Accurate measurement method for titanium tetrachloride dust collection slag

Abstract

The invention relates to the technical field of chemical engineering, in particular to an accurate measurement method for titanium tetrachloride dust collection slag, which comprises an operation platform, a drying box placed on the right side of the upper surface of the operation platform and a muffle furnace placed on the right end of the lower side of the operation platform, the drying box comprises a box body, an electric heating piece installed on the lower side surface of the interior of the box body and a supporting platform fixedly installed in the middle of the interior of the box body, a collecting mechanism is placed in the supporting platform, and a lifting mechanism is fixedly installed on the upper side wall of the interior of the box body. According to the method, the situation that a sample in the crucible is splashed or the crucible is exploded in the sample melting process can be avoided, meanwhile, the components of main amount C, volatile components, ash content, TiO2 and microelements in the titanium tetrachloride dust collection slag can be accurately measured, and an index basis is provided for subsequent recycling.

Description

Technical Field

[0001] The invention relates to the technical field of chemical industry, in particular to a method for accurately measuring titanium tetrachloride dust collection residue. Background Art

[0002] There are two main methods for preparing TiCl4 in industry: boiling chlorination method and molten salt chlorination method. In both chlorination methods, unreacted fine particles will be discharged from the furnace with the flue gas and collected by the dust collector. The collected slag mainly includes fine particles of high-titanium slag, petroleum coke and high-boiling point metal chlorides, etc., which are mainly processed by pulping. After pulping, they are separated by filter pressing to separate the filtrate and dust slag. The filtrate is neutralized, and the hydroxide precipitate generated by the metal chloride is separated by the filter press to form hydroxide slag, which is pulled to the slag yard for storage. The filtrate is treated by MVR. The dust slag is usually recovered by flotation + gravity separation. Flotation is used to select coke, and gravity separation is used to select titanium. The separated titanium and coke are returned to production.

[0003] The daily detection method of titanium tetrachloride dust residue is to add cellulose powder to the dust residue sample, press it into shape, and then put it into an X-ray fluorescence spectrometer for analysis. This method can only perform qualitative analysis and observe the trend, but cannot accurately perform quantitative analysis. In the subsequent recycling and reuse process, it is often necessary to know its true component content to facilitate the calculation of indicators such as yield and recovery rate. Therefore, accurate measurement of various indicators is particularly important; secondly, in the process of measuring titanium tetrachloride dust residue TiO2, it needs to be melted at high temperature. However, due to the presence of a large amount of carbon in the dust residue, a large amount of heat will be released during the melting process, causing splashing or damage to the crucible. Splashing will cause inaccurate measurement results, and damage to the crucible will reduce sample measurement efficiency and waste labor costs. Summary of the invention

[0004] In order to overcome the defects in the prior art, the purpose of the present invention is to provide a method for accurately measuring titanium tetrachloride dust residue to solve the problems raised in the above background technology.

[0005] To achieve the above object, the present invention provides a method for accurately measuring titanium tetrachloride dust slag, comprising an operating platform, a drying box placed on the right side of the upper surface of the operating platform, and a muffle furnace placed on the right end of the lower side of the operating platform, comprising the following steps:

[0006] S1. First, the staff will place the collected titanium tetrachloride dust residue into the inner filter cartridge in the collection mechanism, then remove the inner filter cartridge and place it in the sink, seal the drain, and wash the titanium tetrachloride dust residue in the inner filter cartridge with water through the faucet. At the same time, after meeting the liquid-to-solid ratio requirements, repeatedly stir and wash in the sink;

[0007] S2. The washed inner filter cartridge is inserted back into the outer cartridge, and the limit rod is aligned with the auxiliary hole. Then the collecting mechanism is placed as a whole in the placement hole opened on the inner support platform of the drying box, and the limit rod is aligned with the limit hole. At the same time, the filtrate is collected and filtered out, and the filter cake is dried and ground after drying to make it completely dispersed.

[0008] S3. After placing, close the box door and start the electric heating sheet in the drying box to dry. After drying, start and control the cylinder to extend, send the crushing blade and the rotating rod into the inner filter cylinder until the closing plate contacts the inner support ring, start the motor to crush, and make it all pass through the inner filter cylinder;

[0009] S4. The ground filter cake sample and the crushed sample are fully mixed, and then reduced to 10 to 20 g. The reduced samples are placed in ziplock bags and wait for analysis;

[0010] S5. Place the porcelain crucible in a muffle furnace at 850℃±10℃ and burn for 1 hour, take it out, place it in a desiccator to cool for 30 minutes, weigh it to an accuracy of 0.0001g, repeat the burning, weigh it to constant weight, weigh the m1 sample to an accuracy of 0.0001g, place it in the porcelain crucible with constant weight, cover it with a lid, weigh the mass m2 to an accuracy of 0.001g, then place the porcelain crucible in a muffle furnace at 900℃±10℃ and burn for 15 minutes, take it out, and place the porcelain crucible in a desiccator to cool for 30 minutes, then weigh m3 to an accuracy of 0.0001g, measure twice in parallel, take the average value, and obtain the amount of volatile matter;

[0011] Calculation process:

[0012] The original weight of the sample m1

[0013] The mass of the porcelain crucible, cover and sample before firing m2

[0014] The mass of the porcelain crucible, cover and residue after burning m3

[0015] Volatile matter = m3-m2

[0016] Volatile matter ratio = (m3-m2) / m1;

[0017] S6. Weigh the m4 sample and put it into a crucible. Add a solvent to cover the sample. Use a high-frequency infrared carbon-sulfur analyzer to select a suitable carbon standard curve for determination. Read the data directly on the instrument. Measure twice in parallel and take the average value to obtain the carbon content.

[0018] S7, place the porcelain ark in a muffle furnace at 850℃±10℃ and burn for 1 hour, take it out, place it in a desiccator to cool for 30 minutes, weigh it to an accuracy of 0.0001g, repeat the burning, weigh it to constant weight, weigh the m5 sample to an accuracy of 0.0001g, place it in the porcelain ark that has been constant weight, spread it evenly, weigh the total mass to be m6 to an accuracy of 0.0001g, put it in a muffle furnace again, burn it at 850℃±10℃ until it is completely ash, take it out and place it in a desiccator to cool for 30 minutes, weigh the mass to be m7 to an accuracy of 0.0001g, measure it twice in parallel, take the average value, and get the amount of ash;

[0019] Calculation process:

[0020] The original mass of the sample m5

[0021] The quality of porcelain ark m6

[0022] Mass of the porcelain ark and the residue after burning m7

[0023] Ash mass = m7-m6

[0024] Ash content = (m7-m6) / m5;

[0025] S8. Add 3g of sodium peroxide to the bottom of the corundum crucible, weigh m8 ash and put it on the sodium peroxide, and cover it with 3g of sodium peroxide again to ensure that the sodium peroxide completely covers the sample, put the corundum crucible into the muffle furnace, set the heating time to 15 minutes, the heating temperature to 650℃ and the insulation time to 10min respectively, take it out and cool it after melting, cool it to room temperature, wipe the outer wall of the crucible, completely leach the sample, slowly add 60ml of 1:1 hydrochloric acid, 40ml of 1:1 sulfuric acid, 0.1g of iron powder, and 6 aluminum particles, wait until the solution reacts to dark gray, add 20ml of saturated ammonium sulfate solution, cover it with a Geiger funnel, and add 10ml of saturated ammonium sulfate solution to the crucible. Add saturated sodium bicarbonate to the funnel, wait until the aluminum particles are completely dissolved and the solution emits large bubbles, take it out and cool it. At the same time, pay attention to the fact that the saturated sodium bicarbonate solution in the Geiger funnel cannot be evacuated. It should be replenished with saturated sodium bicarbonate solution at any time. Calibrate, remove the Geiger funnel, quickly add 10ml of 300g / L ammonium thiocyanate solution to the conical flask, and immediately titrate with ammonium ferric sulfate standard solution until the test solution turns a stable orange-red color, which is the end point. Make blank samples and parallel samples in the same batch, and take the average of the parallel sample results. Calculate the titanium content based on the amount of ammonium ferric sulfate solution consumed by the sample minus the amount of ammonium ferric sulfate solution consumed by the blank. At the same time, the titanium content in the dust collection residue is inferred based on the titanium content in the ash;

[0026] Calculation process:

[0027] TiO2% (ash content) = M*C1*(V1-V0) / (m8*1000)*100%

[0028] TiO2% (dust collection residue) = TiO2% (ash content) * (m7-m6) / m5

[0029] C1——Molar concentration of ammonium ferric sulfate solution, mol / L

[0030] V1——The volume of ammonium ferric sulfate standard solution consumed by the titration test solution, ml

[0031] V0——The volume of ammonium ferric sulfate standard solution consumed in titrating the blank sample, ml

[0032] m8——ash weight, g

[0033] M——molar mass of titanium dioxide, 79.9 g / mol;

[0034] S9, prepare standard solutions of Si, Al, Ca, Mg, and Mn elements, draw standard curves on ICP, weigh 0.3g sodium tetraborate, 0.9g anhydrous sodium carbonate, and m9 ash sample to be tested in a platinum crucible, mix the reagent and sample evenly in the platinum crucible, put into a muffle furnace, program the temperature to 920°C, keep warm for 10min, take out, cool slightly, then put the mixed sample into a polytetrafluoroethylene beaker, and leach the sample with a boiling 1:1 hydrochloric acid solution until the solution is clear, wash the platinum crucible with distilled water and take it out, transfer the leaching solution to a 100ml colorimetric tube and make up the volume, measure it on ICP, obtain the content of each element according to the intensity of each element peak, directly select the results on the instrument together with the blank test, calculate the content of the trace element in the ash, convert it into the percentage of oxides, and at the same time, infer the content of each oxide in the dust collection slag according to the content of each oxide in the ash;

[0035] Calculation process:

[0036] W=C2*100*10-6 / m9*100%

[0037] The content of each oxide in the ash: the percentage of each trace element in the ash * the molecular weight of the oxide / the molar mass of the element

[0038] XSiO2%(ash content)=WSiO2×2.1392

[0039] XAl2O3%(ash content)=WAl2O3×1.8895

[0040] XCaO% (ash content) = WCaO × 1.3992

[0041] XMgO% (ash content) = WMgO × 1.6582

[0042] XMnO% (ash content) = WMnO × 1.2912

[0043] XCr2O3%(ash content)=WCr2O3×1.4615

[0044] The content of each oxide in the dust collection residue: the percentage of each oxide in the ash * the percentage of ash in the dust collection residue

[0045] YSiO2% (dust collection residue) = XSiO2% (ash content) * (m7-m6) / m5

[0046] YAl2O3% (dust collection) = XAl2O3% (ash content) * (m7-m6) / m5

[0047] YCaO% (dust collection residue) = XCaO% (ash content) * (m7-m6) / m5

[0048] YMgO% (dust collection) = XMgO% (ash content) * (m7-m6) / m5

[0049] YMnO% (dust collection residue) = XMnO% (ash content) * (m7-m6) / m5

[0050] YCr2O3% (dust collection residue) = XCr2O3% (dust collection residue) * (m7-m6) / m5

[0051] Where:

[0052] C2——The value of each element in ICP determination, μg / ml

[0053] m9——mass of the sample, g

[0054] W——Percentage of each trace element in the ash, %

[0055] X——Percentage of each oxide in the ash, %

[0056] Y——the percentage of each oxide in the dust collection residue;

[0057] The above steps use an operating platform, a muffle furnace and a drying box to achieve accurate measurement of titanium tetrachloride dust collection residue;

[0058] Support legs are welded at the four corners of the lower surface of the operating platform, a water tank is arranged on the left side of the upper surface of the operating platform, a faucet is arranged on the left side of the water tank, and an operating table is arranged in the middle of the upper surface of the operating platform;

[0059] The drying box includes a box body, an electric heating plate installed on the lower surface of the box body, and a support platform fixedly installed in the middle position of the box body, a collecting mechanism is placed in the support platform, and a lifting mechanism is fixedly installed on the upper side wall of the box body;

[0060] A placement hole is provided in the middle of the upper surface of the support platform, and limiting holes are provided on the upper surface of the support platform at the left and right sides of the upper end of the placement hole.

[0061] As a further improvement of the present technical solution, the collecting mechanism includes an outer cylinder and an outer support ring welded to the top of the outer cylinder, auxiliary holes are opened on both sides of the upper surface of the outer support ring, an inner filter cylinder is arranged in the outer cylinder, an inner support ring is welded to the top of the inner filter cylinder, and limiting rods are welded on both sides of the lower surface of the inner support ring.

[0062] As a further improvement of the present technical solution, the lifting mechanism includes a closing plate, a motor installed in the middle position of the upper surface of the closing plate, and two cylinders installed on the left and right sides of the upper surface of the closing plate. The lower surface of the closing plate is rotatably connected to a rotating rod, and a number of crushing blades are welded to the side surface of the rotating rod.

[0063] As a further improvement of the technical solution, the mesh number of the inner filter cylinder is 200 meshes, and the outer cylinder is a closed cylinder.

[0064] As a further improvement of the technical solution, a drain outlet which can be closed as needed is provided at the lower end of the water tank, the water-solid ratio of the washing liquid is 3:1 or 4:1, the drying temperature of the drying box is 105°C to 115°C, and the reduction method used is the cone quartering method or the grid method.

[0065] As a further improvement of the technical solution, when measuring volatile matter, after the porcelain crucible is placed in the muffle furnace, the internal temperature of the muffle furnace must be restored to 900°C±10°C within 3 minutes, otherwise the experimental results will be invalidated. The sample mass m4g when measuring the carbon content is between 0.1500g and 0.2000g.

[0066] As a further improvement of the technical solution, when measuring the molten ash content of TiO2, sodium peroxide or potassium pyrosulfate is used. When performing sample analysis, if the sample is too heavy, in order to avoid inaccurate test results, the measurement is performed after separation and dilution.

[0067] As a further improvement of the technical solution, when conducting ash analysis, the burning time is determined according to the ash reduction situation, and it must be ensured that all the samples are ash reduced. When measuring the trace element content, the ICP method is used for analysis or the X-ray fluorescence spectrometer is used for analysis.

[0068] As a further improvement of the technical solution, the molecular mass of the trace element adopts the molecular mass on the periodic table, accurate to two decimal places.

[0069] As a further improvement of the technical solution, an electronic scale for weighing and a crucible tongs auxiliary tool for taking the crucible are placed on the upper surface of the operating table.

[0070] Compared with the prior art, the present invention has the following beneficial effects:

[0071] 1. The accurate measurement method of titanium tetrachloride dust collection residue can accurately know the actual content of each component in the titanium tetrachloride dust collection residue through analysis of the titanium tetrachloride dust collection residue, providing an indicator basis for subsequent recycling.

[0072] 2. The accurate measurement method of titanium tetrachloride dust slag can infer the content of TiO2 and trace elements in the dust slag according to the proportion of ash in the dust slag, which can prevent splashing or crucible damage caused by high carbon content during the melting process, inaccurate measurement and repeated sampling. BRIEF DESCRIPTION OF THE DRAWINGS

[0073] The accompanying drawings described herein are only for explanation purposes and are not intended to limit the scope of the present invention in any way. In addition, the shapes and proportional dimensions of the various components in the figures are only schematic, used to help understand the present invention, and are not specifically limited to the shapes and proportional dimensions of the various components of the present invention. Those skilled in the art can select various possible shapes and proportional dimensions to implement the present invention according to the teachings of the present invention.

[0074] Figure 1 It is a schematic diagram of the overall assembly structure of the present invention;

[0075] Figure 2 It is a schematic diagram of the structure of the operating platform of the present invention;

[0076] Figure 3 It is a schematic diagram of the drying box structure of the present invention;

[0077] Figure 4 It is a schematic diagram of the supporting platform structure of the present invention;

[0078] Figure 5 is a cross-sectional view of the support platform of the present invention;

[0079] Figure 6 It is a schematic diagram of the structure of the collecting mechanism of the present invention;

[0080] Figure 7 It is a schematic diagram of the lifting mechanism structure of the present invention;

[0081] The meaning of each number in the figure is:

[0082] 1. Operating platform; 11. Faucet; 12. Sink; 13. Operating table; 2. Support feet; 3. Muffle furnace;

[0083] 4. Drying box; 41. Box body; 42. Electric heating plate; 43. Support platform; 431. Placement hole; 432. Limit hole; 44. Collecting mechanism; 441. Outer cylinder; 442. Outer support ring; 443. Auxiliary hole; 444. Inner filter cylinder; 445. Inner support ring; 446. Limiting rod; 45. Lifting mechanism; 451. Closing plate; 452. Cylinder; 453. Motor; 454. Crushing blade; 455. Rotating rod. DETAILED DESCRIPTION

[0084] The details of the present invention can be more clearly understood by combining the accompanying drawings with the description of the specific embodiments of the present invention. However, the specific embodiments of the present invention described herein are only used for the purpose of explaining the present invention and cannot be understood as limiting the present invention in any way. Under the guidance of the present invention, technicians can conceive of any possible variations based on the present invention, which should be regarded as falling within the scope of the present invention. The terms "installation" and "connection" should be understood in a broad sense, which can be directly connected or indirectly connected through an intermediate medium.

[0085] The terms "central axis", "vertical", "horizontal", "front", "back", "up", "down", "left", "right", "top", "bottom", "inside", "outside" and the like used herein to indicate positions or positional relationships are based on the positions or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the equipment or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, in the description of the present invention, the meaning of "several" is two or more, unless otherwise clearly and specifically defined.

[0086] See also Figure 1-Figure 7 As shown, the present invention provides a precise measurement method for titanium tetrachloride dust collection slag, comprising an operating platform 1, a drying box 4 placed on the right side of the upper surface of the operating platform 1, and a muffle furnace 3 placed on the right end of the lower side of the operating platform 1, comprising the following steps:

[0087] S1. First, the staff puts the collected titanium tetrachloride dust residue into the inner filter cartridge 444 in the collection mechanism 44, then removes the inner filter cartridge 444 and places it in the water tank 12, seals the drain, and washes the titanium tetrachloride dust residue in the inner filter cartridge 444 with water through the faucet 11. After the liquid-to-solid ratio requirement is met, the dust residue is repeatedly stirred and washed in the water tank;

[0088] S2, the washed inner filter cartridge 444 is inserted back into the outer cartridge 441, and the limiting rod 446 is aligned with the auxiliary hole 443, and then the collecting mechanism 44 is placed as a whole in the placement hole 431 opened on the inner support platform 43 of the drying box 4, and the limiting rod 446 is ensured to be aligned with the limiting hole 432, and the filtrate is collected and filtered out at the same time, and the filter cake is dried, and then ground to make it completely dispersed after drying;

[0089] S3, after placing, close the box door, start the electric heating plate 42 in the drying box 4 to dry, after drying, start and control the cylinder 452 to extend, send the crushing blade 454 and the rotating rod 455 into the inner filter cylinder 444, until the closing plate 451 contacts the inner support ring 445, start the motor 453 to crush, so that all of them pass through the inner filter cylinder;

[0090] S4. The ground filter cake sample and the crushed sample are fully mixed, and then reduced to 10 to 20 g. The reduced samples are placed in ziplock bags and wait for analysis;

[0091] S5. Place the porcelain crucible in a muffle furnace at 850℃±10℃ and burn for 1 hour, take it out, place it in a desiccator to cool for 30 minutes, weigh it to an accuracy of 0.0001g, repeat the burning, weigh it to constant weight, weigh the m1 sample to an accuracy of 0.0001g, place it in the porcelain crucible with constant weight, cover it with a lid, weigh the mass m2 to an accuracy of 0.001g, then place the porcelain crucible in a muffle furnace at 900℃±10℃ and burn for 15 minutes, take it out, and place the porcelain crucible in a desiccator to cool for 30 minutes, then weigh m3 to an accuracy of 0.0001g, measure twice in parallel, take the average value, and obtain the amount of volatile matter;

[0092] Calculation process:

[0093] The original weight of the sample m1

[0094] The mass of the porcelain crucible, cover and sample before firing m2

[0095] The mass of the porcelain crucible, cover and residue after burning m3

[0096] Volatile matter = m3-m2

[0097] Volatile matter ratio = (m3-m2) / m1;

[0098] S6. Weigh the m4 sample and put it into a crucible. Add a solvent to cover the sample. Use a high-frequency infrared carbon-sulfur analyzer to select a suitable carbon standard curve for determination. Read the data directly on the instrument. Measure twice in parallel and take the average value to obtain the carbon content.

[0099] S7, place the porcelain ark in a muffle furnace at 850℃±10℃ and burn for 1 hour, take it out, place it in a desiccator to cool for 30 minutes, weigh it to an accuracy of 0.0001g, repeat the burning, weigh it to constant weight, weigh the m5 sample to an accuracy of 0.0001g, place it in the porcelain ark that has been constant weight, spread it evenly, weigh the total mass to be m6 to an accuracy of 0.0001g, put it in a muffle furnace again, burn it at 850℃±10℃ until it is completely ash, take it out and place it in a desiccator to cool for 30 minutes, weigh the mass to be m7 to an accuracy of 0.0001g, measure it twice in parallel, take the average value, and get the amount of ash;

[0100] Calculation process:

[0101] The original mass of the sample m5

[0102] The quality of porcelain ark m6

[0103] Mass of the porcelain ark and the residue after burning m7

[0104] Ash mass = m7-m6

[0105] Ash content = (m7-m6) / m5;

[0106] S8. Add 3g of sodium peroxide to the bottom of the corundum crucible, weigh m8 ash and put it on the sodium peroxide, and cover it with 3g of sodium peroxide again to ensure that the sodium peroxide completely covers the sample, put the corundum crucible into the muffle furnace, set the heating time to 15 minutes, the heating temperature to 650℃ and the insulation time to 10min respectively, take it out and cool it after melting, cool it to room temperature, wipe the outer wall of the crucible, completely leach the sample, slowly add 60ml of 1:1 hydrochloric acid, 40ml of 1:1 sulfuric acid, 0.1g of iron powder, and 6 aluminum particles, wait until the solution reacts to dark gray, add 20ml of saturated ammonium sulfate solution, cover it with a Geiger funnel, and add 10ml of saturated ammonium sulfate solution to the crucible. Add saturated sodium bicarbonate to the funnel, wait until the aluminum particles are completely dissolved and the solution emits large bubbles, take it out and cool it. At the same time, pay attention to the fact that the saturated sodium bicarbonate solution in the Geiger funnel cannot be evacuated. It should be replenished with saturated sodium bicarbonate solution at any time. Calibrate, remove the Geiger funnel, quickly add 10ml of 300g / L ammonium thiocyanate solution to the conical flask, and immediately titrate with ammonium ferric sulfate standard solution until the test solution turns a stable orange-red color, which is the end point. Make blank samples and parallel samples in the same batch, and take the average of the parallel sample results. Calculate the titanium content based on the amount of ammonium ferric sulfate solution consumed by the sample minus the amount of ammonium ferric sulfate solution consumed by the blank. At the same time, the titanium content in the dust collection residue is inferred based on the titanium content in the ash;

[0107] Calculation process:

[0108] TiO2% (ash content) = M*C1*(V1-V0) / (m8*1000)*100%

[0109] TiO2% (dust collection residue) = TiO2% (ash content) * (m7-m6) / m5

[0110] Where:

[0111] C1——Molar concentration of ammonium ferric sulfate solution, mol / L

[0112] V1——The volume of ammonium ferric sulfate standard solution consumed by the titration test solution, ml

[0113] V0——The volume of ammonium ferric sulfate standard solution consumed in titrating the blank sample, ml

[0114] m8——ash weight, g

[0115] M——molar mass of titanium dioxide, 79.9 g / mol;

[0116] S9, prepare standard solutions of Si, Al, Ca, Mg, and Mn elements, draw standard curves on ICP, weigh 0.3g sodium tetraborate, 0.9g anhydrous sodium carbonate, and m9 ash sample to be tested in a platinum crucible, mix the reagent and sample evenly in the platinum crucible, put into a muffle furnace, program the temperature to 920°C, keep warm for 10min, take out, cool slightly, then put the mixed sample into a polytetrafluoroethylene beaker, and leach the sample with a boiling 1:1 hydrochloric acid solution until the solution is clear, wash the platinum crucible with distilled water and take it out, transfer the leaching solution to a 100ml colorimetric tube and make up the volume, measure it on ICP, obtain the content of each element according to the intensity of each element peak, directly select the results on the instrument together with the blank test, calculate the content of the trace element in the ash, convert it into the percentage of oxides, and at the same time, infer the content of each oxide in the dust collection slag according to the content of each oxide in the ash;

[0117] Calculation process:

[0118] W=C2*100*10-6 / m9*100%

[0119] The content of each oxide in the ash: the percentage of each trace element in the ash * the molecular weight of the oxide / the molar mass of the element

[0120] XSiO2%(ash content)=WSiO2×2.1392

[0121] XAl2O3%(ash content)=WAl2O3×1.8895

[0122] XCaO% (ash content) = WCaO × 1.3992

[0123] XMgO% (ash content) = WMgO × 1.6582

[0124] XMnO% (ash content) = WMnO × 1.2912

[0125] XCr2O3%(ash content)=WCr2O3×1.4615

[0126] The content of each oxide in the dust collection residue: the percentage of each oxide in the ash * the percentage of ash in the dust collection residue

[0127] YSiO2% (dust collection residue) = XSiO2% (ash content) * (m7-m6) / m5

[0128] YAl2O3% (dust collection) = XAl2O3% (ash content) * (m7-m6) / m5

[0129] YCaO% (dust collection residue) = XCaO% (ash content) * (m7-m6) / m5

[0130] YMgO% (dust collection) = XMgO% (ash content) * (m7-m6) / m5

[0131] YMnO% (dust collection residue) = XMnO% (ash content) * (m7-m6) / m5

[0132] YCr2O3% (dust collection residue) = XCr2O3% (dust collection residue) * (m7-m6) / m5

[0133] Where:

[0134] C2——The value of each element in ICP determination, μg / ml

[0135] m9——mass of the sample, g

[0136] W——Percentage of each trace element in the ash, %

[0137] X——Percentage of each oxide in the ash, %

[0138] Y——the percentage of each oxide in the dust collection residue;

[0139] The above steps use the operating platform 1, the muffle furnace 3 and the drying box 4 to cooperate to complete the accurate measurement method of titanium tetrachloride dust collection residue;

[0140] Support legs 2 are welded at the four corners of the lower surface of the operating platform 1, a water tank 12 is arranged on the left side of the upper surface of the operating platform 1, a faucet 11 is arranged on the left side of the water tank 12, and an operating table 13 is arranged in the middle of the upper surface of the operating platform 1;

[0141] The drying box 4 includes a box body 41, an electric heating plate 42 installed on the lower surface of the box body 41, and a support platform 43 fixedly installed in the middle position of the box body 41. A collecting mechanism 44 is placed in the support platform 43, and a lifting mechanism 45 is fixedly installed on the upper side wall of the box body 41.

[0142] A placement hole 431 is provided in the middle of the upper surface of the support platform 43 , and limiting holes 432 are provided on the upper surface of the support platform 43 on both sides of the upper end of the placement hole 431 .

[0143] Specifically, the collecting mechanism 44 includes an outer cylinder 441 and an outer support ring 442 welded to the top of the outer cylinder 441, auxiliary holes 443 are opened on both sides of the upper surface of the outer support ring 442, an inner filter cylinder 444 is arranged in the outer cylinder 441, an inner support ring 445 is welded to the top of the inner filter cylinder 444, and limiting rods 446 are welded on both sides of the lower surface of the inner support ring 445.

[0144] Furthermore, the lifting mechanism 45 includes a closing plate 451, a motor 453 installed in the middle position of the upper surface of the closing plate 451, and two cylinders 452 installed on the left and right sides of the upper surface of the closing plate 451. The lower surface of the closing plate 451 is rotatably connected to a rotating rod 455, and a plurality of crushing blades 454 are welded to the side surface of the rotating rod 455.

[0145] Specifically, the mesh number of the inner filter cylinder 444 is 200 meshes, and the outer cylinder 441 is a closed cylinder, ensuring that the material in the inner filter cylinder 444 can reach the 200 mesh standard under the crushing of the crushing blade 454 and can smoothly enter the outer cylinder 441.

[0146] In addition, a drain port which can be closed as required is provided at the lower end of the water tank 12, the water-solid ratio of the washing liquid is 3:1 or 4:1, the drying temperature of the drying box 4 is 105°C to 115°C, and the reduction method used is the cone quartering method or the grid method.

[0147] Furthermore, when measuring the volatile matter, after the porcelain crucible is placed in the muffle furnace 3, the internal temperature of the muffle furnace 3 must be restored to 900°C±10°C within 3 minutes, otherwise the experimental results will be invalid. The sample mass m4g when measuring the carbon content is between 0.1500g and 0.2000g.

[0148] Specifically, when measuring the molten ash content of TiO2, in addition to using sodium peroxide or potassium pyrosulfate, when performing sample analysis, if the sample is too heavy, in order to avoid inaccurate test results, the measurement is performed after separation and dilution.

[0149] It is worth noting that when conducting ash analysis, the burning time is determined according to the ash reduction situation, and it must be ensured that all the samples are reduced to ash. When measuring the content of trace elements, the ICP method or X-ray fluorescence spectrometer is used for analysis.

[0150] Furthermore, the molecular mass of the trace element adopts the molecular mass on the periodic table, accurate to two decimal places.

[0151] Furthermore, an electronic scale for weighing and a crucible tongs auxiliary tool for taking the crucible are placed on the upper surface of the operating table 13 , so as to facilitate operation on the operating table 13 .

[0152] Among them, it is worth mentioning that the structures and working principles of the faucet 11, muffle furnace 3, electric heating plate 42, cylinder 452, motor 453, infrared carbon and sulfur analyzer, and ICP-OES involved in this embodiment are well known to those skilled in the art and will not be elaborated here.

[0153] It should be noted that the above embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with the technology to understand the content of the present invention and implement it accordingly, and they cannot be used to limit the protection scope of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention.

[0154] Schedule:

[0155] Table 1 Titanium tetrachloride dust collection slag detection index

[0156]

Claims

1. A method for accurately measuring titanium tetrachloride dust slag, comprising an operating platform (1), a drying box (4) placed on the right side of the upper surface of the operating platform (1), and a muffle furnace (3) placed on the right end of the lower side of the operating platform (1). The method comprises the following steps: S1. First, the staff places the collected titanium tetrachloride dust residue into the inner filter cartridge (444) in the collection mechanism (44), then removes the inner filter cartridge (444) and places it in a water tank (12), seals the drain, and washes the titanium tetrachloride dust residue in the inner filter cartridge (444) with water through the faucet (11). After the liquid-to-solid ratio requirement is met, the residue is repeatedly stirred and washed in the water tank; S2, the washed inner filter cartridge (444) is inserted back into the outer cartridge (441), and the limiting rod (446) is aligned with the auxiliary hole (443) for placement, and then the collecting mechanism (44) is placed as a whole inside the placement hole (431) provided on the inner support platform (43) of the drying box (4), and the limiting rod (446) is ensured to be aligned with the limiting hole (432), and at the same time, the filtrate is collected and filtered out, and the filter cake is dried, and after drying, it is ground to be completely dispersed; S3. After placing, close the box door and start the electric heating plate (42) in the drying box (4) to dry. After drying, start and control the cylinder (452) to extend, send the crushing blade (454) and the rotating rod (455) into the inner filter cartridge (444) until the closing plate (451) contacts the inner support ring (445), and start the motor (453) to crush so that all of the particles pass through the inner filter cartridge; S4. The ground filter cake sample and the crushed sample are fully mixed, and then reduced to 10 to 20 g. The reduced samples are placed in ziplock bags and wait for analysis; S5. Place the porcelain crucible in a muffle furnace (3) at 850°C ± 10°C and burn for 1 hour, then take it out, place it in a desiccator to cool for 30 minutes, weigh it to an accuracy of 0.0001g, repeat the burning, weigh it to constant weight, weigh the m1 sample to an accuracy of 0.0001g, place it in the porcelain crucible with a constant weight, cover it with a lid, weigh the mass m2 to an accuracy of 0.001g, then place the porcelain crucible in a muffle furnace (3) at 900°C ± 10°C and burn for 15 minutes, take it out, and place the porcelain crucible in a desiccator to cool for 30 minutes, then weigh m3 to an accuracy of 0.0001g, measure twice in parallel, take the average value, and obtain the amount of volatile matter; Calculation process: The original weight of the sample m1 The mass of the porcelain crucible, cover and sample before firing m2 The mass of the porcelain crucible, cover and residue after burning m3 Volatile matter = m3-m2 Volatile matter ratio = (m3-m2) / m1; S6. Weigh the m4 sample and put it into a crucible. Add a solvent to cover the sample. Use a high-frequency infrared carbon-sulfur analyzer to select a suitable carbon standard curve for determination. Read the data directly on the instrument. Measure twice in parallel and take the average value to obtain the carbon content. S7, place the porcelain ark in a muffle furnace (3) at 850℃±10℃ and burn for 1 hour, take it out, place it in a desiccator to cool for 30 minutes, weigh it to an accuracy of 0.0001g, repeat the burning, weigh it to constant weight, weigh the m5 sample to an accuracy of 0.0001g, place it in the porcelain ark that has been constant weight, spread it evenly, weigh the total mass to be m6 to an accuracy of 0.0001g, put it in the muffle furnace (3), burn it at 850℃±10℃ until it is completely ash, take it out and place it in a desiccator to cool for 30 minutes, weigh the mass to be m7 to an accuracy of 0.0001g, measure it twice in parallel, take the average value, and get the amount of ash; Calculation process: The original mass of the sample m5 The quality of porcelain ark m6 Mass of the porcelain ark and the residue after burning m7 Ash mass = m7-m6 Ash content = (m7-m6) / m5; S8, add 3g of sodium peroxide to the bottom of the corundum crucible, weigh m8 ash and put it on the sodium peroxide, and cover it with 3g of sodium peroxide again to ensure that the sodium peroxide completely covers the sample, put the corundum crucible into the muffle furnace (3), set the heating time to 15 minutes, the heating temperature to 650°C and the insulation time to 10min respectively, take it out and cool it after melting, cool it to room temperature, wipe the outer wall of the crucible, completely leach the sample, slowly add 60ml of hydrochloric acid with a ratio of 1:1, 40ml of sulfuric acid with a ratio of 1:1, 0.1g of iron powder, and 6 aluminum particles, wait until the solution reacts and turns dark gray, add 20ml of saturated ammonium sulfate solution, cover it with a Geiger funnel, and cover it with a lid. Add saturated sodium bicarbonate to the Geiger funnel, wait until the aluminum particles are completely dissolved and the solution emits large bubbles, then take it out and cool it. At the same time, pay attention to the fact that the saturated sodium bicarbonate solution in the Geiger funnel cannot be evacuated, and the saturated sodium bicarbonate solution should be added at any time. Calibrate, remove the Geiger funnel, quickly add 10ml of 300g / L ammonium thiocyanate solution to the conical flask, and immediately titrate with ammonium ferric sulfate standard solution until the test solution turns a stable orange-red color, which is the end point. Make blank samples and parallel samples in the same batch, and take the average of the parallel sample results. Calculate the titanium content based on the amount of ammonium ferric sulfate solution consumed by the sample minus the amount of ammonium ferric sulfate solution consumed by the blank. At the same time, infer the content of titanium in the dust collection slag based on the content of titanium in the ash; Calculation process: TiO2% (ash content) = M*C1*(V1-V0) / (m8*1000)*100% TiO2% (dust collection residue) = TiO2% (ash content) * (m7-m6) / m5 C1——Molar concentration of ammonium ferric sulfate solution, mol / L V1——The volume of ammonium ferric sulfate standard solution consumed by the titration test solution, ml V0——The volume of ammonium ferric sulfate standard solution consumed in titrating the blank sample, ml m8——ash weight, g M——molar mass of titanium dioxide, 79.9 g / mol; S9, prepare standard solutions of Si, Al, Ca, Mg and Mn, draw standard curves on ICP, weigh 0.3g sodium tetraborate, 0.9g anhydrous sodium carbonate and m9 ash sample to be tested in a platinum crucible, mix the reagent and sample evenly in the platinum crucible, put into a muffle furnace (3), raise the temperature to 920°C, keep warm for 10 min, take out, cool slightly, put the mixed sample into a polytetrafluoroethylene beaker, leach the sample with a boiling 1:1 hydrochloric acid solution until the solution is clear, wash the platinum crucible with distilled water and take out, transfer the leached solution to a 100ml colorimetric tube and make up the volume, measure on ICP, obtain the content of each element according to the intensity of each element peak, directly select the result on the instrument together with the blank test, calculate the content of the trace element in the ash, convert it into the percentage of oxide, and at the same time, infer the content of each oxide in the dust collection residue according to the content of each oxide in the ash; Calculation process: W=C2*100*10-6 / m9*100% The content of each oxide in the ash: the percentage of each trace element in the ash * the molecular weight of the oxide / the molar mass of the element XSiO2%(ash content)=WSiO2×2.1392 XAl2O3%(ash content)=WAl2O3×1.8895 XCaO% (ash content) = WCaO × 1.3992 XMgO% (ash content) = WMgO × 1.6582 XMnO% (ash content) = WMnO × 1.2912 XCr2O3%(ash content)=WCr2O3×1.4615 The content of each oxide in the dust collection residue: the percentage of each oxide in the ash * the percentage of ash in the dust collection residue YSiO2% (dust collection residue) = XSiO2% (ash content) * (m7-m6) / m5 YAl2O3% (dust collection) = XAl2O3% (ash content) * (m7-m6) / m5 YCaO% (dust collection residue) = XCaO% (ash content) * (m7-m6) / m5 YMgO% (dust collection) = XMgO% (ash content) * (m7-m6) / m5 YMnO% (dust collection residue) = XMnO% (ash content) * (m7-m6) / m5 YCr2O3% (dust collection residue) = XCr2O3% (dust collection residue) * (m7-m6) / m5 Where: C2——the value of each element in ICP determination, μg / ml; m9——mass of the sample, g W——Percentage of each trace element in the ash, % X——Percentage of each oxide in the ash, % Y——the percentage of each oxide in the dust collection residue; The above steps use the operating platform (1), the muffle furnace (3) and the drying box (4) to complete the accurate measurement method of titanium tetrachloride dust collection residue; Support legs (2) are welded at the four corners of the lower surface of the operating platform (1); a water tank (12) is arranged on the left side of the upper surface of the operating platform (1); a faucet (11) is arranged on the left side of the water tank (12); and an operating table (13) is arranged in the middle of the upper surface of the operating platform (1); The drying box (4) comprises a box body (41), an electric heating plate (42) installed on the lower surface of the box body (41), and a support platform (43) fixedly installed in the middle position of the box body (41), a collecting mechanism (44) is placed in the support platform (43), and a lifting mechanism (45) is fixedly installed on the upper side wall of the box body (41); A placement hole (431) is provided in the middle of the upper surface of the support platform (43), and limiting holes (432) are provided on the upper surface of the support platform (43) on both left and right sides of the upper end of the placement hole (431).

2. The method for accurately measuring titanium tetrachloride dust collection residue according to claim 1, characterized in that: The collecting mechanism (44) comprises an outer cylinder (441) and an outer support ring (442) welded to the top end of the outer cylinder (441); auxiliary holes (443) are provided on both sides of the upper surface of the outer support ring (442); an inner filter cylinder (444) is arranged inside the outer cylinder (441); an inner support ring (445) is welded to the top end of the inner filter cylinder (444); and limiting insertion rods (446) are welded to both left and right sides of the lower surface of the inner support ring (445).

3. The accurate measurement method of titanium tetrachloride dust collection residue according to claim 2, characterized in that: The lifting mechanism (45) comprises a closing plate (451), a motor (453) installed at the middle position of the upper surface of the closing plate (451), and two cylinders (452) installed at the left and right sides of the upper surface of the closing plate (451); a rotating rod (455) is rotatably connected to the lower surface of the closing plate (451), and a plurality of crushing blades (454) are welded to the side surface of the rotating rod (455).

4. The accurate measurement method of titanium tetrachloride dust collection residue according to claim 3, characterized in that: The mesh number of the inner filter cylinder (444) is 200 meshes, and the outer cylinder (441) is a closed cylinder.

5. The method for accurately measuring titanium tetrachloride dust collection residue according to claim 3, characterized in that: The lower end of the water tank (12) is provided with a drain port which can be closed as required, the water-wash liquid-solid ratio is 3:1 or 4:1, the drying temperature of the drying box (4) is 105° C. to 115° C., and the reduction method used is the cone quartering method or the grid method.

6. The method for accurately measuring titanium tetrachloride dust collection residue according to claim 3, characterized in that: When measuring the volatile matter, after the porcelain crucible is placed in the muffle furnace (3), the internal temperature of the muffle furnace (3) must be restored to 900°C±10°C within 3 minutes, otherwise the experimental results will be invalid. When measuring the carbon content, the sample mass m4g is between 0.1500g and 0.2000g.

7. The method for accurately measuring titanium tetrachloride dust collection residue according to claim 3, characterized in that: When measuring the molten ash content of TiO2, sodium peroxide or potassium pyrosulfate is used. When analyzing the sample, if the sample is too heavy, in order to avoid inaccurate test results, the measurement should be performed after separation and dilution.

8. The method for accurately measuring titanium tetrachloride dust collection residue according to claim 3, characterized in that: When conducting ash analysis, the burning time is determined according to the ash reduction situation, and it must be ensured that all the samples are reduced to ash. When measuring the trace element content, the ICP method or X-ray fluorescence spectrometer is used for analysis.

9. The method for accurately measuring titanium tetrachloride dust collection residue according to claim 3, characterized in that: The molecular mass of trace elements adopts the molecular mass on the periodic table, accurate to two decimal places.

10. The method for accurately measuring titanium tetrachloride dust collection residue according to claim 3, characterized in that: An electronic scale for weighing and a crucible tongs auxiliary tool for taking the crucible are placed on the upper surface of the operating table (13).

Images