CN115974009A - Method and device for efficiently removing glycerin in tellurium beads - Google Patents
Method and device for efficiently removing glycerin in tellurium beads Download PDFInfo
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- CN115974009A CN115974009A CN202211721522.1A CN202211721522A CN115974009A CN 115974009 A CN115974009 A CN 115974009A CN 202211721522 A CN202211721522 A CN 202211721522A CN 115974009 A CN115974009 A CN 115974009A
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- tellurium
- beads
- glycerol
- efficiently removing
- glycerin
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 title claims abstract description 197
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 108
- 239000011324 bead Substances 0.000 title claims abstract description 97
- 235000011187 glycerol Nutrition 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 10
- 239000010453 quartz Substances 0.000 claims description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 31
- 238000004821 distillation Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000009835 boiling Methods 0.000 abstract description 8
- 238000007796 conventional method Methods 0.000 abstract description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000003599 detergent Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method and a device for efficiently removing glycerin from tellurium beads, wherein the method utilizes the high boiling point difference between the glycerin and the tellurium beads, and completely distills and removes the glycerin and water from the tellurium beads by a vacuum distillation method. The device provided by the invention is simple in structure, the method is simple and easy to implement, and the problems of small treatment amount, long time consumption, low efficiency and incomplete glycerol removal existing in the conventional method for removing glycerol from tellurium beads are solved.
Description
Technical Field
The invention relates to the technical field of tellurium bead production, in particular to a method and a device for efficiently removing glycerin in tellurium beads.
Background
Tellurium is known as "industrial vitamin", 30% of which is used in the metallurgical industry. The product form of tellurium mainly comprises tellurium ingots, tellurium powder and tellurium beads. The tellurium ingot is too large in size and needs to be crushed when in use; the tellurium powder is too fine, and dust is easy to generate during feeding; compared with the prior art, the tellurium beads are spherical small particles, are suitable in size, do not need to be crushed, are convenient to measure, can be directly used, and do not generate raise dust. Therefore, the preparation of tellurium beads is becoming more and more important. The tellurium beads are mainly used as an additive for castings or special steel materials to improve the cutting processability and the hardness of the castings or used as a raw material for manufacturing a thermal analysis sample cup for detecting the contents of Si and C in molten iron in front of a furnace.
At present, the preparation method of tellurium beads takes a glycerol forming method as a mainstream technology, the method is low in cost, and the prepared tellurium beads are high in sphericity. The glycerol forming method takes glycerol as a forming agent, the molten solution of tellurium forms drops through a dropping liquid pipe and falls into the forming agent glycerol to form tellurium beads, but the glycerol easily enters shrinkage cavities of the tellurium beads in the forming process of the tellurium beads, and the glycerol can be mixed with water in any proportion and has strong hygroscopicity, so that the tellurium beads are oxidized, the product quality is influenced, and the glycerol in the tellurium beads needs to be removed.
The existing method for removing the glycerol in the tellurium beads mainly comprises an ultrasonic cleaning method and a detergent cleaning method, wherein the ultrasonic cleaning method is used for removing the glycerol by adopting ultrasonic cleaning, but the ultrasonic cleaning treatment capacity is small, only 3-5 kg of tellurium beads can be treated each time, and the ultrasonic cleaning cannot guarantee that all the tellurium beads are cleaned and the complete removal of the glycerol cannot be guaranteed, so that the application of the ultrasonic cleaning to enterprise production has great limitation, and is time-consuming and labor-consuming. The detergent cleaning method is to add detergent into tellurium beads, and generally remove glycerin through cleaning for 12-14 times and drying for 2-3 times (drying time is 8-12 h), but the method has the disadvantages of many cleaning times, complex procedures, long drying time and long time consumption, and is easy to cause detergent residue, generates a large amount of chemical wastewater and is not environment-friendly.
Disclosure of Invention
In view of the above, the present invention provides a method and an apparatus for efficiently removing glycerol from tellurium beads, so as to solve the problems of small processing amount, long time consumption, low efficiency, incomplete glycerol removal, etc. of the existing method for removing glycerol from tellurium beads.
In order to solve the technical problems, on one hand, the technical scheme of the invention firstly provides a method for efficiently removing glycerol from tellurium beads, which utilizes the boiling point difference of the glycerol and the tellurium beads and adopts a vacuum distillation method to volatilize and remove the glycerol in the tellurium beads through distillation, thereby achieving the purpose of deeply removing the glycerol from the tellurium beads, and the volatilized glycerol is collected through condensation to realize recycling.
The vacuum distillation method specifically comprises the following steps: placing the tellurium beads in a vacuum condition of 1-10 Pa, heating to 290-320 ℃, and preserving heat for 3-5 h.
The boiling point of the tellurium under normal pressure is 1390 ℃, the boiling point of the glycerol under normal pressure is 290 ℃, and the saturated vapor pressure difference of the glycerol and the tellurium is large, so the glycerol is removed by adopting a vacuum distillation method. But the volatilization of the glycerol under normal pressure is difficult, and the required energy consumption is high, so the invention puts the tellurium beads under vacuum condition, reduces the boiling point of the glycerol, and volatilizes the water and the glycerol with low boiling points from the tellurium beads through vacuum distillation. The temperature of vacuum distillation is controlled to be a proper temperature which is far lower than the melting point of tellurium and slightly higher than the volatilization temperature of glycerin, and the distillation temperature is determined to be 290-320 ℃.
On the other hand, based on the method for efficiently removing the glycerol in the tellurium beads, the invention also provides a device for efficiently removing the glycerol in the tellurium beads, which comprises a tellurium bead containing pipe, a heater and a condensed liquid recoverer, wherein the tellurium bead containing pipe is horizontally and obliquely arranged in the heater, the tellurium bead containing pipe is provided with a condensation outlet which is connected with the condensed liquid recoverer, and a cooler is arranged at the position of the condensation outlet of the tellurium bead containing pipe.
Furthermore, the tellurium pearl holds the pipe and is provided with the connector and is connected with evacuation equipment, and evacuation equipment evacuation makes the tellurium pearl hold the inside environment for the vacuum.
In some embodiments of the present invention, the tellurium bead holding tube is a quartz tube with openings at both ends sealed by cover plates, wherein a connection port is formed on one side of the cover plate and connected to a vacuum pumping device, and the vacuum pumping device includes a mechanical pump and the like.
In some embodiments of the present invention, the horizontal inclination angle of the tellurium bead holding tube is 5 to 10 °, which can avoid the backflow of water and glycerin condensed out by volatilization.
In some embodiments of the invention, the heater is a horizontal distillation furnace.
In some embodiments of the invention, the cooler is a water jacket.
Compared with the prior art, the method and the device for efficiently removing the glycerol in the tellurium beads provided by the invention have the advantages that the vacuum distillation method is adopted, the glycerol and the water are completely distilled and removed from the tellurium beads by utilizing the boiling point difference of the water, the glycerol and the tellurium beads, the surface brightness, the quality stability and the production efficiency of the obtained tellurium beads are greatly improved, the glycerol can be collected and recycled, and the use cost of the forming agent for producing the tellurium beads is reduced. The device provided by the invention is simple in structure, the method is simple and easy to implement, and the problems of small treatment amount, long time consumption, low efficiency and incomplete glycerol removal existing in the conventional method for removing glycerol from tellurium beads are solved.
Drawings
Fig. 1 is a schematic structural diagram of a device for efficiently removing glycerol from tellurium beads according to an embodiment of the present invention.
The labels in the figure are:
1-a quartz tube; 2-a bottom cover plate; 3-top cover plate; 4-connecting port; 5-a condensate collector; 6-switching a valve; 7-water cooling jacket; 8-a heater; 9-tellurium beads.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and the detailed description. In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
Referring to fig. 1, the invention provides a device for efficiently removing glycerin from tellurium beads, comprising a quartz tube 1 horizontally and obliquely arranged in a heater 8, wherein two ends of the quartz tube 1 are in an open structure and are sealed by a bottom cover plate 2 and a top cover plate 3. And a connecting port 4 is formed on the top cover plate 3 and is used for connecting a vacuumizing device to vacuumize the quartz tube. A condensation outlet is formed in the quartz tube 1 and connected with a condensate collector 5, and a water cooling sleeve 7 is sleeved on the quartz tube 1. When the device is used, the top cover plate 3 of the quartz tube 1 is opened, tellurium beads to be treated are filled into the quartz tube 1, the top cover plate 3 is covered, the vacuumizing equipment is started for vacuumizing, after the vacuum condition is achieved, the heater is started for heating and distilling the interior of the quartz tube 1, and during the distillation process, evaporated glycerin and water can be gathered to the front end of the quartz tube 1 and are condensed and gathered into the condensate collector 5 under the action of the water cooling sleeve 7.
In the embodiment of the invention, the heater 8 is a horizontal distillation furnace and adopts three-stage heating. The tellurium bead treatment capacity of the quartz tube 1 is 30-50 kg tellurium beads/tube. The vacuum pumping equipment is a mechanical pump.
Example 1:
a method for efficiently removing glycerol in tellurium beads specifically comprises the following steps:
referring to fig. 1, tellurium beads fished out of glycerin were filtered and loaded into quartz tubes 1, each tube being charged with 30kg; the quartz tube 1 filled with the tellurium beads 9 is placed into a heater 8, the quartz tube 1 is horizontally and obliquely placed in the heater 8, the inclination angle is 10 degrees, so that the tail part of the quartz tube 1 is higher than the head part, and the backflow of moisture and glycerin is avoided. Covering a top cover plate 3 of the quartz tube after the tellurium beads are charged, connecting a mechanical pump through a connecting port 4 on the top cover plate 3, starting vacuumizing, stopping vacuumizing when the vacuum degree reaches 10Pa, starting a heater 8 to work to increase the temperature in the quartz tube 1 to 290 ℃, and stopping after the temperature is kept for 3 hours. And opening a switch valve 6 of the condensate collector 5 to lead out the water and the glycerol condensed in the collector for repeatedly producing the tellurium beads, opening the bottom cover plate 2 to pour out the treated tellurium beads, and observing the surface quality of the tellurium beads. Wherein the heater 8 adopts a horizontal distillation furnace with three-stage heating.
The tellurium beads treated by the method have good surface glossiness, no glycerin residue and treatment efficiency of 10kg/h.
Example 2:
a method for efficiently removing glycerol in tellurium beads specifically comprises the following steps:
referring to fig. 1, tellurium beads fished out of glycerin were filtered and loaded into a quartz tube 1, 50kg per tube; the quartz tube 1 filled with the tellurium beads 9 is placed in a heater 8, the quartz tube 1 is horizontally and obliquely placed in the heater 8, the tail part of the quartz tube 1 is higher than the head part by the inclination angle of 10 degrees, and the backflow of moisture and glycerin is avoided. After the tellurium beads are charged, the top cover plate 3 of the quartz tube is covered, a mechanical pump is connected through a connecting port 4 on the top cover plate 3, the vacuumizing is started, the vacuumizing is stopped when the vacuum degree reaches 10Pa, the heater 8 starts to work, the temperature in the quartz tube 1 is raised to 320 ℃, and the heat preservation is stopped after 4 hours. And opening a switch valve 6 of the condensate collector 5 to lead out the water and the glycerol condensed in the collector for repeatedly producing the tellurium beads, opening the bottom cover plate 2 to pour out the treated tellurium beads, and observing the surface quality of the tellurium beads. Wherein the heater 8 adopts a horizontal distillation furnace with three-stage heating.
The tellurium beads treated by the method have good surface glossiness and no glycerin residue, and the treatment efficiency is 12.5kg/h.
Example 3:
a method for efficiently removing glycerol in tellurium beads specifically comprises the following steps:
referring to fig. 1, tellurium beads fished out of glycerin were filtered and loaded into quartz tubes 1, each tube containing 45kg; the quartz tube 1 filled with the tellurium beads 9 is placed into a heater 8, the quartz tube 1 is horizontally and obliquely placed in the heater 8, the inclination angle is 10 degrees, so that the tail part of the quartz tube 1 is higher than the head part, and the backflow of moisture and glycerin is avoided. Covering a top cover plate 3 of the quartz tube after the tellurium beads are charged, connecting a mechanical pump through a connecting port 4 on the top cover plate 3, starting to vacuumize, stopping vacuumizing after the vacuum degree reaches 10Pa, starting to work by a heater 8 to enable the temperature in the quartz tube 1 to rise to 300 ℃, and stopping after the temperature is kept for 5 hours. And opening a switch valve 6 of the condensate collector 5 to lead out the water and the glycerol condensed in the collector for repeatedly producing the tellurium beads, opening the bottom cover plate 2 to pour out the treated tellurium beads, and observing the surface quality of the tellurium beads. Wherein the heater 8 adopts a horizontal distillation furnace with three-section heating.
The tellurium beads treated by the method have good surface glossiness, no glycerin residue and treatment efficiency of 9kg/h.
In summary, the method and the device for efficiently removing the glycerol from the tellurium beads provided by the invention adopt the vacuum distillation method, utilize the boiling point difference of water, the glycerol and the tellurium beads, completely distill and remove the glycerol and the water from the tellurium beads, improve the surface brightness and the quality stability of the tellurium beads, greatly improve the production efficiency of the tellurium beads, collect and recycle the glycerol, and reduce the use cost of the forming agent for producing the tellurium beads.
While there have been shown and described what are at present considered to be the basic principles and essential features of the invention and advantages thereof, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, but is capable of other embodiments without departing from the spirit or essential characteristics thereof; the present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
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 alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method for efficiently removing glycerin in tellurium beads is characterized by comprising the following steps: and removing the glycerol in the tellurium beads by adopting a vacuum distillation method.
2. The method for efficiently removing the glycerol from the tellurium beads as claimed in claim 1, wherein: the vacuum distillation method comprises the following steps:
placing the tellurium beads in a vacuum condition of 1-10 Pa, heating to 290-320 ℃, and preserving heat for 3-5 h.
3. The utility model provides a device of glycerine in high-efficient removal tellurium pearl which characterized in that: the device comprises a tellurium bead containing pipe, a heater and a condensate liquid recoverer, wherein the tellurium bead containing pipe is horizontally and obliquely arranged in the heater, a condensation outlet is formed in the tellurium bead containing pipe and connected with the condensate liquid recoverer, and a cooler is arranged at the position of the condensation outlet of the tellurium bead containing pipe.
4. The device for efficiently removing the glycerol in the tellurium beads as claimed in claim 3, wherein: the tellurium pearl holds the pipe and is provided with the connector and is connected with evacuation equipment.
5. The device for removing the glycerol in the tellurium beads efficiently as claimed in claim 3 or 4, wherein: the tellurium bead holding pipe is a quartz pipe with openings at two ends sealed by cover plates.
6. The device for efficiently removing the glycerol in the tellurium beads as claimed in claim 3, wherein: the horizontal inclination angle of the tellurium bead holding pipe is 5-10 degrees.
7. The device for efficiently removing the glycerol in the tellurium beads as claimed in claim 3, wherein: the heater is a horizontal distillation furnace.
8. The device for efficiently removing the glycerol in the tellurium beads as claimed in claim 3, wherein: the cooler is a water cooling jacket.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211721522.1A CN115974009A (en) | 2022-12-30 | 2022-12-30 | Method and device for efficiently removing glycerin in tellurium beads |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211721522.1A CN115974009A (en) | 2022-12-30 | 2022-12-30 | Method and device for efficiently removing glycerin in tellurium beads |
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| CN115974009A true CN115974009A (en) | 2023-04-18 |
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| CN202211721522.1A Pending CN115974009A (en) | 2022-12-30 | 2022-12-30 | Method and device for efficiently removing glycerin in tellurium beads |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20140029739A (en) * | 2012-08-29 | 2014-03-11 | 충남대학교산학협력단 | Apparatus for manufacturing of tellurium powder by vacuum distillation and controlling particle size |
| CN106946233A (en) * | 2017-04-18 | 2017-07-14 | 昆明鼎邦科技股份有限公司 | A kind of method of impure selenium material vacuum Refining |
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| WO2021180900A1 (en) * | 2020-03-13 | 2021-09-16 | Gommers Development Group S.R.O. | Device and method for distillation |
-
2022
- 2022-12-30 CN CN202211721522.1A patent/CN115974009A/en active Pending
Patent Citations (6)
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| WO2021180900A1 (en) * | 2020-03-13 | 2021-09-16 | Gommers Development Group S.R.O. | Device and method for distillation |
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