CN101786635B - Method for preparation of sodium metasilicate pentahydrate by fly ash - Google Patents
Method for preparation of sodium metasilicate pentahydrate by fly ash Download PDFInfo
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- CN101786635B CN101786635B CN201010125797XA CN201010125797A CN101786635B CN 101786635 B CN101786635 B CN 101786635B CN 201010125797X A CN201010125797X A CN 201010125797XA CN 201010125797 A CN201010125797 A CN 201010125797A CN 101786635 B CN101786635 B CN 101786635B
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Abstract
The invention discloses a method for the preparation of sodium metasilicate pentahydrate by fly ash, which comprises the steps: using sodium hydroxide solution to alkaline-hydrolyze sodium silicate solution with the silicon dioxide preparation modulus of 0.4-0.8 in the fly ash, carbonizing amorphous hydrated silicon dioxide with the partial sodium hydroxide solution, then re-dissolving the amorphous hydrated silicon dioxide with the sodium hydroxide solution to formulate crystallization solution with the ratio of SiO2 to Na2O of 1:0.8-1.2, removing suspended matters by filtration, heating and concentration, cooling and crystallizing, and performing solid-liquid separation at 35 DEG C to result in sodium metasilicate pentahydrate. The method has the advantages of simple process, inexpensive raw material, great easiness for industrialization and tremendous economical and environmental benefits.
Description
Technical field
The invention belongs to the recycling category of flyash, be specifically related to a kind of method of utilizing the fly-ash Preparation metasilicate pentahydrate sodium.
Background technology
Last century the seventies; After some developed countries (states such as the U.S., Canada, Japan, Switzerland) begin to pay attention to phosphorus-containing detergent waste water gradually and enter rivers and lakes; Cause the water quality eutrophication, make the water pollution anoxic, the phenomenon that aquatic organism is threatened; The production and the use of phosphorus-containing detergent are forbidden and limited to the rules of enacting a law in succession.After getting into 21st century, China also has many provinces and cities to issue the relevant regulations of forbidding selling and using phosphorus-containing detergent.These are prohibited the phosphorus behave and have effectively promoted research and development and production for the phosphorus washing auxiliary detergent.
At present; In industrialized generation,, the phosphorus washing auxiliary detergent mainly was three kinds of 4A zeolite, metasilicate pentahydrate sodium and ZX-Is; Wherein the 4A zeolite belongs to aluminium salt (sodium aluminium silicate), because aluminium salt can cause plant, animal and human's class chronic poisoning, therefore; The a large amount of use still has future trouble, so the main developing direction of following free phosphate detergent is Starso and ZX-I.
Starso (mainly being metasilicate pentahydrate sodium) production technique is simple relatively, and product cost is low, and this washing auxiliary detergent to have a dispersing property good; Keep solution alkalescence ability strong; Advantages such as the pH buffer capacity is big, and soil removability is strong, the consumption in washing composition increases year by year.Its working method mainly contains three kinds: comminution granulation, aqueous solution crystallization process and crystallization comminuting method.It is raw material that these three kinds of methods all adopt industrial metasilicate and industrial caustic soda bar none; And its industrial metasilicate all is the dry production that adopts highly energy-consuming, and specific practice is that silica sand that mill is good and soda ash prepare mixing and goes into kiln, frit reaction number hour under nearly 1550 ℃ high temperature; Then with the fused salt shrend; With the improved grinding after the shrend, dilution is clarified again; And then with the clear liquor heating, evaporation concentration becomes the industrial metasilicate of required modulus.Adopt this method manufacture water glass, complex process, resource consumption is big; Energy consumption is high, and seriously polluted, and cost is high; Be not suitable for the requirement of current development low-carbon economy, also be helpless to reduce production cost, promote the development of free phosphate detergent for the phosphorus washing auxiliary detergent.
Summary of the invention
The purpose of this invention is to provide a kind of cheap waste that utilizes--the method for-fly-ash Preparation metasilicate pentahydrate sodium.This method can not only be prepared qualified metasilicate pentahydrate sodium product under low-temperature atmosphere-pressure, and technical process is simple, and energy-saving and emission-reduction consumption reduction advantage is remarkable, and product cost is low.
The present invention utilizes the method for fly-ash Preparation metasilicate pentahydrate sodium may further comprise the steps:
A) with the sodium hydroxide solution of flyash and 25～40wt% according to 1～2: 1 liquid-solid ratio is mixed; Silicon-dioxide under the sodium hydroxide solution boiling temperature in the alkaline hydrolysis flyash; Make it to generate water glass and get in the solution, to obtain modulus be 0.4～0.8 sodium silicate solution to dilute filtration then;
B) get the above-mentioned sodium silicate solution of part, divide preparation amorphous hydrated SiO 2 with dioxide gas carbon, filtering separation obtains sodium carbonate solution and amorphous hydrated SiO 2 filter cake;
C) the amorphous hydrated SiO 2 filter cake that the sodium silicate solution dissolving b to make in a)) obtains is mixed with SiO
2: Na
2O=1: 0.8～1.2 crystallization stoste, filter and remove suspended substances heat up to concentrate, and adds the crystallisation cycle mother liquor that filtering separation last time obtains and process crystal solution;
D) make the crystal solution decrease temperature crystalline, carry out solid-liquid separation to 35 ℃, obtain metasilicate pentahydrate sodium.
Wherein, being used for the dioxide gas that carbon divides can be the desulfurization flue gas of carbonic acid gas volumetric concentration >=10%.
In the aforesaid method, after the sodium carbonate solution that step b) obtains can be used the milk of lime causticization, mend dense causticity liquid caustic soda or sheet alkali and turn back to alkaline hydrolysis flyash operation and recycle.The filtrating that the step d) solid-liquid separation obtains can be used as the crystallisation cycle mother liquor, returns to be blended in the spissated crystallization stoste to recycle.
Metasilicate pentahydrate sodium preparation method of the present invention is particularly suitable for handling aluminous fly-ash; Through the silicon-dioxide in the alkaline hydrolysis flyash; Propose the element silicon in the flyash, be made into large industriallization raw material, promptly promoted economic benefit; Again enrichment the aluminium in the flyash, for the subsequent extractions aluminum oxide has been created condition.Therefore, the present invention will play the important techniques supporting role to the aluminous fly-ash recycling, and enterprise can obtain remarkable economic efficiency.
Embodiment
Get that dioxide-containing silica is about 50%, the dry powder coal ash of aluminium sesquioxide content about 40%; With concentration be that 35% sodium hydroxide solution is by 1.5: 1 mixed pulps of liquid-solid ratio; 120 ℃ of following stirring reactions 20 minutes, make most silicon-dioxide and sodium hydroxide reaction in the flyash generate water glass and get into solution.It is 0.6 low modulus sodium silicate solution that the following washings appropriateness diluted slurry collected of step washing leaching cake, filtering separation promptly obtain modulus.
Filter cake is after the second adverse current washing, as the raw material that extracts aluminium sesquioxide.Washings is collected the back as diluent, is used to dilute above-mentioned reaction paste.
Get the above-mentioned sodium silicate solution that obtains of part,, fully react after-filtration separation carbon and divide slurries, obtain sodium carbonate solution and amorphous hydrated SiO 2 filter cake to the desulfurization flue gas that wherein feeds gas concentration lwevel 17%.
Sodium carbonate solution with the milk of lime causticization after, mend dense causticity liquid caustic soda or sheet alkali again, be made into 35% sodium hydroxide solution, be pumped to alkaline hydrolysis flyash operation and recycle.
The amorphous hydrated SiO 2 filter cake that obtains dissolves with above-mentioned sodium silicate solution, is mixed with SiO
2: Na
2O=1: 1 crystallization stoste after the filter and remove suspended substances, is warming up to 120 ℃; Evaporation concentration to solution mesosilicic acid sodium content reaches about 55%, is cooled to 95 ℃ again, is blended into the crystallisation cycle mother liquor that filtering separation last time obtains; Be cooled to 60～65 ℃, add an amount of metasilicate pentahydrate sodium crystal seed, control rate of temperature fall and stir speed (S.S.); Treat that solution is cooled to about 35 ℃, filtering separation obtains the metasilicate pentahydrate sodium filter cake of water ratio＜5%.
The filtrating that filtering separation obtains is the crystallisation cycle mother liquor, can pump in the crystallization stoste to recycle.
The metasilicate pentahydrate sodium filter cake is sent in the rotary drying kiln, and with 130 ℃ hot-air seasoning, control kiln discharge temperature of charge remains between 60～65 ℃, collects the oven dry material and is the metasilicate pentahydrate sodium product.
Claims (2)
1. method of utilizing the fly-ash Preparation metasilicate pentahydrate sodium may further comprise the steps:
A) with the sodium hydroxide solution of flyash and 25～40wt% according to 1～2: 1 liquid-solid ratio is mixed; Silicon-dioxide under the sodium hydroxide solution boiling temperature in the alkaline hydrolysis flyash; Make it to generate water glass and get in the solution, to obtain modulus be 0.4～0.8 sodium silicate solution to dilute filtration then;
B) get the above-mentioned sodium silicate solution of part, divide preparation amorphous hydrated SiO 2 with dioxide gas carbon, filtering separation obtains sodium carbonate solution and amorphous hydrated SiO 2 filter cake;
C) the amorphous hydrated SiO 2 filter cake that the sodium silicate solution dissolving b to make in a)) obtains is mixed with SiO
2: Na
2O=1: 0.8～1.2 crystallization stoste, filter and remove suspended substances heat up to concentrate, and adds the crystallisation cycle mother liquor that filtering separation last time obtains and process crystal solution;
D) make the crystal solution decrease temperature crystalline, carry out filtering separation to 35 ℃, obtain metasilicate pentahydrate sodium, and the filtrating that separation is obtained is as the crystallisation cycle mother liquor.
2. the method for utilizing the fly-ash Preparation metasilicate pentahydrate sodium according to claim 1 is characterized in that the desulfurization flue gas that in sodium silicate solution, feeds carbonic acid gas volumetric concentration >=10% carries out carbon branch preparation amorphous hydrated SiO 2.
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| CN201010125797XA CN101786635B (en) | 2010-03-17 | 2010-03-17 | Method for preparation of sodium metasilicate pentahydrate by fly ash |
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| CN201010125797XA CN101786635B (en) | 2010-03-17 | 2010-03-17 | Method for preparation of sodium metasilicate pentahydrate by fly ash |
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| CN101786635A CN101786635A (en) | 2010-07-28 |
| CN101786635B true CN101786635B (en) | 2012-03-28 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920967A (en) * | 2010-08-20 | 2010-12-22 | 朔州市润泽投资发展有限公司 | Method for extracting silicon dioxide from flyash |
| RU2473465C2 (en) * | 2010-12-08 | 2013-01-27 | Общество с ограниченной ответственностью "Руслэнд" | Method of obtaining pentahydrate, hexahydrate, nonahydrate crystallohydrates of sodium metasilicate |
| CN102190310B (en) * | 2011-01-06 | 2013-03-06 | 内蒙古大唐国际再生资源开发有限公司 | Method for manufacturing sodium metasilicate nonahydrate with fly ashes |
| CN102701228A (en) * | 2012-05-28 | 2012-10-03 | 朔州市润泽投资发展有限公司 | Recycling method of caustic alkaline liquid for treatment of high-silicon aluminum ore material |
| CN104556080A (en) * | 2015-01-15 | 2015-04-29 | 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 | Method for preparing sodium silicate by virtue of desilication alkaline liquor |
| CN106517222A (en) * | 2016-11-14 | 2017-03-22 | 清华大学 | Method for synthesizing ordered mesopore nano-silica through pulverous coal |
| CN110272053B (en) * | 2018-03-16 | 2021-05-11 | 国家能源投资集团有限责任公司 | Preparation method of high-purity water glass, low-iron white carbon black and ultra-white glass raw materials |
| CN113213497B (en) * | 2021-05-15 | 2022-08-05 | 江西省欧陶科技有限公司 | Process and tool for preparing sodium metasilicate pentahydrate by using crystallization crushing method |
| CN113753906A (en) * | 2021-09-16 | 2021-12-07 | 中国建设基础设施有限公司 | Wet grinding preparation method of water glass excitant for geopolymer |
| CN115215418A (en) * | 2022-07-27 | 2022-10-21 | 聊城鲁西聚酰胺新材料科技有限公司 | Method for removing silicate in ammoximation wastewater by using CO2 |
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| CN101318663A (en) * | 2008-07-23 | 2008-12-10 | 平朔煤炭工业公司 | Method for preparing high-modulus sodium silicate |
| CN101327932A (en) * | 2008-07-31 | 2008-12-24 | 云南云天化国际化工股份有限公司 | Method for producing sodium metasilicate pentahydrate with fluorine-containing silica gel |
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