A method and device for efficiently removing glycerol from tellurium beads

Abstract

The present invention discloses a method and device for efficiently removing glycerol from tellurium beads. The method utilizes the high boiling point difference between glycerol and tellurium beads, and adopts a vacuum distillation method to completely distill and remove glycerol and water from the tellurium beads. The device comprises a tellurium bead holding tube, a heater, and a condensed liquid recovery device. The tellurium bead holding tube is horizontally and tiltedly placed in the heater, the tellurium bead holding tube is provided with a condensation outlet connected to the condensation liquid recovery device, and a cooler is provided at the condensation outlet of the tellurium bead holding tube. The device of the present invention has a simple structure and a simple and easy method, and solves the problems of small processing capacity, long time consumption, low efficiency, and incomplete glycerol removal in the existing method for removing glycerol from tellurium beads.

Description

Technical Field

[0001] The invention relates to the technical field of tellurium bead production, and in particular to a method and a device for efficiently removing glycerol from tellurium beads. Background Art

[0002] Tellurium is known as the "vitamin of industry", and 30% of it is used in the metallurgical industry. The main product forms of tellurium are tellurium ingots, tellurium powder, and tellurium beads. Tellurium ingots are too large and need to be crushed when used; tellurium powder is too fine and easily generates dust when added; in contrast, tellurium beads are small spherical particles with suitable sizes, no need to be crushed, easy to measure, can be used directly, and will not generate dust. Therefore, the preparation of tellurium beads is becoming more and more important. Tellurium beads are mainly used as additives for castings or special steels to improve their cutting performance and increase hardness, or as raw materials for making thermal analysis sample cups for detecting Si and C content in molten iron in front of the furnace.

[0003] At present, the mainstream technology for preparing tellurium beads is the glycerol molding method, which is low-cost and produces tellurium beads with high sphericity. The glycerol molding method uses glycerol as a molding agent, and the molten solution of tellurium forms droplets through a dropper and falls into the molding agent glycerol to form tellurium beads. However, during the molding process of tellurium beads, glycerol can easily enter the shrinkage pores of the tellurium beads. Since glycerol can be mixed with water in any proportion and has strong hygroscopicity, the tellurium beads are oxidized, affecting the product quality. Therefore, it is necessary to remove the glycerol in the tellurium beads.

[0004] There are two main methods for removing glycerol from tellurium beads: ultrasonic cleaning and detergent cleaning. The ultrasonic cleaning method uses ultrasonic cleaning to remove glycerol, but the processing capacity of ultrasonic cleaning is small, and only 3 to 5 kg of tellurium beads can be processed each time. In addition, ultrasonic cleaning cannot ensure that all tellurium beads are cleaned, and it cannot ensure that glycerol is completely removed. Therefore, the application of ultrasonic cleaning in enterprise production has great limitations and is time-consuming and labor-intensive. The detergent cleaning method is to add detergent to the tellurium beads, generally through 12 to 14 times of cleaning and 2 to 3 times of drying (drying time 8 to 12 hours) to remove glycerol. This method undoubtedly has the disadvantages of many cleaning times, complex procedures, long drying time, and long time consumption. It is easy to cause detergent residues and generate a large amount of chemical wastewater, which is not environmentally friendly. Summary of the invention

[0005] In view of this, and in response to the above-mentioned deficiencies in the prior art, the present invention provides a method and device for efficiently removing glycerol from tellurium beads, so as to solve the problems of small processing capacity, long time consumption, low efficiency, incomplete glycerol removal, etc. in the existing methods for removing glycerol from tellurium beads.

[0006] In order to solve the above technical problems, on the one hand, the technical solution of the present invention first provides a method for efficiently removing glycerol from tellurium beads. It utilizes the boiling point difference between glycerol and tellurium beads and adopts a vacuum distillation method to volatilize and remove the glycerol in the tellurium beads by distillation, thereby achieving the purpose of deeply removing glycerol from the tellurium beads. The volatilized glycerol is collected by condensation and reused.

[0007] The above vacuum distillation method specifically includes the following steps: placing the tellurium beads under a vacuum condition of 1 to 10 Pa, heating to 290 to 320° C., and keeping the temperature for 3 to 5 hours.

[0008] The boiling point of tellurium at normal pressure is 1390°C, and the boiling point of glycerol at normal pressure is 290°C. Since the saturated vapor pressures of glycerol and tellurium are quite different, the present invention uses a vacuum distillation method to remove glycerol. However, the volatilization of glycerol at normal pressure is relatively difficult and requires high energy consumption. Therefore, the present invention places the tellurium beads under vacuum conditions to reduce the boiling point of glycerol, and evaporates low-boiling-point water and glycerol from the tellurium beads through vacuum distillation. The temperature of vacuum distillation is controlled at an appropriate temperature far below the melting point of tellurium and slightly above the volatilization temperature of glycerol. The present invention determines the distillation temperature to be 290-320°C.

[0009] On the other hand, based on the above-mentioned method for efficiently removing glycerol from tellurium beads, the present invention also provides a device for efficiently removing glycerol from tellurium beads, which includes a tellurium bead holding tube, a heater, and a condensate liquid recovery device. The tellurium bead holding tube is horizontally and tiltedly placed in the heater, the tellurium bead holding tube is provided with a condensate outlet connected to the condensate liquid recovery device, and a cooler is provided at the condensate outlet of the tellurium bead holding tube.

[0010] Furthermore, the tellurium bead containing tube is provided with a connection port connected to a vacuum pumping device, and the vacuum pumping device performs vacuum pumping to make the internal environment of the tellurium bead containing tube a vacuum.

[0011] In some embodiments of the present invention, the tellurium bead containing tube is a quartz tube with openings at both ends and sealed with a cover plate, wherein the cover plate on one side is provided with a connection port to connect with a vacuum pumping device, and the vacuum pumping device includes a mechanical pump and the like.

[0012] In some embodiments of the present invention, the horizontal inclination angle of the tellurium bead containing tube is 5-10°, which can prevent the reflux of the volatilized and condensed water and glycerin.

[0013] In some embodiments of the present invention, the heater is a horizontal distillation furnace.

[0014] In some embodiments of the present invention, the cooler is a water cooling jacket.

[0015] Compared with the prior art, the present invention provides a method and device for efficiently removing glycerol from tellurium beads. The vacuum distillation method is used to completely distill and remove glycerol and water from the tellurium beads by utilizing the boiling point difference between water, glycerol and tellurium beads. The surface brightness, quality stability and production efficiency of the obtained tellurium beads are greatly improved, and the glycerol can be collected and reused, reducing the cost of using the tellurium bead production molding agent. The device structure of the present invention is simple and the method is simple and easy to implement, which solves the problems of small processing capacity, long time consumption, low efficiency and incomplete glycerol removal in the existing method for removing glycerol from tellurium beads. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 A schematic diagram of the structure of a device for efficiently removing glycerol from tellurium beads provided in an embodiment of the present invention.

[0017] Markings in the figure:

[0018] 1-quartz tube; 2-bottom cover plate; 3-top cover plate; 4-connection port; 5-condensate collector; 6-switch valve; 7-water cooling jacket; 8-heater; 9-tellurium bead. DETAILED DESCRIPTION

[0019] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments. In the description of the present invention, it should be understood that the terms "upper", "lower", "front", "back", "left", "right", "top", "bottom", "inside", "outside" and the like indicate directions or positional relationships based on the directions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and therefore cannot be understood as limiting the present invention.

[0020] See also Figure 1 The present invention provides a device for efficiently removing glycerol from tellurium beads, comprising a quartz tube 1 horizontally and tiltedly placed in a heater 8, wherein both ends of the quartz tube 1 are open structures and are sealed by a bottom cover plate 2 and a top cover plate 3. A connection port 4 is provided on the top cover plate 3 for connecting a vacuum pumping device to vacuum the quartz tube. A condensation outlet is provided on the quartz tube 1, and the condensation outlet is connected to a condensate collector 5. A water cooling jacket 7 is provided on the quartz tube 1. When in use, the top cover plate 3 of the quartz tube 1 is opened, the tellurium beads to be treated are loaded into the quartz tube 1, the top cover plate 3 is covered, the vacuum pumping device is started to vacuum, and after the vacuum condition is reached, the heater is started to heat and distill the inside of the quartz tube 1. During the distillation process, the evaporated glycerol and water will gather at the front end of the quartz tube 1, and condense into the condensate collector 5 under the action of the water cooling jacket 7.

[0021] In the embodiment of the present invention, the heater 8 is a horizontal distillation furnace, which adopts three-stage heating. The tellurium bead processing capacity of the quartz tube 1 is 30-50 kg tellurium bead / tube. The vacuum pumping device is a mechanical pump.

[0022] Embodiment 1:

[0023] A method for efficiently removing glycerol from tellurium beads comprises the following steps:

[0024] See also Figure 1 , filter the tellurium beads removed from the glycerol and load them into the quartz tube 1, with 30kg of material in each tube; put the quartz tube 1 loaded with tellurium beads 9 into the heater 8, and the quartz tube 1 is placed horizontally and tilted in the heater 8, with an inclination angle of 10° so that the tail of the quartz tube 1 is higher than the head to prevent water and glycerol from flowing back. After the tellurium beads are loaded, cover the top cover plate 3 of the quartz tube, connect the mechanical pump through the connection port 4 on the top cover plate 3 and start vacuuming. When the vacuum degree reaches 10Pa, stop vacuuming. The heater 8 starts to work to raise the temperature in the quartz tube 1 to 290℃, and keep it warm for 3h before stopping. Open the switch valve 6 of the condensate collector 5 to guide the condensed water and glycerol in the collector to be used for repeated production of tellurium beads, open the bottom cover plate 2 to pour out the treated tellurium beads, and observe their surface quality. The heater 8 adopts a three-stage heated horizontal distillation furnace.

[0025] The tellurium beads treated by the above method have good surface gloss, no glycerin residue, and the treatment efficiency is 10kg / h.

[0026] Embodiment 2:

[0027] A method for efficiently removing glycerol from tellurium beads comprises the following steps:

[0028] See also Figure 1 , filter the tellurium beads removed from the glycerol and load them into the quartz tube 1, with 50kg of material in each tube; put the quartz tube 1 loaded with tellurium beads 9 into the heater 8, and the quartz tube 1 is placed horizontally and tilted in the heater 8, with an inclination angle of 10° so that the tail of the quartz tube 1 is higher than the head to prevent water and glycerol from flowing back. After the tellurium beads are loaded, cover the top cover plate 3 of the quartz tube, connect the mechanical pump through the connection port 4 on the top cover plate 3 and start vacuuming. When the vacuum degree reaches 10Pa, stop vacuuming, and start the heater 8 to raise the temperature in the quartz tube 1 to 320℃, and keep it warm for 4h before stopping. Open the switch valve 6 of the condensate collector 5 to guide the condensed water and glycerol in the collector to be used for repeated production of tellurium beads, open the bottom cover plate 2 to pour out the treated tellurium beads, and observe their surface quality. The heater 8 adopts a three-stage heated horizontal distillation furnace.

[0029] The tellurium beads treated by the above method have good surface gloss, no glycerin residue, and a treatment efficiency of 12.5kg / h.

[0030] Embodiment 3:

[0031] A method for efficiently removing glycerol from tellurium beads comprises the following steps:

[0032] See also Figure 1 , filter the tellurium beads removed from the glycerol and load them into the quartz tube 1, with 45kg loaded into each tube; put the quartz tube 1 loaded with tellurium beads 9 into the heater 8, and the quartz tube 1 is placed horizontally and tilted in the heater 8, with an inclination angle of 10° so that the tail of the quartz tube 1 is higher than the head to prevent water and glycerol from flowing back. After the tellurium beads are loaded, cover the top cover plate 3 of the quartz tube, connect the mechanical pump through the connection port 4 on the top cover plate 3 and start vacuuming. When the vacuum reaches 10Pa, stop vacuuming, and start the heater 8 to raise the temperature in the quartz tube 1 to 300℃, and keep it warm for 5h before stopping. Open the switch valve 6 of the condensate collector 5 to guide the condensed water and glycerol in the collector to be used for repeated production of tellurium beads, open the bottom cover plate 2 to pour out the treated tellurium beads, and observe their surface quality. The heater 8 adopts a horizontal distillation furnace with three-stage heating.

[0033] The tellurium beads treated by the above method have good surface gloss, no glycerin residue, and a treatment efficiency of 9kg / h.

[0034] In summary, the present invention provides a method and device for efficiently removing glycerol from tellurium beads. The vacuum distillation method is used to utilize the boiling point difference among water, glycerol and tellurium beads to completely distill and remove glycerol and water from the tellurium beads, thereby improving the surface brightness and quality stability of the tellurium beads. The production efficiency of the tellurium beads is greatly improved, and glycerol can be collected and reused, thereby reducing the cost of using the tellurium bead production molding agent.

[0035] The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention. For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and the present invention can be implemented in other specific forms without departing from the spirit or basic features of the present invention; therefore, no matter from which point of view, the embodiments should be regarded as exemplary and non-restrictive. The scope of the present invention is limited by the attached claims rather than the above description. Therefore, it is intended to include all changes within the meaning and scope of the equivalent elements of the claims in the present invention, and any figure marks in the claims should not be regarded as limiting the claims involved.

[0036] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A device for efficiently removing glycerol from tellurium beads, characterized in that: It includes a tellurium bead holding tube, a heater, and a condensed liquid recovery device. The tellurium bead holding tube is horizontally and tiltedly placed in the heater. The tellurium bead holding tube is provided with a condensation outlet connected to the condensed liquid recovery device. A cooler is provided at the condensation outlet of the tellurium bead holding tube. The tellurium bead holding tube is provided with a connection port connected to a vacuum pumping device. The tellurium bead holding tube is a quartz tube with openings at both ends and sealed with a cover plate. The device uses a vacuum distillation method to remove glycerol from tellurium beads, and the vacuum distillation method includes the following steps: Place the tellurium beads under a vacuum condition of 1 to 10 Pa, heat to 290 to 320°C, and keep warm for 3 to 5 hours.

2. The device for efficiently removing glycerol from tellurium beads according to claim 1, characterized in that: The horizontal inclination angle of the tellurium bead containing tube is 5 to 10 degrees.

3. The device for efficiently removing glycerol from tellurium beads according to claim 1, characterized in that: The heater is a horizontal distillation furnace.

4. The device for efficiently removing glycerol from tellurium beads according to claim 1, characterized in that: The cooler is a water cooling jacket.

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