CN109399940A - A kind of preparation method of nickel slag microcrystalline glass - Google Patents
A kind of preparation method of nickel slag microcrystalline glass Download PDFInfo
- Publication number
- CN109399940A CN109399940A CN201811500405.6A CN201811500405A CN109399940A CN 109399940 A CN109399940 A CN 109399940A CN 201811500405 A CN201811500405 A CN 201811500405A CN 109399940 A CN109399940 A CN 109399940A
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- Prior art keywords
- glass
- nickel slag
- nickel
- melted
- agent
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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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/004—Refining agents
Abstract
The invention discloses a kind of preparation methods of nickel slag microcrystalline glass, set the mass percent range of each oxide are as follows: Al2O3: 7 ~ 12；MgO:10 ~ 20；CaO:8 ~ 5；SiO2: 48 ~ 52；Parent glass match ratio range are as follows: nickel slag 30 ~ 34%, flyash 27 ~ 33%, silica sand 8 ~ 10%, fluorite 9 ~ 11%, clarifying agent 8 ~ 11%, nucleating agent 3 ~ 6%, reducing agent 3 ~ 4%；Parent glass liquid is prepared using fusion method, while realizing the reduction and recycling of iron in nickel slag；Then nickel slag microcrystalline glass is prepared using the heat treatment of one-step method controlled micro crystallization.The present invention can be excellent with processability as primary raw material using nickel slag devitrified glass；The incorporation of nickel slag is up to 30% or more, can a large amount of consumable nickel slags, reduce the waste of waste resource；The reduction and separation that iron may be implemented while manufacturing nickel slag, further improve the recycling and reuse of efficient resource.
Description
Technical field
The present invention relates to nickel slags to recycle field, and in particular to a kind of preparation method of nickel slag microcrystalline glass.
Background technique
With the development of economy, industrial production is while consumption of natural resource, along with the output of a large amount of wastes,
In it is particularly evident with industrial residue, its main feature is that poor fluidity, yield are big, wide in variety, ingredient is changeable, processing difficulty is big.Now
Common processing method is stockpiling, not only wastes soil in this way, but also can generate secondary pollution to environment by various modes, very
To directly endangering human health.How proper treatment and recycle these wastes have become the whole world focal issue.
After the Soviet Union trial-produces cinder microcrystalline glass successfully, devitrified glass and its performance boost are prepared using industrial residue
Research made significant headway, but the preparation research in relation to nickel slag microcrystalline glass is less.The preparation of nickel slag microcrystalline glass is ground
Studying carefully in the processing to a large amount of commercial nickel slags has very important meaning.
Summary of the invention
To solve the above problems, the present invention provides a kind of preparation methods of nickel slag microcrystalline glass.
To achieve the above object, the technical scheme adopted by the invention is as follows:
A kind of preparation method of nickel slag microcrystalline glass, includes the following steps:
S1, according to the chemical composition analysis of nickel slag as a result, determining that glass system is CaO-SiO2-MgO-Al2O3-Li2O system, in advance
If the principal crystalline phase of devitrified glass is pyroxene；
Using flash smelting water quenching nickel slag and flyash as major ingredient, fluorite and silica sand are that auxiliary material is counted using phasor using diminishing method
Calculate the proportion of various raw materials, wherein set the mass percent range of each oxide are as follows: Al2O3: 7 ~ 12；MgO:10 ~ 20；CaO:
8~5；SiO2: 48 ~ 52；
S2, the match ratio for determining devitrified glass
Using fluorine system compound, carbonate respectively as cosolvent and clarifying agent, and composite nucleating agent is added, is melted by repeatedly trying
Parent glass match ratio range is finally determined afterwards are as follows: nickel slag 30 ~ 34%, flyash 27 ~ 33%, silica sand 8 ~ 10%, fluorite 9 ~ 11% are clear
Clear agent 8 ~ 11%, nucleating agent 3 ~ 6%, reducing agent 3 ~ 4%；The incorporation efficiency of its nickel slag is up to 30% or more；
S3, being melted for parent glass is carried out
Parent glass liquid is prepared using fusion method, while realizing the reduction and recycling of iron in nickel slag；Specifically, raw material is being melted
1 ~ 2h of heat preservation is poured into the mold preheated in advance after raw material sufficiently melts and is homogenized under conditions of temperature is 1450 DEG C
In, it is placed in high temperature box furnace, is preheated to 400 DEG C, after keeping the temperature 1h, close power supply by it and cool to room temperature with the furnace, it is therefore an objective to drop
Low glass because cooling rate it is too fast caused by internal stress；
S4, devitrified glass is prepared；
Nickel slag microcrystalline glass is prepared using one-step method controlled micro crystallization heat treatment, the condition of heat treatment is 768 DEG C of heat preservation 1.5h.
Wherein, in the step S3, in the melted stage of devitrified glass, graphite is used to complete the reduction of iron simultaneously as reducing agent
And the separation of iron and glass metal is realized using Gravity Separation.
The invention has the following advantages:
The present invention can be excellent with processability as primary raw material using nickel slag devitrified glass；The incorporation of nickel slag is up to 30% or more,
Can a large amount of consumable nickel slags, reduce the waste of waste resource；The reduction and separation that iron may be implemented while manufacturing nickel slag, into
One step improves the recycling and reuse of efficient resource.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
The embodiment of the invention provides a kind of preparation methods of nickel slag microcrystalline glass, include the following steps:
S1, according to the chemical composition analysis of nickel slag as a result, determining that glass system is CaO-SiO2-MgO-Al2O3-Li2O system, in advance
If the principal crystalline phase of devitrified glass is pyroxene；
Using flash smelting water quenching nickel slag and flyash as major ingredient, fluorite and silica sand are that auxiliary material is counted using phasor using diminishing method
Calculate the proportion of various raw materials, wherein set the mass percent range of each oxide are as follows: Al2O3: 7 ~ 12；MgO:10 ~ 20；CaO:
8~5；SiO2: 48 ~ 52；
S2, the match ratio for determining devitrified glass
Using fluorine system compound, carbonate respectively as cosolvent and clarifying agent, and composite nucleating agent is added, is melted by repeatedly trying
Parent glass match ratio range is finally determined afterwards are as follows: nickel slag 30 ~ 34%, flyash 27 ~ 33%, silica sand 8 ~ 10%, fluorite 9 ~ 11% are clear
Clear agent 8 ~ 11%, nucleating agent 3 ~ 6%, reducing agent 3 ~ 4%；Its industrial residue utilization rate be up to 60%(nickel slag incorporation efficiency be up to 30% with
On)；
S3, being melted for parent glass is carried out
Parent glass liquid is prepared using fusion method, while realizing the reduction and recycling of iron in nickel slag；Specifically, raw material is being melted
1 ~ 2h of heat preservation is poured into the mold preheated in advance after raw material sufficiently melts and is homogenized under conditions of temperature is 1450 DEG C
In, it is placed in high temperature box furnace, is preheated to 400 DEG C, after keeping the temperature 1h, close power supply by it and cool to room temperature with the furnace；
S4, devitrified glass is prepared
It is melted before terminating and dips a small amount of glass metal, water quenching obtains parent glass powder, and levigate 200 mesh of mistake prepares Thermal Synthetic point
Sample is analysed, is measured using Thermal Synthetic Analysis differential thermal analyzer, analysis curve obtains glass nucleation, crystallization temperature to set basis
The controlled micro crystallization heat treating regime of glass.The present embodiment prepares nickel slag crystallite using the heat treatment of one-step method controlled micro crystallization based on the analysis results
Glass, i.e. coring, crystallization carry out and complete simultaneously at the same temperature glass-ceramic process, and the condition of heat treatment is 768 DEG C of guarantors
Warm 1.5h is cooled to room temperature the good, devitrified glass based on pyroxene phase up to crystalline condition.
Embodiment 1
Step 1: being computed the theoretical match ratio of determining parent glass；Nickel slag 32%, flyash 34%, silica sand 10%, fluorite 11%,
Clarifying agent 9%, nucleating agent 4%；
Step 2: carrying out being melted for parent glass in high-temperature energy-conservation Cinker clew furnace, glass melting temperature is 1450 DEG C, and at such a temperature
1h is kept the temperature to guarantee that raw material is sufficiently melted, is homogenized and clarified, then pours into glass metal in the mold for being preheated to 200 DEG C in advance,
The separation for realizing glass metal and iron liquid using Gravity Separation simultaneously, obtains glass specimen；
Step 3: glass specimen is put into 400 DEG C of annealing furnaces the 1h that anneals, room temperature is cooled to the furnace, obtain parent glass sample；
Step 4: controlled micro crystallization heat treatment is carried out to parent glass using one-step method heat treatment process, specifically, by prepared base
Plinth glass then cools to room temperature the good, devitrified glass based on pyroxene phase up to crystalline condition in 768 DEG C of heat preservation 1.5h.
Embodiment 2
Devitrified glass match ratio is finally determined Step 1: being melted by repeatedly examination are as follows: nickel slag 33%, flyash 32%, silica sand 9%, firefly
Stone 9%, clarifying agent 9%, graphite 3%, nucleating agent 5%；
Step 2: carrying out being melted for parent glass in high-temperature energy-conservation Cinker clew furnace, glass melting temperature is 1450 DEG C, and at such a temperature
1h is kept the temperature to guarantee that raw material is sufficiently melted, is homogenized and clarified, then pours into glass metal in the mold for being preheated to 200 DEG C in advance,
The separation for realizing glass metal and iron liquid using Gravity Separation simultaneously, obtains glass specimen；
Step 3: glass specimen is put into 400 DEG C of annealing furnaces the 1h that anneals, room temperature is cooled to the furnace, obtain parent glass sample；
Step 4: controlled micro crystallization heat treatment is carried out to parent glass using one-step method heat treatment process, specifically, by prepared base
Plinth glass then cools to room temperature the good, devitrified glass based on pyroxene phase up to crystalline condition in 768 DEG C of heat preservation 1.5h.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or modify within the scope of the claims, this not shadow
Ring substantive content of the invention.In the absence of conflict, the feature in embodiments herein and embodiment can any phase
Mutually combination.
Claims (2)
1. a kind of preparation method of nickel slag microcrystalline glass, characterized by the following steps:
S1, according to the chemical composition analysis of nickel slag as a result, determining that glass system is CaO-SiO2-MgO-Al2O3-Li2O system, in advance
If the principal crystalline phase of devitrified glass is pyroxene；
Using flash smelting water quenching nickel slag and flyash as major ingredient, fluorite and silica sand are that auxiliary material is counted using phasor using diminishing method
Calculate the proportion of various raw materials, wherein set the mass percent range of each oxide are as follows: Al2O3: 7 ~ 12；MgO:10 ~ 20；CaO:
8~5；SiO2: 48 ~ 52；
S2, the match ratio for determining devitrified glass
Using fluorine system compound, carbonate respectively as cosolvent and clarifying agent, and composite nucleating agent is added, is melted by repeatedly trying
Parent glass match ratio range is finally determined afterwards are as follows: nickel slag 30 ~ 34%, flyash 27 ~ 33%, silica sand 8 ~ 10%, fluorite 9 ~ 11% are clear
Clear agent 8 ~ 11%, nucleating agent 3 ~ 6%, reducing agent 3 ~ 4%；
S3, being melted for parent glass is carried out
Parent glass liquid is prepared using fusion method, while realizing the reduction and recycling of iron in nickel slag；Specifically, raw material is being melted
1 ~ 2h of heat preservation is poured into the mold preheated in advance after raw material sufficiently melts and is homogenized under conditions of temperature is 1450 DEG C
In, it is placed in high temperature box furnace, is preheated to 400 DEG C, after keeping the temperature 1h, close power supply by it and cool to room temperature with the furnace；
S4, devitrified glass is prepared
Nickel slag microcrystalline glass is prepared using one-step method controlled micro crystallization heat treatment, the condition of heat treatment is 768 DEG C of heat preservation 1.5h.
2. a kind of preparation method of nickel slag microcrystalline glass as described in claim 1, it is characterised in that: in the step S3,
The melted stage of devitrified glass uses graphite as reducing agent and completes the reduction of iron and realize iron and glass metal using Gravity Separation
Separation.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811500405.6A CN109399940A (en) | 2018-12-10 | 2018-12-10 | A kind of preparation method of nickel slag microcrystalline glass |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811500405.6A CN109399940A (en) | 2018-12-10 | 2018-12-10 | A kind of preparation method of nickel slag microcrystalline glass |
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| CN109399940A true CN109399940A (en) | 2019-03-01 |
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| CN201811500405.6A Pending CN109399940A (en) | 2018-12-10 | 2018-12-10 | A kind of preparation method of nickel slag microcrystalline glass |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111992724A (en) * | 2020-08-21 | 2020-11-27 | 内蒙古科技大学 | Pyroxene-based metal Fe interlayer composite material and preparation method thereof |
| CN112851123A (en) * | 2021-02-24 | 2021-05-28 | 中南大学 | Method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101020968A (en) * | 2006-12-29 | 2007-08-22 | 金川集团有限公司 | Process of comprehensively utilizing high temperature nickel smelting slag |
| CN103708731A (en) * | 2013-12-30 | 2014-04-09 | 中国科学院过程工程研究所 | Nickel-slag porous microcrystalline material and preparation method thereof |
| CN103951193A (en) * | 2014-05-08 | 2014-07-30 | 中国科学院过程工程研究所 | Glass ceramics prepared from tailings obtained by nickel-molybdenum ore dressing and smelting and preparation method thereof |
| CN104556702A (en) * | 2014-12-16 | 2015-04-29 | 北京科技大学 | Method for preparing high-alkalinity glass ceramic from metallurgical slag |
-
2018
- 2018-12-10 CN CN201811500405.6A patent/CN109399940A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101020968A (en) * | 2006-12-29 | 2007-08-22 | 金川集团有限公司 | Process of comprehensively utilizing high temperature nickel smelting slag |
| CN103708731A (en) * | 2013-12-30 | 2014-04-09 | 中国科学院过程工程研究所 | Nickel-slag porous microcrystalline material and preparation method thereof |
| CN103951193A (en) * | 2014-05-08 | 2014-07-30 | 中国科学院过程工程研究所 | Glass ceramics prepared from tailings obtained by nickel-molybdenum ore dressing and smelting and preparation method thereof |
| CN104556702A (en) * | 2014-12-16 | 2015-04-29 | 北京科技大学 | Method for preparing high-alkalinity glass ceramic from metallurgical slag |
Non-Patent Citations (2)
| Title |
|---|
| 南雪丽等: "废渣微晶玻璃析晶行为分析及热处理制度的优化", 《人工晶体学报》 * |
| 高一智: "镍渣微晶玻璃的制备及性能研究", 《中国优秀硕士学位论文全文数据库-工程科技I辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111992724A (en) * | 2020-08-21 | 2020-11-27 | 内蒙古科技大学 | Pyroxene-based metal Fe interlayer composite material and preparation method thereof |
| CN112851123A (en) * | 2021-02-24 | 2021-05-28 | 中南大学 | Method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag |
| CN112851123B (en) * | 2021-02-24 | 2022-08-12 | 中南大学 | Method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag |
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Application publication date: 20190301 |
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