CN108191247A - A kind of preparation method of silica sludge glass ceramics - Google Patents
A kind of preparation method of silica sludge glass ceramics Download PDFInfo
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- CN108191247A CN108191247A CN201810252092.0A CN201810252092A CN108191247A CN 108191247 A CN108191247 A CN 108191247A CN 201810252092 A CN201810252092 A CN 201810252092A CN 108191247 A CN108191247 A CN 108191247A
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- 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
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- Crystallography & Structural Chemistry (AREA)
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- General Chemical & Material Sciences (AREA)
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Abstract
The present invention provides a kind of preparation methods of silica sludge glass ceramics, this method is raw material using the wastewater sludge of 60%wt or so and a certain proportion of silica, feldspar, aluminium oxide, calcium oxide, it is sufficiently mixed, is sieved after ball milling, being molded, burying burning sintering with stove heating fusing, brine hardening and with stove heating, so as to form glass ceramics.This method raw material proportioning is simple, and process repeatability is good, and it is higher that glass ceramics density is made.
Description
Technical field
The present invention relates to alum sludge process fields, and in particular to a kind of preparation of silica sludge glass ceramics
Method.
Background technology
In recent years, due to the intensive growth of population, the quickening of industrialization and urbanization process, produce a large amount of waste and
Byproduct, such as sludge, coal ash and mud, wastewater sludge are treated as an ever-increasing economy and the burden of environment.
It is Hesperian economically developed, it is more early for the processing starting of sludge, it is advanced for the treatment technology of sludge, handle the journey of sludge
Degree compared with other countries' height, they be generally with indirect heat drying or landfill, it is agricultural based on.For our Asia, compared with
For flourishing Japan of country they mainly using burning.Although and our in country's starting evenings, by exerting in recent years
Power, the method that we still summarize the various adaptation to local conditions such as Sludge landfill, sludge incineration, the processing of sludge ocean, agricultural sludge
（Certainly foreign countries' most countries are also to handle sludge with these modes）.
Sewage sludge contains a large amount of Fe2O3、P2O5、SiO2And ZnO, they are builder and the centre of glass reticular structure
Body.Therefore, glass ceramics can be produced using it as a kind of raw material sources.Japanese Tsukishima Kikai Co., Ltds
Hisashi Endo etc. were tried between nineteen ninety-five having carried out fundamental research and half industrialness with sludge potting porcelain in 1991
The research of equipment is tested, develops and sludge is converted into slag（Devitrified glass）Melting process technology and industrialized.
Syaharudin Zaibon et al. composite wastes sludge and soda-lime-silica glass devitrified glass are successful, have glass phase in finished product.
In a kind of methods that glass ceramics is prepared using waterworks wastewater sludge of patent ZL201210396941.2, lead to
It crosses into waterworks wastewater sludge and adds a certain proportion of feldspar, a small amount of MgO and Al2O3, glass ceramics can be made, but it burns
Junction temperature needs to be maintained at 1400-1500 DEG C, and to pass through the terrible grinding process of quenched glass, and workload is bigger.
Invention content
The present invention proposes a kind of preparation method of silica sludge glass ceramics, by adding higher ratio into sludge
Silica and a certain proportion of feldspar, a small amount of CaO and Al of example2O3, glass ceramics can be made, technique is sintered to bury burning, without
The grinding of frit is carried out, it is simple for process, it is produced on a large scale.
Realize the technical scheme is that：A kind of preparation method of silica sludge glass ceramics, step are as follows：
（1）Drying wastewater sludge and silica, feldspar, aluminium oxide, calcium oxide are fully ground and be uniformly mixed, is mixed
Material；
（2）By step（1）Mixture 1000-1300 DEG C of heat preservation 1-3h is heated in sintering furnace, salt bath water quenching after sintering obtains
Obtain frit；
（3）By step（2）Obtained frit carries out burying burning, obtains glass ceramics.
Step（1）Middle wastewater sludge heats 20-36h at 100-120 DEG C, obtains drying wastewater sludge.
The step（1）It is total that middle drying wastewater sludge accounts for drying wastewater sludge, silica, feldspar, aluminium oxide, calcium oxide
The 50-80% of quality, silica, feldspar, aluminium oxide and calcium oxide account for drying wastewater sludge, silica, feldspar, aluminium oxide,
The 20-50% of calcium oxide gross mass；The mass ratio of each substance is in silica, feldspar, aluminium oxide, calcium oxide（10-15）：
（10-15）：（50-60）：（20-30）.
The step（1）Middle material grinds 30-36h, crosses 100-150 mesh sieve, obtains mixture.
The step（3）In using mass ratio as 1:1 SiO2And Al2O3Mixture as burying material, frit is placed in and is buried
Burning is buried in material.
The step（3）In to bury the temperature of burning be 800-1000 DEG C, time 1-4h.
The key component of feldspar is silica, and aluminium oxide is glass network main composition object, adds in higher proportion in addition
Silica, which is used as, coheres phase and CaO, Na2O, K2Conditioning agents of the O as glass sintering temperature.Wastewater sludge also contains SiO2,
Al2O3And P2O5As the main composition object of glass network, the Fe contained simultaneously2O3Intermediate as a glass network.
The beneficial effects of the invention are as follows：The mixing of porcelain and wastewater sludge that the present invention is formed using silica, feldspar
Object is raw material, so as to which waste is become more stable and small toxicity material, and makes glass ceramics；The present invention is with higher
The silica of ratio and a certain proportion of feldspar and 60wt% or so wastewater sludge prepare glass ceramics for primary raw material.This hair
The features such as bright simple for process, cost of material is low, and acquisition glass ceramics density is high, suitable for commercial scale.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's all other embodiments obtained under the premise of not making the creative labor, belong to this hair
The range of bright protection.
Embodiment 1
The specific method that glass ceramics is prepared using waterworks wastewater sludge is as follows：
Wastewater sludge by weight 60% the ratio silica with 40%, feldspar and calcium oxide, alumina powder mixture respectively
Dispensing, porcelain proportioning are 19.78wt%SiO2、26.00 wt%CaO、51.5 0wt%Al2O3、2.72 wt%K2O and Na2O.It is useless
Sewage sludge heats 36 hours in insulating box in 120 DEG C in advance, drying.Abrasive lapping mixed above is uniform, and crosses 150 mesh sieve.So
Ball milling 24 hours afterwards, are molded in grinding tool.
Above-mentioned molding material strip is put into alumina crucible in resistance furnace keeps the temperature 3 hours with stove heating in 1270 DEG C.Then
Salt bath（10%）Quenching.
Above-mentioned frit is moved into again to heat up with stove in resistance furnace and buries burning in 1000 DEG C（SiO2And Al2O3According to 1:1 ratio
Example mixing, which is used as, buries material）And 2 hours crystallizations are kept the temperature, obtain glass ceramics.
The ceramics relative density is more than 88%.
Embodiment 2
The specific method that glass ceramics is prepared using waterworks wastewater sludge is as follows：
Wastewater sludge by weight 60% the ratio silica with 40%, feldspar and calcium oxide, alumina powder mixture respectively
Dispensing, porcelain proportioning are 24.78wt%SiO2、21.00 wt%CaO、51.50 wt%Al2O3、2.72 wt%K2O and Na2O.It is useless
Sewage sludge heats 36 hours in insulating box in 100 DEG C in advance, drying.Abrasive lapping mixed above is uniform, and crosses 150 mesh sieve.So
Ball milling 36 hours afterwards, are molded in grinding tool.
Above-mentioned molding material strip is put into alumina crucible in resistance furnace to melt and to keep the temperature 2 small with stove heating in 1270 DEG C
When.Then salt bath（10%）150 mesh sieve is crossed after quenching, grinding.
Above-mentioned frit is moved into again to heat up with stove in resistance furnace and buries burning in 800 DEG C（SiO2And Al2O3According to 1:1 ratio
Mixing is used as and buries material）And 2 hours crystallizations are kept the temperature, obtain glass ceramics.
The ceramics relative density is more than 88%.
Embodiment 3
The specific method that glass ceramics is prepared using waterworks wastewater sludge is as follows：
（1）Wastewater sludge heats 36 hours in insulating box in 100 DEG C；It will drying wastewater sludge and silica, feldspar, oxidation
Aluminium, calcium oxide are fully ground and are uniformly mixed, drying wastewater sludge account for drying wastewater sludge, silica, feldspar, aluminium oxide,
The 50% of calcium oxide gross mass, silica, feldspar, aluminium oxide and calcium oxide account for drying wastewater sludge, silica, feldspar, oxygen
The 50% of change aluminium, calcium oxide gross mass；The mass ratio of each substance is 10 in silica, feldspar, aluminium oxide, calcium oxide：10：50：
20, and sieve that is levigate respectively and crossing 100 mesh；Then ball milling 20 hours.
（2）After material mixed above molding, in sintering furnace being heated to 1000 DEG C with stove heating keeps the temperature 3 hours, then by object
Material directly carries out salt bath water quenching, obtains frit.
（3）More than glass material carries out burying burning.Frit is in SiO2And Al2O3Mixture（According to 1:1 ratio mixing）
It is sintered 4 hours as 800 DEG C of material is buried.Obtain glass ceramics.
Embodiment 4
（1）Wastewater sludge heats 30 hours in insulating box in 110 DEG C；It will drying wastewater sludge and silica, feldspar, oxidation
Aluminium, calcium oxide are fully ground and are uniformly mixed, drying wastewater sludge account for drying wastewater sludge, silica, feldspar, aluminium oxide,
The 70% of calcium oxide gross mass, silica, feldspar, aluminium oxide and calcium oxide account for drying wastewater sludge, silica, feldspar, oxygen
The 30% of change aluminium, calcium oxide gross mass；The mass ratio of each substance is 12 in silica, feldspar, aluminium oxide, calcium oxide：13：55：
25, and sieve that is levigate respectively and crossing 120 mesh；Then ball milling 30 hours.
（2）After material mixed above molding, in sintering furnace being heated to 1200 DEG C with stove heating keeps the temperature 2 hours, then by object
Material directly carries out salt bath water quenching, obtains frit.
（3）More than glass material carries out burying burning.Frit is in SiO2And Al2O3Mixture（According to 1:1 ratio mixing）
It is sintered 2 hours as 900 DEG C of material is buried.Obtain glass ceramics.
Embodiment 5
（1）Wastewater sludge heats 20 hours in insulating box in 120 DEG C；It will drying wastewater sludge and silica, feldspar, oxidation
Aluminium, calcium oxide are fully ground and are uniformly mixed, drying wastewater sludge account for drying wastewater sludge, silica, feldspar, aluminium oxide,
The 80% of calcium oxide gross mass, silica, feldspar, aluminium oxide and calcium oxide account for drying wastewater sludge, silica, feldspar, oxygen
The 20% of change aluminium, calcium oxide gross mass；The mass ratio of each substance is 15 in silica, feldspar, aluminium oxide, calcium oxide：15：60：
30, and sieve that is levigate respectively and crossing 150 mesh；Then ball milling 36 hours.
（2）After material mixed above molding, in sintering furnace being heated to 1000-1300 DEG C with stove heating keeps the temperature 1-3 hours, so
Material is directly carried out to salt bath water quenching afterwards, obtains frit.
（3）More than glass material carries out burying burning.Frit is in SiO2And Al2O3Mixture（According to 1:1 ratio mixing）
It is sintered 1 hour as 1000 DEG C of material is buried.Obtain glass ceramics.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (6)
1. a kind of preparation method of silica sludge glass ceramics, it is characterised in that step is as follows：
（1）Drying wastewater sludge and silica, feldspar, aluminium oxide, calcium oxide are fully ground and be uniformly mixed, is mixed
Material；
（2）By step（1）Mixture 1000-1300 DEG C of heat preservation 1-3h is heated in sintering furnace, salt bath water quenching after sintering obtains
Obtain frit；
（3）By step（2）Obtained frit carries out burying burning, obtains glass ceramics.
2. the preparation method of silica sludge glass ceramics according to claim 1, it is characterised in that：Step（1）In
Wastewater sludge heats 20-36h at 100-120 DEG C, obtains drying wastewater sludge.
3. the preparation method of silica sludge glass ceramics according to claim 1, it is characterised in that：The step
（1）It is middle drying wastewater sludge account for drying wastewater sludge, silica, feldspar, aluminium oxide, calcium oxide gross mass 50-80%；Two
The mass ratio of each substance is in silica, feldspar, aluminium oxide, calcium oxide（10-15）：（10-15）：（50-60）：（20-30）.
4. the preparation method of silica sludge glass ceramics according to claim 1, it is characterised in that：The step
（1）Middle material grinds 30-36h, crosses 100-150 mesh sieve, obtains mixture.
5. the preparation method of silica sludge glass ceramics according to claim 1, it is characterised in that：The step
（3）In using mass ratio as 1:1 SiO2And Al2O3Mixture as burying material, frit is placed in bury expect in bury burning.
6. the preparation method of silica sludge glass ceramics according to claim 1, it is characterised in that：The step
（3）In to bury the temperature of burning be 800-1000 DEG C, time 1-4h.
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| CN201810252092.0A CN108191247A (en) | 2018-03-26 | 2018-03-26 | A kind of preparation method of silica sludge glass ceramics |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114835396A (en) * | 2022-03-30 | 2022-08-02 | 国家能源集团宁夏煤业有限责任公司 | Composition for microcrystalline glass, microcrystalline glass and preparation method thereof |
Citations (3)
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| CN101576262A (en) * | 2008-05-05 | 2009-11-11 | 王永清 | Method for treating sludge in sewage plant and device thereof |
| CN102887642A (en) * | 2012-10-18 | 2013-01-23 | 中原工学院 | Method for preparing glass ceramic by utilizing wastewater sludge from water works |
| CN107555986A (en) * | 2017-09-04 | 2018-01-09 | 济南大学 | A kind of low-loss salt mine structure microwave-medium ceramics and preparation method |
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2018
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101576262A (en) * | 2008-05-05 | 2009-11-11 | 王永清 | Method for treating sludge in sewage plant and device thereof |
| CN102887642A (en) * | 2012-10-18 | 2013-01-23 | 中原工学院 | Method for preparing glass ceramic by utilizing wastewater sludge from water works |
| CN107555986A (en) * | 2017-09-04 | 2018-01-09 | 济南大学 | A kind of low-loss salt mine structure microwave-medium ceramics and preparation method |
Non-Patent Citations (1)
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| 张小立等: "利用废水污泥制备玻璃陶瓷的试验研究", 《中原工学院学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114835396A (en) * | 2022-03-30 | 2022-08-02 | 国家能源集团宁夏煤业有限责任公司 | Composition for microcrystalline glass, microcrystalline glass and preparation method thereof |
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Address after: 451191 No. 1 Huaihe Road, Shuang Hu Economic and Technological Development Zone, Xinzheng, Zhengzhou, Henan Applicant after: Zhongyuan University of Technology Address before: 451191 No. 1 Huaihe Road, Shuanghu Town Economic and Technological Development Zone, Zhengzhou City, Henan Province Applicant before: Zhongyuan University of Technology |
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