CN117025969A - Vacuum furnace and method for extracting lead from waste CRT cone glass - Google Patents
Vacuum furnace and method for extracting lead from waste CRT cone glass Download PDFInfo
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- CN117025969A CN117025969A CN202311065801.1A CN202311065801A CN117025969A CN 117025969 A CN117025969 A CN 117025969A CN 202311065801 A CN202311065801 A CN 202311065801A CN 117025969 A CN117025969 A CN 117025969A
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- 239000011521 glass Substances 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000002699 waste material Substances 0.000 title claims abstract description 23
- 229910000464 lead oxide Inorganic materials 0.000 claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 15
- 230000008569 process Effects 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 238000004321 preservation Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims abstract description 3
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 claims description 42
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000005192 partition Methods 0.000 claims description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 abstract description 30
- 238000006722 reduction reaction Methods 0.000 abstract description 15
- 238000011084 recovery Methods 0.000 abstract description 4
- 239000004566 building material Substances 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 abstract 3
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 238000009833 condensation Methods 0.000 abstract 1
- 239000011133 lead Substances 0.000 description 40
- 230000009467 reduction Effects 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000004876 x-ray fluorescence Methods 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 238000004846 x-ray emission Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 239000010793 electronic waste Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The application discloses a vacuum furnace and a method for extracting lead from waste CRT cone glass, belonging to the fields of high pollution control and treatment of waste lead-containing glass and comprehensive recovery of secondary resources. Firstly, placing a granular carbonaceous reducing agent in an upper layer distributing device of a vacuum furnace for carbothermic reduction reaction, placing conical glass in a lower layer distributing device, and sealing the vacuum furnace; and (3) under the conditions of 5-10 Pa and 1300 ℃ of vacuum chamber pressure, preserving heat for 120min, volatilizing lead oxide in the conical glass, and performing carbothermic reaction on the volatilized lead oxide and a carbonaceous reducing agent in the process of passing through a carbon layer at the upper part of the graphite crucible to generate gaseous metallic lead, and condensing the gaseous metallic lead in a condensing disc. After the heat preservation is finished, naturally cooling, obtaining metallic lead in a condensation area, wherein the purity of the metallic lead is more than 99%, and lead oxide in residual glass is effectively removed, so that the metallic lead can be used for preparing novel lead-free glass, building materials and ceramic materials, and harmless treatment and comprehensive utilization of resources of the conical glass are realized.
Description
The application relates to a divisional application of a method for extracting lead from waste CRT cone glass, which has the application date of 2018, 8, 20, the application number of 201810946758.2 and the name of 'method for extracting lead from waste CRT cone glass'.
Technical Field
The application relates to a vacuum furnace and a method for extracting lead from waste CRT cone glass, belonging to the fields of high pollution control and treatment of waste lead-containing glass and comprehensive recovery of secondary resources.
Background
In particular, since the 21 st century, electronic technology has rapidly progressed, flat panel display industry has rapidly grown, a large number of Cathode Ray Tube (CRT) cone glasses used for televisions and computers for display screens have been eliminated, and China has entered the peak period of lead-containing CRT cone glass rejection. One predictive study estimated that by 2020, the amount of waste CRT cone glass in the entire asian range would increase to around 1500 tons. Moreover, the cone glass mainly contains a large amount of silicon dioxide, lead oxide and the like, wherein the silicon dioxide content is about 50%, and the lead oxide content is about 20%, so that the lead oxide in the cone glass is one of important sources of lead resources. Meanwhile, since the CRT cone glass contains heavy metal lead, the CRT cone glass is considered as dangerous electronic waste, the key of the safe treatment of the waste CRT cone glass is that lead oxide in the waste CRT cone glass is treated, if the lead oxide is treated improperly, the ecological environment such as water source, soil and the like is difficult to estimate, and the health of human beings is endangered, so the removal and comprehensive utilization of lead-containing resources of the waste CRT cone glass are a problem which must be solved in the current electronic garbage treatment of China. At present, the technology of detoxification of secondary resources in cone glass and comprehensive recycling is not mature enough, so that reasonable resource utilization method and approach of waste CRT glass become the problem to be solved urgently in China or even in the world.
In recent years, numerous researchers in China put forward a method mainly for extracting metallic lead from the pyrometallurgical cone glass around the principles of environmental protection, economy, process feasibility and the like, so that secondary recovery and utilization of lead resources in waste CRT cone glass are greatly promoted, and various problems still exist, such as lower extraction rate of lead, complex process, environmental pollution and the like. Ma Zhilai A method and apparatus for recovering metallic lead from waste CRT cone glass (application No. 201310361538.0, 201320505904.0) features that waste CRT cone glass, lead concentrate, lead oxide ore and coke are mixed together in a certain proportion, and smelted in a blast furnace to obtain coarse lead, slag and fume, the yield of coarse lead being up to 20%, the content of lead in coarse lead being up to 98.52%, and the content of lead in slag being over 1%. The core of the method for extracting the metallic lead from the lead oxide in the iron thermal reduction cone glass disclosed by the application number 201210345035 is that after iron powder and the cone glass are uniformly mixed, the mixture of the metallic lead and the residual glass is obtained by heat treatment at 600-1000 ℃, and then the lead is purified by a floatation or chemical method, so that the extraction rate of the lead in the cone glass is about 60%.
Disclosure of Invention
The application aims to provide a vacuum furnace and a method for extracting lead from waste CRT (cathode ray tube) cone glass, which are used for efficiently removing lead oxide in the cone glass, recycling metal lead and realizing harmless treatment and comprehensive utilization of the waste lead-containing CRT cone glass.
The application provides a vacuum furnace, which comprises a lower-layer distributing device, an upper-layer distributing device and a graphite condensing device, wherein a lead oxide volatilizing chamber is arranged between the lower-layer distributing device and the upper-layer distributing device, and a gaseous lead volatilizing chamber and a condensing chamber are arranged between the upper-layer distributing device and the graphite condensing device;
the upper layer material distribution device is a porous stainless steel net and is fixed on the side wall of the reactor through a clamping groove; the gaseous lead volatilizing chamber is separated from the condensing chamber by a partition board, and the partition board is provided with air holes.
The application also provides a method for extracting lead from waste CRT cone glass, which is carried out by adopting the vacuum furnace according to the scheme, and specifically comprises the following steps:
(1) Placing the conical glass in a lower layer distributing device of a vacuum furnace, placing a carbonaceous reducing agent in an upper layer distributing device, and sealing the vacuum furnace;
(2) Carrying out cold vacuumizing on the vacuum furnace, starting other operations when the cold pressure is less than 30Pa, heating to 1300 ℃ at a heating rate of 10 ℃/min, heating, and preserving the temperature for 120min, wherein the hot pressure in the hot process of the vacuum furnace is 5-10 Pa;
(3) And after the heat preservation is finished, naturally cooling the high-temperature furnace body at room temperature, and after the furnace body is naturally cooled to the room temperature, collecting condensate lead in a condensing chamber, and obtaining the lead-removed glass in a volatilizing chamber.
Preferably, the ratio of the carbon content of the carbonaceous reducing agent to the lead oxide content of the conical glass is greater than 0.1%.
Preferably, the lead oxide content of the conical glass is 28.54%.
Preferably, the components of the lead-removed glass are as follows: siO (SiO) 2 64.87％，PbO 0.03％，K 2 O 11.12％，Na 2 O 5.89％，CaO 4.96％，SrO 3.36％，Al 2 O 3 3.47%, mgO 2.88%, baO 2.75% and the other 0.67%.
The application also provides condensate lead obtained by the method according to the scheme, and the grain size of the condensate lead is smaller than 50 mu m.
The principle of the application is as follows: when the pressure of the system reaches 5-15 Pa and the temperature is higher than 1150 ℃, the-O-P-O-Si-O-network structure in the conical glass is destroyed, so that lead oxide is released and reacts with a carbon layer arranged on the upper part of the crucible to obtain metallic lead, and the metallic lead volatilizes and condenses on a condensing disc because the system reaches the saturated vapor pressure of the metallic lead, thereby realizing the fundamental purpose of recovering the metallic lead; the reaction type is as follows:
PbSiO 3 →PbO(s)+SiO 2 (s)(1)
PbO(s)→PbO(l)→PbO(g)(2)
PbO(g)+C(s)→Pb(s)+CO(g)(3)
Pb(s)→Pb(l)→Pb(g)(4)
the application has the beneficial effects that:
(1) The application designs a novel vacuum volatilization and carbothermic reduction device, which enables lead oxide volatilized in the conical glass and a carbon layer at the upper part in the device to generate carbothermic reduction reaction.
(2) The application realizes the carbothermic reduction reaction of gaseous lead oxide through the novel device structure.
(3) The application realizes the one-step method for recovering the metallic lead from the conical glass, and compared with the existing treatment process, the application has the advantages of shorter process flow and simple operation; the process of treating the lead-containing cone glass has no additive, reduces secondary pollution, and the whole process is carried out in a completely closed vacuum furnace, thereby being beneficial to environmental protection and labor health.
(4) The application realizes the high-efficiency removal of lead in the lead-containing conical glass, when the heat treatment temperature is 1300 ℃, and the heat preservation is carried out for 120min, the lead removal rate can reach 99.85 percent, the purity of the recovered metallic lead can reach more than 99.45 percent, and meanwhile, the residual glass containing 0.03 percent of lead oxide can be obtained, and the lead-containing conical glass can be used for preparing novel lead-free glass, building materials, ceramic materials and the like.
Drawings
FIG. 1 is a process flow diagram of the present application;
FIG. 2 is a scanning electron microscope picture of metallic lead recovered at different temperatures;
FIG. 3 is a schematic diagram of a vacuum furnace bed apparatus.
Detailed Description
The application will be described in further detail with reference to the drawings and examples, but the scope of the application is not limited to the description.
The devices used in embodiments 1 to 5 of the application are shown in fig. 3, and comprise a lower layer distributing device, an upper layer distributing device and a graphite condensing device, wherein a lead oxide volatilization chamber in conical glass is arranged between the lower layer distributing device and the upper layer distributing device, and a gaseous lead volatilization chamber and a condensing chamber are arranged between the upper layer distributing device and the graphite condensing device; the upper layer material distribution device is a porous stainless steel net and is fixed on the side wall of the reactor through a clamping groove; the gaseous lead volatilizing chamber is separated from the condensing chamber by a partition board, and the partition board is provided with air holes.
Example 1
Firstly, cleaning the surface of the cone glass, and crushing the large cone glass into block cone glass (50 g, wherein the lead oxide content is 28.54%) which is suitable for being put into a vacuum furnace by using a jaw crusher; the granular carbonaceous reducing agent is placed in an upper layer distributing device of a vacuum furnace for carbothermic reduction reaction, the carbon content in the carbonaceous reducing agent is 5g, and the conical glass is placed in a lower layer distributing device; vacuum carbothermal reduction treatment is carried out, the temperature is raised to 1150 ℃, the heating rate is 5 ℃/min, the system thermal pressure is within the range of 5Pa to 8Pa, the temperature is kept for 30min, the room temperature is naturally cooled by a furnace body, metallic lead is obtained in a condensing disc, and residual glass after lead oxide removal is obtained in a volatilizing chamber.
The elemental content of the residual glass was analyzed by an X-ray fluorescence spectrometer to obtain a recovery rate of 43.34% of metallic lead, and the purity of the volatilized metallic lead was 99.23% by chemical analysis.
Example 2
Firstly, cleaning the surface of the cone glass, and crushing the large cone glass into block cone glass (50 g, wherein the lead oxide content is 28.54%) which is suitable for being put into a vacuum furnace by using a jaw crusher; the granular carbonaceous reducing agent is placed in an upper layer distributing device of a vacuum furnace for carbothermic reduction reaction, the carbon content in the carbonaceous reducing agent is 15g, and the conical glass is placed in a lower layer distributing device; vacuum carbothermal reduction treatment is carried out, the temperature is raised to 1300 ℃, the heating rate is 10 ℃/min, the thermal state pressure of the system is within the range of less than 10Pa, the temperature is kept for 30min, the room temperature is naturally cooled by a furnace body, metallic lead is obtained in a condensing disc, and residual glass after lead oxide removal is obtained in a volatilizing chamber.
The elemental content of the residue was analyzed by X-ray fluorescence spectrometer to give a removal rate of 92.71% of metallic lead, and the purity of the volatilized metallic lead was 99.12% by chemical analysis.
Example 3
Firstly, cleaning the surface of the cone glass, and crushing the large cone glass into block cone glass (50 g, wherein the lead oxide content is 28.54%) which is suitable for being put into a vacuum furnace by using a jaw crusher; the granular carbonaceous reducing agent is placed in an upper layer distributing device of a vacuum furnace for carbothermic reduction reaction, the carbon content in the carbonaceous reducing agent is 20g, and the conical glass is placed in a lower layer distributing device; vacuum carbothermal reduction treatment is carried out, the temperature is raised to 1400 ℃, the heating rate is 20 ℃/min, the thermal state pressure of the system is within the range of 10Pa to 15Pa, the temperature is kept for 30min, the room temperature is naturally cooled by a furnace body, metallic lead is obtained in a condensing disc, and residual glass after lead oxide removal is obtained in a volatilizing chamber.
The elemental content of the residue was analyzed by X-ray fluorescence spectrometer to give a removal rate of 99.80% of metallic lead, and the purity of the volatilized metallic lead was 99.40% by chemical analysis.
Example 4
Firstly, cleaning the surface of the cone glass, and crushing the large cone glass into block cone glass (50 g, wherein the lead oxide content is 28.54%) which is suitable for being put into a vacuum furnace by using a jaw crusher; the granular carbonaceous reducing agent is placed in an upper layer distributing device of a vacuum furnace for carbothermic reduction reaction, the carbon content in the carbonaceous reducing agent is 15g, and the conical glass is placed in a lower layer distributing device; vacuum carbothermal reduction treatment is carried out, the temperature is raised to 1300 ℃, the heating rate is 10 ℃/min, the thermal state pressure of the system is within the range of less than 10Pa, the temperature is kept for 60min, the room temperature is naturally cooled by a furnace body, metallic lead is obtained in a condensing disc, and residual glass after lead oxide removal is obtained in a volatilizing chamber.
The elemental content of the residue was analyzed by X-ray fluorescence spectroscopy to give a removal of 99.45% of lead oxide from the conical glass, and the purity of the volatilized metallic lead was 99.36% by chemical analysis.
Example 5
Firstly, cleaning the surface of the cone glass, and crushing the large cone glass into block cone glass (50 g, wherein the lead oxide content is 28.54%) which is suitable for being put into a vacuum furnace by using a jaw crusher; the granular carbonaceous reducing agent is placed in an upper layer distributing device of the vacuum furnace for carbothermic reduction reaction, and the conical glass is placed in a lower layer distributing device; vacuum carbothermal reduction treatment is carried out, the temperature is raised to 1300 ℃, the heating rate is 10 ℃/min, the thermal state pressure of the system is within the range of less than 10Pa, the temperature is kept for 120min, the room temperature is naturally cooled by a furnace body, metallic lead is obtained in a condensing disc, and residual glass after lead oxide removal is obtained in a volatilizing chamber;
the elemental content of the residue was analyzed by X-ray fluorescence spectroscopy to give a removal of 99.85% of lead oxide from the conical glass, and the purity of the volatilized metallic lead was 99.45% by chemical analysis.
To verify the effect of different heat treatment temperatures, soak times, etc. on the present application, elemental measurements were performed on the residual glasses in examples 1 to 5, and the results are shown in table 1:
table 1 examined the influence of different heat treatment temperatures on the content of each element in the residual glass
| Project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| SiO 2 (％) | 51.43 | 62.68 | 64.35 | 66.13 | 64.87 |
| PbO(％) | 18.42 | 3.08 | 0.08 | 0.68 | 0.03 |
| K 2 O(％) | 9.65 | 10.61 | 11.02 | 10.23 | 11.12 |
| Na 2 O(％) | 5.25 | 5.74 | 5.31 | 5.54 | 5.89 |
| CaO(％) | 4.01 | 5.55 | 4.98 | 5.06 | 4.96 |
| SrO(％) | 3.02 | 3.11 | 3.12 | 3.22 | 3.36 |
| Al 2 O 3 (％) | 2.60 | 3.08 | 3.92 | 2.78 | 3.47 |
| MgO(％) | 1.94 | 2.27 | 2.45 | 3.03 | 2.88 |
| BaO(％) | 2.37 | 2.95 | 3.13 | 2.15 | 2.75 |
| Others(％) | 1.04 | 0.93 | 1.64 | 1.18 | 0.67 |
It can be seen from table 1 that with the increase of the heat treatment temperature and the heat preservation time, the content of lead oxide in the residual glass is obviously reduced, namely the removal effect of lead oxide is obviously improved, and the removal of lead oxide is 99.83% under the optimal condition (the temperature is 1300min, and the heat preservation is 120 min).
Fig. 2 is a scanning electron microscope image of metallic lead recovered under different conditions, and it can be seen from the image that the lead product obtained under different conditions has substantially similar morphology and a particle size of less than 50 μm.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the application.
Claims (6)
1. The vacuum furnace is characterized by comprising a lower-layer distributing device, an upper-layer distributing device and a graphite condensing device, wherein a lead oxide volatilizing chamber is arranged between the lower-layer distributing device and the upper-layer distributing device, and a gaseous lead volatilizing chamber and a condensing chamber are arranged between the upper-layer distributing device and the graphite condensing device;
the upper layer material distribution device is a porous stainless steel net and is fixed on the side wall of the reactor through a clamping groove; the gaseous lead volatilizing chamber is separated from the condensing chamber by a partition board, and the partition board is provided with air holes.
2. A method for extracting lead from waste CRT cone glass, which is characterized by adopting the vacuum furnace as claimed in claim 1, and specifically comprising the following steps:
(1) Placing the conical glass in a lower layer distributing device of a vacuum furnace, placing a carbonaceous reducing agent in an upper layer distributing device, and sealing the vacuum furnace;
(2) Carrying out cold vacuumizing on the vacuum furnace, starting other operations when the cold pressure is less than 30Pa, heating to 1300 ℃ at a heating rate of 10 ℃/min, heating, and preserving the temperature for 120min, wherein the hot pressure in the hot process of the vacuum furnace is 5-10 Pa;
(3) And after the heat preservation is finished, naturally cooling the high-temperature furnace body at room temperature, and after the furnace body is naturally cooled to the room temperature, collecting condensate lead in a condensing chamber, and obtaining the lead-removed glass in a volatilizing chamber.
3. The method for extracting lead from waste CRT cone glass as claimed in claim 2, wherein: the ratio of the carbon content in the carbonaceous reducing agent to the lead oxide content in the conical glass is more than 0.1%.
4. The method for extracting lead from waste CRT cone glass as claimed in claim 2, wherein: the lead oxide content of the conical glass is 28.54%.
5. The method for extracting lead from waste CRT cone glass as claimed in claim 2, wherein: the components of the lead-removed glass are as follows: siO (SiO) 2 64.87％，PbO 0.03％，K 2 O 11.12％，Na 2 O5.89％，CaO 4.96％，SrO 3.36％，Al 2 O 3 3.47%, mgO 2.88%, baO 2.75%, other 0.67%％。
6. Condensate lead obtained by the method according to any one of claims 2 to 5, characterized in that: the condensate lead has a particle size of less than 50 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311065801.1A CN117025969A (en) | 2018-08-20 | 2018-08-20 | Vacuum furnace and method for extracting lead from waste CRT cone glass |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311065801.1A CN117025969A (en) | 2018-08-20 | 2018-08-20 | Vacuum furnace and method for extracting lead from waste CRT cone glass |
| CN201810946758.2A CN109182778A (en) | 2018-08-20 | 2018-08-20 | A method of extracting lead from discarded CRT cone glass |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810946758.2A Division CN109182778A (en) | 2018-08-20 | 2018-08-20 | A method of extracting lead from discarded CRT cone glass |
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| CN201810946758.2A Pending CN109182778A (en) | 2018-08-20 | 2018-08-20 | A method of extracting lead from discarded CRT cone glass |
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| CN115418494B (en) * | 2022-09-06 | 2024-01-19 | 湖南水口山有色金属集团有限公司 | Method for recycling lead in CRT lead-containing glass by fuming furnace |
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| CN102002593B (en) * | 2010-12-01 | 2012-12-26 | 中国科学院生态环境研究中心 | Process for synthesizing nano-lead from waste cathode-ray tube (CRT) lead-containing glass by one-step method |
| CN103184349B (en) * | 2011-12-29 | 2014-07-23 | 广东先导稀材股份有限公司 | High purity zinc preparation device and method |
| CN103280390B (en) * | 2013-06-09 | 2016-08-10 | 南开大学 | A kind of method for innocent treatment of discarded cathode ray tube lead bearing glass |
| CN104962744A (en) * | 2015-06-23 | 2015-10-07 | 河南理工大学 | Method for harmlessly removing lead from waste CRT (cathode ray tube) cone glass and preparing glass micro-spheres |
| CN107881345A (en) * | 2017-12-19 | 2018-04-06 | 江苏省冶金设计院有限公司 | A kind of equipment and recovery method for reclaiming metallic lead zinc |
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2018
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