CN105152536B - A kind of method that microcrystal glass material is synthesized using ferrochrome slag - Google Patents
A kind of method that microcrystal glass material is synthesized using ferrochrome slag Download PDFInfo
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- CN105152536B CN105152536B CN201510603618.1A CN201510603618A CN105152536B CN 105152536 B CN105152536 B CN 105152536B CN 201510603618 A CN201510603618 A CN 201510603618A CN 105152536 B CN105152536 B CN 105152536B
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Abstract
The present invention relates to the synthesis technical field of inorganic non-metallic material, the purpose of invention is to provide a kind of method using solid waste (ferrochrome slag and cullet), lime stone, soda ash and fluorite synthesis pyroxene type microcrystal glass material.The raw material of synthesis of the present invention is mainly solid waste, and wherein ferrochrome slag belongs to weight toxic waste, it is necessary to individually handle.The present invention has synthesized waste residue microcrystal glass material only with normal pressure-sintered, and properties are satisfied by industrial needs, not only solve solid waste bulk deposition pollution on the environment, the slag class microcrystal glass material of synthesis can apply to building and ornament materials, and meet the industrial policy of " recycling economy " that country advocates, there is higher economic value and Significance for Environment.
Description
Technical field
The present invention relates to the synthesis technical field of inorganic non-metallic material, particularly with solid waste (ferrochrome slag,
Cullet), lime stone, the method that soda ash and fluorite are Material synthesis microcrystal glass material.
Background technology
China's stainless steel production in recent years is in increase trend rapidly, also increasing to the demand of ferrochrome.Meanwhile ferrochrome
The environmental pressure that alloy smelting enterprise is faced is also increasingly urgent, especially the discharge of ferrochrome factory solid waste, it is necessary to
Meet national requirements for environmental protection.In ferrochrome factory solid waste be mainly derived from high temperature production technique caused clinker and
Dirt mud.Ferrochrome slag viscosity is big, fusing point is high, and slag iron can not be kept completely separate.In general, often production 1t ferrochromes will be about
Produce 1.1~1.3t waste residues；Simultaneously during ferrochrome submerged-arc smelting, because the high temperature evaporation of element, electrode hole splash
Furnace charge fine particle can also produce about 25kg flue dust or sludge with tail gas discharge in the waste residue and charging process that go out.So can
Find out clean method and utilize ferrochrome slag, and synthesize the material with certain added value, protected for energy-saving and emission-reduction and environment
Protector plays a very important role.
Domestic and international ferrochrome residues processing technique sums up, the main technique for including recovery alloy or fine chrome mine, circulation
Recycle technique etc..The technique for wherein reclaiming alloy or fine chrome mine was reclaimed using the methods of magnetic separation, gravity treatment, and circulation and stress
It is to be raw material production refractory material, slag former with ferrochrome slag or for cement admixture and pave the way.Due to ferrochrome slag
In remaining chrome ore there is weak magnetic, and ferrochrome has ferromagnetism, it is therefore possible to use the technique of magnetic separation is reclaimed in slag
Ferrochrome particle and remaining chrome ore.In addition, many producers and research institution all once research both at home and abroad is using gravity treatment
Method reclaims the metal in ferrochrome slag, and some ferroalloy works and researcher use circulation and stress ferrochrome slag, and
For producing substitute and making cement admixture and the paving of refractory material (do not burn magnesite-chrome brick and do not burn magnesia brick) and stifled eye magnesia
Road.
Devitrified glass is the novel glass to grow up the fifties, and it is with microcrystal and the mutually equally distributed material of glass
Material, therefore also known as glass ceramics or sintered glass ceramics；Cinder microcrystalline glass is as an important composition in microcrystal glass area
Part, it is the devitrified glass prepared with flyash of various metallurgical slags, industrial and mineral tailings and steam power plant etc. for primary raw material.Utilize
Industrial residue slakin devitrified glass, has obtained rapid development in the past 20 years.Cinder microcrystalline glass has higher machinery
Intensity, wear-resisting, good electric property and chemical stability, it has also become a kind of good structural material.Current slag crystallite
Glass is mainly manufactured using blast-furnace slag, because the chemical composition of blast-furnace slag is more stable, and adapts to CaO-Al2O3-
SiO2The requirement of microcrystalline glass in series.Ferrochrome slag is close with blast furnace slag composition, is equally applicable to prepare microcrystal glass material, but
It is due to that high-melting-point substances are more in ferrochrome slag, so ferrochrome slag ratio blast furnace slag tapping temperature is higher by 500 DEG C or so；
And it is more compared with blast furnace slag that material is nucleated in ferrochrome slag, the more difficult control of Crystallization Process, therefore the present invention is from these difficult points,
Ferrochrome slag microcrystalline glass preparation temperature is successfully reduced, and by batching control devitrified glass crystalline phase, solves and uses ferrochrome
Fe alloy slag prepares these defects of microcrystal glass material, has synthesized the devitrified glass of better performances.
Because ferrochrome slag ingredient is more complicated, it is seldom to prepare the correlative study of devitrified glass on ferrochrome slag,
It is final to determine but in order to make industrialization of the cinder microcrystalline glass in China as early as possible, research prepares devitrified glass with ferrochrome slag
Optimal preparation flow and preparation condition, have very important significance for the recycling of ferrochrome slag discarded object.
The content of the invention
It is an object of the invention to provide one kind to utilize solid waste (ferrochrome slag and cullet), lime stone, pure
The method of alkali and fluorite synthesis pyroxene type microcrystal glass material.The raw material of synthesis of the present invention is mainly solid waste, wherein
Ferrochrome slag belongs to weight toxic waste, it is necessary to individually handle.The present invention has synthesized waste residue microcrystal glass only with normal pressure-sintered
Material, and properties are satisfied by industrial needs, have higher economic value and Significance for Environment.
It is a kind of using ferrochrome slag synthesize microcrystal glass material method, with ferrochrome slag, cullet, lime stone,
Soda ash and fluorite are raw material, and preparation process is as follows：
(1) raw material prepares：Fine powder is made by grinding in ferrochrome slag and both discarded objects of cullet, and is all led to
Cross the sieve of 200 mesh；The composition of described solid waste is：SiO in ferrochrome slag2Account for 25~30%, MgO account for 35~
40%, Al2O3Account for 20~25%, Cr2O3Account for 1~10%, CaO and account for 1~3%, Fe2O3Account for 1~5%, remaining for it is a small amount of containing potassium,
The oxide of sodium；SiO in the cullet powder2Account for 75~78%, Na2O account for 8~10%, CaO account for 7~10%, MgO account for 3~
5%, remaining is a small amount of oxide containing potassium；CaO accounts for 55~56% in the lime stone, Na in the soda ash2O accounts for 58~
59%, CaF in the fluorite2Account for 98~99%.
(2) mix：The ratio of ferrochrome slag in synthesis material, cullet, lime stone, soda ash and fluorite is controlled, according to
Quality than ferrochrome slag 30~50%, cullet 50~30%, lime stone 10~20%, soda ash 5~10%, match somebody with somebody fluorite 5 outside
~10%, the raw material dosage according to needed for calculating design, by load weighted ferrochrome slag, cullet, lime stone, soda ash and fluorite
Mixing 30min~120min is carried out using ball mill；
(3) melt：Raw material after mixing is put into alumina crucible, under air atmosphere, is warming up in Muffle furnace with stove
1500 DEG C~1550 DEG C are melted, and soaking time is 1~4h；
(4) cast annealing：After melting insulation, take out crucible, by fused raw material be poured into advance in 500 DEG C of Muffle furnaces it is pre-
In the stainless steel mould of heat, and 0.5~2h of annealing, then furnace cooling in 500 DEG C of Muffle furnaces are put into rapidly；
(5) it is heat-treated：Sample after annealing, the temperature schedule made with the coring determined and crystallization temperature carry out heat
Processing, using second order heat-treating methods, sample is put into Muffle furnace from room temperature to 630~660 DEG C, and insulation 0.5~
2h, 830~860 DEG C are continuously heating to, are incubated 0.5~2h, then furnace cooling.
The advantage of the invention is that：Devitrified glass has been synthesized with ferrochrome slag, cullet, lime stone, soda ash and fluorite
Material, the raw material of preparation is caused in caused heavy inert solid discarded object ferrochrome slag in ferrochrome production and life
Scrap glass, this all suitable abundant, microcrystal glass material (example 4) of the slag class of synthesis of solid waste reserves in two,
Its rupture strength is 104MPa, microhardness 9859.78Mpa, bulk density 2.87g/cm3, and its microstructure is uniform,
With good performance.Not only solve solid waste bulk deposition pollution on the environment, the slag class of synthesis
Microcrystal glass material can apply to building and ornament materials, and meet the industrial policy of " recycling economy " that country advocates.
Brief description of the drawings
Fig. 1 devitrified glass preparation flows.
Fig. 2 devitrified glass X ray diffracting spectrums.
Fig. 3 devitrified glass microscopic structures.
Fig. 4 devitrified glass microhardnesses.
Fig. 5 devitrified glass bending strengths.
Embodiment
Ferrochrome slag, cullet, lime stone, soda ash and fluorite are used as raw material, it matches as shown in table 1.1500
DEG C~1550 DEG C of temperature melting 1~4h of normal pressure heat-insulating, synthesis slag class crystallite glass after heat treatment will be passed through after obtained basic glass
Glass material.X-ray diffraction analysis and sem analysis are carried out to synthesis sample.
Table 1 synthesizes the raw material proportioning and synthesis condition of ferrochrome slag microcrystalline glass material
By preparing design flow diagram, as shown in figure 1, having obtained the ferrochrome slag microcrystalline glass material of heterogeneity proportioning
Material, distinguish as shown in Figure 2 and Figure 3 according to X-ray diffraction and the ESEM result figure of experimental design synthetic material, can from figure
To find out, the principal crystalline phase of synthetic material is diopside and nepheline, and with ferrochrome slag percentage composition in the feed
Increase, devitrified glass generation crystal grain be gathered into mutually diminish, the mechanical performance for so directly resulting in devitrified glass is (such as micro- hard
Degree, bending strength) change is also produced therewith, as shown in Figure 4, Figure 5.With the increase of ferrochrome slag ingredient, microhardness with
Increase, reach 104MPa when ferrochrome slag content increases to 50%；It is rear to reduce and bending strength first increases,
Vickers hardness reaches maximum, i.e. 9859.78MPa when ferrochrome slag content reaches 45%.
Claims (1)
1. it is a kind of using ferrochrome slag synthesize microcrystal glass material method, it is characterised in that with ferrochrome slag, cullet,
Lime stone, soda ash and fluorite are raw material, and specific preparation process is as follows：
(1) raw material prepares：Fine powder is made by grinding in ferrochrome slag, cullet, makes its all sieve by 200 mesh；
(2) mix：The ratio of ferrochrome slag in synthesis material, cullet, lime stone, soda ash and fluorite is controlled, according to quality
Than ferrochrome slag 30~50%, cullet 30~50%, lime stone 10~20%, soda ash 5~10%, outside with fluorite 5~
10%, and mixed, the raw material dosage according to needed for calculating design, by load weighted ferrochrome slag, waste glass powder, lime
Stone, soda ash and fluorite carry out 30~120min of mixing with ball mill；
(3) melt：Raw material after mixing is put into alumina crucible, under air atmosphere, 1500 are warming up to stove in Muffle furnace
DEG C~1550 DEG C melted, soaking time is 1~4h；
(4) cast annealing：After melting insulation, crucible is taken out, fused raw material is poured into what is preheated in advance in 500 DEG C of Muffle furnaces
In stainless steel mould, and furnace cooling anneal 0.5~2h after is put into 500 DEG C of Muffle furnaces rapidly；
(5) it is heat-treated：Sample after annealing, it is heat-treated using second order heat-treating methods, the sample for cooling of annealing is put
Enter from room temperature to 630~660 DEG C in Muffle furnace, be incubated 0.5~2h, be continuously heating to 830~860 DEG C, insulation 0.5~
2h, then furnace cooling；
SiO in the ferrochrome slag2Account for 25~30%, MgO and account for 35~40%, Al2O3Account for 20~25%, Cr2O3Account for 1~
10%, CaO account for 1~3%, Fe2O31~5% is accounted for, remaining is a small amount of oxide containing potassium, sodium；In the cullet powder
SiO2Account for 75~78%, Na2O, which accounts for 8~10%, CaO and accounts for 7~10%, MgO, accounts for 3~5%, and remaining is a small amount of oxidation containing potassium
Thing；CaO accounts for 55~56% in the lime stone, Na in the soda ash2O accounts for 58~59%, CaF in the fluorite2Account for 98~
99%.
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| CN105837041A (en) * | 2016-05-19 | 2016-08-10 | 台玻安徽玻璃有限公司 | Manufacturing method of float glass |
| CN106698954A (en) * | 2016-12-21 | 2017-05-24 | 江苏省冶金设计院有限公司 | Cordierite microcrystalline glass prepared from high carbon ferrochrome slag and coal gangue and preparation method of cordierite microcrystalline glass |
| CN106698953A (en) * | 2016-12-21 | 2017-05-24 | 江苏省冶金设计院有限公司 | Cordierite microcrystalline glass prepared by using high-carbon ferrochrome slag and preparation method of cordierite microcrystalline glass |
| CN108640524A (en) * | 2018-07-31 | 2018-10-12 | 合肥利裕泰玻璃制品有限公司 | A kind of method that high carbon chromium scum prepares devitrified glass |
| CN113087398B (en) * | 2021-04-13 | 2022-12-09 | 山东建筑大学 | Microcrystalline glass prepared from coal gasification furnace slag and preparation method thereof |
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| CN103395995B (en) * | 2013-08-01 | 2015-07-08 | 湖南永鑫环保科技有限公司 | Production method for producing microcrystalline glass by using waste glass and smelting waste |
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