CN102936016B - 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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- CN102936016B CN102936016B CN201210452429.5A CN201210452429A CN102936016B CN 102936016 B CN102936016 B CN 102936016B CN 201210452429 A CN201210452429 A CN 201210452429A CN 102936016 B CN102936016 B CN 102936016B
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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 is prepared soluble glass.
Background technology
Taking coal gangue, kaolin or flyash etc. when raw material is prepared polymerize aluminum chloride or Tai-Ace S 150, can produce a large amount of waste residues, in waste residue, contain a large amount of silicon-dioxide, 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 and mainly contains 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 industrial main method of preparing water glass (water glass) is 1100-1450 DEG C of melting in High Temperature Furnaces Heating Apparatus by quartz sand and sodium carbonate (or salt of wormwood), then the water glass fragment obtaining is water-soluble under 100 DEG C of normal pressures, or in autoclave sterilizer 150 DEG C water-soluble.Also can adopt hydrothermal method, under the pressure of 200 DEG C and 20bar in autoclave sterilizer melting sand and sodium hydroxide or potassium hydroxide, directly make aqueous silicate solution.The people such as Yi Ding, in the time utilizing water glass to prepare mesoporous silicon oxide SBA-15 nanometer rod, adopt silica powder (350 order) and sodium carbonate mixture to obtain sodium silicate solid in 1450 DEG C of frit reactions, the then water-soluble sodium silicate solution that obtains in autoclave.
In a kind of white carbon black preparation method that patent 200610016584.7 is reported, the preparation of water glass is with silicon dioxide powder and sodium bicarbonate 1:1 ~ 2 in molar ratio, under 1150-1650 DEG C of high temperature, calcines.Too high calcining temperature is not only high to equipment requirements, and energy consumption increases.
Summary of the invention
The object 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 is prepared water glass.
A kind of coal gangue that utilizes provided by the invention is put forward the method that waste slag of aluminum is prepared soluble glass, step comprises: the waste residue of first coal gangue being carried after aluminium mixes with mol ratio 1:0.3 ~ 1 of sodium carbonate by silicon-dioxide in waste residue with sodium carbonate, grind to form the particle of 1 ~ 50 μ m, then be warming up to 500 ~ 850 DEG C of roastings 1 ~ 5 hour at retort furnace Program, be transferred to rapidly in boiling water and carry out shrend, obtain thick water glass solid; Above-mentioned thick water glass solid is placed in to autoclave, adds and be equivalent to waste residue weight 400-600 distilled water doubly, stir, be warming up to 150 DEG C, dissolve after 5 hours, cool the temperature to room temperature, filtering separation, obtains water white sodium silicate solution and filter residue; To after sodium silicate solution crystallization, obtain soluble glass.
A kind of coal gangue that utilizes provided by the invention is put forward the method that waste slag of aluminum is prepared soluble glass, step comprises: the waste residue of first coal gangue being carried after aluminium mixes with mol ratio 1:0.3 ~ 1:0.005 ~ 0.05 of sodium carbonate, sodium-chlor by silicon-dioxide in waste residue with sodium carbonate, sodium-chlor, grind to form the particle of 1 ~ 50 μ m, then be warming up to 500 ~ 850 DEG C of roastings 1 ~ 5 hour at retort furnace Program, be transferred to rapidly in boiling water and carry out shrend, obtain thick water glass solid; Above-mentioned thick water glass solid is placed in to autoclave, adds and be equivalent to waste residue weight 400-600 distilled water doubly, stir, be warming up to 150 DEG C, dissolve after 5 hours, cool the temperature to room temperature, filtering separation, obtains water white sodium silicate solution and filter residue; To after sodium silicate solution crystallization, obtain soluble glass.
The carbonic acid gas producing when above roasting can be reclaimed for carborization and be prepared white carbon black by purification.After roasting, undissolved micro-filter residue can be used for the non-burning brick preparation of high strength coal gangue.
Described coal gangue is carried waste slag of aluminum can propose waste slag of aluminum replacement with flyash, kaolin or bauxitic clay.
Described sodium carbonate 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, control coal gangue and put forward proportioning and the granularity of waste slag of aluminum and sodium carbonate (or salt of wormwood), after the two is evenly mixed, there is frit reaction in (500 ~ 850 DEG C) under eutectic temperature, form soluble glass, more than silicon extraction rate reached to 90%.The temperature that the method is not only prepared traditional Method of Soda water glass has reduced by 600 DEG C of left and right, has greatly reduced energy consumption, has also avoided the deep-etching of traditional caustic soda alkali solution technique to production unit and the alkali pollution that environment is produced simultaneously.In addition, the carbon dioxide that roasting produces can be recycled, and after roasting, undissolved micro-residue can be used for the non-burning brick preparation of high strength coal gangue, and whole technique, in a closed cycle, is that a kind of eco-friendly waste residue efficiently utilizes scheme.
Brief description of the drawings
Thermogravimetric differential thermal check analysis result figure under Fig. 1 and embodiment 1 same process condition
Thermogravimetric differential thermal check analysis result figure under Fig. 2 and embodiment 2 same process conditions
Thermogravimetric differential thermal check analysis result figure under Fig. 3 and embodiment 3 same process conditions
Thermogravimetric differential thermal check analysis result figure under Fig. 4 and embodiment 4 same process conditions
The dissolving crystallized solid of product of Fig. 5 embodiment 1 and 4 preparations and the infrared spectra comparison diagram of filter residue,
In figure: a. represents that embodiment 1 dissolves the IR spectra of PVDC of filter residue, b. represent the IR spectra of PVDC of embodiment 1 lysate crystalline solid product, c. represent that embodiment 4 dissolves the IR spectra of PVDC of filter residue, d. represents the IR spectra of PVDC of embodiment 4 lysate crystalline solid products
Embodiment
Raw material is prepared:
Carry the waste residue (white residue) after 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 100g white residue becomes 5 μ m left and right particle with sodium carbonate 110g mixed grinding in ball mill, be placed in retort furnace Program and heat up, is 10 DEG C/min between temperature rise rate: 0-500 DEG C; 500-850 DEG C is 2 DEG C/min; 850 DEG C of constant temperature stopped after 3 hours, were placed in rapidly boiling water and carried out shrend, obtained thick water glass solid.Above-mentioned thick water glass solid is placed in to the autoclave of 1 liter, adds 500 ml distilled waters, be warming up to 150 DEG C, after stirring and dissolving 5 hours, cool the temperature to room temperature, filtering separation, obtain water white sodium silicate solution and filter residue, sodium silicate solution evaporative crystallization is obtained to 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).Under same process condition, thermogravimetric differential thermal check analysis result is if the results of IR of Fig. 1, filter residue is as Fig. 5 (a), and after sodium silicate solution crystallization, the results of IR of sample is as Fig. 5 (b), and water glass dissolution rate is 92.4%.
Table 2 product analysis of components table
From Fig. 1 differential thermal analysis, mixture starts to occur solid-solid reaction at about 500 DEG C, discharges carbon dioxide, occurs obviously weightlessness in figure, illustrates that also not reaching eutectic point just starts to react.No longer weightless to 800 DEG C of left and right, but found out by the endotherm(ic)peak of DSC curve in figure, and frit reaction is still being carried out, 812 DEG C of melt temperatures; From Fig. 5, a, b line can be found out, impurity after reaction, shrend, separated and dissolved is almost all present in filter residue, the sodium silicate solution obtaining and the purity of the sodium silicate solid product after sodium silicate solution condensing crystal is reached to 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 Si-O-Al key, and the impurity aluminum in filter residue is mainly at high temperature to have formed the water-fast mixture such as sodium silicoaluminate and titanium sodium aluminate with silicon, titanium.
Take 100g white residue and sodium carbonate 70g mixed grinding, all the other conditions, with embodiment 1, adopt ICP to measure its silicone content and foreign matter content (table 3) to sodium silicate solution and filter residue (alkali solution technique) philosophy.The thermogravimetric differential thermal analysis result contrasting under same process condition as Fig. 2, water glass dissolution rate be 90.0%.
Table 3 product analysis of components table
From the known (see figure 2) of differential thermal analysis, thermogravimetric analysis result is with embodiment 1, and DSC curve can obtain 805 DEG C of melt temperatures.
Take 100g white residue and sodium carbonate 164g mixed grinding, all the other conditions are with embodiment 1.Adopt ICP to measure its silicone content and foreign matter content (table 3) to sodium silicate solution and filter residue (alkali solution technique) philosophy.The thermogravimetric differential thermal analysis result contrasting under same process condition as Fig. 3, water glass dissolution rate be 90.2%.
From the known (see figure 3) of differential thermal analysis, thermogravimetric analysis result is with embodiment 1, and DSC curve can obtain 829 DEG C of melt temperatures.
Embodiment 4
Taking 100g white residue becomes 5 μ m left and right particle with sodium carbonate 110g sodium-chlor 1g mixed grinding, set retort furnace Program and heat up, is 10 DEG C/min between temperature rise rate: 0-500 DEG C; 500-850 DEG C is 2 DEG C/min; 850 DEG C of constant temperature stopped after 3 hours, were placed in rapidly boiling water and carried out shrend, obtained thick water glass solid.Above-mentioned thick water glass solid is placed in to the autoclave of 1 liter, adds 500 ml distilled waters, be warming up to 150 DEG C, stirring and dissolving, after 5 hours, cools the temperature to room temperature, and filtering separation obtains water white sodium silicate solution and filter residue.The thermogravimetric differential thermal analysis result contrasting under same process condition is if the results of IR of Fig. 4, filter residue is as c line in Fig. 5, and after sodium silicate solution crystallization, the results of IR of sample is as the d line in Fig. 5, and water glass dissolution rate is 89.5%.
From the differential thermal analysis of Fig. 4, thermogravimetric analysis result is with embodiment 1, and DSC curve can obtain 780 DEG C of melt temperatures, and after adding assistant NaCl, melt temperature is reduced to 780 DEG C by 812 DEG C.
Comparing embodiment
The mixture (take 100g white residue and become the particle about 5 μ m with sodium carbonate 100g mixed grinding) of getting identical proportioning with embodiment 1, changes heating schedule in its retort furnace, and setting program heats up, and between temperature rise rate: 0-500 DEG C, is 10 DEG C/min; 500-850 DEG C is 5 DEG C/min; 850-1400 DEG C is 2 DEG C/min, and 1400 DEG C of constant temperature stopped after 3 hours, and water glass dissolution rate is 54.6%.
Through relatively finding out, there is frit reaction formation soluble glass in (500 ~ 850 DEG C) under eutectic temperature, and water glass dissolution rate reaches more than 90%.There is frit reaction in (1100 ~ 1400 DEG C) under high temperature eutectic temperature, forms soluble glass, and water glass dissolution rate is only more than 54.6%.The temperature that the method is not only prepared traditional Method of Soda water glass has reduced by 600 DEG C of left and right, has greatly reduced energy consumption, has also avoided the deep-etching of traditional caustic soda alkali solution technique to production unit and the alkali pollution that environment is produced simultaneously.That a kind of eco-friendly waste residue efficiently utilizes method.
Claims (4)
1. one kind is utilized coal gangue to put forward the method that waste slag of aluminum is prepared soluble glass, it is characterized in that, step comprises: the waste residue of first coal gangue being carried after aluminium mixes with mol ratio 1:0.3～1 of sodium carbonate by silicon-dioxide in waste residue with sodium carbonate, grind to form the particle of 1～50 μ m, then be warming up to 500～850 DEG C of roastings 1～5 hour at retort furnace Program, be transferred to rapidly in boiling water and carry out shrend, obtain thick water glass solid; Above-mentioned thick water glass solid is placed in to autoclave, adds distilled water to stir, be warming up to 150 DEG C, dissolve after 5 hours, cool the temperature to room temperature, filtering separation, will obtain soluble glass after sodium silicate solution crystallization.
2. one kind is utilized coal gangue to put forward the method that waste slag of aluminum is prepared soluble glass, it is characterized in that, step comprises: the waste residue of first coal gangue being carried after aluminium mixes with mol ratio 1:0.3～1:0.005～0.05 of sodium carbonate, sodium-chlor by silicon-dioxide in waste residue with sodium carbonate, sodium-chlor, grind to form the particle of 1～50 μ m, then be warming up to 500～850 DEG C of roastings 1～5 hour at retort furnace Program, be transferred to rapidly in boiling water and carry out shrend, obtain thick water glass solid; Above-mentioned thick water glass solid is placed in to autoclave, adds distilled water to stir, be warming up to 150 DEG C, dissolve after 5 hours, cool the temperature to room temperature, filtering separation, will obtain soluble glass after 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 is prepared soluble glass, it is characterized in that described sodium carbonate salt of wormwood replaces.
4. a kind of coal gangue that utilizes as claimed in claim 2 is put forward the method that waste slag of aluminum is prepared soluble glass, it is characterized in that described sodium-chlor Repone K or Sodium Fluoride replace.
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| CN103420386A (en) * | 2013-08-05 | 2013-12-04 | 山西大学 | Method for preparing silica through coal gangue aluminum extraction waste slag |
| CN104477928B (en) * | 2014-12-03 | 2017-01-11 | 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 |
| 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 |
| 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 |
| CN109183194B (en) * | 2018-07-18 | 2020-08-28 | 山西载驰科技有限公司 | Method for preparing high-purity aluminum silicate fiber from coal gangue on large scale |
| CN110937608B (en) * | 2019-12-30 | 2020-11-03 | 安徽龙泉硅材料有限公司 | Preparation method of high-quality sodium silicate for silicon dioxide |
| CN111422878B (en) * | 2020-04-20 | 2023-03-07 | 武汉工程大学 | Method for treating silico-calcium collophanite |
| 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 |
| CN111747423B (en) * | 2020-06-22 | 2023-03-17 | 安徽龙泉硅材料有限公司 | Preparation method of ultrapure sodium silicate |
| CN111747422B (en) * | 2020-06-22 | 2023-07-28 | 安徽龙泉硅材料有限公司 | Preparation method of ultrapure sodium silicate for silicon dioxide |
| CN114212797B (en) * | 2021-12-03 | 2023-07-18 | 内蒙古科技大学 | Method for extracting liquid silica gel from coal gangue |
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| JPH09187750A (en) * | 1996-01-11 | 1997-07-22 | Kanegafuchi Chem Ind Co Ltd | Waste treating agent and waste treatment method |
| CN101296865B (en) * | 2005-11-10 | 2011-10-12 | 科学与工业研究委员会 | Process for the preparation of sodium silicate from kimberlite tailing |
| CN102337397B (en) * | 2011-10-28 | 2013-04-10 | 中南大学 | High-efficient separation and extraction process of silicon and vanadium in stone coal |
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