CN109354416A - It is a kind of to utilize the once sintered process for preparing devitrified glass of lithium porcelain stone tailing - Google Patents

It is a kind of to utilize the once sintered process for preparing devitrified glass of lithium porcelain stone tailing Download PDF

Info

Publication number
CN109354416A
CN109354416A CN201811496009.0A CN201811496009A CN109354416A CN 109354416 A CN109354416 A CN 109354416A CN 201811496009 A CN201811496009 A CN 201811496009A CN 109354416 A CN109354416 A CN 109354416A
Authority
CN
China
Prior art keywords
devitrified glass
porcelain stone
lithium porcelain
stone tailing
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.)
Pending
Application number
CN201811496009.0A
Other languages
Chinese (zh)
Inventor
李异洪
Original Assignee
李异洪
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by 李异洪 filed Critical 李异洪
Priority to CN201811496009.0A priority Critical patent/CN109354416A/en
Publication of CN109354416A publication Critical patent/CN109354416A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C10/00Devitrified 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
    • C03C10/0063Devitrified 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 present invention relates to a kind of using the once sintered process for preparing devitrified glass of lithium porcelain stone tailing, its main feature is that adding a certain amount of calcite and Nucleating Agent using lithium porcelain stone tailing as primary raw material, prepares devitrified glass using once sintered method.Its basic process is that raw material mixed grinding is sieved, and is melted, and is kept the temperature, and annealing, cooling obtains devitrified glass.The present invention prepares high-strength wearable devitrified glass by primary raw material of lithium porcelain stone tailing, realize the comprehensive utilization of resources of lithium porcelain stone tailing, its in devitrified glass raw material highest doping up to 80%, devitrified glass production cost is significantly reduced, lithium porcelain stone tailing is efficiently solved and stacks a series of safety and environmental problem generated naturally.In addition, clarifying agent is not added using once sintered method, reduce the corrosion to equipment and the discharge of nitrogen oxides while reducing energy consumption.

Description

It is a kind of to utilize the once sintered process for preparing devitrified glass of lithium porcelain stone tailing
Technical field
The present invention relates to a kind of preparation process of devitrified glass more particularly to a kind of utilization once sintered systems of lithium porcelain stone tailing The process of standby devitrified glass.
Background technique
In recent years, environmental pressure brought by exploitation of mineral resources activity is also got over the fast development of China's economy Come bigger, the discharge amount of industrial solid castoff is increasing.And a major class of the tailing as industrial solid castoff, refer to mine The dressing plant on mountain by ore reduction, screening, grinding, classification, again through selecting process such as gravity-floatations, after selecting useful metal Remainder, generally using SiO2 as main component.According to incompletely statistics, the tail that China is generated due to exploitation of mineral resources The accumulation stockpiling total amount of mine up to 11,000,000,000 tons or more, year quantum of output reached 1,200,000,000 tons, account for the 50 of whole world tailing quantum of output % or more.Tailing is removed as the building materials raw material such as low value-added cement, wall body brick at present, and most of also air storage is both made in this way At land occupation, environmental pollution, security risk, also make the wasting of resources.Therefore, how that these resource entirety high level are sharp With, especially developing low-cost, high performance devitrified glass building, ornament materials, widely paid close attention to.
Devitrified glass is also known as microlite or glass ceramics, is the polycrystalline solids material as obtained from controlling the crystallization of glass Material, was succeeded in developing and was commercialized for the first time in 1957 by Corning Incorporated.Devitrified glass compares traditional ceramics and glass, tool There are excellent high temperature resistant, wearability and chemical corrosion resistance, also there is high intensity, high rigidity, high-insulativity, low-dielectric loss Equal excellent performances, are widely used in fields such as national defence, aerospace, electronics, biomedicine, building materials.Traditional crystallite glass Glass is mainly based on chemical raw material, and high production cost, resource and energy consumption are bigger, and the chemical component in tailing mainly has SiO2, Al2O3, Fe2O3, MgO and CaO etc., needed for these ingredients all prepare devitrified glass, so using based on tailing Raw material is wanted to prepare devitrified glass, it has also become the important directions of devitrified glass development.In recent years, to the research of tailing microcrystal glass and Application and development is very active, it has also become one of the hot spot of new material development and application.
In recent years, due to the lithium porcelain stone tailing of lithium ion battery largely caused after a large amount of extraction lithiums In the presence of, how by the tailing effective use be a problem to be solved.Currently available technology is mostly by lithium porcelain stone raw ore with extremely low Ratio is added into the preparation of devitrified glass, and can not play the role of digestion and a large amount of lithium porcelain stone tailings of processing turns waste into wealth.
Summary of the invention
In order to make up the deficiency that the prior art is recycled in recycling lithium porcelain stone tailing, lithium is utilized the present invention provides a kind of The once sintered process for preparing devitrified glass of porcelain stone tailing is solving lithium porcelain stone tailings pollution, is improving the same of mine environment When, it prepares and has excellent performance, the devitrified glass product with high added value.
In order to achieve the above object, the present invention adopts the following technical scheme:
It is a kind of using the once sintered process for preparing devitrified glass of lithium porcelain stone tailing, include the following steps:
(1) mixed raw material: lithium porcelain stone tailing, calcite, Nucleating Agent are mixed, and mixing is made after crossing 0.100mm square hole screen in grinding Material;
(2) it is heat-treated: the above mixture is obtained into devitrified glass first product through melting, heat preservation, annealing, cooling;
(3) it grinds, polish, cutting: devitrified glass first product being ground, polish, is cut, obtaining the micro- of different size and brightness Crystal glass finished product.
Raw material in the step (1) does not include cosolvent.
Raw material in the step (1) does not include clarifying agent.
Raw material in the step (1) includes: lithium porcelain stone tailing 60-80%, calcite 10-30% by percentage to the quality, Nucleating Agent 3-5%.
The lithium porcelain stone tailing ingredient by mass percentage, SiO2 65-75%, Al2O3 15-25%, Na2O 2- 5%, K2O 2-5%, CaF2 1-2%, impurity 1-2%.
Nucleating Agent in the step (2) is P2O5;The additional amount of P2O5 is 3-5% by percentage to the quality.
Heat treatment in the step (2) specifically: heated up with the heating rate of 6-9 DEG C/min, at 1100-1200 DEG C Lower heat preservation, soaking time 120 minutes;Then anneal, temperature be 600-650 DEG C, soaking time 20 minutes, in air from It is so cooling.
Compared with the existing technology, beneficial effects of the present invention are as follows:
(1) present invention prepares high-strength wearable devitrified glass by primary raw material of lithium porcelain stone tailing, realizes the money of lithium porcelain stone tailing Sourceization comprehensive utilization, highest doping significantly reduces devitrified glass and is produced into up to 80% in devitrified glass raw material This, and efficiently solve lithium porcelain stone tailing and stack a series of safety and environmental problem generated naturally.
(2) fluxing agent is not added additionally by the present invention, but utilizes the Na itself contained in lithium porcelain stone tailing2O、K2O and CaF is combined as fluxing agent, melting temperature effectively can be down to 1100-1200 DEG C from 1600 DEG C, be greatly reduced energy consumption, simultaneously Reduce the corrosion to equipment.
(3) clarifying agent is not added additionally by the present invention.Routine prepares devitrified glass and needs to use antimony containing compounds as clear Clear agent can cause adverse effect to environment and equipment, and it usually requires to be used cooperatively with nitrate, also will increase nitrogen oxidation The discharge amount of object generates atmosphere pollution.
(4) present invention forms Composite Nucleation Agents using the CaF2 itself contained in the lithium porcelain stone tailing and P2O5 of addition, should Composite Nucleation Agents can effectively reduce the crystallization activation energy of devitrified glass, promote the formation of devitrified glass integrally crystallization.
(5) present invention has the intensity for being better than lithotome, wearability, resistance to using devitrified glass made from lithium porcelain stone tailing The performances such as sour, alkaline-resisting, resistant to chemical etching, and there is no radioactivity, it is harmless, it is ideal house decorative material.
Detailed description of the invention
Fig. 1 is the process flow chart provided by the invention for preparing lithium porcelain stone tailing microcrystal glass.
Fig. 2 is 1 gained lithium porcelain stone tailing microcrystal glass photo of embodiment provided by the invention.
Fig. 3 is 1 gained lithium porcelain stone tailing microcrystal glass photo of comparative example provided by the invention.
Specific embodiment
With reference to the accompanying drawing and the present invention is discussed in detail in specific embodiment.Embodiment below is only limitted to explain the present invention, Protection scope of the present invention should include the full content of claim, be not limited only to the present embodiment.And under the present invention passes through Face embodiment, those skilled in the art are all the elements that can fully achieve the claims in the present invention record.
Embodiment 1
It is provided in this embodiment using the once sintered process for preparing devitrified glass of lithium porcelain stone tailing, include the following steps:
(1) mixed raw material: will be mixed by the lithium porcelain stone tailing, calcite, Nucleating Agent of ingredient described in table 1 by proportion described in table two, Mixture is made after crossing 0.100mm square hole screen in grinding;
(2) it is heat-treated: being heated up, kept the temperature at 1100-1200 DEG C, soaking time 120 minutes with the heating rate of 6-9 DEG C/min; Then it anneals, temperature is 600-650 DEG C, and soaking time 20 minutes, natural cooling obtained devitrified glass photo such as in air Shown in Fig. 2, surface is smooth, and structure is uniform, and integrally crystallization degree is higher.
Following table 1 is lithium porcelain stone tailing used in embodiment 1 at being grouped as.
Following table 2 is the material composition and composition in the method that embodiment 1 provides.
The lithium porcelain stone tailing used in embodiment 1 of table 1 at being grouped as
The material composition and composition in method that 2 embodiment 1 of table provides
Comparative example 1
Method as described in Example 1, the difference is that forming Composite Nucleation Agents that P2O5 is not added, this example is used once sintered Method is difficult to complete whole crystallization under the conditions of no Composite Nucleation Agents, and gained devitrified glass photo is as shown in figure 3, surface is thick Rough, stomata increases, and crystallization degree is lower.
It should be noted that those skilled in the art are that the present invention may be implemented completely according to the above embodiment of the present invention Independent claims and the full scope of appurtenance, realize process and the same above-described embodiment of method;And the present invention is not detailed Elaboration partly belongs to techniques well known.
The above, part specific embodiment only of the present invention, but scope of protection of the present invention is not limited thereto, appoints In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of, should all cover by what those skilled in the art Within protection scope of the present invention.

Claims (7)

1. it is a kind of using the once sintered process for preparing devitrified glass of lithium porcelain stone tailing, include the following steps:
(1) mixed raw material: lithium porcelain stone tailing, calcite, Nucleating Agent are mixed, and mixing is made after crossing 0.100mm square hole screen in grinding Material;
(2) it is heat-treated: the above mixture is obtained into devitrified glass first product through melting, heat preservation, annealing, cooling;
(3) it grinds, polish, cutting: devitrified glass first product being ground, polish, is cut, obtaining the micro- of different size and brightness Crystal glass finished product.
2. it is according to claim 1 a kind of using the once sintered process for preparing devitrified glass of lithium porcelain stone tailing, It is characterized in that, the raw material in the step (1) includes: lithium porcelain stone tailing 60-80%, calcite 10- by percentage to the quality 30%, Nucleating Agent 3-5%.
3. it is according to claim 2 a kind of using the once sintered process for preparing devitrified glass of lithium porcelain stone tailing, It is characterized in that, the raw material in the step (1) does not include cosolvent.
4. it is according to claim 2 a kind of using the once sintered process for preparing devitrified glass of lithium porcelain stone tailing, It is characterized in that, the raw material in the step (1) does not include clarifying agent.
5. it is according to claim 2 a kind of using the once sintered process for preparing devitrified glass of lithium porcelain stone tailing, Be characterized in that: the lithium porcelain stone tailing ingredient by mass percentage, SiO2 65-75%, Al2O3 15-25%, Na2O 2- 5%, K2O 2-5%, CaF2 1-2%, impurity 1-2%.
6. it is according to claim 2 a kind of using the once sintered process for preparing devitrified glass of lithium porcelain stone tailing, Be characterized in that: the Nucleating Agent in the step (2) is the Composite Nucleation Agents that the CaF2 in P2O5 and lithium porcelain stone tailing is formed; The additional amount of P2O5 is 3-5% by percentage to the quality.
7. it is according to claim 1 a kind of using the once sintered process for preparing devitrified glass of lithium porcelain stone tailing, It is characterized in that, the heat treatment in the step (2) specifically: heated up with the heating rate of 6-9 DEG C/min, in 1100-1200 It is kept the temperature at DEG C, soaking time 120 minutes;Then anneal, temperature be 600-650 DEG C, soaking time 20 minutes, in air Natural cooling.
CN201811496009.0A 2018-12-07 2018-12-07 It is a kind of to utilize the once sintered process for preparing devitrified glass of lithium porcelain stone tailing Pending CN109354416A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811496009.0A CN109354416A (en) 2018-12-07 2018-12-07 It is a kind of to utilize the once sintered process for preparing devitrified glass of lithium porcelain stone tailing

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811496009.0A CN109354416A (en) 2018-12-07 2018-12-07 It is a kind of to utilize the once sintered process for preparing devitrified glass of lithium porcelain stone tailing

Publications (1)

Publication Number Publication Date
CN109354416A true CN109354416A (en) 2019-02-19

Family

ID=65331774

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811496009.0A Pending CN109354416A (en) 2018-12-07 2018-12-07 It is a kind of to utilize the once sintered process for preparing devitrified glass of lithium porcelain stone tailing

Country Status (1)

Country Link
CN (1) CN109354416A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111348895A (en) * 2020-04-07 2020-06-30 江西鼎盛新材料科技有限公司 Lepidolite tailing once-sintered ceramic foam belt microcrystal decorative integrated board
CN111470773A (en) * 2019-12-20 2020-07-31 吉林省梓楗新型建材股份有限公司 Method for one-time sintering of microcrystalline jade

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1091399A (en) * 1993-02-26 1994-08-31 湖州玻璃厂二分厂 The colour devitrified glass and the manufacture method thereof that contain lithium tailings 〉=80%
CN1117029A (en) * 1994-08-13 1996-02-21 山东建材工业学院分院科研生产处科技开发中心 Method for producing nucleated glass product with golden tailings
CN101224949A (en) * 2008-01-25 2008-07-23 浙江大学 Ecological glass-ceramic and preparation method thereof
CN101298366A (en) * 2008-07-04 2008-11-05 沈阳建筑大学 Metal tailings construction nucleated glass and one-step sintering preparation thereof
CN102079625A (en) * 2010-12-07 2011-06-01 淮安乔氏建材发展有限公司 Microcrystal glass manufactured by using tailing solid waste and manufacturing method thereof
CN102531394A (en) * 2011-12-28 2012-07-04 淄博钰晶新型材料科技有限公司 Formula and production process for producing microcrystal panels using lithium tailings
CN104261677A (en) * 2014-09-16 2015-01-07 新疆大学 Method for preparing microcrystalline glass from lithium beryllium tailings
CN105884200A (en) * 2016-04-11 2016-08-24 大连理工大学 Method for producing microcrystalline glass-ceramic composite material from industrial fly ash and vitrification slag
CN108395105A (en) * 2018-05-24 2018-08-14 苏州大学 A method of preparing devitrified glass using copper silver tailing and cullet

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1091399A (en) * 1993-02-26 1994-08-31 湖州玻璃厂二分厂 The colour devitrified glass and the manufacture method thereof that contain lithium tailings 〉=80%
CN1117029A (en) * 1994-08-13 1996-02-21 山东建材工业学院分院科研生产处科技开发中心 Method for producing nucleated glass product with golden tailings
CN101224949A (en) * 2008-01-25 2008-07-23 浙江大学 Ecological glass-ceramic and preparation method thereof
CN101298366A (en) * 2008-07-04 2008-11-05 沈阳建筑大学 Metal tailings construction nucleated glass and one-step sintering preparation thereof
CN102079625A (en) * 2010-12-07 2011-06-01 淮安乔氏建材发展有限公司 Microcrystal glass manufactured by using tailing solid waste and manufacturing method thereof
CN102531394A (en) * 2011-12-28 2012-07-04 淄博钰晶新型材料科技有限公司 Formula and production process for producing microcrystal panels using lithium tailings
CN104261677A (en) * 2014-09-16 2015-01-07 新疆大学 Method for preparing microcrystalline glass from lithium beryllium tailings
CN105884200A (en) * 2016-04-11 2016-08-24 大连理工大学 Method for producing microcrystalline glass-ceramic composite material from industrial fly ash and vitrification slag
CN108395105A (en) * 2018-05-24 2018-08-14 苏州大学 A method of preparing devitrified glass using copper silver tailing and cullet

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王艺慈: "《包钢高炉渣制备微晶玻璃的析晶行为》", 31 January 2014, 冶金工业出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111470773A (en) * 2019-12-20 2020-07-31 吉林省梓楗新型建材股份有限公司 Method for one-time sintering of microcrystalline jade
CN111348895A (en) * 2020-04-07 2020-06-30 江西鼎盛新材料科技有限公司 Lepidolite tailing once-sintered ceramic foam belt microcrystal decorative integrated board

Similar Documents

Publication Publication Date Title
CN109354416A (en) It is a kind of to utilize the once sintered process for preparing devitrified glass of lithium porcelain stone tailing
CN109020231B (en) Method for preparing alloy iron and microcrystalline glass
CN104926131A (en) Vanadium titano-magnetite tailing glass-ceramic and preparation method thereof
CN105441683B (en) A kind of integrated conduct method of mixed sludge
CN108516709B (en) Sulphoaluminate cement clinker taking lead-zinc tailings as raw materials and preparation method thereof
CN108275974B (en) Water permeable brick and method for preparing water permeable brick by using fly ash
CN104788011B (en) A kind of tailings of high silicon iron foam pyroceram and its production method
CN105924014A (en) Microcrystalline glass produced from fly ash through all-electric melting calendaring process and production method thereof
CN110335693A (en) A kind of preparation method for radioactive waste glass solidification basic material and glass solidified body
CN104649784A (en) Method for preparing silicon-potash fertilizer based on magnesium slag
CN108264233B (en) Method for comprehensively utilizing electrolytic manganese slag and preparing microcrystalline glass
CN104193171A (en) Silicon manganese alloy slag glass ceramic and preparation method thereof
CN104058591A (en) Method for producing foam microcrystal thermal insulating decoration board by use of fluorite tailings
CN104478329A (en) Preparation method for producing autoclaved aerated concrete block by using antimony ore tailing
CN109265010A (en) A kind of lithium porcelain stone tailing microcrystal glass and preparation method thereof
CN110590170B (en) Fly ash-based inorganic fiber and preparation method thereof
CN106145686B (en) A kind of complicated utilization Pb-Zn tailings, devitrified glass of electrolytic manganese waste residue and preparation method thereof
CN110092587B (en) Method for preparing microcrystalline glass by using waste
CN106007364B (en) A method of preparing devitrified glass using ardealite
CN103526049B (en) The method of a kind of pyrometallurgical smelting antimony arsenic removal
CN109081677B (en) Antique brick body made of high-calcium-magnesium skarn type iron tailings and manufacturing method thereof
CN110335695A (en) A kind of preparation method of solidification of radwaste basic material and glass solidified body
CN106116161B (en) A method of preparing devitrified glass using yellow phosphorus furnace slag and chromium slag
CN105293929B (en) The method that devitrified glass mill ball is prepared using molybdic tailing
CN106630644A (en) Rare-earth slag glass-ceramic and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190219