CN104129798A - Method for preparing layered crystal sodium disilicate by using rice hull ash - Google Patents
Method for preparing layered crystal sodium disilicate by using rice hull ash Download PDFInfo
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- CN104129798A CN104129798A CN201410288749.0A CN201410288749A CN104129798A CN 104129798 A CN104129798 A CN 104129798A CN 201410288749 A CN201410288749 A CN 201410288749A CN 104129798 A CN104129798 A CN 104129798A
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- rice hull
- hull ash
- sodium disilicate
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- sodium hydroxide
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Abstract
The invention discloses a method for preparing layered crystal sodium disilicate by using rice hull ash, and belongs to the field of resource utilization and chemical production. The method comprises the following steps of adding sodium hydroxide in the rice hull ash; then adding water; grinding thoroughly and mixing uniformly; drying the uniformly ground and mixed material; heating the dried material to a temperature of 700-740 DEG C in 30-60 minutes; keeping the temperature for 10-60 minutes; and then cooling to obtain the layered crystal sodium disilicate. The layered crystal sodium disilicate prepared by using the rice hull ash can be used as a phosphorous-free washing assistant, is friendly to a biological environment, and fits requirements of environment protection. Waste rice hull is used as a silicon source, so that a positive effect for protecting the environment is achieved; and effective resource recycle can be realized, thereby increasing resource utilization rate. Besides, the method is simple in production process, is not high in requirements for production equipment and production conditions, and can be operated easily.
Description
Technical field
The present invention relates to chemical industry preparation field.Be particularly related to rice hull ash preparing washing auxiliary agent laminated crystal of sodium disilicate.
Background technology
Tripoly phosphate sodium STPP (STPP) is a kind of common detergent builder.Because phosphate cpd is drained in rivers and lakes with wash water, can cause Water Eutrophication, will make a large amount of breeding of algae, oxygen content in water is showing and is declining, serious harm the growth of animal in water, also make water quality deterioration simultaneously.For this reason, from 20 century 70s, many countries successively promulgate and the phosphoric acid salt using in synthetic detergent are strictly limited or forbidden relevant law, the substitute of the STPP of Efforts To Develop research and development simultaneously, the related development development work of increasing non-phosphorus washing assistant.
Current STPP substitute employed both at home and abroad mainly contains Starso and 4A zeolite, but due to 4A zeolite to calcium and magnesium ion exchange capacity relatively a little less than, and the technique of raw material and production has very large impact to the ion-exchange capacity of 4 A zeolites.And 4 A zeolite insoluble in water, life-time service can deposit on substrate, and Starso is relatively poor to calcium ion removal ability simultaneously, although five water things and nine water things have relatively strong water-absorbent, but easily deliquescence and make powdered detergent caking, therefore, application has been subject to certain restriction.
So people start to seek new multifunctional phosphateless washing agent.Wherein, crystalline layered silicate not only can be avoided the shortage of free phosphate detergent well as laminated crystal of sodium disilicate, and has more good scourability and therefore get more and more people's extensive concerning gradually.
Sodium disilicate be the mol ratio of silicon-dioxide and sodium oxide close to 2 water glass, under normal circumstances, sodium disilicate is amorphous, by certain pyroprocessing, can realize the ordered arrangement of silicon-oxy tetrahedron, becomes crystal.This crystal shows as the laminate structure of non-complete cleavage, and crystal formation has several forms such as δ, β, α, γ, and wherein δ, β type commodity value are obvious, and the laminated crystal of sodium disilicate softening water ability that accounts for main component with δ type is the strongest.
The preparation method of δ laminated crystal of sodium disilicate adopts quartz sand to react and make with sodium hydroxide at present, or adopt dry method water glass (sodium carbonate method) and mirabilite method water glass to make, all there is the problems such as production cost is high or high to equipment requirements, and operation easier is larger in these methods.
In addition, rice husk is the byproduct of rice processing, and its quality accounts for 22% of paddy.In paddy main producing region, a large amount of rice husks are piled into mountain, and in the north, the modal mode of utilizing is the fuel as warming.But this mode still can generate a large amount of rice hull ash.Other of rice husk utilize mode to comprise to prepare wall brick, feed etc., these utilize mode also exist cost higher, utilize the shortcomings such as limited, added value is lower.
In rice hull ash, dioxide-containing silica, up to 59%, uses this feature in prior art, by rice hull ash for the preparation of high-purity silicon dioxide.
Utilize mode except above-mentioned, a large amount of rice husks need the recycling mode that makes new advances of exploitation, realizes resource circulation utilization realizing environmental protection when.
Summary of the invention
Goal of the invention of the present invention is: utilize rice hull ash to prepare a kind of laminated crystal of sodium disilicate washing assistant with good item property, to solve the above-mentioned problem existing.
The technical solution used in the present invention is:
In rice hull ash, add sodium hydroxide and add again that fully ground and mixed is even after a certain amount of distilled water;
Uniform ground and mixed dry materials is dewatered;
Again dried material is risen to 700 DEG C-740 DEG C through 30-60min;
Insulation 10-60min, then cooling, obtain laminated crystal of sodium disilicate.
The preparation principle of present method is: 2SiO
2+ 2NaOH----Na
2si
2o
5+ H
2o.
In the prior art, there is the rice hull ash of employing to prepare the report of water glass, still, this chemical substance of the amorphous silica in rice hull ash that to prepare water glass be simple application, its product is worth lower.And the present invention adopts rice hull ash to prepare laminated crystal of sodium disilicate, just do not utilize this chemical substance, also utilize this chemical substance to there is at a certain temperature this feature of high reactivity, adopt directly synthetic high value products of simple step, be equivalent to water glass and be worth 3 times of left and right, its economic worth also significantly improves; In addition, synthetic water glass is a kind of Amorphous silicate, but method of the present invention prepare laminated crystal of sodium disilicate be directly by unformed silicon-dioxide and sodium hydroxide at high temperature one-step synthesis there is the water glass of specific crystal structure, the method technique is simpler, and preparation cost and efficiency are higher.
As preferred technical scheme: described rice hull ash is to be prepared from the temperature of 300 DEG C-600 DEG C with the heat-up rate of 2 DEG C of-6 DEG C/min.
Present inventor is through experimental results demonstrate, the form of rice hull ash and the activity of amorphous silicon di-oxide prepared by different heat-up rates and different outlet temperatures have certain difference, in building-up process on laminated crystal of sodium disilicate and product, the content of δ-laminated crystal of sodium disilicate has impact, is conducive to the composition that organism in rice husk etc. can volatilize and fully discharges and prepare rice hull ash under this temperature condition.
As preferred technical scheme: the water adding is distilled water.Can avoid like this introducing of impurity, the quality of the laminated crystal of sodium disilicate obtaining is higher.
As preferred technical scheme, dried material is risen to 720 DEG C through 60min.
Laminated crystal of sodium disilicate is doing the washing auxiliary detergent used time, the laminated crystal of sodium disilicate of δ type wherein must account for main component just can reach strong softening outlet capacity, the laminated crystal of sodium disilicate accounting of the δ type that the mode that adopts process 60min to rise to 720 DEG C obtains is maximum, and the product softening water ability obtaining is also just the strongest.
As preferred technical scheme:, described heating and heat preservation step is all carried out in retort furnace.
In sum, owing to having adopted technique scheme, the invention has the beneficial effects as follows: utilizing layered sodium disilicate prepared by rice hull ash to can be used as not phosphorous washing assistant, is friendly to ecotope, meets environmental requirement; Using discarded rice husk as silicon source, not only can play active effect to the protection of environment, can also effectively carry out resource recirculation, improve resource utilization; Production technique is simple, less demanding to production unit and working condition, processing ease.
Embodiment
The present invention is described in detail below.
In order to make object of the present invention, technical scheme and advantage clearer, 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, is not intended to limit the present invention.
Embodiment 1:
Be the rice hull ash that 2 DEG C/min makes at 400 DEG C by temperature rise rate, in prepared rice hull ash, add sodium hydroxide, add the amount of sodium hydroxide, be calculated in molar ratio as the SiO in rice hull ash
2: the NaOH=1:1 adding, and add distilled water, add distilled water amount be meter in mass ratio, distilled water: (rice hull ash+sodium hydroxide)=2:1, then in mortar, ground and mixed is even, uniform ground and mixed dry materials is dewatered, and the dry method dewatering is for rising to 100 DEG C from room temperature through 40min; Again dried material is risen to 700 DEG C through 30min and be then incubated 10min, then cooling, to obtain final product.
Embodiment 2:
Be the rice hull ash that 2 DEG C/min makes at 300 DEG C by temperature rise rate, in prepared rice hull ash, add sodium hydroxide, add the amount of sodium hydroxide, be calculated in molar ratio as the SiO in rice hull ash
2: the NaOH=1:1 adding, and add distilled water, add distilled water amount be meter in mass ratio, distilled water: (rice hull ash+sodium hydroxide)=2:1, then in mortar, ground and mixed is even, and uniform ground and mixed dry materials is dewatered; Again dried material is risen to 700 DEG C through 60min and be then incubated 30min, then cooling, to obtain final product.
Embodiment 3:
Be the rice hull ash that 2 DEG C/min makes at 400 DEG C by temperature rise rate, in prepared rice hull ash, add sodium hydroxide, add the amount of sodium hydroxide, be calculated in molar ratio as the SiO in rice hull ash
2: the NaOH=1:1 adding, add distilled water amount be meter in mass ratio, distilled water: (rice hull ash+sodium hydroxide)=2:1, then in mortar, ground and mixed is even, and uniform ground and mixed dry materials is dewatered; Again dried material is risen to 720 DEG C through 50min and be then incubated 10min, then cooling, to obtain final product.
Embodiment 4:
Be the rice hull ash that 3 DEG C/min makes at 400 DEG C by temperature rise rate, in prepared rice hull ash, add sodium hydroxide, add the amount of sodium hydroxide, be calculated in molar ratio as the SiO in rice hull ash
2: the NaOH=1:1 adding, add distilled water amount be meter in mass ratio, distilled water: (rice hull ash+sodium hydroxide)=2:1, then in mortar, ground and mixed is even, and uniform ground and mixed dry materials is dewatered; Again dried material is risen to 720 DEG C through 30min and be then incubated 30min, then cooling, to obtain final product.
Embodiment 5:
Be the rice hull ash that 6 DEG C/min makes at 500 DEG C by temperature rise rate, in prepared rice hull ash, add sodium hydroxide, add the amount of sodium hydroxide, be calculated in molar ratio as the SiO in rice hull ash
2: the NaOH=1:1 adding, add distilled water amount be meter in mass ratio, distilled water: (rice hull ash+sodium hydroxide)=2:1, then in mortar, ground and mixed is even, and uniform ground and mixed dry materials is dewatered; Again dried material is risen to 720 DEG C through 60min again and be then incubated 10min, then cooling, to obtain final product.
Embodiment 6:
Be the rice hull ash that 2 DEG C/min makes at 500 DEG C by temperature rise rate, in prepared rice hull ash, add sodium hydroxide, add the amount of sodium hydroxide, be calculated in molar ratio as the SiO in rice hull ash
2: the NaOH=1:1 adding, add distilled water amount be meter in mass ratio, distilled water: (rice hull ash+sodium hydroxide)=2:1, then in mortar, ground and mixed is even, and uniform ground and mixed dry materials is dewatered; Again dried material is risen to 720 DEG C through 40min and be then incubated 30min, then cooling, to obtain final product.
Embodiment 7:
Be the rice hull ash that 2 DEG C/min makes at 600 DEG C by temperature rise rate, in prepared rice hull ash, add sodium hydroxide, add the amount of sodium hydroxide, be calculated in molar ratio as the SiO in rice hull ash
2: the NaOH=1:1 adding, add distilled water amount be meter in mass ratio, distilled water: (rice hull ash+sodium hydroxide)=2:1, then in mortar, ground and mixed is even, and uniform ground and mixed dry materials is dewatered; Again dried material is risen to 720 DEG C through 50min again and be then incubated 10min, then cooling, to obtain final product.
Embodiment 8:
Be the rice hull ash that 4 DEG C/min makes at 600 DEG C by temperature rise rate, in prepared rice hull ash, add sodium hydroxide, add the amount of sodium hydroxide, be calculated in molar ratio as the SiO in rice hull ash
2: the NaOH=1:1 adding, add distilled water amount be meter in mass ratio, distilled water: (rice hull ash+sodium hydroxide)=2:1, then in mortar, ground and mixed is even, and uniform ground and mixed dry materials is dewatered; Again dried material is risen to 740 DEG C through 60min and be then incubated 60min, then cooling, to obtain final product.
By laminated crystal of sodium disilicate correlated performance test prepared embodiment 1-8, test-results is as shown in table 1.
Table 1 laminated crystalline two silicic acid detect data
Claims (5)
1. utilize rice hull ash to prepare a method for laminated crystal of sodium disilicate, it is characterized in that, comprise the following steps:
In rice hull ash, add sodium hydroxide and add again that fully ground and mixed is even after water;
By uniform ground and mixed dry materials;
Again dried material is risen to 700 DEG C-740 DEG C through 30-60min; Insulation 10-60min, then cooling, obtain laminated crystal of sodium disilicate.
2. the method for utilizing rice hull ash to prepare laminated crystal of sodium disilicate as claimed in claim 1, is characterized in that, described rice hull ash is to be prepared from the temperature of 300 DEG C-600 DEG C with the heat-up rate of 2 DEG C of-6 DEG C/min.
3. the method for utilizing rice hull ash to prepare laminated crystal of sodium disilicate as claimed in claim 1, is characterized in that, the water adding is distilled water.
4. the method for utilizing rice hull ash to prepare laminated crystal of sodium disilicate as claimed in claim 1, is characterized in that, dried material is risen to 720 DEG C through 60min.
5. the method for utilizing rice hull ash to prepare laminated crystal of sodium disilicate as claimed in claim 1, is characterized in that, described heating and heat preservation step is all carried out in retort furnace.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088547A (en) * | 1991-12-21 | 1994-06-29 | 赫彻斯特股份公司 | The crystalline sodium disilicate preparation method |
| CN1613760A (en) * | 2004-11-22 | 2005-05-11 | 河北科技大学 | Method for preparing laminated crystalline sodium disilicate by alta-mud |
| CN1762802A (en) * | 2005-09-09 | 2006-04-26 | 四川省宜宾五粮液集团有限公司 | Method for industrial production of white carbon black using rice husk |
| CN101007636A (en) * | 2007-01-13 | 2007-08-01 | 淮阴工学院 | Process for preparation of delta-layed crystalline sodium disilicate using attapulgite |
-
2014
- 2014-06-25 CN CN201410288749.0A patent/CN104129798A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088547A (en) * | 1991-12-21 | 1994-06-29 | 赫彻斯特股份公司 | The crystalline sodium disilicate preparation method |
| CN1613760A (en) * | 2004-11-22 | 2005-05-11 | 河北科技大学 | Method for preparing laminated crystalline sodium disilicate by alta-mud |
| CN1762802A (en) * | 2005-09-09 | 2006-04-26 | 四川省宜宾五粮液集团有限公司 | Method for industrial production of white carbon black using rice husk |
| CN101007636A (en) * | 2007-01-13 | 2007-08-01 | 淮阴工学院 | Process for preparation of delta-layed crystalline sodium disilicate using attapulgite |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Application publication date: 20141105 |