CN104591197A - Method for preparing high-purity alpha-layered sodium silicate by using rice husk ash - Google Patents
Method for preparing high-purity alpha-layered sodium silicate by using rice husk ash Download PDFInfo
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- CN104591197A CN104591197A CN201510033360.6A CN201510033360A CN104591197A CN 104591197 A CN104591197 A CN 104591197A CN 201510033360 A CN201510033360 A CN 201510033360A CN 104591197 A CN104591197 A CN 104591197A
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Abstract
The invention discloses a method for preparing high-purity alpha-layered sodium silicate by using rice husk ash, and belongs to the field of inorganic applied materials and chemical preparation. The method comprises the following steps: putting the rice husk ash in a sodium hydroxide solution to be leached for 1 to 6h, filtering, adjusting the molar ratio of Na to Si in a filtrate to 0.90 to 1.1 with NaOH, drying the filtrate at a temperature of 100 to 200 DEG C, and then carrying out heat preservation for 30min to 210min at a temperature of 760 to 820 DEG C; and then cooling to obtain the alpha-layered sodium silicate. Without adding seed crystals, uniformly mixed materials are dried, fired at a high temperature and cooled to obtain the layered sodium silicate with the alpha-phase content of 100%, and the purity of the layered sodium silicate is more that 8% higher than that of the existing industrial product. The method has the advantages of simple process, low preparation cost and high efficiency. The prepared product has a high additional value due to the high purity, and has obvious economic benefits.
Description
Technical field
The present invention relates to inorganic application material and field of chemical preparation, particularly a kind of rice hull ash that utilizes is prepared as the method for the α-lamina sodium silicate of solid lubricant.
Background technology
α-lamina sodium silicate (layer silicon) is the inorganic crystal material that a class has intercalation compound feature, there is silicon-oxy tetrahedron layer with negative charge and regularly arranged, pass through Na between layers in crystalline structure
+balancing charge and support, there is the performance-extreme-pressure anti-wear similar to layered inorganic material such as graphite, molybdenumdisulphide, tungsten disulfides and rub and improve, industrially having wider application prospect, and its complete function, use pollution-free, is the solid lubricant with huge potentiality to be exploited.
The preparation method of current α-lamina sodium silicate has following several: evaporation drying crystallization process, liquid soluble glass one-step calcinations, quick dissolved sodium silicate Synthesis method, hydrothermal synthesis method, solid water glass direct translation method.Often there is the shortcomings such as production cost is high, high to equipment requirements, operation easier is comparatively large, complicated process of preparation in the method for the existing α of preparation-lamina sodium silicate.In current art, α-lamina sodium silicate the purity of producing is relatively low, although report and synthesized high-purity α-lamina sodium silicate, if application number is the Chinese patent application of 200410012440.5, adopt modulus to be 2.0 ± 0.05 liquid soluble glass, be placed in the high temperature of 750-800 DEG C, reaction 30-360 minute, synthesis α-lamina sodium silicate, but water glass wherein adds the mixing crystal seed of 3-30%, and also the reaction times is relatively long; And for example, application number is the Chinese patent application of 200410064556.3, although overcome the shortcoming that soluble glass method cost is high and quartz/Method of Soda working pressure is high, have employed cheap wilkinite, through a series of process, but what prepare is the laminated crystal of sodium disilicate product of β and δ crystal formation, and complex manufacturing.
China is Rice Cropping country maximum in the world, and paddy annual production is about 200,000,000 tons, and rice husk accounts for 20% of paddy usually, and rice husk resource is very abundant.But rice husk surface is hard, and silicone content is high, is not easily bacterially decomposed, and tap density is little, discarded welding, burns and causes topsoil, so the exploitation of rice husk are significant.The Land use systems of China's rice husk comprises prepares wall brick, feed, pyrolysis etc., these Land use systems also exist cost higher, utilize the shortcomings such as limited, added value is lower.In rice hull ash, dioxide-containing silica is up to more than 90%, has and use the production of this feature as the report of the silicon-containing compounds such as sodium silicate, white carbon black, silicon-dioxide in prior art.But this chemical substance of amorphous silica in these rice hull ash that have been simple application, its product added value is lower.
Summary of the invention
The object of the invention is, provides a kind of method utilizing rice hull ash to prepare high-purity α-lamina sodium silicate.
To achieve these goals, the technical solution used in the present invention is.
Utilize rice hull ash to prepare a method for high-purity α-lamina sodium silicate, comprise the following steps:
(1) rice hull ash is put into sodium hydroxide solution to leach, leaching time is 1 ~ 6h;
(2) solution in step (1) is filtered, with NaOH, the mol ratio of Na:Si in filtrate is adjusted to 0.90 ~ 1.1,
(3) filtrate after step (2) being adjusted is dry at 100 DEG C ~ 200 DEG C;
(4) step (3) dried material is incubated 30min ~ 210min at 760 DEG C ~ 820 DEG C; Then cool, obtain α-lamina sodium silicate.
The purity of α-lamina sodium silicate in the present invention, unless stated otherwise, all refers to the purity of mass percent.
The method that the present invention prepares α-lamina sodium silicate be by rice hull ash and sodium hydroxide solution even according to certain mixed in molar ratio, without the need to adding crystal seed, again by the dry materials after mixing, then at high temperature burn till, the lamina sodium silicate that α phase content reaches as high as 100% after cooling, can be obtained, higher by more than 8% than existing Industrial products purity, the method technique is simple, preparation cost is low and efficiency is higher, and obtained product makes its added value high because purity is high, remarkable in economical benefits.
The invention has the advantages that.
(1) the present invention adopts rice hull ash as silicon source, and the raw materials cost of product is low, effectively carries out resource recirculation, improves resource utilization, has significant environment protection significance and social benefit.
(2) calcination time needed for preparation technology of the present invention is relatively short, is conducive to significantly reducing energy consumption, thus reduces production cost, decreases resource consumption, improves economic benefit.
(3) the present invention synthesizes α-lamina sodium silicate, and content reaches as high as 100%, and added value of product is high, remarkable in economical benefits.
(4) production technique of the present invention is simple, to production unit (without the need to spraying dry) and working condition (quartz/Method of Soda working pressure is high) less demanding, processing ease.
Accompanying drawing explanation
The XRD figure spectrum that Fig. 1 is the embodiment of the present invention 6, the sample of synthesis in embodiment 7, embodiment 8 carries out XRD determining, in figure, X-coordinate is diffraction angle " 2-theta "; Ordinate zou is " diffracted intensity ".
Embodiment
The present invention is described in detail below.
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
embodiment 1:
By the SiO in rice hull ash
2content, with SiO
2: the mol ratio of NaOH=1:1 takes rice hull ash and NaOH respectively, puts into rice hull ash by after NaOH wiring solution-forming, and dipping 3h, filters and obtain filtrate, the mol ratio of Na:Si in filtrate is adjusted to 0.9, then by filtrate drying and dehydrating at 100 DEG C; Again dried material is incubated 150min at 760 DEG C, then cools, namely obtain the α-lamina sodium silicate of 97%.
embodiment 2:
By the SiO in rice hull ash
2content, with SiO
2: the mol ratio of NaOH=1:1 takes rice hull ash and NaOH respectively, puts into rice hull ash by after NaOH wiring solution-forming, and dipping 3h, filters and obtain filtrate, the mol ratio of Na:Si in filtrate is adjusted to 0.9, by the solution of gained drying and dehydrating at 100 DEG C; Again dried material is incubated 150min at 780 DEG C, then cools, namely obtain the α-lamina sodium silicate of 98%.
embodiment 3:
By the SiO in rice hull ash
2content, with SiO
2: the mol ratio of NaOH=1:1 takes rice hull ash and NaOH respectively, puts into rice hull ash by after NaOH wiring solution-forming, and dipping 3h, filters and obtain filtrate, the mol ratio of Na:Si in filtrate is adjusted to 1.0, by the solution of gained drying and dehydrating at 150 DEG C; Again dried material is incubated 150min at 800 DEG C, then cools, namely obtain the α-lamina sodium silicate of 99%.
embodiment 4:
By the SiO in rice hull ash
2content, with SiO
2: the mol ratio of NaOH=1:1 takes rice hull ash and NaOH respectively, puts into rice hull ash by after NaOH wiring solution-forming, and dipping 3h, filters and obtain filtrate, the mol ratio of Na:Si in filtrate is adjusted to 1.0, by the solution of gained drying and dehydrating at 150 DEG C; Again dried material is incubated 120min at 800 DEG C, then cools, namely obtain the α-lamina sodium silicate of 97%.
embodiment 5:
By the SiO in rice hull ash
2content, with SiO
2: the mol ratio of NaOH=1:1 takes rice hull ash and NaOH respectively, puts into rice hull ash by after NaOH wiring solution-forming, and dipping 3h, filters and obtain filtrate, the mol ratio of Na:Si in filtrate is adjusted to 1.0, by the solution of gained drying and dehydrating at 200 DEG C; Again dried material is incubated 120min at 800 DEG C, then cools, namely obtain the α-lamina sodium silicate of 98%.
embodiment 6:
By the SiO in rice hull ash
2content, with SiO
2: the mol ratio of NaOH=1:1 takes rice hull ash and NaOH respectively, puts into rice hull ash by after NaOH wiring solution-forming, and dipping 3h, filters and obtain filtrate, the mol ratio of Na:Si in filtrate is adjusted to 1.05, by the solution of gained drying and dehydrating at 200 DEG C; Again dried material is incubated 60min at 800 DEG C, then cools, namely obtain the α-lamina sodium silicate of 97%.
embodiment 7:
By the SiO in rice hull ash
2content, with SiO
2: the mol ratio of NaOH=1:1 takes rice hull ash and NaOH respectively, puts into rice hull ash by after NaOH wiring solution-forming, and dipping 3h, filters and obtain filtrate, the mol ratio of Na:Si in filtrate is adjusted to 1.05, by the solution of gained drying and dehydrating at 150 DEG C; Again dried material is incubated 120min at 800 DEG C, then cools, namely obtain the α-lamina sodium silicate of 99%.
embodiment 8:
By the SiO in rice hull ash
2content, with SiO
2: the mol ratio of NaOH=1:1 takes rice hull ash and NaOH respectively, puts into rice hull ash by after NaOH wiring solution-forming, and dipping 3h, filters and obtain filtrate, the mol ratio of Na:Si in filtrate is adjusted to 1.1, by the solution of gained drying and dehydrating at 150 DEG C; Again dried material is incubated 180min at 800 DEG C, then cools, namely obtain the α-lamina sodium silicate of 100%.
embodiment 9:
By the SiO in rice hull ash
2content, with SiO
2: the mol ratio of NaOH=1:1 takes rice hull ash and NaOH respectively, puts into rice hull ash by after NaOH wiring solution-forming, and dipping 3h, filters and obtain filtrate, the mol ratio of Na:Si in filtrate is adjusted to 1.1, by the solution of gained drying and dehydrating at 150 DEG C; Again dried material is incubated 120min at 800 DEG C, then cools, namely obtain the α-lamina sodium silicate of 100%.
Tested by α-lamina sodium silicate prepared by embodiment 1-9, test-results is as shown in table 1.
The purity of table 1 each embodiment α-lamina sodium silicate
Carry out XRD determining to the sample of synthesis in embodiment 6, embodiment 7, embodiment 8, its XRD figure spectrum as shown in Figure 1.In Fig. 1, X-coordinate is diffraction angle " 2-theta "; Ordinate zou is " diffracted intensity ".
Claims (4)
1. utilize rice hull ash to prepare a method for high-purity α-lamina sodium silicate, it is characterized in that, comprise the following steps:
(1) rice hull ash is put into sodium hydroxide solution to leach, leaching time is 1 ~ 6h;
(2) solution in step (1) is filtered, with NaOH, the mol ratio of Na:Si in filtrate is adjusted to 0.90 ~ 1.1,
(3) filtrate after step (2) being adjusted is dry at 100 DEG C ~ 200 DEG C;
(4) step (3) dried material is incubated 30min ~ 210min at 760 DEG C ~ 820 DEG C; Then cool, obtain α-lamina sodium silicate.
2. utilize rice hull ash to prepare the method for high-purity α-lamina sodium silicate as claimed in claim 1, it is characterized in that, in step (1), adopt the silicon-dioxide in sodium hydroxide solution extraction rice hull ash.
3. utilize rice hull ash to prepare the method for high-purity α-lamina sodium silicate as claimed in claim 1, it is characterized in that, in step (1), the mol ratio of filtering Na:Si in the filtrate obtained is 0.90 ~ 1.1.
4. utilize rice hull ash to prepare the method for high-purity α-lamina sodium silicate as claimed in claim 1, it is characterized in that, in step (3), step (2) dried material is incubated 30min ~ 210min at 760 DEG C ~ 820 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115720A (en) * | 2016-08-14 | 2016-11-16 | 皖西学院 | A kind of method utilizing rice hull ash to prepare nano silicon |
| CN111592005A (en) * | 2020-05-08 | 2020-08-28 | 山西大学 | Method for preparing alpha-layered sodium silicate at low temperature from coal powder furnace fly ash acid method aluminum extraction tailings |
| CN113636811A (en) * | 2021-08-10 | 2021-11-12 | 成都精准混凝土有限公司 | Concrete for 3D printing and preparation method thereof |
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| CN1613760A (en) * | 2004-11-22 | 2005-05-11 | 河北科技大学 | Method for preparing laminated crystalline sodium disilicate by alta-mud |
| CN104129798A (en) * | 2014-06-25 | 2014-11-05 | 成都理工大学 | Method for preparing layered crystal sodium disilicate by using rice hull ash |
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2015
- 2015-01-23 CN CN201510033360.6A patent/CN104591197A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1613760A (en) * | 2004-11-22 | 2005-05-11 | 河北科技大学 | Method for preparing laminated crystalline sodium disilicate by alta-mud |
| CN104129798A (en) * | 2014-06-25 | 2014-11-05 | 成都理工大学 | Method for preparing layered crystal sodium disilicate by using rice hull ash |
Non-Patent Citations (3)
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| 刘娟等: "稻壳灰制水玻璃的正交试验研究", 《粮食与饲料工业》 * |
| 刘毅等: "δ - 层状结晶二硅酸钠的制备", 《淮阴工学院学报》 * |
| 马鸿文: "《中国富钾岩石——资源与清洁利用技术》", 28 February 2010, 化学工业出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115720A (en) * | 2016-08-14 | 2016-11-16 | 皖西学院 | A kind of method utilizing rice hull ash to prepare nano silicon |
| CN106115720B (en) * | 2016-08-14 | 2017-07-14 | 皖西学院 | A kind of method that utilization rice hull ash prepares nano silicon |
| CN111592005A (en) * | 2020-05-08 | 2020-08-28 | 山西大学 | Method for preparing alpha-layered sodium silicate at low temperature from coal powder furnace fly ash acid method aluminum extraction tailings |
| 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 |
| CN113636811A (en) * | 2021-08-10 | 2021-11-12 | 成都精准混凝土有限公司 | Concrete for 3D printing and preparation method thereof |
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