A process for diagnosing the performance of reducing agent in titanium dioxide bleaching process and degassing equipment

Abstract

The invention discloses a reductant performance diagnosis process and degassing equipment in a titanium dioxide bleaching process, relates to the technical field of titanium dioxide production, and comprises the following steps; S1: accurately measure 1-2 ml reductant sample and add it to a conical flask; S2: add 50 ml of distilled water treated by a degassing equipment and at room temperature to the conical flask, wherein the degassing equipment is mainly used for gases dissolved in distilled water; S3: then drip sulfuric acid with a mass fraction of 20% to the conical flask, and control the pH of the solution system to be 1-3; S4: then titrate with a potassium permanganate standard solution with a concentration of 0.4921 mol / l, from colorless titration to red at the end point, and the end point is that the color does not fade for 30 seconds, and the titration volume V is recorded; S5: evaluate the reducing ability of the reductant by multiplying the concentration of the potassium permanganate standard solution by the volume divided by the sampling volume. The process is simple and can quickly and accurately detect the reducing ability of the reductant.

Description

Technical Field

[0001] The invention relates to the technical field of titanium dioxide production, and in particular to a reducing agent performance diagnosis process and degassing equipment in a titanium dioxide bleaching process. Background Art

[0002] Titanium dioxide (titanium dioxide) is widely used in coatings, plastics, paper and other industries due to its excellent hiding power, weather resistance and non-reactive properties with most chemicals. In the production process of titanium dioxide, the bleaching step is one of the key links. Its purpose is to reduce the trivalent iron ions in the metatitanic acid slurry to divalent iron ions, so as to facilitate the subsequent water washing to remove the iron ions and improve the purity and whiteness of the product. The commonly used bleaching method is mainly to add metatitanic acid to concentrated sulfuric acid to dissolve it, then use aluminum powder to reduce tetravalent titanium to trivalent titanium, and then use trivalent titanium as a reducing agent for bleaching. This process is costly, and the preparation process of trivalent titanium is also dangerous. Therefore, more and more titanium dioxide bleaching processes use reducing agents for direct bleaching. However, there are many types of reducing agents on the market, and the reducing ability of various reducing agents cannot be accurately quantified. Titanium dioxide manufacturers cannot accurately select suitable reducing agents in the bleaching process, resulting in product quality fluctuations. Providing a simple and accurate reducing ability detection method has important practical application value. Therefore, the present application provides a reducing ability detection method and degassing equipment for reducing agent used for titanium dioxide bleaching to meet the needs. Summary of the invention

[0003] The purpose of the present application is to provide a reducing agent performance diagnosis process and degassing equipment in a titanium dioxide bleaching process. The process is simple and can quickly and accurately detect the reducing ability of the reducing agent.

[0004] To achieve the above-mentioned purpose, the present application provides the following technical solutions: A process for diagnosing the performance of a reducing agent in a titanium dioxide bleaching process, comprising the following steps;

[0005] S1: Add 50 ml of distilled water at room temperature that has been treated with a degassing device into a 250 ml conical flask. The degassing device is mainly used to discharge the gas dissolved in the distilled water;

[0006] S2: Accurately measure 1-2 ml of reducing agent sample and add it to the conical flask;

[0007] S3: Add 20% sulfuric acid to the conical flask to control the pH of the solution system to 1-3;

[0008] S4: Then titrate with a potassium permanganate standard solution with a concentration of 0.4921 mol / l, from colorless to red at the end point. The end point is when the color does not fade within 30 seconds, and record the titration volume V;

[0009] S5: Evaluate the reducing ability of the reducing agent by multiplying the concentration of the potassium permanganate standard solution by its volume and dividing it by the sampling volume.

[0010] A degassing device, comprising a water bath heating tank with an electric heater, a liquid receiving tank, a cooling bottle, a self-driving unit and a self-triggering cooling unit;

[0011] A placing table is arranged in the water bath heating tank, a through hole is arranged at the axis of the placing table and a carrying net is installed in the through hole;

[0012] The bottom of the water bath heating tank is integrally formed and protrudes with a convex block, the mounting cavity of the convex block is communicated with the inner cavity of the water bath heating tank, a first liquid discharge pipe is provided on the outer wall of the convex block, a first manual valve is provided on the first liquid discharge pipe, and the liquid outlet of the first liquid discharge pipe is located above the liquid receiving tank;

[0013] The cooling bottle is located above the liquid receiving tank, a liquid injection port is provided at the upper end of the cooling bottle, a second liquid discharge pipe with a second manual valve is provided at the lower end of the cooling bottle, and a liquid outlet of the second liquid discharge pipe is located above the water bath heating tank;

[0014] The self-driving unit comprises an inner hollow tube filled with water, and an outer hollow tube is provided on the outer wall of the inner hollow tube in a sealing sliding sleeve, the inner cavity of the inner hollow tube is communicated with the inner cavity of the outer hollow tube, the lower end of the inner hollow tube is fixedly installed in the installation cavity through a connecting rod, the lower end of the inner hollow tube is sealed by a heat-conducting copper block, the inner hollow tube and the outer hollow tube are both made of heat-insulating materials, the first drain pipe is located above the heat-conducting copper block, an L-shaped tooth plate is fixed to the upper end of the outer hollow tube, the L-shaped tooth plate is provided with a tooth connection section adapted to the first gear provided on the regulating rod of the first manual valve, and the tooth connection section is initially located below the first gear;

[0015] The self-triggered cooling unit includes a movable slot rotatably arranged on the second manual valve through a rotating shaft, a contact rod installed at the lower part of the outer hollow tube, and a first blocking rod and a second blocking rod installed up and down on the second liquid discharge pipe;

[0016] A sliding block is slidably arranged in the movable cavity of the movable groove, a rectangular opening is arranged at the bottom of the inner cavity of the movable groove, the adjusting handle of the second manual valve vertically passes through the rectangular opening, and a push switch for controlling the electric heater to stop working is installed in the inner cavity of the rectangular opening, and two inclined surfaces are symmetrically arranged on the upper end of the push switch, and the inclined surfaces are located above the rectangular opening. At the beginning, the movable groove is arranged with the left side lower and the right side higher, and is in contact with the first blocking rod.

[0017] As a preferred implementation manner in this embodiment, it also includes a rapid cooling unit, which is installed on the water bath heating tank and is used to pour the room temperature water in the cooling bottle from top to bottom on the rotating conical flask to accelerate the cooling of the conical flask and the distilled water inside.

[0018] As a preferred implementation in this embodiment, the rapid cooling unit includes a worm gear ring rotatably arranged in the through hole and a ring tube installed at the liquid outlet of the second liquid discharge pipe, and a worm engaged with the worm gear ring is arranged on the placement table, and one end of the worm passes through the water bath heating tank and is gear-connected with the L-shaped gear plate through a second gear;

[0019] The bearing net is installed in the inner cavity of the worm gear ring, the worm gear ring is coaxially arranged with the ring tube, and a plurality of liquid outlet heads are arranged on the ring tube in a circular shape and obliquely downward, and the inner circle diameter surrounded by the plurality of liquid outlet heads is larger than the maximum diameter of the conical flask.

[0020] As a preferred implementation manner in this embodiment, the liquid outlet ports of the plurality of liquid outlet heads are located at one half to two thirds of the height of the conical flask.

[0021] As a preferred implementation in this embodiment, it also includes a water lifting mechanism and a temporary water storage bucket with an opening at the upper end, the lower end discharge port of the temporary water storage bucket is connected to the liquid injection port at the upper end of the cooling bottle, and a third manual valve is installed on the discharge port, and the cooling bottle is provided with a vent pipe;

[0022] Water lifting mechanism: used to lift the water with a certain amount of heat in the liquid receiving tank to the temporary water storage barrel, and after the warm water is cooled to room temperature, it is discharged into the cooling bottle through the third manual valve.

[0023] As a preferred implementation in this embodiment, the water lifting mechanism includes a crankshaft rotatably arranged on the outer wall of the water bath heating tank, two cylinders fixedly arranged on the outer wall of the water bath heating tank and having an opening at the upper end, and a liquid infusion tube installed on the temporary water storage bucket;

[0024] The lower ends of the two cylinders are provided with a liquid inlet pipe with a liquid inlet check valve and a liquid outlet pipe with a liquid outlet check valve, the two liquid outlet pipes are connected to the liquid infusion pipe through a hose, and the two liquid inlet pipes are connected to the liquid receiving tank through a hose, and pistons are sealed and movably provided in the two cylinders, and the two pistons are movably connected to the crankshaft through corresponding movable rods, and the two movable rods are arranged one above and one below;

[0025] The crankshaft upper fixed sleeve is provided with a third gear and the third gear is gear-connected with the L-shaped gear plate.

[0026] In summary, the technical effects and advantages of the present invention are as follows:

[0027] The process is simple and can quickly and accurately detect the reducing ability of the reducing agent;

[0028] In the present invention, the degassing device is provided with a water bath heating tank, a liquid receiving tank, a cooling bottle, a self-driving unit and a self-triggering cooling unit, which can realize the heating and automatic cooling of the distilled water in the conical flask;

[0029] In the present invention, a rapid cooling unit is provided, and the distilled water can be cooled uniformly and effectively accelerated by a rotating and pouring method. Meanwhile, the rotating conical flask is beneficial to promoting the overflow of gas in the distilled water. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For those skilled in the art, other drawings can be obtained based on these drawings without paying any creative work.

[0031] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention;

[0032] Figure 2 for Figure 1 Schematic diagram of the local structure;

[0033] Figure 3 for Figure 1 Schematic diagram of the structure of the first liquid discharge pipe;

[0034] Figure 4 for Figure 3 Schematic diagram of the cross-section structure of the middle movable groove;

[0035] Figure 5 for Figure 3 Schematic diagram of the cross-sectional structure of the middle convex block;

[0036] Figure 6 for Figure 1 Enlarged structural diagram at A in the middle.

[0037] In the figure: 1, water bath heating tank; 2, liquid receiving tank; 3, cooling bottle; 301, air permeable tube; 302, second liquid discharge pipe; 4, placing table; 401, carrying net; 5, third manual valve; 6, bump; 601, first liquid discharge pipe; 602, first manual valve; 603, first gear; 604, gear section; 7, self-driving unit; 701, inner hollow tube; 702, outer hollow tube; 703, heat-conducting copper block; 8, L-shaped tooth plate; 9, second manual valve; 901. Adjusting handle; 10. Push switch; 11. Movable groove; 12. Sliding block; 13. First blocking rod; 14. Second blocking rod; 15. Inclined surface; 16. Annular tube; 17. Liquid outlet head; 18. Worm ring; 19. Worm; 20. Second gear; 21. Crankshaft; 22. Third gear; 23. Movable rod; 24. Piston; 25. Cylinder; 26. Liquid inlet pipe; 27. Liquid outlet pipe; 28. Temporary water storage barrel; 29. ​​Infusion tube; 30. Contact rod. DETAILED DESCRIPTION

[0038] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0039] A process for diagnosing the performance of a reducing agent in a titanium dioxide bleaching process comprises the following steps:

[0040] S1: Add 50 ml of distilled water at room temperature that has been treated with a degassing device into a 250 ml conical flask. The degassing device is mainly used to discharge the gas dissolved in the distilled water;

[0041] Although distilled water itself is obtained through the distillation process, most of the dissolved gases in the water have been removed, but in actual operation, a certain amount of dissolved gases still remain in the distilled water. The gases dissolved in the distilled water (such as oxygen) can react chemically with the reducing agent or the potassium permanganate standard solution, thereby affecting the chemical balance in the titration process. For example, oxygen can react with the reducing agent as an oxidant, resulting in a decrease in the effective concentration of the reducing agent, thereby interfering with the accurate determination of the reducing ability; and some dissolved gases (such as nitrogen, carbon dioxide, etc.) do not react directly with the reducing agent or potassium permanganate, but their presence may affect the color or transparency of the solution. This will interfere with the judgment of the titration endpoint, making the color change at the endpoint not obvious or difficult to accurately judge, thereby affecting the accuracy of the titration volume. Therefore, distilled water needs to be degassed by a degassing device before testing.

[0042] S2: Accurately measure 1-2 ml of reducing agent sample and add it to the conical flask;

[0043] S3: Add 20% sulfuric acid to the conical flask to control the pH of the solution system to 1-3;

[0044] S4: Then titrate with a potassium permanganate standard solution with a concentration of 0.4921 mol / l, from colorless to red at the end point. The end point is when the color does not fade within 30 seconds, and record the titration volume V;

[0045] S5: Evaluate the reducing ability of the reducing agent by multiplying the concentration of the potassium permanganate standard solution by its volume and dividing it by the sampling volume. Embodiment 1:

[0046] Add 50 ml of degassed and room temperature distilled water (measured with a 50 ml measuring cylinder) into the conical flask;

[0047] Use a pipette to accurately measure 1 ml of reducing agent sample and add it to a 250 ml conical flask;

[0048] Add 20% sulfuric acid to the solution and control the pH of the solution to 4-5.

[0049] Titrate with a potassium permanganate standard solution with a concentration of 0.4921 mol / l. Titrate from colorless to red at the end point. If the color does not fade within 30 seconds, that is the end point. Record the titration volume V.

[0050] The reducing ability of the reducing agent was evaluated by multiplying the concentration of the potassium permanganate standard solution by its volume and dividing it by the sample volume. Embodiment 2:

[0051] Add 50 ml of degassed and room temperature distilled water (measured with a 50 ml measuring cylinder) into the conical flask;

[0052] Use a pipette to accurately measure 2 ml of reducing agent sample and add it to a 250 ml conical flask;

[0053] Add 20% sulfuric acid to the solution and control the pH of the solution to 3-4.

[0054] Titrate with a standard potassium permanganate solution with a concentration of 0.4921 mol / l. Titrate from colorless to red at the end point. If the color does not fade within 30 seconds, that is the end point. Record the titration volume V.

[0055] The reducing ability of the reducing agent was evaluated by multiplying the concentration of the potassium permanganate standard solution by its volume and dividing it by the sample volume. Embodiment 3:

[0056] Add 50 ml of degassed and room temperature distilled water (measured with a 50 ml measuring cylinder) into the conical flask;

[0057] Use a pipette to accurately measure 2 ml of reducing agent sample and add it to a 250 ml conical flask;

[0058] Add 20% sulfuric acid to the solution and control the pH of the solution to 2-3.

[0059] Titrate with a potassium permanganate standard solution with a concentration of 0.4921 mol / l. Titrate from colorless to red at the end point. If the color does not fade within 30 seconds, that is the end point. Record the titration volume V.

[0060] The reducing ability of the reducing agent was evaluated by multiplying the concentration of the potassium permanganate standard solution by its volume and dividing it by the sample volume. Embodiment 4:

[0061] Add 50 ml of degassed and room temperature distilled water (measured with a 50 ml measuring cylinder) into the conical flask;

[0062] Use a pipette to accurately measure 2 ml of reducing agent sample and add it to a 250 ml conical flask;

[0063] Add 20% sulfuric acid to the solution and control the pH of the solution to 1-2.

[0064] Titrate with a potassium permanganate standard solution with a concentration of 0.4921 mol / l. Titrate from colorless to red at the end point. If the color does not fade within 30 seconds, that is the end point. Record the titration volume V.

[0065] The reducing ability of the reducing agent was evaluated by multiplying the concentration of the potassium permanganate standard solution by its volume and dividing it by the sample volume.

[0066] Experimental data 1:

[0067]

[0068] Examples 1, 2, 3 and 4 show that the reducing agent reducing ability detection method needs to ensure that the pH of the detection system is in the range of 1-3. If the pH is too high, the measurement results vary greatly and the detection endpoint is unclear. Embodiment 5:

[0069] Add 50 ml of degassed and room temperature distilled water (measured with a 50 ml measuring cylinder) into the conical flask;

[0070] Use a pipette to accurately measure 1 ml of reducing agent sample and add it to a 250 ml conical flask;

[0071] Add 20% sulfuric acid to the system and control the pH of the system to be between 1 and 3;

[0072] Titrate with a potassium permanganate standard solution with a concentration of 0.4921 mol / l. Titrate from colorless to red at the end point. If the color does not fade within 30 seconds, that is the end point. Record the titration volume V.

[0073] The reducing ability of the reducing agent was evaluated by multiplying the concentration of the potassium permanganate standard solution by its volume and dividing it by the sample volume. Embodiment 6:

[0074] Add 50 ml of degassed and room temperature distilled water (measured with a 50 ml measuring cylinder) into the conical flask;

[0075] Use a pipette to accurately measure 2 ml of reducing agent sample and add it to a 250 ml conical flask;

[0076] Add 20% sulfuric acid to the system and control the pH of the system to be between 1 and 3;

[0077] Titrate with a potassium permanganate standard solution with a concentration of 0.4921 mol / l. Titrate from colorless to red at the end point. If the color does not fade within 30 seconds, that is the end point. Record the titration volume V.

[0078] The reducing ability of the reducing agent was evaluated by multiplying the concentration of the potassium permanganate standard solution by its volume and dividing it by the sample volume. Embodiment 7:

[0079] Add 50 ml of degassed and room temperature distilled water (measured with a 50 ml measuring cylinder) into the conical flask;

[0080] Use a pipette to accurately measure 3 ml of reducing agent sample and add it to a 250 ml conical flask;

[0081] Add 20% sulfuric acid to the system and control the pH of the system to be between 1 and 3;

[0082] Titrate with a potassium permanganate standard solution with a concentration of 0.4921 mol / l. Titrate from colorless to red at the end point. If the color does not fade within 30 seconds, that is the end point. Record the titration volume V.

[0083] The reducing ability of the reducing agent was evaluated by multiplying the concentration of the potassium permanganate standard solution by its volume and dividing it by the sample volume.

[0084] Experimental data 2:

[0085]

[0086] Examples 5, 6 and 7 show that the parallelism of the process detection results meets the detection requirements.

[0087] like Figure 1-5As shown, a degassing device comprises a water bath heating tank 1 with an electric heater, a liquid receiving tank 2, a cooling bottle 3, a self-driving unit 7 and a self-triggering cooling unit;

[0088] A placing table 4 is arranged in the water bath heating tank 1, a through hole is arranged at the axis center of the placing table 4 and a carrying net 401 is installed in the through hole;

[0089] The bottom of the water bath heating tank 1 is integrally formed and protrudes with a convex block 6, the installation cavity of the convex block 6 is communicated with the inner cavity of the water bath heating tank 1, a first liquid discharge pipe 601 is provided on the outer wall of the convex block 6, a first manual valve 602 is provided on the first liquid discharge pipe 601, and the liquid outlet of the first liquid discharge pipe 601 is located above the liquid receiving tank 2;

[0090] The cooling bottle 3 is located above the liquid receiving tank 2, the upper end of the cooling bottle 3 is provided with a liquid injection port, the lower end of the cooling bottle 3 is provided with a second liquid discharge pipe 302 with a second manual valve 9, and the liquid outlet of the second liquid discharge pipe 302 is located above the water bath heating tank 1;

[0091] The self-driving unit 7 includes an inner hollow tube 701 filled with water, and an outer hollow tube 702 is provided on the outer wall of the inner hollow tube 701 in a sealing sliding sleeve, the inner cavity of the inner hollow tube 701 is communicated with the inner cavity of the outer hollow tube 702, the lower end of the inner hollow tube 701 is fixedly installed in the installation cavity through a connecting rod, the lower end of the inner hollow tube 701 is sealed by a heat-conducting copper block 703, the inner hollow tube 701 and the outer hollow tube 702 are both made of heat-insulating materials, the first drain pipe 601 is located above the heat-conducting copper block 703, an L-shaped tooth plate 8 is fixed to the upper end of the outer hollow tube 702, and a toothed section 604 adapted to the first gear 603 provided on the regulating rod of the first manual valve 602 is provided on the L-shaped toothed plate 8, and the toothed section 604 is initially located below the first gear 603;

[0092] The self-triggered cooling unit includes a movable slot 11 arranged on the second manual valve 9 through a rotating shaft, a contact rod 30 installed at the lower part of the outer hollow tube 702, and a first blocking rod 13 and a second blocking rod 14 installed up and down on the second liquid discharge pipe 302;

[0093] A slider 12 is slidably arranged in the movable cavity of the movable groove 11, a rectangular opening is arranged at the bottom of the inner cavity of the movable groove 11, an adjusting handle 901 of the second manual valve 9 vertically passes through the rectangular opening, and a push switch 10 for controlling the electric heater to stop working is installed in the inner cavity of the rectangular opening, and two inclined surfaces 15 are symmetrically arranged on the upper end of the push switch 10, and the inclined surfaces 15 are located above the rectangular opening. At the beginning, the movable groove 11 is arranged with the left side lower and the right side higher, and contacts with the first blocking rod 13.

[0094] A conical flask filled with distilled water is placed on the carrying net 401, there is water in the accommodating cavity of the water bath heating tank 1 and the lower half of the conical flask is immersed (the immersion water level is basically consistent with the liquid level in the conical flask), the electric heater is controlled to heat the water in the water bath heating tank 1, and the water in the inner hollow tube 701 can be heated by the heat conduction effect of the heat conductive copper block 703. After the water in the water bath heating tank 1 is heated and boiled, the distilled water in the conical flask will also boil, so that the gas in the distilled water will escape, and at the same time, the water in the inner hollow tube 701 will also boil and vaporize, so that the air pressure in the inner hollow tube 701 increases, thereby causing the outer hollow tube 702 to move upward, and the rise of the outer hollow tube 702 will drive The L-shaped toothed plate 8 rises, and after the L-shaped toothed plate 8 rises for a certain distance (that is, the process provides sufficient degassing time for the distilled water after boiling), the toothed section 604 is toothed with the first gear 603, and drives the first gear 603 to rotate and open the first liquid discharge pipe 601 (the toothed connection is separated after opening), so that the hot water in the water bath heating tank 1 enters the liquid receiving tank 2. After all the hot water in the water bath heating tank 1 except the hot water in the installation cavity flows into the liquid receiving tank 2, the contact rod 30 contacts the bottom of the movable tank 11 and makes the movable tank 11 rotate around the rotation axis. When the movable tank 11 changes from left low and right high to left high and right low, the slider 12 will slide to the right. In this process, the slider 12 will contact the inclined surface 15 on the press switch 10. The push switch 10 contacts and squeezes it, causing the electric heater to stop heating. The slider 12 that passes the push switch 10 will contact the adjusting handle 901 and drive it to rotate, thereby opening the second liquid discharge pipe 302 (ultimately, its slider 12 makes the movable groove 11 higher on the left and lower on the right, and the lower right end of the movable groove 11 contacts the second blocking rod 14). The cooling water in the cooling bottle 3 enters the water bath heating tank 1, and the cooling water enters the accommodating cavity of the water bath heating tank 1 and the mounting cavity of the protrusion 6, exchanges heat with the inner wall of the water bath heating tank 1 and the hot water in the mounting cavity, and discharges the water with a certain temperature after the exchange to the liquid receiving tank 2 (at this time, the temperature of the water bath heating tank 1 itself drops), and the hot water temperature in the mounting cavity The gas in the inner hollow tube 701 is cooled by heat conduction, so that the internal air pressure of the inner hollow tube 701 decreases and moves downward. As the L-shaped tooth plate 8 moves downward, the tooth connection section 604 will be again engaged with the first gear 603 and drive it to rotate, thereby closing the pipeline of the first liquid discharge pipe 601. At this time, the water in the water bath heating tank 1 cannot enter the liquid receiving tank 2. As the water level in the water bath heating tank 1 rises, the lower part of the conical flask is finally immersed (at this time, the cooling water in the lowering bottle 3 is used up, and the water level at this time is basically the same as the water level in the water bath heating tank 1 during heating), the lower part of the conical flask is immersed in the cooling water to cool it down, and the water in the conical flask can be cooled to room temperature after waiting for a period of time.

[0095] It should be noted that: 1. The liquid outlet of the second liquid discharge pipe 302 deviates from the position directly below the mounting cavity of the protrusion 6 (the liquid outlet of the second liquid discharge pipe 302 can be moved as far away from the protrusion 6 as possible, so that the movement path of the cooling water in the water bath heating tank 1 becomes longer, which is beneficial for the discharged cooling water to maximize the contact area with the inner wall of the water bath heating tank 1 and absorb the heat, which is beneficial for reducing the temperature of the cooling water in the water bath heating tank 1 when the lower part of the conical flask is immersed, thereby accelerating the cooling of the conical flask), the cooling water first enters the water bath heating tank 1 to absorb the heat of the residual hot water in the water bath heating tank 1 and the mounting cavity, and the cooling water after absorbing heat will flow into the liquid receiving tank 2 (The water in the waiting liquid receiving tank 2 can be used as cooling water after being cooled and added to the cooling bottle 3 for use), which can effectively reduce the temperature of the cooling water after being stored in the storage water bath heating tank 1, so that when the lower part of the conical flask is immersed, the temperature of the cooling water is not much different from the actual room temperature (basically maintained at about 5 to 10°), which is conducive to the rapid cooling of the conical flask, and at the same time, the cooling water that has absorbed heat and flows into the liquid receiving tank 2 is mixed with the boiling water in the liquid receiving tank 2, thereby reducing the temperature of the water in the liquid receiving tank 2, which is conducive to its temperature quickly lowering to room temperature, and thus is conducive to shortening the heating time of the next conical flask (after each conical heating and degassing is completed, the reducing agent needs to be immediately carried out). The detection time of the capacity is to avoid that the air will be dissolved into the distilled water of the conical flask again due to too long a time. This detection process provides enough time for the cooling of the water); second, the water level of the cooling water in the water bath heating tank 1 is consistent with the water level during heating. After the distilled water is cooled by the cooling water, the cooling water is prepared to be used as the heating water for the next time; third, the bearing net 401 is set to increase the direct contact area between the bottom of the conical flask and the cooling water, which is conducive to accelerating the heat dissipation of the distilled water; fourth, after the conical flask has finished cooling the water, the movable groove 11, the slider 12 and the adjustment handle 901 are controlled to return to their original positions; fifth, the liquid inlet of the first discharge pipe 601 is The end is arranged below the bottom surface of the inner cavity of the water bath heating tank 1 and above the heat-conducting copper block 703, so that after the hot water in the accommodating cavity of the water bath heating tank 1 is completely discharged, there is still hot water in the installation cavity of the protrusion 6 to heat the heat-conducting copper block 703, so that the outer hollow tube 702 can continue to move upward and contact with the movable groove 11, and finally turn off the electric heater and open the second manual valve 9; six, the water capacity in the cooling bottle 3 is consistent with the water volume in the water bath heating tank 1 during heating; seven, the outer wall fixed sleeve of the upper end of the inner hollow tube 701 is provided with an elastic sealing sleeve, and the outer wall of the elastic sealing sleeve slides against the inner wall of the outer hollow tube 702 to form a seal.

[0096] As a preferred implementation in this embodiment, it also includes a rapid cooling unit installed on the water bath heating tank 1, which is used to pour the room temperature water in the cooling bottle 3 from top to bottom on the rotating conical flask to accelerate the cooling of the conical flask and the distilled water inside.

[0097] As a preferred implementation in this embodiment, Figure 1As shown, the rapid cooling unit includes a worm gear ring 18 rotatably arranged in the through hole and a ring tube 16 installed at the liquid outlet of the second liquid discharge pipe 302, and a worm 19 meshingly connected with the worm gear ring 18 is arranged on the placement table 4, and one end of the worm 19 passes through the water bath heating tank 1 and is gear-connected with the L-shaped gear plate 8 through the second gear 20;

[0098] The carrier net 401 is installed in the inner cavity of the worm gear ring 18. The worm gear ring 18 is coaxially arranged with the ring tube 16. A plurality of liquid outlet heads 17 are arranged on the ring tube 16 in a circular shape and obliquely downward. The inner diameter of the circle surrounded by the plurality of liquid outlet heads 17 is larger than the maximum diameter of the conical flask.

[0099] After the distilled water in the conical flask boils, the outer hollow tube 702 drives the L-shaped tooth plate 8 to move upward under the action of the internal air pressure. The upward moving L-shaped tooth plate 8 is driven by the second gear 20, so that the worm 19 drives the worm ring 18 to rotate, and then drives the conical flask to rotate (at a lower speed). When the conical flask rotates at a low speed, the distilled water also moves. This change in the state of motion will affect the microstructure inside the liquid, making it easier for the gas molecules that were originally "trapped" due to intermolecular interactions to find a path to escape. In other words, the rotation increases the chance of gas molecules contacting the liquid surface, thereby promoting the overflow of the gas. At the same time, the rotation can also generate a certain centrifugal force, which helps to push the gas molecules into the liquid The edge of the L-shaped tooth plate 8 further increases the possibility of gas escape. When the L-shaped tooth plate 8 moves downward, the cooling water in the cooling bottle 3 is discharged from the liquid outlet head 17 of the ring tube 16, and the rotating conical bottle is poured from top to bottom, so that a continuous cooling rain curtain can be formed on the bottle body, so that the conical bottle absorbs heat evenly everywhere. By adopting this cooling method, when the cooling water in the water bath heating tank 1 reaches the initial heating water level, the temperature of the distilled water in the conical bottle and the cooling water in the water bath heating tank 1 is basically consistent with the room temperature, and the difference between the upper and lower is not more than 2°. The conical bottle can be directly taken out for use without waiting for a period of time, which can greatly improve the cooling speed. The distilled water can be evenly cooled and the cooling of the distilled water can be effectively accelerated by the rotation and pouring method.

[0100] It should be noted that: first, the absorbed water falling from the conical flask will exchange with the hot water in the installation cavity, thereby reducing the temperature of the hot water, and exchanging heat with the hot air in the inner hollow tube 701, thereby reducing the internal gas temperature, and finally causing the outer hollow tube 702 to move downward; second, in the initial stage of heating the conical flask, since the conical flask is not rotated, the bubbles tend to rise to the water surface along a fixed path after they are formed. This fixed rising path helps the bubbles to merge into larger bubbles during the rising process, making them easier to observe and discharge. By not rotating the conical flask in the initial stage to allow the bubbles to gather and rise on a fixed path, and then combining the rotation operation of the conical flask after boiling, the gas in the distilled water can be more effectively discharged. This operation mode combines static and dynamic modes, which not only ensures the effective gathering and rising of the gas, but also accelerates the release and overflow of the gas through rotation, which is more conducive to completely discharging the gas dissolved in the distilled water.

[0101] As a preferred implementation in this embodiment, the liquid outlet ports of the plurality of liquid outlet heads 17 are located at one-half to two-thirds of the height of the conical flask.

[0102] In this height range, the water discharged from the liquid outlet 17 forms a water curtain that can completely cover the lower bottle body of the conical flask (in the rotating state), and ensure that the cooling water forms a relatively uniform water film on the rotating conical flask. The uniform water film can absorb heat more effectively and avoid local overheating or uneven cooling.

[0103] At the same time, cooling at this height can reduce the thermal stress caused by excessive temperature gradient, which helps to extend the service life of the conical flask and prevent cracking or deformation caused by excessive thermal stress.

[0104] It should be noted that the distilled water contained in the conical flask is located below one-half the height of the conical flask.

[0105] As a preferred implementation in this embodiment, it also includes a water lifting mechanism and a temporary water storage bucket 28 with an opening at the upper end, the lower end discharge port of the temporary water storage bucket 28 is connected to the liquid injection port at the upper end of the cooling bottle 3, and a third manual valve 5 is installed on the discharge port, and the cooling bottle 3 is provided with a vent pipe 301;

[0106] Water lifting mechanism: used to lift the water with a certain amount of heat in the liquid receiving tank 2 to the temporary water storage bucket 28, and after the warm water is cooled to room temperature, it is discharged into the cooling bottle 3 through the third manual valve 5.

[0107] The water in the liquid receiving tank 2 can be lifted to the temporary water storage bucket 28 by the water lifting mechanism, and after being cooled, it can be transported to the cooling bottle 3 for standby use.

[0108] As a preferred implementation in this embodiment, Figure 1 and Figure 6 As shown, the water lifting mechanism includes a crankshaft 21 rotatably arranged on the outer wall of the water bath heating tank 1, two cylinders 25 fixedly arranged on the outer wall of the water bath heating tank 1 and having an opening at the upper end, and a liquid infusion pipe 29 installed on a temporary water storage barrel 28;

[0109] The lower ends of the two cylinders 25 are provided with a liquid inlet pipe 26 with a liquid inlet check valve and a liquid outlet pipe 27 with a liquid outlet check valve. The two liquid outlet pipes 27 are connected to the liquid infusion pipe 29 through a hose. The two liquid inlet pipes 26 are connected to the liquid receiving tank 2 through a hose. Pistons 24 are sealed and movably provided in the two cylinders 25, and the two pistons 24 are movably connected to the crankshaft 21 through corresponding movable rods 23, and the two movable rods 23 are arranged one above and one below.

[0110] A third gear 22 is fixedly sleeved on the crankshaft 21 and the third gear 22 is gear-engaged with the L-shaped gear plate 8 .

[0111] When the L-shaped toothed plate 8 moves downward or upward, it will drive the crankshaft 21 to rotate. As the crankshaft 21 rotates, it will drive the two pistons 24 to move up and down through the activity, thereby continuously pumping the water in the liquid receiving tank 2 to the temporary water storage barrel 28. After the cooling water in the cooling bottle is discharged and the second manual valve 9 is closed, the water in the temporary water storage barrel 28 that has been cooled to room temperature can be released into the cooling bottle 3. The operation is convenient and simple, the labor intensity is low (avoiding manual pouring of the water in the liquid receiving tank 2 into the cooling bottle 3), and the recycling of water is realized.

[0112] It should be noted that: first, the temporary water storage barrel 28 is made of heat dissipation material, which is conducive to quickly dissipating the heat of the water contained therein, and the cooling bottle 3 is made of insulation material, which prevents the heat in the temporary water storage barrel 28 from being transferred to the cooling water in the cooling bottle 3, thereby increasing the temperature of the cooling water, which is not conducive to the subsequent rapid heat dissipation of the distilled water; second, no matter whether the L-shaped tooth plate 8 moves downward or upward, the water in the liquid receiving tank 2 will be transported to the temporary water storage barrel 28, which is conducive to obtaining enough cooling water.

[0113] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A degassing device, characterized in that: It comprises a water bath heating tank (1) with an electric heater, a liquid receiving tank (2), a cooling bottle (3), a self-driving unit (7) and a self-triggering cooling unit; A placement table (4) is arranged in the water bath heating tank (1), a through hole is arranged at the axis of the placement table (4), and a carrying net (401) is installed in the through hole; The bottom of the water bath heating tank (1) is integrally formed and protrudes with a protrusion (6); the mounting cavity of the protrusion (6) is communicated with the inner cavity of the water bath heating tank (1); a first liquid discharge pipe (601) is provided on the outer wall of the protrusion (6); a first manual valve (602) is provided on the first liquid discharge pipe (601); and the liquid outlet of the first liquid discharge pipe (601) is located above the liquid receiving tank (2); The cooling bottle (3) is located above the liquid receiving tank (2), a liquid injection port is provided at the upper end of the cooling bottle (3), a second liquid discharge pipe (302) with a second manual valve (9) is provided at the lower end of the cooling bottle (3), and a liquid outlet of the second liquid discharge pipe (302) is located above the water bath heating tank (1); The self-driving unit (7) comprises an inner hollow tube (701) filled with water, and an outer hollow tube (702) is provided on the outer wall of the inner hollow tube (701) in a sealing sliding sleeve, the inner cavity of the inner hollow tube (701) is communicated with the inner cavity of the outer hollow tube (702), the lower end of the inner hollow tube (701) is fixedly installed in the installation cavity via a connecting rod, the lower end of the inner hollow tube (701) is sealed via a heat-conducting copper block (703), and the inner hollow tube (701) is sealed with a heat-conducting copper block (703). ) and the outer hollow tube (702) are both made of heat-insulating materials, the first liquid discharge pipe (601) is located above the heat-conducting copper block (703), an L-shaped tooth plate (8) is fixed to the upper end of the outer hollow tube (702), the L-shaped tooth plate (8) is provided with a toothed section (604) adapted to the first gear (603) provided on the regulating rod of the first manual valve (602), and the toothed section (604) is initially located below the first gear (603); The self-triggered cooling unit comprises a movable groove (11) arranged on the second manual valve (9) by rotating the rotating shaft, a contact rod (30) installed at the lower part of the outer hollow tube (702), and a first blocking rod (13) and a second blocking rod (14) installed on the second liquid discharge pipe (302) in an upper and lower manner; A slider (12) is slidably arranged in the movable cavity of the movable groove (11), a rectangular opening is arranged at the bottom of the inner cavity of the movable groove (11), an adjusting handle (901) of the second manual valve (9) vertically passes through the rectangular opening, and a push switch (10) for controlling the electric heater to stop working is installed in the inner cavity of the rectangular opening, and two inclined surfaces (15) are symmetrically arranged at the upper end of the push switch (10), and the inclined surfaces (15) are located above the rectangular opening. At the beginning, the movable groove (11) is arranged to be lower on the left and higher on the right, and is in contact with the first blocking rod (13).

2. A degassing device according to claim 1, characterized in that: It also includes a rapid cooling unit installed on the water bath heating tank (1) and used to pour the room temperature water in the cooling bottle (3) from top to bottom onto the rotating conical flask, thereby accelerating the cooling of the conical flask and the distilled water inside.

3. A degassing device according to claim 2, characterized in that: The rapid cooling unit comprises a worm wheel ring (18) rotatably arranged in the through hole and a ring tube (16) installed at the liquid outlet of the second liquid discharge pipe (302); a worm (19) meshingly connected to the worm wheel ring (18) is arranged on the placement table (4); one end of the worm (19) passes through the water bath heating tank (1) and is gear-connected to the L-shaped toothed plate (8) via a second gear (20); The carrier net (401) is installed in the inner cavity of the worm gear ring (18), the worm gear ring (18) is coaxially arranged with the ring tube (16), and a plurality of liquid outlet heads (17) are arranged on the ring tube (16) in a circular shape and obliquely downward, and the diameter of the inner circle surrounded by the plurality of liquid outlet heads (17) is greater than the maximum diameter of the conical flask.

4. A degassing device according to claim 3, characterized in that: The liquid outlet ports of the plurality of liquid outlet heads (17) are located at one-half to two-thirds of the height of the conical flask.

5. A degassing device according to claim 1, characterized in that: It also includes a water lifting mechanism and a temporary water storage bucket (28) with an opening at the upper end, the liquid discharge port at the lower end of the temporary water storage bucket (28) is connected to the liquid injection port at the upper end of the cooling bottle (3), and a third manual valve (5) is installed on the liquid discharge port, and the cooling bottle (3) is provided with a vent pipe (301); Water lifting mechanism: used to lift water with a certain amount of heat in the liquid receiving tank (2) into the temporary water storage bucket (28), and after the water temperature is cooled to room temperature, discharge it into the cooling bottle (3) through the third manual valve (5).

6. A degassing device according to claim 5, characterized in that: The water lifting mechanism comprises a crankshaft (21) rotatably arranged on the outer wall of the water bath heating tank (1), two cylinders (25) fixedly arranged on the outer wall of the water bath heating tank (1) and having an opening at the upper end, and a liquid infusion tube (29) installed on the temporary water storage barrel (28); A liquid inlet pipe (26) with a liquid inlet check valve and a liquid outlet pipe (27) with a liquid outlet check valve are provided at the lower ends of the two cylinders (25); the two liquid outlet pipes (27) are connected to the liquid infusion pipe (29) through a hose; the two liquid inlet pipes (26) are connected to the liquid receiving tank (2) through a hose; pistons (24) are sealed and movably provided in the two cylinders (25); the two pistons (24) are movably connected to the crankshaft (21) through corresponding movable rods (23); and the two movable rods (23) are arranged one above the other; A third gear (22) is fixedly sleeved on the crankshaft (21), and the third gear (22) is gear-engaged with the L-shaped gear plate (8).

7. A process for diagnosing the performance of a reducing agent in a titanium dioxide bleaching process, characterized in that: The method comprises the following steps: S1: Add 50 ml of distilled water at room temperature that has been treated by a degassing device into a 250 ml conical flask, wherein the degassing device is mainly used to discharge the gas dissolved in the distilled water, and the degassing device is any one of claims 1 to 6; S2: Accurately measure 1-2 ml of reducing agent sample and add it to the conical flask; S3: Add 20% sulfuric acid to the conical flask to control the pH of the solution system to 1-3; S4: Then titrate with a potassium permanganate standard solution with a concentration of 0.4921 mol / l, from colorless to red at the end point. The end point is when the color does not fade within 30 seconds, and record the titration volume V; S5: Evaluate the reducing ability of the reducing agent by multiplying the concentration of the potassium permanganate standard solution by its volume and dividing it by the sampling volume.

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