CN103539138B - A kind of method utilizing desiliconization alkali lye to prepare xonotlite - Google Patents
A kind of method utilizing desiliconization alkali lye to prepare xonotlite Download PDFInfo
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- CN103539138B CN103539138B CN201310557731.1A CN201310557731A CN103539138B CN 103539138 B CN103539138 B CN 103539138B CN 201310557731 A CN201310557731 A CN 201310557731A CN 103539138 B CN103539138 B CN 103539138B
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Abstract
The invention provides a kind of method utilizing desiliconization alkali lye to prepare xonotlite, adopt single step reaction method, desiliconization alkali lye and milk of lime mixed by silico-calcium mol ratio 0.9-1.1 and react, reaction product carries out filtering and drying treatment successively, obtains xonotlite; Wherein, in described desiliconization alkali lye, silica concentration is 15-30g/L, and naoh concentration is 51.6-129.0g/L, and sodium metaaluminate concentration is less than 5g/L, and concentration of sodium carbonate is less than 17.1g/L.Present invention also offers a kind of xonotlite utilizing above-mentioned method to prepare.The present invention utilizes desiliconization alkali lye to prepare xonotlite, and the siliceous raw material of its desiliconization alkali lye adopts power plant's waste coal ash or coal gangue, greatly reduces the production cost of xonotlite, meanwhile, the method preparing xonotlite of the present invention is simple, and the reaction times is short, is suitable for Industry Promotion.
Description
Technical field
The present invention relates to a kind of method utilizing desiliconization alkali lye to prepare xonotlite, belong to metallurgical technology field.
Background technology
Xonotlite is the main mineral constituent of calcium-silicate thermal insulation material, consisting of lagging material use temperature can reach 1000 DEG C, simultaneously xonotlite have again that unit weight is little, high high-temp stability and the advantage such as thermal conductivity is low, be thus widely used in the main raw material as light heat-insulating fire-retardant material.
At present, preparation method's mainly hydrothermal synthesis method of xonotlite, the method mixes by a certain percentage to be placed in autoclave by calcareous raw material and siliceous raw material to carry out being obtained by reacting xonotlite.The siliceous raw material adopted in this method is the solid materials such as the high white carbon black of the quartz sand of complete crystallization or price mostly, and time required for reaction process is longer, therefore, the method for prior art production xonotlite has the shortcoming that production cost is high, produce length consuming time.How to find a kind of with low cost, siliceous raw material that the market supply is sufficient, the production time that simultaneously can shorten again xonotlite is people's problem demanding prompt solution always.
Summary of the invention
Technical problem solved by the invention, is to provide a kind of method utilizing desiliconization alkali lye to prepare xonotlite, and the method adopts desiliconization alkali lye as siliceous raw material, and this raw material has wide material sources, advantage with low cost.
The invention provides a kind of method utilizing desiliconization alkali lye to prepare xonotlite, adopt single step reaction method, desiliconization alkali lye and milk of lime mixed by silico-calcium mol ratio 0.9-1.1 and react, reaction product carries out filtering and drying treatment successively, obtains xonotlite; Wherein, in described desiliconization alkali lye, silica concentration is 15-30g/L, and naoh concentration is 51.6-129.0g/L, and sodium metaaluminate concentration is less than 5g/L, and concentration of sodium carbonate is less than 17.1g/L.
The desiliconization alkali lye used in the present invention can be prepared by existing technology, such as can by the technique of preparing sodium potassium silicate solution by predesiliconizing potassium-rich rock (application number: 201010121250.2) make; Also can carry out desilication reaction as the flyash of siliceous raw material or coal gangue and sodium hydroxide solution and obtain by utilizing, its concrete preparation process is as follows: be in the sodium hydroxide solution of 6-15% using joining mass percent as the flyash of siliceous raw material or coal gangue, the mass ratio controlling sodium hydroxide and siliceous raw material is (0.4-0.6): 1, temperature of reaction is 90-130 DEG C, reaction times is that 1-3h carries out desilication reaction, solid-liquid separation is carried out after reaction terminates, solid matter is as the raw material producing aluminum oxide, and liquid substance is desiliconization alkali lye.
Utilize desiliconization alkali lye to synthesize in the method for xonotlite in the present invention, in the milk of lime used, the concentration of calcium oxide is 100-220g/L.
Desiliconization alkali lye is utilized to synthesize in the method for xonotlite in the present invention, control reaction process heats up, 260 DEG C are warming up to by 130 DEG C, being specially described temperature-rise period is temperature-gradient method: 130-150 DEG C of insulation 10-15min, 150-180 DEG C of insulation 10-12min, 180-210 DEG C of insulation 8-12min, 210-260 DEG C of insulation 1-8h.This process of reaction system being carried out to temperature-gradient method, is more conducive to xonotlite and carries out crystallization in reaction process, form good crystal formation, is meanwhile also conducive to the physicals promoting xonotlite.
Utilize desiliconization alkali lye to synthesize in the method for xonotlite in the present invention, control reaction pressure is 0.6-3.5MPa.
Utilize desiliconization alkali lye to synthesize in the method for xonotlite in the present invention, control drying temperature is 90-120 DEG C, and time of drying is 1-3h.
Utilize the xonotlite that method of the present invention prepares, the mass percent of its water ratio is less than 2.0% after tested, and the water ratio of the xonotlite obtained with prior art preparation method is suitable, meets relevant criterion level
The present invention utilizes desiliconization alkali lye to prepare xonotlite, and the siliceous raw material of its desiliconization alkali lye adopts power plant's waste coal ash or coal gangue, greatly reduces the production cost of xonotlite, meanwhile, the method preparing xonotlite of the present invention is simple, and the reaction times is short, is suitable for Industry Promotion.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of xonotlite of the present invention.
Fig. 2 is the SEM collection of illustrative plates of xonotlite of the present invention.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
Raw material choose:
1) desiliconization alkali lye: in desiliconization alkali lye, silica concentration is 20g/L, naoh concentration is 64.5g/L, and sodium metaaluminate concentration is less than 5g/L, and concentration of sodium carbonate is less than 17.1g/L;
2) milk of lime: in milk of lime, the concentration of calcium oxide is 150g/L;
Be put into reactor after 1.0 stirring and evenly mixings by desiliconization alkali lye and milk of lime by silico-calcium mol ratio, control reaction pressure under 2.5MPa, react heat temperature raising: 130-150 DEG C of insulation 12min, 150-180 DEG C of insulation 10min, 180-210 DEG C of insulation 8min, 210-260 DEG C is stirred insulation reaction 3h with the speed of 100rpm, reaction terminates rear cooled product to 90 DEG C, then reaction product is filtered, and distill moisture three washing leaching cakes with 600mL, obtained filter cake after dry 2h, can be obtained xonotlite at temperature is 90-120 DEG C.
Learn after tested:
1) the water ratio mass percent of xonotlite obtained above is less than 2.0%;
2) as shown in Figure 1, under scanning electron microscope, its microscopic appearance is observed: xonotlite is fibrous crystallization body;
3) as shown in Figure 2, in X ray diffracting spectrum, we are known: the product obtained after calcining is xonotlite.
Embodiment 2
Raw material choose:
1) desiliconization alkali lye: in desiliconization alkali lye, silica concentration is 15g/L, naoh concentration is 90.3g/L, and sodium metaaluminate concentration is less than 5g/L, and concentration of sodium carbonate is less than 17.1g/L;
2) milk of lime: in milk of lime, the concentration of calcium oxide is 200g/L;
Be put into reactor after 0.96 stirring and evenly mixing by desiliconization alkali lye and milk of lime by silico-calcium mol ratio, control reaction pressure under 3.0MPa, react heat temperature raising: 130-150 DEG C of insulation 15min, 150-180 DEG C of insulation 12min, 180-210 DEG C of insulation 12min, 210-260 DEG C is stirred insulation reaction 2h with the speed of 100rpm, reaction terminates rear cooled product to 90 DEG C, then reaction product is filtered, and distill moisture three washing leaching cakes with 600mL, obtained filter cake after dry 2h, can be obtained xonotlite at temperature is 90-120 DEG C.
Learn after tested: the water ratio mass percent of xonotlite obtained above is less than 2.0%;
Under scanning electron microscope, observe its microscopic appearance and X-ray diffraction test is carried out to it and obtain result as identical in embodiment 1.
Embodiment 3
Raw material choose:
1) desiliconization alkali lye: in desiliconization alkali lye, silica concentration is 30g/L, naoh concentration is 77.4g/L, and sodium metaaluminate concentration is less than 5g/L, and concentration of sodium carbonate is less than 17.1g/L;
2) milk of lime: in milk of lime, calcia concentration is 150g/L;
Be put into reactor after 1.03 stirring and evenly mixings by desiliconization alkali lye and milk of lime by silico-calcium mol ratio, control reaction pressure under 3.0MPa, react heat temperature raising: 130-150 DEG C of insulation 12min, 150-180 DEG C of insulation 12min, 180-210 DEG C of insulation 10min, 210-260 DEG C is stirred insulation reaction 2h with the speed of 100rpm, reaction terminates rear cooled product to 90 DEG C, then reaction product is filtered, and distill moisture three washing leaching cakes with 600mL, obtained filter cake after dry 2h, can be obtained xonotlite at temperature is 90-120 DEG C.
Learn after tested: the water ratio mass percent of xonotlite obtained above is less than 2.0%;
Under scanning electron microscope, observe its microscopic appearance and X-ray diffraction test is carried out to it and obtain result as identical in embodiment 1.
Last it is noted that above embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (4)
1. utilize desiliconization alkali lye to prepare a method for xonotlite, it is characterized in that, adopt single step reaction method, desiliconization alkali lye and milk of lime mixed by silico-calcium mol ratio 0.9-1.1 and react, reaction product carries out filtering and drying treatment successively, obtains xonotlite;
Wherein, in described desiliconization alkali lye, silica concentration is 15-30g/L, and naoh concentration is 51.6-129.0g/L, and sodium metaaluminate concentration is less than 5g/L, and concentration of sodium carbonate is less than 17.1g/L;
Control reaction process heats up, and is warming up to 260 DEG C by 130 DEG C, and described reaction process heats up as temperature-gradient method: 130-150 DEG C of insulation 10-15min, 150-180 DEG C of insulation 10-12min, 180-210 DEG C of insulation 8-12min, 210-260 DEG C of insulation 1-8h; Control reaction pressure is 0.6-3.5MPa.
2. method according to claim 1, is characterized in that, in described milk of lime, the concentration of calcium oxide is 100-220g/L.
3. method according to claim 1, is characterized in that, control drying temperature is 90-120 DEG C, and time of drying is 1-3h.
4. one kind utilizes the xonotlite that described in any one of claim 1-3, method prepares.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104528745A (en) * | 2014-12-02 | 2015-04-22 | 郭建文 | Method for preparing synthetic wollastonite with fly ash |
| CN105439156A (en) * | 2015-12-10 | 2016-03-30 | 内蒙古伊能煤炭转化与循环经济研究院 | Method for preparing rubber and plastics filler by use of microsilica and carbide slag |
| CN105819458B (en) * | 2016-03-28 | 2018-01-12 | 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 | A kind of method that eakleite is prepared using disodium metasilicate calcium |
| CN105836752B (en) * | 2016-03-28 | 2018-01-12 | 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 | A kind of method that eakleite is prepared using disodium metasilicate calcium |
| CN108946748B (en) * | 2018-08-24 | 2022-07-12 | 内蒙古中建亚太建材科技有限公司 | Method for synthesizing xonotlite composite thermal insulation material from high-alumina fly ash |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59169923A (en) * | 1983-03-16 | 1984-09-26 | Aoki Masayoshi | Xonotlite-type calcium silicate and its preparation |
| CN102825650A (en) * | 2012-07-20 | 2012-12-19 | 郭立平 | Making method of high-strength light-weight integral-hydrophobic xonotlite fireproof insulation board |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59169923A (en) * | 1983-03-16 | 1984-09-26 | Aoki Masayoshi | Xonotlite-type calcium silicate and its preparation |
| CN102825650A (en) * | 2012-07-20 | 2012-12-19 | 郭立平 | Making method of high-strength light-weight integral-hydrophobic xonotlite fireproof insulation board |
Non-Patent Citations (2)
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| 陈淑祥等.超轻硬硅钙石型硅酸钙绝热材料制备技术国内外研究现状.《保温材料与建筑节能》.2004,(第1期),第53-55页. * |
| 马世林等.煤矸石脱硅滤液制备纳米级硅灰石粉体的研究.《矿物岩石地球化学通报》.2011,第30卷第299页. * |
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Address after: 010206, Hohhot City, Togtoh province the Inner Mongolia Autonomous Region County Electric Power Industry Park Patentee after: Inner Mongolia Datang International Hohhot aluminum and Electricity Co., Ltd Address before: 010206, Hohhot City, Togtoh province the Inner Mongolia Autonomous Region County Electric Power Industry Park Patentee before: INNER MONGOLIA DATANG INTERNATIONAL RECYCLING RESOURCE DEVELOPMENT Co.,Ltd. |
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