is a view showing an assembled configuration of the heating tank body according to the present invention;
FIG. 9 is a view of the assembled components of the heating tank body of the present invention;
FIG. 10 is a structural assembly view of the cloth assembly of the present invention;
FIG. 11 is a bottom view of the adjustment assembly of the present invention;
FIG. 12 is a top view of the adjustment assembly of the present invention;
fig. 13 is an isometric view of a gas collection assembly of the present invention.
In the figure: 1. placing a rack; 2. a pretreatment mechanism; 21. a dissolution component; 211. a communicating pipe; 212. a liquid outlet pipe; 213. a recovery tank; 214. a liquid pump; 22. a baking assembly; 221. baking the box; 222. a material pumping air pump; 223. drawing a pipe; 224. a bake plate; 225. a wind collecting cover with a pipe; 226. a material pumping pipe; 227. baking the resistor; 3. an extension frame; 4. a carbon sulfur analyzer; 5. a screening mechanism; 51. heating the tank body; 52. an oxygen injection pipe; 53. a feed pipe; 54. a gas discharge pipe; 55. a valve pipe is communicated; 56. sealing the upper cover; 57. a heating resistor; 6. a material pumping pump; 7. a storage component; 71. a reaction cylinder; 72. a sealing cover; 73. placing a funnel; 74. a filler tube; 75. a communication gap; 76. a micro motor; 77. a stirring paddle; 8. a cloth component; 81. a cloth motor; 82. a threaded post; 83. a cloth propeller; 84. a material storage basin; 85. a threaded pipe; 86. the cloth is raised; 9. an adjustment assembly; 91. an adjustment cover; 92. adjusting the turning plate; 93. a connecting arm; 94. a communicating hole; 95. a through hole; 10. a gas collection assembly; 101. a gas collecting pipe; 102. a stressed handle; 103. an addition pipe; 104. a particle trap; 105. and a flow guide pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that in the description of the present invention, the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, which are only for convenience of description and simplification of description, and do not indicate or imply that the referred device or element must have a specific orientation, be configured in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
Further, it will be appreciated that the dimensions of the various elements shown in the figures are not drawn to scale, for ease of description, and that the thickness or width of some layers may be exaggerated relative to other layers, for example.
It should be noted that like reference numerals and letters refer to like items in the following figures, and thus, once an item is defined or illustrated in one figure, it will not need to be further discussed or illustrated in detail in the description of the following figure.
As shown in fig. 1 to 13, the present invention provides a technical solution: the device for detecting the carbon content in the lithium iron phosphate comprises a carbon-sulfur analyzer 4.
It should be noted that, carbon sulfur analyzer 4 is a prior art device that uses in the iron and steel material detection field in this application, it should be emphasized that, in this application, carbon sulfur analyzer 4 is infrared absorption analyzer, through the device through with the high temperature heating of the carbon under the oxygen-rich condition in the sample, the oxidation is carbon dioxide, and let gas enter corresponding absorption cell, absorb corresponding infrared radiation, it is the signal to retransmit by the detector, output result through computer processing, finally obtain the content of carbon in the lithium iron phosphate, wherein need supplement be, in this application, the concrete model of carbon sulfur analyzer 4 is the sharp 5 high frequency infrared carbon sulfur analyzer of Bao ying scientific and technological production.
It should be further noted that, in the present application, the carbon sulfur analyzer 4 needs to be equipped with a processing system having the screening mechanism 5 as a main processing member.
The following begins a detailed description of the processing system:
wherein refer to fig. 1 to know, screening mechanism 5 is installed at the collection end department of carbon sulfur analyzer 4 in this application, refer to fig. 7 and 8 to know, in this application, screening mechanism 5 includes heating tank 51, the sealed upper cover 56 that has gas discharge pipe 54 is installed on the top of heating tank 51, one side fixedly connected with oxygen injection pipe 52 of heating tank 51 outside, one end of gas discharge pipe 54 and the collection end of carbon sulfur analyzer 4 are fixed and communicate, material distribution component 8, adjusting part 9 and gas collection component 10 are installed from outside to inside in proper order to heating tank 51, wherein material distribution component 8 has played the effect for laying the lithium iron phosphate negative pole material, adjusting part 9 has played the effect for laying the raw materials that absorb sulfur dioxide in the reactant gas, wherein gas collection component 10 has played the effect of leading-in reactant gas into carbon sulfur analyzer 4.
It should be further noted that, in the present application, one end of the top of the upper sealing cover 56 is provided with a communicating valve pipe 55, the communicating valve pipe 55 is matched with the adding pipe 103, and the adding pipe 103 is communicated with the outside of the heating tank 51 through the communicating valve pipe 55, and it should be emphasized that, in the present application, the communicating valve pipe 55 is a pipeline with an electronic butterfly valve installed inside, and the sealing of the heating tank 51 when the calcium hydroxide slurry is injected is realized by closing the electronic butterfly valve.
It should also be noted that, the output end inside the heating tank 51 is heating resistor 57 in this application, heating resistor 57 is wholly spirally wound and fixed on the inner wall of the heating tank 51, one side fixedly connected with inlet pipe 53 outside the heating tank 51, one end of inlet pipe 53 is fixed and communicated with one side outside the gas collecting pipe 101, material pumping pump 6 is installed at the other end of inlet pipe 53, pretreatment mechanism 2 is installed at the material pumping end of material pumping pump 6, wherein, screening mechanism 5 and pretreatment mechanism 2 constitute the treatment system of the device.
Beginning with the description of the features of the gas collecting assembly 10 in the screening mechanism 5, referring to fig. 13, in the present application, the gas collecting assembly 10 includes a gas collecting tube 101, one end of the exterior of the gas collecting tube 101 is fixed and communicated with one end of the oxygen injecting tube 52, the bottom of the gas collecting tube 101 is fixed with the bottom of the interior of the heating tank 51, a guiding tube 105 is disposed on the top of the gas collecting tube 101, wherein two times of the exterior end of the guiding tube 105 are respectively and fixedly connected with a stressed handle 102, the stressed handle 102 is made of glass, the overall appearance structure of the stressed handle 102 is a ring structure, in the present application, the guiding tube 105 is integrally inverted funnel structure, one end of the exterior of the guiding tube 105 is fixedly connected with an adding tube 103, one end of the exterior of the adjusting hood 91 is provided with a through hole 95, one end of the adding tube 103 penetrates through the sealing upper cover 56 and is communicated with the exterior of the heating tank 51, the other end of the adding pipe 103 is communicated with the inside of the storing basin 84 through the through hole 95. Further, a particle trap 104 is screwed to an end of the inside of the flow guide tube 105, and a support handle is fixedly connected to a top of the particle trap 104, wherein a stainless steel screen is installed inside the particle trap 104, it should be noted that, in the present application, the particle trap 104 is a ceramic filter originally installed in an exhaust system of a diesel engine, and the inside thereof is generally provided with a stainless steel screen through which particulate emissions can be captured and blocked before entering the atmosphere.
Starting with a detailed description of the features of the adjusting assembly 9 in the screening mechanism 5, it can be seen from fig. 11 and 12 that the adjusting assembly 9 includes an adjusting cover 91 with through holes distributed therein, wherein the top end of the adjusting cover 91 is fixed to the bottom end of the flow guide pipe 105, an adjusting turning plate 92 is fixedly connected to the bottom end of the adjusting cover 91, a connecting arm 93 is fixed to the top of the adjusting cover 91, a communication hole 94 is formed in the top of the adjusting cover 91, wherein the connecting arm 93 is fixed to the flow guide pipe 105, and the communication hole 94 is used for conveying gas.
Finally, the characteristics of the material distribution assembly 8 in the screening mechanism 5 will be described in detail, wherein, referring to fig. 10, it can be seen that the material distribution assembly 8 includes a material distribution motor 81, the material distribution motor 81 is fixed at the bottom of the heating tank 51, the output end of the material distribution motor 81 is fixedly connected with a threaded column 82, the top end of the threaded column 82 penetrates through the bottom of the heating tank 51, and a material distribution screw 83 and a threaded pipe 85 are installed from bottom to top, the top end of the threaded pipe 85 is fixed with a material storage basin 84 with through holes fully distributed therein, the interior of the material storage basin 84 is in contact with one end of an adjusting turning plate 92, in addition, in the present application, the outer wall of the material storage basin 84 and the outer wall of the adjusting cover 91 are respectively attached to the two ends of the inner wall of the gas collection pipe 101, it should be noted that, wherein the material distribution screw 83 includes an assembly ring, the inner wall of the assembly ring is screwed to the outer wall of the threaded column 82, a screw is fixedly connected to the outer wall of the assembly ring, the protruding 86 of bottom fixedly connected with cloth of screw, the bottom of the protruding 86 of cloth contacts with the inside bottom of the heating jar body 51, it needs to emphasize, this device is when specifically using, when the raw materials enters into the inside of collecting main 101, cloth motor 81 is through driving screw thread post 82, make screw thread post 82 rotate through driving cloth screw 83 and screwed pipe 85, the protruding 86 of cloth that has not only realized cloth screw 83 bottom when rotating, promote the raw materials and make it disperse and spread in the inside of collecting main 101, and also realized throwing in the calcium hydrate slurry on adjusting cover 91, through the separation of pivoted storage basin 84 and the regulation that keeps motionless turning plate 92, make the calcium hydrate slurry disperse and spread in storage basin 84.
Starting with the description of the pretreatment mechanism 2, it can be seen from fig. 2 that in the present application, the pretreatment mechanism comprises a dissolving assembly 21 and a baking assembly 22, the dissolving assembly 21 comprises a recovery tank 213, a liquid outlet pipe 212 is installed at one end outside the recovery tank 213, a liquid pump 214 is installed at the top of the recovery tank 213, a communicating pipe 211 is installed at the output end of the liquid pump 214, and a storage assembly 7 is fixed at one end of the communicating pipe 211.
Now, the description starts on the toasting assembly 22, wherein it can be seen from fig. 4 and 5, in the application, the toasting assembly 22 includes a toasting box 221, it is emphasized that in the present application, the output end of the toasting box 221 is a toasting disc 224, the bottom of the toasting disc 224 is provided with a toasting resistor 227, the toasting disc 224 is installed on the top of the toasting box 221, furthermore, a pumping pipe 226 is fixedly connected between one end of the exterior of the toasting box 221 and the bottom of the storage assembly 7, one side of the exterior of the toasting box 221 is provided with a pipe-equipped air-collecting hood 225, one end of the pipe-equipped air-collecting hood 225 is fixedly connected and communicated with the pumping end of the pumping pump 6, the other end of the exterior of the toasting box 221 is provided with a pumping pipe 223, one end of the pumping pipe 223 is provided with a pumping air pump 222, wherein the toasting assembly 22 plays a role of carrying out the toasting treatment of the solution adhered to the pre-treated raw material.
The storage assembly 7 will be described in detail with reference to fig. 6, wherein in this application, the storage assembly includes a reaction cylinder 71, a sealing cover 72 is screwed on a top of the reaction cylinder 71, a filler pipe 74 is fixedly connected to one side of an outside of the reaction cylinder 71, a placing funnel 73 is fixedly connected to one end of the outside of the filler pipe 74, a micro motor 76 is fixedly connected to a bottom of the reaction cylinder 71, a stirring paddle 77 is rotatably connected to a bottom end of the inside of the reaction cylinder 71, and an output end of the micro motor 76 penetrates through the bottom of the reaction cylinder 71 and the stirring paddle 77 and is fixed, wherein the storage assembly 7 drives the stirring paddle 77 to rotate through the micro motor 76 when the storage assembly is in specific operation, so as to accelerate a reaction rate of a negative electrode material with a sulfuric acid solution.
In addition, it should be noted that, referring to fig. 1, the storage assembly 7 and the pretreatment mechanism 2 are both fixedly installed in the placement frame 1, and the extension frame 3 is further fixed outside the placement frame 1, wherein the sieving mechanism 5 is fixedly installed inside the extension frame 3, it should be further noted that, in this application, the device first passes the negative electrode material at the terminal of the lithium iron phosphate battery through a reaction tank with a stirring function, and fills a sulfuric acid solution into the reaction tank, so that substances in the negative electrode material that react with the acid solution are removed in advance, then dries the reacted solution slag, and puts the solution slag into the heating tank to react with the negative electrode material through filling pure oxygen, so that carbon in the negative electrode material of the lithium iron phosphate battery reacts with oxygen to produce carbon dioxide, and finally introduces the carbon dioxide and sulfur into the carbon sulfur analyzer 4 for analysis.
The method for detecting the carbon content in the lithium iron phosphate comprises the following steps:
step one, pouring a negative electrode material in the lithium iron phosphate battery into the reaction cylinder 71 through a filler pipe 74, and pouring a sulfuric acid solution into the reaction cylinder 71 from the filler pipe 74;
step two, driving the stirring paddle 77 to rotate for 10 mm to 15min by the micro motor 76 through an external controller, and after stirring treatment, pumping the reaction liquid into the recovery tank 213 through the liquid pumping pump 214 and recovering the reaction liquid through the liquid outlet pipe 212;
step three, the material pumping air pump 222 works, the reacted raw materials are pumped into the baking box 221 through the material pumping pipe 226 and the communication notch 75, the temperature of the baking box 221 is 200 +/-20 ℃, drying is carried out for 3-5 hours, and then the dried raw materials are conveyed into the heating tank body 51 through the material pumping pump 6;
filling pure oxygen into the heating tank body 51 through the oxygen injection pipe 52, then heating the heating tank body 51 to keep the internal temperature at 260 +/-20 ℃ for 2-2.5 hours, and adding calcium hydroxide slurry to a material storage basin 84 in the heating tank body 51 through an adding pipe 103 before heating, wherein the ratio of the calcium hydroxide slurry to the negative electrode material is 2: 1;
and step five, reacting the raw materials in the heating tank body 51 with pure oxygen to generate carbon dioxide gas and sulfur dioxide gas, reacting and eliminating the sulfur dioxide gas and the calcium hydroxide slurry, and allowing the carbon dioxide gas to enter the carbon-sulfur analyzer 4 along the gas discharge pipe 54 for analysis.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (11)
1. Detect equipment of carbon content in lithium iron phosphate, including carbon sulfur analyzer (4), its characterized in that: a screening mechanism (5) is arranged at the collecting end of the carbon and sulfur analyzer (4);
the screening mechanism (5) comprises a heating tank body (51), a sealing upper cover (56) with a gas discharge pipe (54) is installed at the top end of the heating tank body (51), an oxygen injection pipe (52) is fixedly connected to one side of the outer portion of the heating tank body (51), one end of the gas discharge pipe (54) is fixedly communicated with a collecting end of the carbon-sulfur analyzer (4), and a material distribution assembly (8), an adjusting assembly (9) and a gas collection assembly (10) are sequentially installed inside the heating tank body (51) from outside to inside;
the gas collecting assembly (10) comprises a gas collecting pipe (101), one end of the outside of the gas collecting pipe (101) is fixed and communicated with one end of the oxygen injection pipe (52), the bottom of the gas collecting pipe (101) is fixed with the bottom end of the inside of the heating tank body (51), and a guide pipe (105) is placed at the top of the gas collecting pipe (101);
the adjusting assembly (9) comprises an adjusting cover (91) with through holes distributed therein, the top end of the adjusting cover (91) is fixed with the bottom end of the inside of the guide pipe (105), and the bottom end of the adjusting cover (91) is fixedly connected with an adjusting turning plate (92);
cloth subassembly (8) are including cloth motor (81), and cloth motor (81) are fixed the bottom of the heating jar body (51), the output fixedly connected with screw thread post (82) of cloth motor (81), the top of screw thread post (82) is run through the bottom of the heating jar body (51), cloth screw (83) and screwed pipe (85) are installed from bottom to top to the outside of screw thread post (82), and the top of screwed pipe (85) is fixed with inside storage basin (84) of being covered with the through-hole, the inside of storage basin (84) with the one end of turning over board (92) is contacted in the regulation.
2. The apparatus for detecting carbon content in lithium iron phosphate according to claim 1, characterized in that: the outer wall of the material storage basin (84) and the outer wall of the adjusting cover (91) are respectively attached to two ends of the inner wall of the gas collecting pipe (101).
3. The apparatus for detecting carbon content in lithium iron phosphate according to claim 1, characterized in that: the cloth screw (83) comprises an assembly ring, the inner wall of the assembly ring is in threaded connection with the outer wall of the threaded column (82), the outer wall of the assembly ring is fixedly connected with a screw, the bottom of the screw is fixedly connected with a cloth bulge (86), and the bottom of the cloth bulge (86) is in contact with the bottom inside the heating tank body (51).
4. The apparatus for detecting carbon content in lithium iron phosphate according to claim 1, characterized in that: the whole funnel structure that is put upside down of honeycomb duct (105), honeycomb duct (105) outside one end fixedly connected with add pipe (103), through hole (95) have been seted up to the outside one end of adjusting cover (91), the one end of adding pipe (103) run through sealed upper cover (56) with the outside of the heating jar body (51) is linked together, the other end of adding pipe (103) pass through hole (95) with the inside of storage basin (84) is linked together.
5. The apparatus for detecting carbon content in lithium iron phosphate according to claim 4, wherein: one end of the inside of the flow guide pipe (105) is in threaded connection with a particle catcher (104), the top of the particle catcher (104) is fixedly connected with a supporting handle, and a stainless steel filter screen is arranged inside the particle catcher (104).
6. The apparatus for detecting carbon content in lithium iron phosphate according to claim 4, wherein: both sides of one end of the outer portion of the flow guide pipe (105) are fixedly connected with stressed handles (102) respectively, the stressed handles (102) are made of glass, and the overall appearance structure of the stressed handles (102) is of an annular structure.
7. The apparatus for detecting carbon content in lithium iron phosphate according to claim 4, wherein: and one end of the top of the upper sealing cover (56) is provided with a communicating valve pipe (55), and the communicating valve pipe (55) is matched with the adding pipe (103).
8. The apparatus for detecting carbon content in lithium iron phosphate according to claim 1, characterized in that: the output of the heating tank body (51) inside is heating resistor (57), and heating resistor (57) wholly is spiral winding and fixes on the inner wall of the heating tank body (51), one side fixedly connected with inlet pipe (53) of the heating tank body (51) outside, and the heating tank body (51) is linked together through inlet pipe (53) with gas collecting pipe (101), and material pump (6) are installed to the other end of inlet pipe (53), and preprocessing mechanism (2) are installed to the material end of taking out of material pump (6).
9. The apparatus for detecting carbon content in lithium iron phosphate according to claim 8, wherein: the pretreatment mechanism (2) comprises a dissolving component (21) and a baking component (22), the dissolving component (21) comprises a recovery tank (213), a liquid outlet pipe (212) is installed at one end of the outer portion of the recovery tank (213), a liquid pump (214) is installed at the top of the recovery tank (213), a communicating pipe (211) is installed at the output end of the liquid pump (214), and a storage component (7) is fixed at one end of the communicating pipe (211);
toast subassembly (22) including toasting box (221), fixedly connected with pumping pipe (226) between the outside one end of toasting box (221) and storage subassembly (7) bottom, toast the outside one side of box (221) and install and take a tub wind-collecting cover (225), take the one end of tub wind-collecting cover (225) with the fixed and intercommunication of pumping material end of pumping pump (6), toast the outside other end of box (221) and install pumping pipe (223), pumping material air pump (222) is installed to the one end of pumping pipe (223).
10. The apparatus for detecting carbon content in lithium iron phosphate according to claim 9, characterized in that: storage subassembly (7) include reaction cylinder (71), and the top spiro union of reaction cylinder (71) has sealed lid (72), and one side fixed connection of reaction cylinder (71) outside has filled tube (74), and funnel (73) are placed to the outside one end fixedly connected with of filled tube (74), and bottom fixedly connected with micro motor (76) of reaction cylinder (71), the inside bottom of reaction cylinder (71) is rotated and is connected with stirring rake (77), the bottom that reaction cylinder (71) and stirring rake (77) are run through to the output of micro motor (76) is fixed mutually.
11. The method for detecting the carbon content in the lithium iron phosphate is characterized by comprising the following steps: the method applies the equipment for detecting the carbon content in the lithium iron phosphate according to any one of claims 1 to 10, and comprises the following detection steps:
step one, pouring a negative electrode material in a lithium iron phosphate battery into the reaction cylinder through a filler pipe, and pouring a sulfuric acid solution into the reaction cylinder from the filler pipe;
step two, driving a stirring paddle to rotate for 10 mm to 15min by a micro motor through an external controller, and pumping reaction liquid into a recovery tank for recovery through a liquid pump after stirring treatment;
thirdly, a material pumping air pump works to pump the reacted raw materials into a baking box, the temperature of the baking box is 200 +/-20 ℃, the raw materials are dried for 3-5 hours, and then the dried raw materials are conveyed into a heating tank body by the material pumping air pump;
filling pure oxygen into the heating tank body, heating the heating tank body to keep the internal temperature at 260 +/-20 ℃ for 2-2.5 hours, and adding calcium hydroxide slurry to a storage basin in the heating tank body before heating, wherein the ratio of the calcium hydroxide slurry to the cathode material is 2: 1;
and fifthly, reacting the raw materials in the heating tank body with pure oxygen to generate carbon dioxide gas and sulfur dioxide gas, reacting and eliminating the sulfur dioxide gas and the calcium hydroxide slurry, and allowing the carbon dioxide gas to enter a carbon-sulfur analyzer along a gas discharge pipe for analysis.
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