CN111592005B - Method for preparing alpha-layered sodium silicate at low temperature from coal powder furnace fly ash acid-process aluminum extraction tailings - Google Patents
Method for preparing alpha-layered sodium silicate at low temperature from coal powder furnace fly ash acid-process aluminum extraction tailings Download PDFInfo
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- CN111592005B CN111592005B CN202010381821.XA CN202010381821A CN111592005B CN 111592005 B CN111592005 B CN 111592005B CN 202010381821 A CN202010381821 A CN 202010381821A CN 111592005 B CN111592005 B CN 111592005B
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- C01B33/00—Silicon; Compounds thereof
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- C01B33/32—Alkali metal silicates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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Abstract
A method for preparing alpha-layered sodium silicate at low temperature by acid extraction of aluminum tailings from pulverized coal ash in a pulverized coal furnace belongs to the fields of recycling of industrial solid waste pulverized coal ash and synthesis of layered sodium silicate, and can solve the problems of high raw material cost, need of adding seed crystals, complex process and the like in the existing preparation method of alpha-layered sodium silicate, wherein the pulverized coal ash in the pulverized coal furnace is subjected to sodium carbonate activation, hydrochloric acid leaching, solid-liquid separation, and the solid is washed and dried to obtain the aluminum tailings. Dissolving the aluminum extraction tailings in sodium hydroxide under the ultrasonic action to obtain sodium silicate solution. Taking sodium silicate solution as raw material, heating to 650-740 ℃, roasting for 20-120min, and cooling to obtain alpha-layered sodium silicate product. The method provides a new application way for extracting aluminum tailings by the fly ash acid method, provides a low-cost and high-activity silicon source for the layered sodium silicate product, reduces the crystallization temperature of the alpha-layered sodium silicate, saves the cost and is beneficial to the mass production of the layered sodium silicate product.
Description
Technical Field
The invention belongs to the technical field of resource utilization of industrial solid waste fly ash and synthesis of layered sodium silicate, and particularly relates to a method for preparing alpha-layered sodium silicate at low temperature by acid-process aluminum extraction tailings of fly ash of a pulverized coal furnace.
Background
Fly ash is one of the bulk solid waste produced in coal-fired power plants, and about 1.8 hundred million tons per year are not utilized. The fly ash is rich in a plurality of metal elements such as main metal element aluminum, trace metal element lithium gallium and the like, and multi-element synergistic extraction is one of important ways for realizing high-value utilization of the fly ash. The coal powder furnace has high coal ash discharge amount, is ash slag produced by high-quality coal powder at the ash forming temperature of more than 1200 ℃, and mainly comprises mullite, quartz, corundum and the like which are difficult to activate. The leaching rate of aluminum reaches more than 90 percent by adopting a sodium carbonate activation-hydrochloric acid leaching process, and simultaneously, aluminum extraction tailings are produced as byproducts. In order to realize synchronous utilization of aluminum and silicon in the fly ash, secondary pollution caused by generation of silicon slag is avoided, and high-value utilization of silicon is an urgent need for improving economic, environmental and ecological benefits of the process.
The layered sodium silicate has various crystal forms such as alpha, beta, delta and the like, has the characteristics of large calcium-magnesium ion exchange capacity, strong buffering capacity and environmental friendliness, is used as a builder in a detergent to replace sodium tripolyphosphate, realizes the non-phosphating of the detergent, and has better performance than a non-phosphorus additive 4A zeolite molecular sieve. The application number is 200410012440.5, commercial liquid water glass is used as a silicon source and a sodium source, 3-30% of mixed seed crystal with the alpha phase content of more than 60% is added, and the alpha-layered sodium silicate can be obtained by calcining at a high temperature of 750-800 ℃. The application number is 201510033360.6, the rice hull ash is put into a sodium hydroxide solution for leaching, the leaching is needed for 1-6 hours, sodium hydroxide is added into the filtered filtrate to adjust the silicon-sodium ratio, the mixture is dried at 100-200 ℃, and the mixture is calcined at 760-820 ℃ to obtain the alpha-lamellar sodium silicate. The existing preparation method of the alpha-layered sodium silicate has the problems of high raw material cost, need of adding seed crystals, complex process and the like, and particularly has higher crystallization temperature.
In summary, the inventor takes the aluminum extraction tailings of pulverized coal furnace fly ash subjected to sodium carbonate activation-hydrochloric acid leaching as a raw material, and adopts rapid heating-low-temperature roasting to realize large-scale controllable synthesis of alpha-layered sodium silicate, which is not reported at home and abroad.
Disclosure of Invention
Aiming at the problems of high raw material cost, need of adding seed crystal, complex process and the like in the existing preparation method of the alpha-layered sodium silicate, the invention provides a method for preparing the alpha-layered sodium silicate at low temperature by using the coal ash acid-process aluminum extraction tailings of a coal dust furnace. The method has the advantages of low raw material price, simple process flow, low crystallization temperature, low energy consumption and low synthesis cost; the synthesized layered sodium silicate material has single crystal form and higher alpha phase content, and has wide application prospect in the field of detergents.
The invention adopts the following technical scheme:
the method for preparing alpha-layered sodium silicate at low temperature from the tailings of the acid extraction of aluminum from the pulverized coal ash of a pulverized coal furnace comprises the following steps:
firstly, extracting aluminum tailings: uniformly mixing pulverized coal ash and sodium carbonate in proportion, grinding to an average particle size of 50-100 mu m, roasting at 800-900 ℃ for 0.5-1.5 hours to obtain a roasting product, mixing the roasting product with 5-20wt.% hydrochloric acid in proportion, reacting at 60-100 ℃ for 0.5-1.5 hours, filtering and washing with water to be neutral after the reaction is finished to obtain aluminum extraction tailings;
secondly, preparing a sodium silicate solution: extracting aluminum tailings by SiO 2 Sodium hydroxide solution in terms of Na 2 O is calculated, the aluminum extraction tailings are dissolved in sodium hydroxide solution with the mass fraction of 4-20% under the ultrasonic action according to the proportion, and sodium silicate solution is obtained;
and thirdly, heating the sodium silicate solution to 650-740 ℃, and roasting for 20-120min to obtain an alpha-layered sodium silicate product.
In the first step, the mass ratio of the pulverized coal ash and the sodium carbonate in the pulverized coal furnace is 0.5-1.5:1.
The solid-liquid mass ratio of the roasting product to the hydrochloric acid in the first step is 1:3-1:10.
SiO as described in the second step 2 And Na (Na) 2 The molar ratio of O is 1.5-2.5:1.
And in the third step, the heating rate of the heating is 15-40 ℃/min.
The beneficial effects of the invention are as follows:
the invention adopts the fly ash acid method to extract the aluminum tailings to prepare the alpha-layered sodium silicate, thereby not only increasing the economic, environmental and social benefits of the fly ash acid method to extract the aluminum, but also obviously reducing the formation temperature of the alpha-layered sodium silicate, shortening the formation time, reducing the cost and obviously improving the economic value of the product.
Drawings
FIG. 1 is an XRD pattern of the fly ash acid-process aluminum extraction tailings of the present invention.
Figure 2 is an XRD pattern of alpha-layered sodium silicate prepared in example 1 of the present invention.
Figure 3 is an XRD pattern of alpha-layered sodium silicate prepared in example 2 of the present invention.
Detailed Description
Example 1
Mixing and grinding the fly ash and sodium carbonate according to the mass ratio of the fly ash to the sodium carbonate of the pulverized coal furnace of 1:0.8, and roasting for 1.5 hours at 850 ℃; the roasted product and 15wt percent are mixed according to the solid-liquid mass ratio of 1:5% hydrochloric acid is mixed and reacted for 1.5 hours at 90 ℃, and after the reaction is finished, the mixture is filtered and washed with water until the mixture is neutral, thus obtaining the aluminum extraction tailings. According to SiO 2 With Na and Na 2 The O molar ratio is 2.0, and the aluminum extraction tailings are dissolved in a sodium hydroxide solution with the mass fraction of 5% under the action of ultrasound for 5min to obtain a sodium silicate solution. And (3) roasting the sodium silicate solution at a speed of 20 ℃/min to 680 ℃ for 30min to obtain an alpha-layered sodium silicate product.
Example 2
Mixing and grinding the fly ash and sodium carbonate according to the mass ratio of the fly ash to the sodium carbonate of the pulverized coal furnace of 1:1.3, and roasting for 1.5 hours at 880 ℃; mixing the roasting product with 15wt.% hydrochloric acid according to the solid-liquid mass ratio of 1:7, reacting for 1.5 hours at 90 ℃, filtering after the reaction is finished, and washing with water until the mixture is neutral to obtain the aluminum extraction tailings. According to SiO 2 With Na and Na 2 The O molar ratio is 2.1, and the aluminum extraction tailings are dissolved in a sodium hydroxide solution with the mass fraction of 5% under the action of ultrasound for 10min to obtain a sodium silicate solution. And (3) roasting the sodium silicate solution at a speed of 25 ℃/min to 680 ℃ for 120min to obtain an alpha-layered sodium silicate product.
Claims (1)
1. A method for preparing alpha-layered sodium silicate at low temperature from aluminum tailings extracted by a pulverized coal furnace fly ash acid method is characterized by comprising the following steps: the method comprises the following steps:
mixing and grinding the fly ash and sodium carbonate according to the mass ratio of the fly ash to the sodium carbonate of the pulverized coal furnace of 1:0.8, and roasting for 1.5 hours at 850 ℃; mixing the roasting product with 15wt.% hydrochloric acid according to the solid-liquid mass ratio of 1:5, reacting for 1.5 hours at 90 ℃, filtering after the reaction is finished, and washing with water until the mixture is neutral to obtain aluminum extraction tailings; according to SiO 2 With Na and Na 2 The O molar ratio is 2.0, and the aluminum extraction tailings are dissolved in a sodium hydroxide solution with the mass fraction of 5% under the action of ultrasound for 5min to obtain a sodium silicate solution; and (3) roasting the sodium silicate solution at a speed of 20 ℃/min to 680 ℃ for 30min to obtain an alpha-layered sodium silicate product.
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| CN102936016A (en) * | 2012-11-12 | 2013-02-20 | 山西大学 | Method for preparing soluble glass by using waste residues with aluminum extracted by coal gangue |
| US20130343971A1 (en) * | 2011-05-11 | 2013-12-26 | Inner Mongolia Datang International Recycling Resource Development Co., Ltd. | Method for co-producing alumina and activated calcium silicate from high-alumina fly ash |
| CN104591197A (en) * | 2015-01-23 | 2015-05-06 | 成都理工大学 | Method for preparing high-purity alpha-layered sodium silicate by using rice husk ash |
| CN109384254A (en) * | 2018-07-24 | 2019-02-26 | 山西大学 | The method that crystal aluminum chloride and white carbon black are prepared by flyash or gangue |
| CN109502595A (en) * | 2018-11-22 | 2019-03-22 | 山西大学 | A method of using coal ash for manufacturing for lamina sodium silicate |
| CN109824268A (en) * | 2019-02-25 | 2019-05-31 | 常州市蓝勖化工有限公司 | A kind of preparation method of interface cohesion type high-strength devitrified glass glaze material |
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| US20130343971A1 (en) * | 2011-05-11 | 2013-12-26 | Inner Mongolia Datang International Recycling Resource Development Co., Ltd. | Method for co-producing alumina and activated calcium silicate from high-alumina fly ash |
| CN102936016A (en) * | 2012-11-12 | 2013-02-20 | 山西大学 | Method for preparing soluble glass by using waste residues with aluminum extracted by coal gangue |
| CN104591197A (en) * | 2015-01-23 | 2015-05-06 | 成都理工大学 | Method for preparing high-purity alpha-layered sodium silicate by using rice husk ash |
| CN109384254A (en) * | 2018-07-24 | 2019-02-26 | 山西大学 | The method that crystal aluminum chloride and white carbon black are prepared by flyash or gangue |
| CN109502595A (en) * | 2018-11-22 | 2019-03-22 | 山西大学 | A method of using coal ash for manufacturing for lamina sodium silicate |
| CN109824268A (en) * | 2019-02-25 | 2019-05-31 | 常州市蓝勖化工有限公司 | A kind of preparation method of interface cohesion type high-strength devitrified glass glaze material |
Non-Patent Citations (1)
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| 粉煤灰提铝渣制备δ-层状硅酸钠及其性能研究;张丽宏 等;《无机盐工业》;20181231;第50卷(第12期);第55页第1.1、1.2节，第55-57页第2.1节、第2.2节、第2.3节、表2-4和第58-59页第3节结论部分 * |
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