CN104261677A - Method for preparing microcrystalline glass from lithium beryllium tailings - Google Patents
Method for preparing microcrystalline glass from lithium beryllium tailings Download PDFInfo
- Publication number
- CN104261677A CN104261677A CN201410471994.5A CN201410471994A CN104261677A CN 104261677 A CN104261677 A CN 104261677A CN 201410471994 A CN201410471994 A CN 201410471994A CN 104261677 A CN104261677 A CN 104261677A
- Authority
- CN
- China
- Prior art keywords
- glass
- devitrified glass
- raw material
- lithium beryllium
- mine tailing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000011521 glass Substances 0.000 title claims abstract description 53
- 229910052790 beryllium Inorganic materials 0.000 title claims abstract description 25
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium(0) Chemical compound 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[Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 title claims abstract description 25
- WHXSMMKQMYFTQS-UHFFFAOYSA-N lithium Chemical compound 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- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium monoxide Chemical compound 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[Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 6
- 239000000156 glass melt Substances 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 229910020218 Pb—Zn Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005039 chemical industry Methods 0.000 description 1
- 239000003818 cinder Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0063—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing waste materials, e.g. slags
Abstract
The invention relates to a method for preparing microcrystalline glass from lithium beryllium tailings, which is characterized in that certain amounts of limestone and cupronickel water quenching slag are added to the lithium beryllium tailings used as the main raw material to prepare the microcrystalline glass. The method basically comprises the following steps: drying the raw material, proportioning, mixing, melting, casting, annealing and carrying out heat treatment to obtain the microcrystalline glass. By using the lithium beryllium tailings and cupronickel water quenching slag as the raw materials without adding other chemical raw materials, the microcrystalline glass prepared by a melting process has the characteristics in microcrystal and glass, and has the advantages of favorable mechanical properties, favorable thermal shock performance and favorable chemical stability. The lithium beryllium tailings and cupronickel water quenching slag are coprocessed, thereby lowering the production cost of the microcrystalline glass and having obvious economic and environmental benefits.
Description
Technical field
The present invention relates to a kind of method utilizing lithium beryllium mine tailing to prepare devitrified glass, particularly with lithium beryllium mine tailing be main raw material, Wingdale and copper nickel Water Quenching Slag prepare the method for devitrified glass for auxiliary material, belongs to environmental area and field of metallurgy.
Background technology
Lithium beryllium mine tailing is that after the useful component such as lithium, beryllium that comprehensively extracts through the multiple beneficiation method such as gravity treatment, flotation, magnetic separation, electric separation in ore of rare metal ore, the side product from ore dressing of generation, its main component is SiO
2and Al
2o
3.Due to its SiO
2and Al
2o
3content is higher, and its fusing point is more than 1700 DEG C, and melting homogenizing difficulty is large, and in full-bodied situation, a large amount of bubbles existed in system are not easily discharged, for its recycling brings difficulty.Learn according to existing test and evaluation report, end to 2012, in the mine tailing separating plant Tailings Dam of Koktokay mining area, Powdered mine tailing amount is up to 4,000,000 tons.At present, the main Land use systems of lithium beryllium mine tailing reclaims rare metal in mine tailing and non-metallic minerals, fails to realize its direct whole utilization, reclaims the economic benefit that the methods such as mica create not high simultaneously, cause waste to pile up, problem cannot fundamentally solve.
The relevant report adopting mine tailing waste residue to prepare devitrified glass has much, and ([1] application number: 201310137329.8, application name is called " preparation method based on iron tailings being the composite microcrystallite glass of raw material ".[2] application number: 201210496348.5, application title " without Nucleating Agent devitrified glass preparation method ".[3] application number: 201310080423.4, application title " a kind of method utilizing blast furnace slag to prepare devitrified glass ".[4] application number: 201210103590.1, application title " a kind of method utilizing high-titanium blast furnace slag to prepare devitrified glass ".Application number: 201310217525.6, application title " a kind of Pb-Zn tailings prepares the processing method of dark devitrified glass ".[5] application number: 201310181939.8, application title " a kind of devitrified glass and preparation method thereof ".[6] Zhang Yuanzhi. [J] is inquired in the trial-production of slag, ash glass-Ceramics. Anhui chemical industry, 1998, (6): 31-33.[7] Yang Zhijie, Cang great Qiang, Li Yu etc., molten steel slag prepares the experimental study [J] of devitrified glass, New Building Materials, 2011, (7): 52 ~ 65.Above-mentioned relevant report more or less introduces chemical reagent in devitrified glass preparation process, and major part adopts sintering process, and the production cost of devitrified glass is relatively high, and the physical and mechanical properties of devitrified glass is relatively poor.
In sum, when not adding any chemical reagent, introduce Fe with the form of copper nickel Water Quenching Slag
2o
3as main Nucleating Agent, simultaneously there is high-melting-point and composition and the larger lithium beryllium mine tailing of existing cinder microcrystalline glass composition tolerances adopt scorification to prepare devitrified glass as main raw material have not been reported.
Summary of the invention
The object of the invention is the shortcoming overcoming above-mentioned prior art, provide a kind of method utilizing lithium beryllium mine tailing to prepare devitrified glass, prepare devitrified glass raw materials used based on lithium beryllium mine tailing, Wingdale and copper nickel Water Quenching Slag are auxiliary, do not add any chemical reagent, prepared the devitrified glass with excellent mechanical performances, solve the technical difficult problem that the problem of environmental pollution of mine tailing and lithium beryllium mine tailing are difficult to utilize, reduce the production cost of devitrified glass, improve value-added content of product.
First, by levigate for raw material to 40 orders, and it is dried at 120 DEG C.
Then, according to mass percent by the lithium beryllium mine tailing of 30.07% ~ 47.40%, the Wingdale of 43.97% ~ 52.41% and the copper nickel Water Quenching Slag of 5.44% ~ 17.52% mix, and load in High Temperature Furnaces Heating Apparatus.
The raw material mixed is incubated melting 1 ~ 6h at 1400 DEG C ~ 1600 DEG C, and then watered fast by melt and cast from the annealing 30min ~ 180min that is shaped in the mould of 400 DEG C ~ 600 DEG C of preheatings in advance, last furnace cooling obtains parent glass.
Parent glass is heat-treated, is heated to 700 DEG C ~ 900 DEG C insulation 30 ~ 180min with 5 ~ 10 DEG C/min temperature rise rate, the Fe introduced with copper nickel Water Quenching Slag form
2o
3abundant forming core is carried out as main Nucleating Agent.Again with the temperature rise rate of 5 ~ 10 DEG C/min, be warming up to 850 DEG C ~ 1100 DEG C insulation 1 ~ 5h, then furnace cooling can obtain devitrified glass.
Devitrified glass carries out cutting, polish, polishing, can obtain devitrified glass finished product.
Compared with the present invention prepares devitrified glass with sintering process, technique is short, and energy consumption is low, and raw materials cost is low, and waste utilization rate is high.
Accompanying drawing explanation
Fig. 1 is devitrified glass preparation flow figure
Embodiment
Embodiment 1
The first step, carries out composition analysis to raw material, according to composition analysis result, prepares burden to raw material.Raw material and product composition proportioning are in Table-1 and table-2.
The proportioning raw materials (wt.%) of table-1 devitrified glass product
| Raw material | Lithium beryllium mine tailing | Wingdale | Copper nickel Water Quenching Slag |
| Devitrified glass | 47.40 | 47.15 | 5.45 |
Table-2 raw materials and product chemical constitution (wt.%)
| Component | SiO 2 | Al 2O 3 | CaO | Fe 2O 3 | Other |
| Lithium beryllium mine tailing | 76.72 | 13.28 | 0.18 | 0.34 | 9.48 |
| Wingdale | 1.10 | 0.48 | 54.42 | 0.32 | 43.95 |
| Copper nickel Water Quenching Slag | 34.95 | 8.09 | 2.14 | 44.02 | 10.80 |
| Devitrified glass | 48.60 | 8.72 | 32.40 | 3.00 | 7.28 |
Second step, raw material is dried at 120 DEG C, raw material is mixed by composition proportion, then High Temperature Furnaces Heating Apparatus is put into, rise to 1460 DEG C from room temperature, and melting 2.5h obtains glass melt at 1460 DEG C, glass melt is cast in the mould of 600 DEG C and be shaped, annealing 30min, last furnace cooling finally obtains parent glass.
3rd step, heat-treats parent glass, is heated to 850 DEG C of insulation 60min, the Fe introduced with copper nickel Water Quenching Slag form with 5 DEG C/min temperature rise rate
2o
3as main Nucleating Agent, make the abundant forming core of parent glass; Again with the temperature rise rate of 5 DEG C/min, be warming up to 1100 DEG C of insulation 1h, make its abundant micritization, finally cool to the glass of micritization with the furnace room temperature, described devitrified glass can be obtained.
Embodiment 2
The first step, according to composition analysis result, carries out proportioning to raw material, and raw material and product composition proportioning are in Table-3 and table-4.
The proportioning raw materials (wt.%) of table-3 devitrified glass products
| Raw material | Lithium beryllium mine tailing | Wingdale | Copper nickel Water Quenching Slag |
| Devitrified glass | 44.77 | 46.11 | 9.12 |
Table-4 product chemical constitutions (wt.%)
| Component | CaO | SiO 2 | Al 2O 3 | Fe 2O 3 | Other |
| Devitrified glass | 31.60 | 47.40 | 8.60 | 5.00 | 7.40 |
Raw material is dried at 120 DEG C, and mix by composition proportion, then High Temperature Furnaces Heating Apparatus is put into, 1500 DEG C are risen to from room temperature, and melting 2.5h obtains glass melt at 1500 DEG C, cast in by glass melt in the mould of 600 DEG C and be shaped, annealing 30min, last furnace cooling finally obtains parent glass.
Parent glass is heat-treated, from room temperature with the temperature rise rate of 5 DEG C/min, is warming up to 860 DEG C of insulation 60min, the Fe introduced with copper nickel Water Quenching Slag form
2o
3as main Nucleating Agent, make its abundant forming core, then with the temperature rise rate of 5 DEG C/min, be warming up to 1100 DEG C of insulation 1h, make its abundant micritization, then cool to room temperature with the furnace, can devitrified glass be obtained.
Embodiment 3
The first step, according to composition analysis result, carries out proportioning to raw material, and raw material and product composition proportioning are in Table-5 and table-6.
The proportioning raw materials (wt.%) of table-5 devitrified glass products
| Raw material | Lithium beryllium mine tailing | Wingdale | Copper nickel Water Quenching Slag |
| Devitrified glass | 30.07 | 52.41 | 17.52 |
Table-6 product chemical constitutions (wt.%)
| Component | SiO 2 | CaO | Al 2O 3 | Fe 2O 3 | Other |
| Devitrified glass | 38.24 | 37.25 | 7.27 | 9.80 | 7.44 |
Raw material is dried at 120 DEG C, and mix by composition proportion, then High Temperature Furnaces Heating Apparatus is put into, 1600 DEG C are risen to from room temperature, and melting 2.5h obtains glass melt at 1600 DEG C, cast in by glass melt in the mould of 650 DEG C and be shaped, annealing 30min, last furnace cooling finally obtains parent glass.
Parent glass is heat-treated, from room temperature with the temperature rise rate of 5 DEG C/min, is warming up to 800 DEG C of insulation 60min, the Fe introduced with copper nickel Water Quenching Slag form
2o
3as main Nucleating Agent, make its abundant forming core, then with the temperature rise rate of 5 DEG C/min, be warming up to 1000 DEG C of insulation 1h, make its abundant micritization, then cool to room temperature with the furnace, can devitrified glass be obtained.
Aforesaid method is the invention that professional and technical personnel in the field can realize or use; apparent to the multiple amendment of these embodiments concerning those skilled in the art; therefore; the present invention can not be restricted to embodiment illustrated herein, the distortion done of with good grounds this programme or apparent change all among protection scope of the present invention.
Claims (3)
1. utilize lithium beryllium mine tailing to prepare a method for devitrified glass, it is characterized in that, comprise the step preparing parent glass and step parent glass being obtained devitrified glass by thermal treatment:
(1) by levigate for raw material to 40 orders, and it to be dried under 120 ° of C, then by raw material by proportioning Homogeneous phase mixing, and load in High Temperature Furnaces Heating Apparatus, described raw material comprises lithium beryllium mine tailing, Wingdale and copper nickel Water Quenching Slag;
(2) raw material mixed is incubated melting 1 ~ 6h under 1400 ° of C ~ 1600 ° C, obtain melt, then watered fast by melt and cast from advance in the mould of 400 ° of C ~ 600 ° C preheating, be shaped and the 30min ~ 180min that anneals, last furnace cooling obtains parent glass;
(3) parent glass of step (2) is heat-treated, be heated to 700 ° of C ~ 900 ° C with 5 ~ 10 ° of C/min temperature rise rates and be incubated 30min ~ 180min, the Fe introduced with copper nickel Water Quenching Slag form
2o
3carry out abundant forming core as main Nucleating Agent, then with the temperature rise rate of 5 ~ 10 ° of C/min, be warming up to 850 ° of C ~ 1100 ° C and be incubated 1 ~ 5h, then furnace cooling can obtain devitrified glass;
(4) step (3) described devitrified glass is carried out polish, polishing, cutting can obtain devitrified glass finished product.
2. a kind of method utilizing lithium beryllium mine tailing to prepare devitrified glass according to claim 1, it is characterized in that, described method raw materials quality per-cent composition: lithium beryllium mine tailing 30.07% ~ 47.40%, Wingdale 43.97% ~ 52.41%, copper nickel Water Quenching Slag 5.44% ~ 17.52%.
3. a kind of method utilizing lithium beryllium mine tailing to prepare devitrified glass according to claim 1, it is characterized in that, the principal crystalline phase of devitrified glass is wollastonite and gehlenite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410471994.5A CN104261677B (en) | 2014-09-16 | 2014-09-16 | A kind of method utilizing lithium beryllium mine tailing to prepare devitrified glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410471994.5A CN104261677B (en) | 2014-09-16 | 2014-09-16 | A kind of method utilizing lithium beryllium mine tailing to prepare devitrified glass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104261677A true CN104261677A (en) | 2015-01-07 |
| CN104261677B CN104261677B (en) | 2016-09-14 |
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Cited By (3)
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| CN105819694A (en) * | 2016-04-11 | 2016-08-03 | 新疆有色金属工业（集团）有限责任公司 | Glass ceramic and preparation method thereof |
| CN109354416A (en) * | 2018-12-07 | 2019-02-19 | 李异洪 | It is a kind of to utilize the once sintered process for preparing devitrified glass of lithium porcelain stone tailing |
| CN113149442A (en) * | 2021-03-23 | 2021-07-23 | 广东昊昌智能装备有限公司 | Method for preparing high-temperature-resistant composite crystal by using fly ash |
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| CN113149442A (en) * | 2021-03-23 | 2021-07-23 | 广东昊昌智能装备有限公司 | Method for preparing high-temperature-resistant composite crystal by using fly ash |
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