CN101591023A - A kind of method of utilizing aluminous fly-ash to prepare calcium silicate micro power - Google Patents
A kind of method of utilizing aluminous fly-ash to prepare calcium silicate micro power Download PDFInfo
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- CN101591023A CN101591023A CNA2008101126181A CN200810112618A CN101591023A CN 101591023 A CN101591023 A CN 101591023A CN A2008101126181 A CNA2008101126181 A CN A2008101126181A CN 200810112618 A CN200810112618 A CN 200810112618A CN 101591023 A CN101591023 A CN 101591023A
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- micro power
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- lime
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Abstract
A kind of method of utilizing aluminous fly-ash to prepare calcium silicate micro power relates to material, chemical technology field.Method steps of the present invention is: 1. add exsiccant raw material aluminous fly-ash and stir in sodium hydroxide solution desilication reaction takes place; 2. the mixture behind the desilication reaction is carried out filtering separation, and filter cake washed obtain desiliconization solution and desiliconization flyash, unslaked lime adds water and stirs and obtain pulpous state milk of lime; 3. milk of lime is joined in the desiliconization solution stirring reaction and filtration washing and obtain moisture Calucium Silicate powder and NaOH solution, moisture Calucium Silicate powder oven dry makes calcium silicate micro power, can return step after the NaOH solution concentration and 1. recycle.Compare with prior art, less investment of the present invention, production cost is low, energy consumption is low, simple to operate, and the calcium silicate micro power physical and chemical performance homogeneous that makes, foreign matter content is low, whiteness is high.
Description
Technical field
The present invention relates to material, chemical technology field, particularly prepare the method for calcium silicate micro power with aluminous fly-ash.
Background technology
Calucium Silicate powder, it is Powdered to be white in color, and its chemical formula is CaSiO
3The calcium silicate micro power that foreign matter content is lower has excellent dielectric properties and higher heat resistance, thereby is widely used in pottery, chemical industry, metallurgy, building, machinery, electronics, papermaking, automobile, departments such as agricultural.
In the prior art, " preparation method of degradeable bioactive porous active calcium silicate ceramic material " of Chinese invention patent CN1569736, the core technology of this invention adopts wet chemical method to prepare β-calcium silicate micro power exactly.Concrete steps are: described β-calcium silicate micro power chemical process preparation process is with analytical pure Ca (NO
3)
24H
2O, Na
2SiO
39H
2O, ammoniacal liquor and deionized water are raw material; Be mixed with the Ca (NO of 1.0mol/l
3)
2And Na
2SiO
3The aqueous solution is with Na
2SiO
3Solution joins Ca (NO
3)
2In the solution with etc. the mol ratio material reaction, finish the back continue to stir 8～24 hours, filter and remove residual Na with deionized water and dehydrated alcohol thorough washing
+, oven dry is sieved the back in 800～1000 ℃ of calcinings 1-3 hour, prepares β-calcium silicate micro power.Adopt the calcium silicate micro power chemically reactive of this method preparation stronger, but raw material is relatively costly, the technological process reaction times is long, and energy consumption is higher, so cost of manufacture is higher, is difficult to carry out the popularization of scale operation." artificial tabular spar and the method for making thereof " of Chinese invention patent CN1301677, this technology then drops in stove through pulverizing, mixing raw materials such as natural shape wollastonite, silica, calcite, feldspar, fluorite, heat with combustion gas, fire at 1000～1600 ℃, with naturally cooling or water quenching cooling, form then through grinding.The advantage of the Calucium Silicate powder of this technology manufacturing is to adopt natural crystal as raw material, raw materials cost is relatively low, but material composition is comparatively complicated, the too high performance that will influence wollastonite micro mist (identical) of foreign matter content such as Fe, Na in the raw material with the main component of calcium silicate micro power, and the technology that adopts of this invention also will fire through 1000～1600 ℃, and same energy consumption is higher." method of modifying of wollastonite powder " of Chinese invention patent CN1095732 belongs to a kind of wollastonite powder carried out surface treatment, to replace the method for titanium dioxide, zinc sulfide white in the coating.This technology is mixed high-speed stirring with 100 parts wollastonite powder and 1～3 part dibutyl phthalate, forms a coating layer on the wollastonite powder surface.The raw material of this invention is natural wollastonite equally, and raw materials cost is comparatively cheap, but technological process will consume the comparatively expensive organism of a certain amount of price, is unfavorable for the extensive Industry Promotion of this technology equally.
Summary of the invention
At above-mentioned the deficiencies in the prior art, the purpose of this invention is to provide a kind of method of utilizing aluminous fly-ash to prepare calcium silicate micro power.Its less investment, production cost is low, energy consumption is low, simple to operate, and the calcium silicate micro power physical and chemical performance homogeneous that makes, foreign matter content is low, whiteness is high.
In order to reach the foregoing invention purpose, technical scheme of the present invention realizes as follows:
A kind of method of utilizing aluminous fly-ash to prepare calcium silicate micro power the steps include:
1. in sodium hydroxide solution, add exsiccant raw material aluminous fly-ash and stir desilication reaction takes place;
2. the mixture behind the desilication reaction is carried out filtering separation, and filter cake washed obtain desiliconization solution and desiliconization flyash, unslaked lime adds water and stirs and obtain pulpous state milk of lime;
3. milk of lime is joined in the desiliconization solution stirring reaction and filtration washing and obtain moisture Calucium Silicate powder and NaOH solution, moisture Calucium Silicate powder oven dry makes calcium silicate micro power, can return step after the NaOH solution concentration and 1. recycle.
In aforesaid method, SiO in the described aluminous fly-ash
2Content 〉=35%, Al
2O
3〉=40%, the middle mutually SiO of amorphous glass
2/ Al
2O
3Mass ratio 〉=4.
In aforesaid method, the concentration of described sodium hydroxide solution is 15～20%.
In aforesaid method, the mass ratio of described sodium hydroxide solution and flyash is 0.4～0.6: between 1.
In aforesaid method, the desilication reaction temperature of described sodium hydroxide solution and aluminous fly-ash is 100 ℃～130 ℃, and the desilication reaction time is 1～3 hour.
In aforesaid method, the mass ratio of unslaked lime CaO and water is 1: 3～4 during described preparing lime milk, SiO in CaO and the desiliconization solution in the milk of lime
2Mol ratio be 0.8～1.1: 1.
In aforesaid method, the stirring reaction temperature of described desiliconization solution and milk of lime is 90～110 ℃, and the reaction times is 0.5～1.5 hour.
In aforesaid method, the bake out temperature of described moisture Calucium Silicate powder is 200～400 ℃, and drying time is 0.5～2 hour.
In aforesaid method, the rate of recovery of described sodium hydroxide solution surpasses 95%, and the concentration of sodium hydroxide solution of recovery is 10～15%.
Compared with the prior art, the invention has the advantages that:
(1) the present invention can prepare the high-quality calcium silicate micro power by the raw material powder coal ash and the unslaked lime of cheapness, compare with calcium silicate micro powers that method obtained such as passing through surface activation process by natural wollastonite, calcium silicate micro power whiteness height with this prepared, thin and the even particle size distribution of particle, the chemical composition stability homogeneous, foreign matter contents such as Na, Fe are low.The Industry Promotion of this technology will be for becoming possibility with a large amount of high-quality calcium silicate micro power of aluminous fly-ash production.
(2) the flyash alumina silica ratio significantly improves after the desiliconization, can be used as the system aluminum feedstock, realizes the changing waste into resources utilization.China's high-quality bauxite resource lacks, and the type aluminous fly-ash is huge in the geographic thermal power plant of NORTHWEST CHINA output.Therefore the industrialization of this technology both can solve these power plant because the problem of environmental pollution that flyash caused can be alleviated China's bauxite resource supply crisis again to a certain extent.
(3) used sodium hydroxide can be recycled above 95%, can reduce the preparation cost of high-quality calcium silicate micro power greatly.
(4) equipment that this technology adopted is simple, and is workable, and three-waste free discharge in the whole process of production, and the energy consumption material consumption is lower, meets the circular economy policy of country.
Description of drawings
Accompanying drawing is technological process of production figure of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
Referring to accompanying drawing, production stage of the present invention is:
1. select for use and contain Al
2O
342.5%, SiO
246.7% aluminous fly-ash is as main raw material.According to sodium hydroxide and aluminous fly-ash mass ratio is 0.5: 1 proportioning, the weighing sodium hydroxide solid.It is used water dissolution, and constantly stir, prevent that sodium hydrate solid from condensing, be mixed with concentration and be 15% sodium hydroxide solution.Aluminous fly-ash is added in the prepared sodium hydroxide solution.The sodium hydroxide solution that is dissolved with aluminous fly-ash is carried out desilication reaction under 120 ℃ condition, the desilication reaction time is 2 hours, constantly stirs in desiliconization process, prevents regional area flyash generation agglomeration.
2. after desilication reaction finishes, by the vacuum filtration machine the formed slip system of desiliconization is carried out filtering separation, and filter cake is washed, the filtrate that obtains is desiliconization solution, and filter cake desiliconization flyash is the system aluminum feedstock that alumina silica ratio is significantly improved.According to SiO in CaO in the unslaked lime and the desiliconization solution
2Mol ratio CaO/SiO
2=1.0 take by weighing an amount of unslaked lime, add water at 3.3: 1 with water/unslaked lime mass ratio, stir 30 minutes, are prepared into milk of lime.
3. the milk of lime for preparing is joined in the desiliconization solution, 90 ℃ of following stirring reactions 60 minutes, stir speed (S.S.) was about 120r/min, and the reaction back that finishes is filtered and washed on the vacuum filtration machine, and the filter cake that filters gained is moisture Calucium Silicate powder.Moisture Calucium Silicate powder is calcium silicate micro power behind the oven dry 1h down at 350 ℃.Filtrate filtered is sodium hydroxide solution, additional a little NaOH after its appropriate evaporation concentration is returned step 1. be used for handling the next batch aluminous fly-ash.
The performance of the calcium silicate micro power product that employing the inventive method makes is as follows: CaO and SiO
2Mol ratio between 0.8 to 1.0, Na
2O content＜0.4%, Fe
2O
3＜0.08%, CaO+SiO
2＞96%, calcium silicate micro power 350 mesh sieve surplus＜10%, whiteness＞95%.
Claims (9)
1, a kind of method of utilizing aluminous fly-ash to prepare calcium silicate micro power the steps include:
1. in sodium hydroxide solution, add exsiccant raw material aluminous fly-ash and stir desilication reaction takes place;
2. the mixture behind the desilication reaction is carried out filtering separation, and filter cake washed obtain desiliconization solution and desiliconization flyash, unslaked lime adds water and stirs and obtain pulpous state milk of lime;
3. milk of lime is joined in the desiliconization solution stirring reaction and filtration washing and obtain moisture Calucium Silicate powder and NaOH solution, moisture Calucium Silicate powder oven dry makes calcium silicate micro power, can return step after the NaOH solution concentration and 1. recycle.
2, according to the described method of utilizing aluminous fly-ash to prepare calcium silicate micro power of claim 1, it is characterized in that SiO in the described aluminous fly-ash
2Content 〉=35%, Al
2O
3〉=40%, the middle mutually SiO of amorphous glass
2/ Al
2O
3Mass ratio 〉=4.
3, according to claim 1 or the 2 described methods of utilizing aluminous fly-ash to prepare calcium silicate micro power, it is characterized in that the concentration of described sodium hydroxide solution is 15～20%.
4, according to the described method of utilizing aluminous fly-ash to prepare calcium silicate micro power of claim 3, it is characterized in that the mass ratio of described sodium hydroxide solution and flyash is 0.4～0.6: between 1.
According to the described method of utilizing aluminous fly-ash to prepare calcium silicate micro power of claim 4, it is characterized in that 5, the desilication reaction temperature of described sodium hydroxide solution and aluminous fly-ash is 100 ℃～130 ℃, the desilication reaction time is 1～3 hour.
According to the described method of utilizing aluminous fly-ash to prepare calcium silicate micro power of claim 5, it is characterized in that 6, the mass ratio of unslaked lime CaO and water is 1: 3～4 during described preparing lime milk, SiO in CaO and the desiliconization solution in the milk of lime
2Mol ratio be 0.8～1.1: 1.
According to the described method of utilizing aluminous fly-ash to prepare calcium silicate micro power of claim 6, it is characterized in that 7, the stirring reaction temperature of described desiliconization solution and milk of lime is 90～110 ℃, the reaction times is 0.5～1.5 hour.
According to the described method of utilizing aluminous fly-ash to prepare calcium silicate micro power of claim 7, it is characterized in that 8, the bake out temperature of described moisture Calucium Silicate powder is 200～400 ℃, drying time is 0.5～2 hour.
According to the described method of utilizing aluminous fly-ash to prepare calcium silicate micro power of claim 8, it is characterized in that 9, the rate of recovery of described sodium hydroxide solution surpasses 95%, the concentration of sodium hydroxide solution of recovery is 10～15%.
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| CNA2008101126181A CN101591023A (en) | 2008-05-26 | 2008-05-26 | A kind of method of utilizing aluminous fly-ash to prepare calcium silicate micro power |
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| CNA2008101126181A CN101591023A (en) | 2008-05-26 | 2008-05-26 | A kind of method of utilizing aluminous fly-ash to prepare calcium silicate micro power |
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Cited By (25)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993087A (en) * | 2010-11-29 | 2011-03-30 | 中煤平朔煤业有限责任公司 | Method for preparing water glass by using fly ash |
| CN102190309A (en) * | 2011-01-06 | 2011-09-21 | 内蒙古大唐国际再生资源开发有限公司 | Method for lowering pH value of active calcium silicate |
| CN102417187A (en) * | 2011-08-29 | 2012-04-18 | 天津大学 | Dehydration method in co-producing active calcium silicate by fly ash |
| CN102583409A (en) * | 2012-01-10 | 2012-07-18 | 中国科学院过程工程研究所 | Method for producing mullite and calcium silicate by using high-alumina fly ash |
| CN102583410A (en) * | 2012-01-10 | 2012-07-18 | 中国科学院过程工程研究所 | A method for producing active calcium silicate by using fly ash desiliconization mother liquor |
| CN102605668A (en) * | 2012-03-31 | 2012-07-25 | 陕西科技大学 | Method for making high-bulk paper by adopting chemical wood pulp |
| WO2012151767A1 (en) * | 2011-05-11 | 2012-11-15 | 内蒙古大唐国际再生资源开发有限公司 | Method for preparing alumina from high alumina fly ash and co-producing active calcium silicate |
| CN102912669A (en) * | 2012-11-06 | 2013-02-06 | 大唐国际发电股份有限公司 | Light offset paper filled with synthetic calcium silicate and manufacturing method thereof |
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| CN103193239A (en) * | 2013-02-27 | 2013-07-10 | 陕西科技大学 | Improved preparation method for combined production of calcium silicate filling material for papermaking by using fly ash |
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| CN103373738A (en) * | 2012-04-19 | 2013-10-30 | 中国科学院过程工程研究所 | Fly ash low-temperature wet activating treatment method |
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| CN105985776B (en) * | 2015-01-27 | 2020-07-17 | 中国科学院过程工程研究所 | Preparation method of soil conditioner rich in citric acid soluble silicon |
| CN106148690B (en) * | 2015-04-08 | 2018-06-29 | 贵州宏达环保科技有限公司 | A kind of germanium silicon separation method |
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| CN104891838B (en) * | 2015-05-19 | 2017-05-31 | 河北工程大学 | It is a kind of that the method that silicon, calcium are used to prepare reinforcing agent is extracted from flyash |
| CN104894915A (en) * | 2015-05-20 | 2015-09-09 | 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 | Papermaking adhesive control agent, and preparation method and application of control agent |
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| CN106867502A (en) * | 2017-03-24 | 2017-06-20 | 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 | Using aluminous fly-ash coproduction petroleum fracturing propping agent and the method for eakleite |
| CN108192475A (en) * | 2017-12-12 | 2018-06-22 | 朱文杰 | A kind of preparation method of thick coated type anti-crack floor paint |
| CN111170324A (en) * | 2020-01-21 | 2020-05-19 | 张战军 | Method for preparing light high-whiteness calcium silicate micro powder by using rice hull ash |
| CN111887465A (en) * | 2020-08-25 | 2020-11-06 | 陕西科技大学 | Method for preparing paper-making reconstituted tobacco substrate with high air permeability and high absorptivity |
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