A drying method for preparing beta-ruthenium trichloride

Abstract

The present application relates to the technical field of noble metal production, and discloses a drying method for preparing beta-type ruthenium trichloride, which adopts a drying and stirring device and comprises the following steps: step 1, beta-type ruthenium trichloride solution is added into a tank; step 2, a driving motor drives a stirring shaft to stir the solution at a rotating speed of 150-180 r / min, and meanwhile, an infrared lamp is used to heat the solution until the solution is skinned; step 3, when the solution is skinned, the rotating speed of the driving motor is adjusted to 100-120 r / min, the infrared lamp continues to heat, and the solution is slurried; step 4, when the solution is slurried, the rotating speed of the driving motor is adjusted to 50-80 r / min, the infrared lamp continues to heat, and the solution is agglomerated. Different rotating speeds of the motor are adopted at different stages of the material, the heat transfer efficiency of the material is ensured, the drying efficiency is accelerated, and the material consumption and energy consumption are reduced.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of noble metal production, in particular to a drying method for preparing beta-ruthenium trichloride. BACKGROUND

[0002] Ruthenium trichloride has two crystal forms, alpha and beta. Alpha-ruthenium trichloride belongs to the orthorhombic system, has a large lattice parameter, and is composed of layered structures of ruthenium and chlorine atoms, so it is stable at room temperature and insoluble, and cannot be used as a metal anode coating. Beta-ruthenium trichloride belongs to the hexagonal system, has a compact structure, and is arranged in a hexagonal close-packed manner of ruthenium and chlorine atoms, so it has the characteristics of high temperature resistance, non-passivation, and high stability, and is the main raw material for metal anode coating of electrolytic cells.

[0003] CN201910645571.3 discloses a method for preparing ruthenium trichloride from a ruthenium-containing waste material, comprising the following steps: (1) calcination: the ruthenium-containing waste material is calcined at a temperature of 200-800℃ for 4-8h; (2) preparation of RuO4: the calcined ruthenium-containing waste material is added to a reaction kettle, and sodium chlorate, liquid bromine and water are added, and the mixture is stirred and reacted at 60-100℃ for 1.5-5h, wherein the ruthenium content of the ruthenium-containing waste material is 100 parts by weight, the sodium chlorate is 150-550 parts by weight, the liquid bromine is 2-6 parts by weight, and the water is 300-800 parts by weight; (3) preparation of H2RuCl5 solution: at room temperature, the RuO4 produced in step (2) is absorbed by hydrochloric acid to obtain a H2RuCl5 solution; (4) drying: the generated H2RuCl5 solution is heated and concentrated to crystallize, and then dried by infrared radiation to obtain hydrated ruthenium trichloride crystals.

[0004] The above technical solution heats and concentrates the generated H2RuCl5 solution to crystallize it, and then dries it by infrared radiation to obtain hydrated ruthenium trichloride crystals, but in the drying process, the solution is not stirred, and the convective heat transfer effect of the heat transfer surface on the ruthenium trichloride solution is poor, the heat penetration is uneven, and the efficiency is low. SUMMARY

[0005] The present application aims to solve the above problems, and provides a drying method for preparing beta-ruthenium trichloride, which uses left-handed upper stirring blades and right-handed lower stirring blades. The upper stirring blades have the effect of strengthening the axial downward stirring, and the lower stirring blades have the effect of strengthening the axial upward stirring, so that the material is fully exposed to the heating mechanism area, achieving uniform heating and drying. Different motor speeds are used at different stages of the material to ensure the heat transfer efficiency of the material, thereby speeding up the drying efficiency and reducing material consumption and energy consumption.

[0006] To achieve the above object, the present application provides the following technical solutions:

[0007] A drying method for preparing beta-ruthenium trichloride, the method involves a drying stirring device, the drying stirring device comprises a tank body, a driving motor, a transmission mechanism, a plurality of stirring shafts, the transmission mechanism is connected at the top of the tank body, one end of the plurality of stirring shafts is respectively connected to the transmission mechanism, and the other end is located in the tank body, a plurality of infrared lamps are arranged in the tank body, the plurality of stirring shafts are respectively provided with upper stirring blades and lower stirring blades, the upper stirring blades are left-handed, and the lower stirring blades are right-handed, and the driving motor is used for driving the transmission mechanism to rotate.

[0008] The method comprises the following steps:

[0009] Step 1: the beta-ruthenium trichloride solution is added into the tank body;

[0010] Step 2: the driving motor drives the stirring shaft to stir the solution at a rotating speed of 150-180 r / min, and the infrared lamp is used to heat the solution until the solution is crusty;

[0011] Step 3: when the solution is crusty, the rotating speed of the driving motor is adjusted to 100-120 r / min, and the infrared lamp is continuously used for heating until the solution is slurry;

[0012] Step 4: when the solution is slurry, the rotating speed of the driving motor is adjusted to 50-80 r / min, and the infrared lamp is continuously used for heating until the solution is crumbled.

[0013] In the step 2, the rotating speed of the driving motor includes but is not limited to 150 r / min, 160 r / min, 170 r / min and 180 r / min; in the step 3, the rotating speed of the driving motor includes but is not limited to 100 r / min, 110 r / min and 120 r / min; and in the step 4, the rotating speed of the driving motor includes but is not limited to 50 r / min, 60 r / min, 70 r / min and 80 r / min.

[0014] In the above drying method, the transmission mechanism is a planetary gear transmission mechanism, the planetary gear transmission mechanism comprises a sun gear and a plurality of planet gears meshing with the sun gear, the sun gear and the plurality of planet gears are both rotationally connected to the top of the tank body, the driving motor is connected with the sun gear, and the number of teeth of the sun gear is greater than or less than the number of teeth of the planet gears.

[0015] In the above drying method, a support frame is further included, the support frame is located between the transmission mechanism and the tank body, the support frame is provided with through holes matched with the positions of the sun gear and the plurality of planet gears, and one end of the plurality of stirring shafts respectively passes through the through holes and is connected with the sun gear and the plurality of planet gears.

[0016] In the drying method, the planetary gears are three, and the through holes are four.

[0017] In the drying method, the support frame comprises a first plate body, a second plate body and a third plate body which are integrally formed and connected at one end, and the angles between the first plate body and the second plate body, the second plate body and the third plate body, and the third plate body and the first plate body are all the same, and the through holes are respectively located at the central part, the end of the first plate body, the end of the second plate body and the end of the third plate body.

[0018] In the drying method, the upper stirring blade comprises a first connecting column and a plurality of first blades which are connected to the outer side of the first connecting column and arranged along the circumferential direction of the first connecting column, and the first connecting column is detachably connected to the stirring shaft by bolts.

[0019] The lower stirring blade comprises a second connecting column and a plurality of second blades which are connected to the outer side of the second connecting column and arranged along the circumferential direction of the second connecting column, and the second connecting column is detachably connected to the stirring shaft by bolts, and the plurality of first blades and the plurality of second blades are arranged symmetrically.

[0020] In the drying method, the angles between the plurality of first blades, the plurality of second blades and the horizontal plane are all 40-50°.

[0021] In the drying method, the first blade is four pieces, the second blade is four pieces, the first blade and the first connecting column are integrally formed, and the second blade and the second connecting column are integrally formed.

[0022] In the drying method, the side surface of the tank body is provided with an upper and lower arranged feeding port and discharging port, and an exhaust pipe arranged opposite to the feeding port.

[0023] Compared with the prior art, the beneficial effects of the present application are:

[0024] The present application adopts left-handed upper stirring blades and right-handed lower stirring blades, the upper stirring blades play a role of strengthening the axial downward stirring, the lower stirring blades play a role of strengthening the axial upward stirring, so that the materials are fully exposed in the heating mechanism area, uniform heating and drying are realized, different motor speeds are adopted in different stages of the materials, the heat transfer efficiency of the materials is ensured, the drying efficiency is further accelerated, and the material consumption and energy consumption are reduced. BRIEF DESCRIPTION OF DRAWINGS

[0025] Fig. 1 is a perspective view of the drying and stirring device of example 1;

[0026] Fig. 2 is a schematic diagram of the internal structure of the drying stirring device of embodiment 1;

[0027] Fig. 3 is a front view of Fig. 2 ;

[0028] Fig. 4 is a perspective view of the support frame of the drying stirring device of embodiment 1;

[0029] Fig. 5 is a perspective view of the upper stirring blade of the drying stirring device of embodiment 1;

[0030] Fig. 6 is a perspective view of the lower stirring blade of the drying stirring device of embodiment 1. DETAILED DESCRIPTION

[0031] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the scope of protection of the present application.

[0032] Embodiment 1

[0033] Referring to Figs. 1-6 , a drying stirring device includes a tank body 1, a driving motor 2, a transmission mechanism 3, and a plurality of stirring shafts 4. The transmission mechanism 3 is connected to the top of the tank body 1. One end of each of the plurality of stirring shafts 4 is connected to the transmission mechanism 3, and the other end is located in the tank body 1. A plurality of infrared lamps 11 are arranged in the tank body 1. The plurality of stirring shafts 4 are each provided with an upper stirring blade 41 and a lower stirring blade 42. The upper stirring blade 41 is left-handed, and the lower stirring blade 42 is right-handed. The driving motor 2 is used to drive the transmission mechanism 3 to rotate.

[0034] Under this design, a person skilled in the art adds β-type ruthenium trichloride, which is referred to as material below, into the tank body 1. Under the action of the driving motor 2, the transmission mechanism 3 is rotated, thereby driving the plurality of stirring shafts 4 to stir in the tank body 1 at different rotating speeds. In the process of stirring, the material is heated by the infrared lamps 11 at the same time. The upper stirring blade 41 plays a role in strengthening the stirring in the axial direction downward, and the lower stirring blade 42 plays a role in strengthening the stirring in the axial direction upward, so that the material is fully exposed to the area of the infrared lamps 11, uniform heating and drying are achieved, different rotating speeds of the driving motor 2 and different powers of the infrared lamps 11 are adopted in different stages of the material, the heat transfer efficiency of the material is ensured, the drying efficiency is thus accelerated, material consumption and energy consumption are reduced, and the temperature gradient of the material in the stirring process is reduced.

[0035] In the embodiment, the transmission mechanism 3 is a planetary gear transmission mechanism, which comprises a sun gear 31 and a plurality of planet gears 32 engaged with the sun gear 31, the sun gear 31 and the plurality of planet gears 32 are both rotationally connected to the top of the tank body 1, the driving motor 2 is connected with the sun gear 31, and the number of teeth of the sun gear 31 is greater than or less than that of the planet gears 32.

[0036] In actual application, when the driving motor 2 drives the sun gear 31 to rotate, the plurality of planet gears will also rotate with the sun gear 31, and the purpose of selecting the number of teeth of the sun gear 31 to be greater than or less than that of the planet gears 32 is to make the plurality of stirring shafts 4 stir in the tank body 1 at different rotating speeds. It should be noted that the different rotating speeds refer to that the rotating speed of the stirring shaft 4 connected with the sun gear 31 is different from that of the stirring shaft 4 connected with the planet gears 32, but the rotating speeds of the plurality of planet gears 32 should be the same, so that the rotating speed of the central part in the tank body 1 is different from that between the inner wall and the central part of the tank body 1, so that the material is stirred in the interval area between the stirring paddles, the regular flow area of the material is reduced, the flow range is increased, and the heat transfer efficiency of the material is accelerated.

[0037] Preferably, the support frame 5 is arranged between the transmission mechanism 3 and the tank body 1, the support frame 5 is provided with through holes 54 matched with the positions of the sun gear 31 and the plurality of planet gears 32, and one end of the plurality of stirring shafts 4 respectively passes through the through holes 54 and is connected with the sun gear 31 and the plurality of planet gears 32. The purpose of arranging the support frame 5 is to ensure the stability of the transmission mechanism 3, that is, the stability of the engagement between the sun gear 31 and the plurality of planet gears 32, and also to ensure the stability of the stirring shaft 4 when rotating.

[0038] More preferably, the planet gears 32 are three, and the through holes 54 are four. The number of the through holes 54 should match the number of the planet gears 32, but the number of the planet gears 32 is not limited to three, and can be four, five, six or more, or less than three, but attention should be paid to the stirring distance between the stirring shafts 4. In the embodiment, three planet gears 32 are selected based on economy and meeting the stirring effect.

[0039] In the embodiment, the support frame 5 comprises a first plate body 51, a second plate body 52 and a third plate body 53 which are integrally formed, one end of the first plate body 51, the second plate body 52 and the third plate body 53 are connected, and the included angles between the first plate body 51 and the second plate body 52, the second plate body 52 and the third plate body 53, and the third plate body 53 and the first plate body 51 are all the same, and the through holes 54 are respectively located at the central part, the end of the first plate body 51, the end of the second plate body 52 and the end of the third plate body 53.

[0040] Adopt the structure of one-piece molding can guarantee the strength of the support frame 5 body, by setting the through hole 54 in the center of the support frame 5, the end of the first plate body 51, the end of the second plate body 52, the end of the third plate body 53, so that the sun gear 31 is connected through the through hole 54 in the center, as long as the plurality of planetary gears 32 are connected in the end of the first plate body 51, the end of the second plate body 52, the end of the third plate body 53 can quickly complete the meshing installation.

[0041] In the embodiment, the upper stirring blade 41 comprises a first connecting column 411, a plurality of first blades 412 connected to the outer side of the first connecting column 411 and arranged along the circumferential direction of the first connecting column 411, and the first connecting column 411 is detachably connected to the stirring shaft 4 by bolts; further, the lower stirring blade 42 comprises a second connecting column 421, a plurality of second blades 422 connected to the outer side of the second connecting column 421 and arranged along the circumferential direction of the second connecting column 421, and the second connecting column 421 is detachably connected to the stirring shaft 4 by bolts, and the plurality of first blades 412 and the plurality of second blades 422 are arranged symmetrically.

[0042] Specifically, by detachably connecting the first connecting column 411 to the stirring shaft 4 by bolts and detachably connecting the second connecting column 421 to the stirring shaft 4 by bolts, the distance between the first connecting column 411 and the second connecting column 421 can be adjusted along the length direction of the stirring shaft 4 by detaching the bolts, so that the first blades 412 can be completely immersed in the material, and the second blades 422 can be located on the surface of the material to achieve the best stirring effect.

[0043] Preferably, the included angle between the plurality of first blades 412 and the plurality of second blades 422 and the horizontal plane is 40-50°. Because for the stirring effect, a smaller angle such as 30° may produce a smaller stirring force, resulting in a relatively weak stirring effect. A larger angle such as 60° will produce a larger stirring force, which can more effectively mix the material uniformly, but a larger angle requires more energy input, so the energy consumption will increase relatively, so the embodiment adopts 40-50°, preferably 45°. However, in order to meet the processing requirements, other angles can also be used, and the angle of the stirring blade is not limited in the embodiment, but it is necessary to ensure that the upper stirring blade 41 and the lower stirring blade 42 are symmetrical, and the upper stirring blade 41 is left-handed, and the lower stirring blade 42 is right-handed.

[0044] Preferably, the first blades 412 are four pieces; the second blades 422 are four pieces, the first blades 412 and the first connecting columns 411 are integrally formed; the second blades 422 and the second connecting columns 421 are integrally formed. By designing the first blades 412 and the first connecting columns 411 as an integrally formed structure, and the second blades 422 and the second connecting columns 421 as an integrally formed structure, the strength of the upper stirring blades 41 and the lower stirring blades 42 can be ensured, and the number of the first blades 412 and the second blades 422 is not limited to four pieces, and other numbers of pieces are also possible.

[0045] Preferably, the side of the tank body 1 is provided with an upper and lower arranged feeding port 12 and discharging port 13, and an exhaust pipe 14 arranged opposite to the feeding port 12.

[0046] Specifically, the exhaust pipe 14 is used to exhaust the corrosive or toxic gas generated in the drying process in the tank body 1, so as to avoid the corrosive or toxic gas remaining in the inner wall of the tank body 1 to corrode the container and cause harm. The feeding port 12 and the discharging port 13 are respectively arranged on the side of the tank body 1, wherein the discharging port 13 is in a closed state during the stirring drying process.

[0047] Embodiment 2

[0048] A drying method for preparing β-type ruthenium trichloride, which is carried out by using the drying and stirring device in Embodiment 1, comprising the following steps:

[0049] Step 1: adding a β-type ruthenium trichloride solution into the tank body 1;

[0050] Step 2: driving the motor 2 to drive the stirring shaft 4 to stir the solution at a speed of 150 r / min, and at the same time, using a 275W infrared lamp 11 to heat the solution until the solution is crusty;

[0051] Step 3: when the solution is crusty, the speed of the driving motor 2 is adjusted to 100 r / min, and the heating by the infrared lamp 11 is continued until the solution is slurry;

[0052] Step 4: when the solution is slurry, the speed of the driving motor 2 is adjusted to 50 r / min, and the heating by the infrared lamp 11 is continued until the solution is crumbled.

[0053] Embodiment 3

[0054] The same as Embodiment 2, the difference is that in Step 2, the speed of the driving motor 2 is 180 r / min; in Step 3, the speed of the driving motor 2 is 120 r / min; in Step 4, the speed of the driving motor 2 is 80 r / min.

[0055] Embodiment 4

[0056] The same as Example 2, except that in Step 2, the rotational speed of the driving motor 2 was 150 r / min; in Step 3, the rotational speed of the driving motor 2 was 120 r / min; and in Step 4, the rotational speed of the driving motor 2 was 80 r / min.

[0057] Example 5

[0058] The same as Example 2, except that in Step 2, the rotational speed of the driving motor 2 was 180 r / min; in Step 3, the rotational speed of the driving motor 2 was 100 r / min; and in Step 4, the rotational speed of the driving motor 2 was 50 r / min.

[0059] Example 6

[0060] The same as Example 2, except that in Step 2, the rotational speed of the driving motor 2 was 150 r / min; in Step 3, the rotational speed of the driving motor 2 was 100 r / min; and in Step 4, the rotational speed of the driving motor 2 was 80 r / min.

[0061] Example 7

[0062] The same as Example 2, except that in Step 2, the rotational speed of the driving motor 2 was 180 r / min; in Step 3, the rotational speed of the driving motor 2 was 100 r / min; and in Step 4, the rotational speed of the driving motor 2 was 80 r / min.

[0063] Example 8

[0064] The same as Example 2, except that in Step 2, the rotational speed of the driving motor 2 was 150 r / min; in Step 3, the rotational speed of the driving motor 2 was 120 r / min; and in Step 4, the rotational speed of the driving motor 2 was 50 r / min.

[0065] Example 9

[0066] The same as Example 2, except that in Step 2, the rotational speed of the driving motor 2 was 180 r / min; in Step 3, the rotational speed of the driving motor 2 was 120 r / min; and in Step 4, the rotational speed of the driving motor 2 was 50 r / min.

[0067] Comparative Example 1

[0068] The same as Example 2, except that in Step 2, Step 3, and Step 4, the rotational speed of the driving motor 2 was 150 r / min.

[0069] Comparative Example 2

[0070] The same as Example 2, except that in Step 2, Step 3, and Step 4, the rotational speed of the driving motor 2 was 100 r / min.

[0071] Comparative Example 3

[0072] The same as Example 2, except that the rotating speed of the driving motor 2 in step 2, step 3 and step 4 is 50 r / min.

[0073] Comparative Example 4

[0074] The same as Example 2, except that the rotating speed of the driving motor 2 in step 2 is 130 r / min; the rotating speed of the driving motor 2 in step 3 is 80 r / min; and the rotating speed of the driving motor 2 in step 4 is 30 r / min.

[0075] Comparative Example 5

[0076] The same as Example 2, except that the rotating speed of the driving motor 2 in step 2 is 200 r / min; the rotating speed of the driving motor 2 in step 3 is 140 r / min; and the rotating speed of the driving motor 2 in step 4 is 100 r / min.

[0077] Comparative Example 6

[0078] The same as Example 2, except that the power of the infrared lamp 11 in step 2, step 3 and step 4 is 350 W.

[0079] Comparative Example 7

[0080] The same as Example 2, except that the power of the infrared lamp 11 in step 2, step 3 and step 4 is 200 W.

[0081] After the β-type ruthenium trichloride is obtained by using the drying method described in Examples 2-9 and Comparative Examples 1-7 respectively, the drying condition of the β-type ruthenium trichloride solution is analyzed, and the analysis result is shown in Table 1:

[0082] Table 1 Drying condition of β-type ruthenium trichloride solution

[0083]

[0084]

[0085] Result analysis:

[0086] According to the standard of HG / T·3679-2011, the ruthenium content of the ruthenium trichloride on the metal anode coating of the electrolytic cell is required to be about 35%-38%, and considering the stability and metal content, the industry requires the ruthenium content to be 37%-37.5%.

[0087] 1. From the results of Examples 2-9, it can be seen that before the skinning, the corresponding skinning time of 180 r / min rotation speed used in Example 3, Example 5, Example 7 and Example 9 is shorter than that of 150 r / min rotation speed used in Example 2, Example 4, Example 6 and Example 8; and before the pulping, that is, in the time from skinning to pulping, the corresponding pulping time of 120 r / min rotation speed used in Example 3, Example 4, Example 8 and Example 9 is shorter than that of 100 r / min rotation speed used in Example 2, Example 5, Example 6 and Example 7, but in the time from pulping to caking, the influence of 50 r / min and 80 r / min rotation speed on the caking time is not large, and Example 3 uses the largest rotation speed in the three stages, although the time is short, the overall efficiency is high, but compared with Example 2 which uses the smallest rotation speed in the three stages, although the time is slightly higher than that of Example 3, the overall efficiency is not bad, in terms of ruthenium content, considering that the detection uniformity is within 0-0.5% deviation, the result of Example 2 is slightly better than that of Example 3, because at high speed, it will cause the generation of bubbles and the splashing of solution, thereby reducing the content of ruthenium; the result of Example 6 is most close to that of Example 2, and Example 6 and Example 2 use 150 r / min and 100 r / min before skinning and pulping, the difference is the rotation speed before caking of the two, although the influence of 50 r / min and 80 r / min rotation speed on the caking time is not large, but it still has a subtle influence on the result. Even though Examples 2-9 all meet the range of 35%-38% of ruthenium content, only Example 2 meets the range of 37%-37.5%, Example 6 slightly exceeds the range of 37%-37.5%, and the stability of metal content is slightly weaker than that of Example 2.

[0088] 2. From the results of Example 2 and Comparative Examples 1-3, it can be seen that Example 2 is the best example of effect, and Example 2 uses motor speeds of 150 r / min, 100 r / min, and 50 r / min in the three stages, respectively, while Comparative Example 1 uses the best skinning motor speed of 150 r / min. Compared with Example 2, the skinning time is not much different, the pulping time is significantly better than Example 2, but the lumping time is significantly longer than Example 2. This is because high speed can promote pulping, but also affects the solution lumping, and under high speed, it can cause the generation of bubbles and the splashing of the solution, thereby reducing the content of ruthenium, so the ruthenium content of Comparative Example 1 is significantly lower than that of Example 2. Comparative Example 2 uses the best pulping motor speed of 100 r / min. Compared with Example 2, the speed before skinning is lower than Example 2, so the skinning time reaches 167 min, which is significantly longer than the 121 min of Example 2. The pulping time is not much different from Example 2, but the speed before lumping is 100 r / min, which has a certain effect on lumping, so the lumping time is slightly longer than Example 2. Although the results meet the range of 35% to 38%, they do not meet the range of 37% to 37.5%, and the overall time is longer and the efficiency is lower. Comparative Example 3 uses the best pulping motor speed of 50 r / min. Compared with Example 2, the results are close to Example 2, slightly worse than Example 2, and meet the range of 37% to 37.5%. The skinning time and pulping time are significantly longer than Example 2, and the efficiency is lower.

[0089] 3. From the results of Example 2, Example 3, and Comparative Examples 4 and 5, it can be seen that Comparative Example 4 uses lower speeds in the three stages than the three stages corresponding to Example 2. Compared with Example 2, the skinning time, pulping time, and lumping time are all longer than Example 2. Although the results are close to Example 2, slightly worse than Example 2, and meet the range of 37% to 37.5%, the efficiency is lower. Comparative Example 5 uses higher speeds in the three stages than the three stages corresponding to Example 2 and Example 3. Compared with Example 2 and Example 3, the skinning time and pulping time are slightly better than Example 2 and Example 3. The speed is too high to have a certain effect on lumping, so the lumping time is slightly longer than Example 2 and Example 3. The reason is the same as Example 3, and the results are significantly worse than Example 2 under high speed.

[0090] 4. From the results of Example 2 and Comparative Example 6, Comparative Example 7, it can be seen that Comparative Example 6 and Comparative Example 7 both use the same rotational speed as Example 2, but Comparative Example 6 uses an infrared lamp power of 350W, which indicates that the temperature is higher during stirring, promoting skinning, slurry, and caking, but the ruthenium content is significantly higher than Example 2, up to 38.62%, which does not meet the range of 35% to 38%; while Comparative Example 7 uses an infrared lamp power of 200W, which indicates that the temperature is lower during stirring compared to Example 2, so the skinning time, slurry time, and caking time are all longer than Example 2, and the ruthenium content is also significantly lower than Example 2, although it meets the range of 35% to 38%, it does not meet the range of 37% to 37.5%.

[0091] In summary, the present application uses left-handed upper stirring blades and right-handed lower stirring blades, the upper stirring blades enhance the axial downward stirring effect, and the lower stirring blades enhance the axial upward stirring effect, so that the material is fully exposed to the heating mechanism area, achieving uniform heating and drying, and through experiments, the motor speed is controlled at 150r / min, 100r / min, and 50r / min respectively before skinning, slurry, and caking, and a 275W infrared lamp is used, which not only ensures the heat transfer efficiency of the material, but also speeds up the drying efficiency, reduces material consumption and energy consumption, and ultimately achieves unexpected results, with a ruthenium content of 37.36%, which not only meets the requirement of the electrolytic cell metal anode coating ruthenium trichloride with a ruthenium content of about 35% to 38%, but also meets the industry requirement of a ruthenium content of 37% to 37.5% considering the stability and metal content of the metal.

[0092] The above only describes the preferred embodiments of the present application, and it should be noted that for those skilled in the art, without departing from the principles of the present application, a number of improvements or modifications can be made, and these improvements or modifications should also be considered within the scope of the present application.

Claims

1. A drying method for preparing β-ruthenium trichloride, characterized by, The method relates to a drying stirring device, the drying stirring device comprising a tank body, a driving motor, a transmission mechanism, and multiple stirring shafts, the transmission mechanism being connected at the top of the tank body, one end of the multiple stirring shafts being connected to the transmission mechanism respectively, and the other end being located in the tank body, multiple infrared lamps being arranged in the tank body, upper stirring blades and lower stirring blades being arranged on the multiple stirring shafts, the upper stirring blades being left-handed, and the lower stirring blades being right-handed, the driving motor being used for driving the transmission mechanism to rotate. The method comprises the following steps: Step 1: a beta-type ruthenium trichloride solution is added into the tank body; Step 2: the driving motor drives the stirring shaft to stir the solution at a rotating speed of 150-180 r / min, meanwhile, the solution is heated by the 275W infrared lamp until the solution is skinned; Step 3: when the solution is skinned, the rotating speed of the driving motor is adjusted to 100-120 r / min, and the heating by the infrared lamp is continuously carried out until the solution is slurried; Step 4: when the solution is slurried, the rotating speed of the driving motor is adjusted to 50-80 r / min, and the heating by the infrared lamp is continuously carried out until the solution is lumped.

2. The drying method according to claim 1, characterized in that, The transmission mechanism is a planetary gear transmission mechanism, the planetary gear transmission mechanism comprising a sun gear and multiple planetary gears meshing with the sun gear, the sun gear and the multiple planetary gears being rotationally connected at the top of the tank body, the driving motor being connected with the sun gear, the number of teeth of the sun gear being greater than or less than the number of teeth of the planetary gears.

3. The drying method according to claim 2, characterized in that, Further comprising a support frame, the support frame being located between the transmission mechanism and the tank body, the support frame being provided with through holes matched with the positions of the sun gear and the multiple planetary gears, one end of the multiple stirring shafts penetrating through the through holes and being connected with the sun gear and the multiple planetary gears.

4. The drying method according to claim 3, characterized in that, The planetary gears are three, and the through holes are four.

5. The drying method according to claim 4, characterized in that, The support frame comprises integrally formed first, second and third plate bodies, one end of the first, second and third plate bodies being connected, and the included angles between the first and second plate bodies, the second and third plate bodies and the third and first plate bodies being the same, the through holes being located at the central part, the end of the first plate body, the end of the second plate body and the end of the third plate body respectively.

6. The drying method according to claim 1, wherein The upper stirring blade comprises a first connecting column and multiple first blades, the multiple first blades being connected to the outer side of the first connecting column and being arranged along the circumferential direction of the first connecting column, the first connecting column being detachably connected to the stirring shaft through bolts; The lower stirring blade comprises a second connecting column and multiple second blades, the multiple second blades being connected to the outer side of the second connecting column and being arranged along the circumferential direction of the second connecting column, the second connecting column being detachably connected to the stirring shaft through bolts, the multiple first blades and the multiple second blades being arranged symmetrically above and below.

7. The drying method according to claim 6, characterized in that, The included angles between the multiple first blades, the multiple second blades and the horizontal plane are all 40-50°.

8. The drying method according to claim 6, wherein The first blades are four, the second blades are four, the first blades and the first connecting column are an integrally formed structure, and the second blades and the second connecting column are an integrally formed structure.

9. The drying method according to claim 1, wherein The side of the tank body is provided with an inlet and an outlet arranged in up and down direction, and an exhaust pipe arranged opposite to the inlet.

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