CN104140108B - A kind of method preparing calcium magnesium silicate powder - Google Patents
A kind of method preparing calcium magnesium silicate powder Download PDFInfo
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- CN104140108B CN104140108B CN201410318067.XA CN201410318067A CN104140108B CN 104140108 B CN104140108 B CN 104140108B CN 201410318067 A CN201410318067 A CN 201410318067A CN 104140108 B CN104140108 B CN 104140108B
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- nitrocalcite
- reductive agent
- water glass
- magnesium nitrate
- water
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Abstract
Prepare a method for calcium magnesium silicate powder, belong to inorganic non-metallic ultrafine powder preparation field.First take nitrocalcite, magnesium nitrate, water glass, reductive agent, the mol ratio of described nitrocalcite, magnesium nitrate, water glass, reductive agent is 1 ~ 2:1 ~ 2:1 ~ 2:6 ~ 30; First nitrocalcite, magnesium nitrate and reductive agent are dissolved completely in deionized water, again water glass is dissolved in the water and makes sodium silicate aqueous solution, sodium silicate aqueous solution is poured in the aqueous solution of nitrocalcite, magnesium nitrate and reductive agent formation, 90 ~ 100 DEG C are heated to subsequently with magnetic stirring apparatus, solution, after 0.3 ~ 1 hour, directly moves in the high temperature sintering furnace being heated to 650 ~ 800 DEG C in advance, along with the evaporation of moisture by Keep agitation, there is vigorous combustion, obtain fluffy spumescence product.The present invention adopts the water glass of cost cheaper to be raw material, is conducive to practical application; Obtained powder good dispersion, particle is tiny; Equipment, technique are simple.
Description
Technical field
The invention belongs to inorganic non-metallic ultrafine powder field, particularly relate to a kind of calcium magnesium silicate, specifically a kind of method preparing calcium magnesium silicate powder.
Background technology
Long after glow luminous material is exactly the energy that can absorb and store ambient light radiation by day, the energy stored with the form slow releasing of visible ray to evening thus reach the material of illuminating effect.Compared with sulfide, aluminate long afterglow materials, silicate series long-afterglow material chemical stability is good, and water tolerance is strong, raw material SiO
2inexpensive, be easy to get, therefore the research and development of silicate fluorescent material is subject to extensive concern all over the world.
Obtain long-afterglow material, the preparation of its material is crucial.The preparation of current calcium magnesium silicate base long persistence luminescent material, is mainly undertaken by high temperature solid state reaction and sol-gel method.The powder granule that high temperature solid-state method obtains is comparatively thick, and sintering temperature is higher, long reaction time, needs grinding, but grinding has a certain impact to its luminescent properties, and energy consumption is high, does not meet the theme of current environmental protection.Sol-gel method is a kind of emerging wet chemical synthesis, and obtained powder can reach nano level, affects that it is luminous, and operation is loaded down with trivial details, wayward, and alkoxide used is harmful is unfavorable for scale operation.
Combustion synthesis method is a kind of advanced synthetic technology of material, and it utilizes chemical reaction self-heat generation to prepare material, has the advantages such as technique is simple, energy consumption is low, generated time is short, efficiency is high, product purity is high, less investment.Have at present and adopted combustion synthesis technology to prepare the research report of calcium magnesium silicate, wherein used silicon sol as the source of silicon.But because silicon sol solid content is low, price is high, thus have impact on its large-scale promotion application.
Summary of the invention
For the above-mentioned problems in the prior art, the invention provides a kind of method preparing calcium magnesium silicate powder, described this method will solve in existing preparation method that silicon sol solid content is low, price is high, be difficult to the technical problem of large-scale promotion.
A kind of method preparing calcium magnesium silicate powder of the present invention, comprises the following steps:
1) take nitrocalcite, magnesium nitrate, water glass, reductive agent, the mol ratio of described nitrocalcite, magnesium nitrate, water glass, reductive agent is 1 ~ 2:1 ~ 2:1 ~ 2:6 ~ 30;
2) be dissolved in the water by water glass and make sodium silicate aqueous solution, the concentration of described sodium silicate solution is between 0.5 ~ 2mol/L;
3) nitrocalcite, magnesium nitrate and reductive agent are dissolved completely in deionized water, again sodium silicate aqueous solution is poured into, be heated to 90 ~ 100 DEG C subsequently, Keep agitation is after 0.3 ~ 1 hour, solution is directly moved in the high temperature sintering furnace being heated to 650 ~ 800 DEG C in advance, along with the evaporation of moisture, obtain fluffy spumescence product and calcium magnesium silicate powder.
Further, described reductive agent is any one in urea, citric acid.
Method of the present invention replaces silicon sol for raw material with water glass and adopts combustion synthesis technology to prepare, and thus there is not the problems such as sol-gel method expensive starting materials, technique is loaded down with trivial details, solid content is low, thus has with low cost, the simple technique effect of technique.Method of the present invention does not need external heat source long duration of action, therefore there is not the problems such as sintering temperature is higher, long reaction time, the technique effect that thus to have that thermal treatment temp is low, quick, product is reunited few.
The present invention compares with prior art, and its technical progress is significant.The present invention adopts the water glass of cost cheaper to be raw material, is conducive to practical application.Obtained powder good dispersion, particle is tiny; Equipment, technique are simple.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of embodiment 1.
Fig. 2 is the SEM electromicroscopic photograph of embodiment 1.
Embodiment
Below by specific embodiment, also the present invention is further elaborated by reference to the accompanying drawings, but do not limit the present invention.
Embodiment 1
In nitrocalcite: magnesium nitrate: water glass: the mol ratio=2:1:2:6 ratio batching of urea, nitrocalcite, magnesium nitrate and urea are dissolved completely in deionized water, again the water glass be dissolved in the water is poured into, 90 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 1 hour, solution is directly moved in the high temperature sintering furnace being heated to 650 DEG C in advance, along with the evaporation of moisture, vigorous combustion, obtain fluffy spumescence product, itself XRD and SEM schemes respectively as depicted in figs. 1 and 2, and from XRD figure, product is calcium magnesium silicate Ca substantially
2mgSiO
7phase, as can be seen from SEM figure, the median size of calcium magnesium silicate powder is 0.1mm.
Embodiment 2
In nitrocalcite: magnesium nitrate: water glass: the mol ratio=1:1:1:30 ratio batching of urea, nitrocalcite, magnesium nitrate and urea are dissolved completely in deionized water, again the water glass be dissolved in the water is poured into, 100 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 0.3 hour, solution is directly moved in the high temperature sintering furnace being heated to 800 DEG C in advance, along with the evaporation of moisture, vigorous combustion, obtain fluffy spumescence product, all the other implementation conditions, all with embodiment 1, obtain the CaMgSiO that median size is about 0.38mm
4powder.
Embodiment 3
In nitrocalcite: magnesium nitrate: water glass: the mol ratio=2:2:2:3 ratio batching of citric acid, nitrocalcite, magnesium nitrate and citric acid are dissolved completely in deionized water, again the water glass be dissolved in the water is poured into, 95 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 0.5 hour, solution is directly moved in the high temperature sintering furnace being heated to 700 DEG C in advance, along with the evaporation of moisture, vigorous combustion, obtain fluffy spumescence product, all the other implementation conditions, all with embodiment 1, obtain the CaMgSiO that median size is about 0.12mm
4powder.
Embodiment 4
In nitrocalcite: magnesium nitrate: water glass: the mol ratio=2:1:2:5 ratio batching of citric acid, nitrocalcite, magnesium nitrate and citric acid are dissolved completely in deionized water, again the water glass be dissolved in the water is poured into, 98 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 0.6 hour, solution is directly moved in the high temperature sintering furnace being heated to 750 DEG C in advance, along with the evaporation of moisture, vigorous combustion, obtain fluffy spumescence product, all the other implementation conditions, all with embodiment 1, obtain the Ca that median size is about 0.25mm
2mgSiO
7powder.
The content of above-described embodiment be only the present invention conceive under basic explanation, and according to any equivalent transformation that technical scheme of the present invention is done, all should protection scope of the present invention be belonged to.
Claims (2)
1. prepare a method for calcium magnesium silicate powder, it is characterized in that comprising the following steps:
1) take nitrocalcite, magnesium nitrate, water glass, reductive agent, the mol ratio of described nitrocalcite, magnesium nitrate, water glass, reductive agent is 1 ~ 2:1 ~ 2:1 ~ 2:6 ~ 30;
2) be dissolved in the water by water glass and make sodium silicate aqueous solution, the concentration of described sodium silicate solution is between 0.5 ~ 2mol/L;
3) nitrocalcite, magnesium nitrate and reductive agent are dissolved completely in deionized water, again sodium silicate aqueous solution is poured into, be heated to 90 ~ 100 DEG C subsequently, Keep agitation is after 0.3 ~ 1 hour, solution is directly moved in the high temperature sintering furnace being heated to 650 ~ 800 DEG C in advance, along with the evaporation of moisture, obtain fluffy spumescence product and calcium magnesium silicate powder.
2. a kind of method preparing calcium magnesium silicate powder according to claim 1, is characterized in that: described reductive agent is any one in urea, citric acid.
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| CN201410318067.XA CN104140108B (en) | 2014-07-07 | 2014-07-07 | A kind of method preparing calcium magnesium silicate powder |
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| CN201410318067.XA CN104140108B (en) | 2014-07-07 | 2014-07-07 | A kind of method preparing calcium magnesium silicate powder |
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| CN104140108A CN104140108A (en) | 2014-11-12 |
| CN104140108B true CN104140108B (en) | 2016-04-27 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105219389A (en) * | 2015-10-08 | 2016-01-06 | 上海应用技术学院 | Strontium silicate magnesium raw powder's production technology is prepared in a kind of rare earth Eu, Dy doping |
| CN110127710A (en) * | 2019-06-10 | 2019-08-16 | 河南师范大学 | A kind of silicic acid hydrate calcium and magnesium rheological agent and its energy saving and environment friendly production technology |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101195488A (en) * | 2006-12-05 | 2008-06-11 | 成增勋 | Hydrothermal synthesis production method of magnesium lithium silicate |
| CN101613110A (en) * | 2008-12-16 | 2009-12-30 | 海南美大制药有限公司 | A kind of aluminum-magnesium silicate compound and synthetic method thereof |
| CN101734673A (en) * | 2008-11-20 | 2010-06-16 | 贵阳宝源阳光硅业有限公司 | Calcium silicate and preparation method thereof |
-
2014
- 2014-07-07 CN CN201410318067.XA patent/CN104140108B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101195488A (en) * | 2006-12-05 | 2008-06-11 | 成增勋 | Hydrothermal synthesis production method of magnesium lithium silicate |
| CN101734673A (en) * | 2008-11-20 | 2010-06-16 | 贵阳宝源阳光硅业有限公司 | Calcium silicate and preparation method thereof |
| CN101613110A (en) * | 2008-12-16 | 2009-12-30 | 海南美大制药有限公司 | A kind of aluminum-magnesium silicate compound and synthetic method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Preparation, bioactivity, degradability and primary cell responses to an ordered mesoporous magnesium–calcium silicate;Jingxiong Lu et al.;《Microporous and Mesoporous Materials》;20120711;第163卷;第222页Experimental部分 * |
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