CN102936016A - Method for preparing soluble glass by using waste residues with aluminum extracted by coal gangue - Google Patents
Method for preparing soluble glass by using waste residues with aluminum extracted by coal gangue Download PDFInfo
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- CN102936016A CN102936016A CN2012104524295A CN201210452429A CN102936016A CN 102936016 A CN102936016 A CN 102936016A CN 2012104524295 A CN2012104524295 A CN 2012104524295A CN 201210452429 A CN201210452429 A CN 201210452429A CN 102936016 A CN102936016 A CN 102936016A
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- coal gangue
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Abstract
The invention relates to a method for preparing soluble glass by using waste residues with aluminum extracted by coal gangue. The method comprises firstly mixing and grinding the waste residue with aluminum extracted by coal gangue and sodium carbonate to be 1-50mu m particles, then conducting temperature programming in a muffle furnace, conducting low temperature congruent melting reaction for 1-5 hours at the temperature of 500-850 DEG C, and conducting water quenching to obtain coarse sodium silicate solid; and placing the coarse sodium silicate solid in a high pressure reactor, adding distilled water, heating to be 150 DEG C, stirring and dissolving for 5 hours, cooling to be room temperature, filtering and separating to obtain a colorless and transparent sodium silicate solution, and crystallizing to be the soluble glass. The method lowers the temperature for preparing sodium silicate by using a traditional soda ash method by about 600 DEG C, greatly reduces energy consumption, and simultaneously avoids highly corrosive of a traditional caustic soda alkali-dissolution method on production facilities and alkali pollution on the environment.
Description
Technical field
The present invention relates to the preparation of water glass, specifically belong to a kind of coal gangue that utilizes and put forward the method that waste slag of aluminum prepares soluble glass.
Background technology
When preparing polymerize aluminum chloride or Tai-Ace S 150 take coal gangue, kaolin or flyash etc. as raw material, can produce a large amount of waste residues, contain a large amount of silicon-dioxide in the waste residue, if can not effectively fully utilize, must cause production cost to increase and secondary environmental pollution.
Soluble glass is of many uses, is summed up to mainly contain the following aspects: (1) industrial raw materials: can be used for preparing silicon sol, silica gel, precipitated silica, zeolite, aluminosilicate, Magnesium Silicate q-agent, synthesis of clay, cement or catalyzer etc.; (2) washing agent: as fabric washing powder, dish washing detergent and industrial cleaning agent; (3) tackiness agent: the tackiness agent that can be used as cardboard, moulded coal, roofing tile, brick and cement, refractory cement, gypsum and plaster and welding rod etc.; (4) top coat: can be used for TiO
2Product, concrete, brick and tile or glass surface, flame resistant glass and tunnel construction spraying etc.; (5) deinking of paper pulp and papermaking and bleaching; (6) sanitas of water treatment system.
At present, the main method of industrial preparation water glass (water glass) is 1100-1450 ℃ of melting in High Temperature Furnaces Heating Apparatus with quartz sand and yellow soda ash (or salt of wormwood), then the water glass fragment that obtains is water-soluble under 100 ℃ of normal pressures, or in autoclave sterilizer 150 ℃ water-soluble.Also can adopt hydrothermal method, namely under the pressure of 200 ℃ and 20bar in autoclave sterilizer melting sand and sodium hydroxide or potassium hydroxide, directly make aqueous silicate solution.The people such as Yi Ding adopt silica powder (350 order) and sodium carbonate mixture to obtain sodium silicate solid in 1450 ℃ of frit reactions, then the water-soluble sodium silicate solution that obtains in autoclave when utilizing water glass to prepare mesoporous silicon oxide SBA-15 nanometer rod.
Among a kind of white carbon black preparation method of patent 200610016584.7 report, the preparation of water glass is with silicon dioxide powder and sodium bicarbonate 1:1 ~ 2 in molar ratio, calcines under 1150-1650 ℃ of high temperature.Too high calcining temperature is not only high to equipment requirements, and energy consumption increases.
Summary of the invention
The purpose of this invention is to provide a kind of coal gangue that utilizes that can reduce energy consumption, minimizing pollution and put forward the method that waste slag of aluminum prepares water glass.
A kind of coal gangue that utilizes provided by the invention is put forward the method that waste slag of aluminum prepares soluble glass, step comprises: waste residue and the yellow soda ash first coal gangue carried behind the aluminium mix by the mol ratio 1:0.3 of silicon-dioxide in the waste residue and yellow soda ash ~ 1, grind to form the particle of 1 ~ 50 μ m, then be warming up to 500 ~ 850 ℃ of roastings 1 ~ 5 hour at the retort furnace Program, be transferred to rapidly and carry out shrend in the boiling water, obtain thick water glass solid; Above-mentioned thick water glass solid is placed autoclave, add and be equivalent to waste residue weight 400-600 distilled water doubly, stir, be warming up to 150 ℃, dissolve after 5 hours, cool the temperature to room temperature, filtering separation obtains water white sodium silicate solution and filter residue; To obtain soluble glass after the sodium silicate solution crystallization.
A kind of coal gangue that utilizes provided by the invention is put forward the method that waste slag of aluminum prepares soluble glass, step comprises: first coal gangue is carried waste residue and yellow soda ash behind the aluminium, sodium-chlor and mixed by the mol ratio 1:0.3 of silicon-dioxide in the waste residue and yellow soda ash, sodium-chlor ~ 1:0.005 ~ 0.05, grind to form the particle of 1 ~ 50 μ m, then be warming up to 500 ~ 850 ℃ of roastings 1 ~ 5 hour at the retort furnace Program, be transferred to rapidly and carry out shrend in the boiling water, obtain thick water glass solid; Above-mentioned thick water glass solid is placed autoclave, add and be equivalent to waste residue weight 400-600 distilled water doubly, stir, be warming up to 150 ℃, dissolve after 5 hours, cool the temperature to room temperature, filtering separation obtains water white sodium silicate solution and filter residue; To obtain soluble glass after the sodium silicate solution crystallization.
The carbonic acid gas that produces during above roasting can prepare white carbon black by purifying to reclaim for carborization.Undissolved micro-filter residue can be used for the non-burning brick preparation of high strength coal gangue after the roasting.
Described coal gangue is carried waste slag of aluminum can propose the waste slag of aluminum replacement with flyash, kaolin or bauxitic clay.
Described yellow soda ash can replace with salt of wormwood, and described sodium-chlor can replace with Repone K or Sodium Fluoride.
Compared with prior art advantage of the present invention and effect: the utilization of the present invention principle that balances each other, the control coal gangue is put forward proportioning and the granularity of waste slag of aluminum and yellow soda ash (or salt of wormwood), (500 ~ 850 ℃) generation frit reaction under eutectic temperature after the two is evenly mixed, form soluble glass, more than the silicon extraction rate reached to 90%.The temperature that the method not only prepares traditional Method of Soda water glass has reduced about 600 ℃, has greatly reduced energy consumption, has also avoided simultaneously traditional caustic soda alkali solution technique to the deep-etching of production unit and alkali pollution that environment is produced.In addition, the carbon dioxide that roasting produces can be recycled, and undissolved micro-residue can be used for the non-burning brick preparation of high strength coal gangue after the roasting, and whole technique is in the closed cycle, is that a kind of eco-friendly waste residue efficiently utilizes scheme.
Description of drawings
Thermogravimetric differential thermal check analysis under Fig. 1 and the embodiment 1 same process condition is figure as a result
Thermogravimetric differential thermal check analysis under Fig. 2 and the embodiment 2 same process conditions is figure as a result
Thermogravimetric differential thermal check analysis under Fig. 3 and the embodiment 3 same process conditions is figure as a result
Thermogravimetric differential thermal check analysis under Fig. 4 and the embodiment 4 same process conditions is figure as a result
The dissolving crystallized solid of product of Fig. 5 embodiment 1 and 4 preparations and the infrared spectra comparison diagram of filter residue,
Among the figure: a. represents the IR spectra of PVDC of embodiment 1 dissolving filter residue, b. the IR spectra of PVDC that represents embodiment 1 lysate crystalline solid product, c. represent the IR spectra of PVDC of embodiment 4 dissolving filter residues, d. represents the IR spectra of PVDC of embodiment 4 lysate crystalline solid products
Embodiment
Raw material is prepared:
Carry waste residue (white residue) behind the aluminium by coal gangue, be dried to constant weight (each component concentration sees attached list 1) for subsequent use.
The analysis of components table of table 1 raw material waste residue
Taking by weighing the 100g white residue and become particle about 5 μ m with yellow soda ash 110g mixed grinding in ball mill, place the retort furnace Program to heat up, is 10 ℃/min between temperature rise rate: 0-500 ℃; 500-850 ℃ is 2 ℃/min; 850 ℃ of constant temperature stopped after 3 hours, placed rapidly boiling water to carry out shrend, obtained thick water glass solid.Above-mentioned thick water glass solid is placed 1 liter autoclave, add 500 ml distilled waters, be warming up to 150 ℃, after the stirring and dissolving 5 hours, cool the temperature to room temperature, filtering separation, obtain water white sodium silicate solution and filter residue, the sodium silicate solution evaporative crystallization is got the water glass product.Adopt ICP respectively to sodium silicate solution, filter residue and its silicone content of water glass products measure and foreign matter content (table 2).The results of IR of thermogravimetric differential thermal check analysis result such as Fig. 1, filter residue such as Fig. 5 (a) under the same process condition, the results of IR of sample such as Fig. 5 (b) after the sodium silicate solution crystallization, the water glass dissolution rate is 92.4%.
Table 2 product analysis of components table
From Fig. 1 differential thermal analysis as can be known, mixture begins to occur solid-solid reaction at about 500 ℃, discharges carbon dioxide, occurs obviously weightlessness among the figure, illustrates that also not reaching eutectic point just begins to react.To about 800 ℃ no longer weightless, but found out that by the endotherm(ic)peak of DSC curve among the figure frit reaction is still being carried out, 812 ℃ of melt temperatures; A, b line can be found out from Fig. 5, almost all be present in the filter residue through the impurity after reaction, shrend, the separated and dissolved, resulting sodium silicate solution and the purity of the sodium silicate solid product behind the sodium silicate solution condensing crystal reached 99.7%, product dissolves the infrared spectra of post crystallization water glass solid, has the characteristic peak of water glass.In the infrared spectrogram of filter residue, 1020cm
-1The peak at place can belong to the Si-O-Al key, and the impurity aluminum in the filter residue mainly is at high temperature to have formed the water-fast mixtures such as sodium silicoaluminate and titanium sodium aluminate with silicon, titanium.
Take by weighing 100g white residue and yellow soda ash 70g mixed grinding, all the other conditions adopt ICP that sodium silicate solution and filter residue (alkali solution technique) philosophy are measured its silicone content and foreign matter content (table 3) with embodiment 1.The thermogravimetric differential thermal analysis result who contrasts under the same process condition such as Fig. 2, water glass dissolution rate are 90.0%.
Table 3 product analysis of components table
From differential thermal analysis (see figure 2) as can be known, the thermogravimetric analysis result is with embodiment 1, and the DSC curve can obtain 805 ℃ of melt temperatures.
Take by weighing 100g white residue and yellow soda ash 164g mixed grinding, all the other conditions are with embodiment 1.Adopt ICP that sodium silicate solution and filter residue (alkali solution technique) philosophy are measured its silicone content and foreign matter content (table 3).The thermogravimetric differential thermal analysis result who contrasts under the same process condition such as Fig. 3, water glass dissolution rate are 90.2%.
From differential thermal analysis (see figure 3) as can be known, the thermogravimetric analysis result is with embodiment 1, and the DSC curve can obtain 829 ℃ of melt temperatures.
Embodiment 4
Taking by weighing the 100g white residue and become particle about 5 μ m with yellow soda ash 110g sodium-chlor 1g mixed grinding, set the retort furnace Program and heat up, is 10 ℃/min between temperature rise rate: 0-500 ℃; 500-850 ℃ is 2 ℃/min; 850 ℃ of constant temperature stopped after 3 hours, placed rapidly boiling water to carry out shrend, obtained thick water glass solid.Above-mentioned thick water glass solid is placed 1 liter autoclave, add 500 ml distilled waters, be warming up to 150 ℃, stirring and dissolving cooled the temperature to room temperature after 5 hours, and filtering separation obtains water white sodium silicate solution and filter residue.C line among the results of IR of the thermogravimetric differential thermal analysis result who contrasts under the same process condition such as Fig. 4, filter residue such as Fig. 5, the results of IR of sample such as the d line among Fig. 5 after the sodium silicate solution crystallization, the water glass dissolution rate is 89.5%.
From the differential thermal analysis of Fig. 4 as can be known, the thermogravimetric analysis result is with embodiment 1, and the DSC curve can obtain 780 ℃ of melt temperatures, and melt temperature is reduced to 780 ℃ by 812 ℃ behind the adding assistant NaCl.
Comparing embodiment
Get the mixture (take by weighing the 100g white residue and become particle about 5 μ m with yellow soda ash 100g mixed grinding) of identical proportioning with embodiment 1, change heating schedule in its retort furnace, setting program heats up, and is 10 ℃/min between temperature rise rate: 0-500 ℃; 500-850 ℃ is 5 ℃/min; 850-1400 ℃ is 2 ℃/min, and 1400 ℃ of constant temperature stopped after 3 hours, and the water glass dissolution rate is 54.6%.
Through relatively finding out, frit reaction formation soluble glass occurs in (500 ~ 850 ℃) under eutectic temperature, and the water glass dissolution rate reaches more than 90%.Frit reaction occurs in (1100 ~ 1400 ℃) under the high temperature eutectic temperature, forms soluble glass, and the water glass dissolution rate is only more than 54.6%.The temperature that the method not only prepares traditional Method of Soda water glass has reduced about 600 ℃, has greatly reduced energy consumption, has also avoided simultaneously traditional caustic soda alkali solution technique to the deep-etching of production unit and alkali pollution that environment is produced.That a kind of eco-friendly waste residue efficiently utilizes method.
Claims (5)
1. one kind is utilized coal gangue to put forward the method that waste slag of aluminum prepares soluble glass, it is characterized in that, step comprises: waste residue and the yellow soda ash first coal gangue carried behind the aluminium mix by the mol ratio 1:0.3 of silicon-dioxide in the waste residue and yellow soda ash ~ 1, grind to form the particle of 1 ~ 50 μ m, then be warming up to 500 ~ 850 ℃ of roastings 1 ~ 5 hour at the retort furnace Program, be transferred to rapidly and carry out shrend in the boiling water, obtain thick water glass solid; Above-mentioned thick water glass solid is placed autoclave, add distilled water and stir, be warming up to 150 ℃, dissolve after 5 hours, cool the temperature to room temperature, filtering separation will obtain soluble glass after the sodium silicate solution crystallization.
2. one kind is utilized coal gangue to put forward the method that waste slag of aluminum prepares soluble glass, it is characterized in that, step comprises: first coal gangue is carried waste residue and yellow soda ash behind the aluminium, sodium-chlor and mixed by the mol ratio 1:0.3 of silicon-dioxide in the waste residue and yellow soda ash, sodium-chlor ~ 1:0.005 ~ 0.05, grind to form the particle of 1 ~ 50 μ m, then be warming up to 500 ~ 850 ℃ of roastings 1 ~ 5 hour at the retort furnace Program, be transferred to rapidly and carry out shrend in the boiling water, obtain thick water glass solid; Above-mentioned thick water glass solid is placed autoclave, add distilled water and stir, be warming up to 150 ℃, dissolve after 5 hours, cool the temperature to room temperature, filtering separation will obtain soluble glass after the sodium silicate solution crystallization.
3. a kind of coal gangue that utilizes as claimed in claim 1 or 2 is put forward the method that waste slag of aluminum prepares soluble glass, it is characterized in that described coal gangue replaces with flyash, kaolin or bauxitic clay.
4. a kind of coal gangue that utilizes as claimed in claim 1 or 2 is put forward the method that waste slag of aluminum prepares soluble glass, it is characterized in that described yellow soda ash replaces with salt of wormwood.
5. a kind of coal gangue that utilizes as claimed in claim 1 or 2 is put forward the method that waste slag of aluminum prepares soluble glass, it is characterized in that described sodium-chlor replaces with Repone K or Sodium Fluoride.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420386A (en) * | 2013-08-05 | 2013-12-04 | 山西大学 | Method for preparing silica through coal gangue aluminum extraction waste slag |
| CN104477928A (en) * | 2014-12-03 | 2015-04-01 | 宋英宏 | Method for extracting sodium silicate from coal ashes |
| CN106082245A (en) * | 2016-06-01 | 2016-11-09 | 望江县金峰矿产品科技有限公司 | A kind of method that slag is prepared nanometer grade silica |
| CN106829983A (en) * | 2017-03-31 | 2017-06-13 | 瓮福（集团）有限责任公司 | A kind of preparation method of sodium metasilicate |
| CN107416852A (en) * | 2017-05-25 | 2017-12-01 | 肖飞 | A kind of method that gangue prepares sodium silicate |
| CN107416851A (en) * | 2017-05-25 | 2017-12-01 | 肖飞 | A kind of technique for preparing sodium silicate using flyash wet method |
| CN109183194A (en) * | 2018-07-18 | 2019-01-11 | 山西载驰科技有限公司 | A method of by the high-purity alumina silicate fibre of gangue large scale preparation |
| CN110937608A (en) * | 2019-12-30 | 2020-03-31 | 安徽龙泉硅材料有限公司 | Preparation method of high-quality sodium silicate for silicon dioxide |
| CN111422878A (en) * | 2020-04-20 | 2020-07-17 | 武汉工程大学 | Method for treating silico-calcium collophanite |
| CN111592005A (en) * | 2020-05-08 | 2020-08-28 | 山西大学 | Method for preparing alpha-layered sodium silicate at low temperature from coal powder furnace fly ash acid method aluminum extraction tailings |
| CN111646472A (en) * | 2020-05-22 | 2020-09-11 | 兰州理工大学 | Method for in-situ preparation of porous silicon-carbon composite negative electrode material |
| CN111747422A (en) * | 2020-06-22 | 2020-10-09 | 安徽龙泉硅材料有限公司 | Preparation method of ultrapure sodium silicate for silicon dioxide |
| CN111747423A (en) * | 2020-06-22 | 2020-10-09 | 安徽龙泉硅材料有限公司 | Preparation method of ultrapure sodium silicate |
| CN114212797A (en) * | 2021-12-03 | 2022-03-22 | 内蒙古科技大学 | Method for extracting liquid silica gel from coal gangue |
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| CN101296865A (en) * | 2005-11-10 | 2008-10-29 | 科学与工业研究委员会 | Process for the preparation of sodium silicate from kimberlite tailing |
| CN102337397A (en) * | 2011-10-28 | 2012-02-01 | 中南大学 | High-efficient separation and extraction process of silicon and vanadium in stone coal |
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| CN101296865A (en) * | 2005-11-10 | 2008-10-29 | 科学与工业研究委员会 | Process for the preparation of sodium silicate from kimberlite tailing |
| CN102337397A (en) * | 2011-10-28 | 2012-02-01 | 中南大学 | High-efficient separation and extraction process of silicon and vanadium in stone coal |
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420386A (en) * | 2013-08-05 | 2013-12-04 | 山西大学 | Method for preparing silica through coal gangue aluminum extraction waste slag |
| CN104477928A (en) * | 2014-12-03 | 2015-04-01 | 宋英宏 | Method for extracting sodium silicate from coal ashes |
| CN106082245A (en) * | 2016-06-01 | 2016-11-09 | 望江县金峰矿产品科技有限公司 | A kind of method that slag is prepared nanometer grade silica |
| CN106829983A (en) * | 2017-03-31 | 2017-06-13 | 瓮福（集团）有限责任公司 | A kind of preparation method of sodium metasilicate |
| CN106829983B (en) * | 2017-03-31 | 2020-03-27 | 瓮福（集团）有限责任公司 | Preparation method of sodium silicate |
| CN107416851B (en) * | 2017-05-25 | 2020-11-17 | 阜阳市逸浩专利技术服务有限公司 | Process for preparing sodium silicate by using fly ash wet method |
| CN107416852A (en) * | 2017-05-25 | 2017-12-01 | 肖飞 | A kind of method that gangue prepares sodium silicate |
| CN107416851A (en) * | 2017-05-25 | 2017-12-01 | 肖飞 | A kind of technique for preparing sodium silicate using flyash wet method |
| CN107416852B (en) * | 2017-05-25 | 2020-11-17 | 阜阳市逸浩专利技术服务有限公司 | Method for preparing sodium silicate from coal gangue |
| CN109183194A (en) * | 2018-07-18 | 2019-01-11 | 山西载驰科技有限公司 | A method of by the high-purity alumina silicate fibre of gangue large scale preparation |
| CN110937608A (en) * | 2019-12-30 | 2020-03-31 | 安徽龙泉硅材料有限公司 | Preparation method of high-quality sodium silicate for silicon dioxide |
| CN111422878A (en) * | 2020-04-20 | 2020-07-17 | 武汉工程大学 | Method for treating silico-calcium collophanite |
| CN111422878B (en) * | 2020-04-20 | 2023-03-07 | 武汉工程大学 | Method for treating silico-calcium collophanite |
| CN111592005A (en) * | 2020-05-08 | 2020-08-28 | 山西大学 | Method for preparing alpha-layered sodium silicate at low temperature from coal powder furnace fly ash acid method aluminum extraction tailings |
| CN111592005B (en) * | 2020-05-08 | 2023-07-18 | 山西大学 | Method for preparing alpha-layered sodium silicate at low temperature from coal powder furnace fly ash acid-process aluminum extraction tailings |
| CN111646472A (en) * | 2020-05-22 | 2020-09-11 | 兰州理工大学 | Method for in-situ preparation of porous silicon-carbon composite negative electrode material |
| CN111747422A (en) * | 2020-06-22 | 2020-10-09 | 安徽龙泉硅材料有限公司 | Preparation method of ultrapure sodium silicate for silicon dioxide |
| CN111747423A (en) * | 2020-06-22 | 2020-10-09 | 安徽龙泉硅材料有限公司 | Preparation method of ultrapure sodium silicate |
| CN114212797A (en) * | 2021-12-03 | 2022-03-22 | 内蒙古科技大学 | Method for extracting liquid silica gel from coal gangue |
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