CN103613118B - A kind of preparation method of high-purity magnesium stannate powder - Google Patents
A kind of preparation method of high-purity magnesium stannate powder Download PDFInfo
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Abstract
The invention provides one and be suitable for gas sensor, the preparation method of the high-purity magnesium stannate powder that fire retardant and ceramic industry use, the method is that free alkali is mixed with solution respectively at the SILVER REAGENT sodium stannate crystal of 0.1-0.5% and SILVER REAGENT magnesium chloride, be incubated after first sodium stannate solution being heated to 60 ~ 80 DEG C, get the magnesium chloride solution with molar masss such as sodium stannate solutions again, drop in sodium stannate solution under the condition stirred, the rate of addition controlling magnesium chloride makes the pH value of reaction solution remain on 9.8 ~ 10.8, by reaction solution ageing after magnesium chloride dropwises, sedimentation, washing, three hydrated stannic acid magnesium are obtained after solid-liquid separation and oven dry, the three hydrated stannic acid magnesium calcined dehydration at 700 ~ 850 DEG C will obtained again, cooling obtains anhydrous magnesium stannate finished product.Preparation method of the present invention, operational path is short, and processing parameter easily controls, and the product purity of acquisition is high, particle diameter is little, is suitable for the use of gas sensor, fire retardant and ceramic industry.
Description
Technical field
The present invention relates to a kind of preparation method of stannate, particularly relate to a kind of preparation method of magnesium stannate, more specifically relate to a kind of preparation method being suitable for the high-purity magnesium stannate powder that gas sensor, fire retardant and ceramic industry use.
Background technology
Magnesium stannate, if three hydrated stannic acid magnesium, anhydrous magnesium stannate etc. are a kind of white powders, because it has excellent application performance in dielectric ceramic, gas sensor, humidity sensor, thermally-stabilised electrical equipment, battery electrode material, fire retardant material and architectural pottery, be in recent years subject to extensive concern.But for the synthesis technique of magnesium stannate, the rare open report of document both domestic and external, patent publication No. is the preparation method that the Chinese patent application of CN 101696335A discloses a kind of europium-doped magnesium stannate luminescent material, the method adopts stannic acid, europium nitrate, magnesium nitrate and water to be mixed to form the water-sol, the water-sol flashes to gel, gel obtains europium-doped magnesium stannate luminescent powder after calcining, its complex manufacturing process, be not suitable for suitability for industrialized production, and the method is not the preparation method of pure magnesium stannate, reference value is little; Also there is people to decompose under 850 degree of high temperature with mixing sodium stannate and magnesium sulfate and within 4 hours, prepare the electrode that magnesium stannate is used as lithium cell, owing to being solid state reaction, sodium stannate can not contact cmpletely with magnesium sulfate, the magnesium stannate of preparation mixes a large amount of tindioxide or magnesium oxide, is therefore not suitable for using in gas sensor, fire retardant and ceramic industry.
Summary of the invention
The object of the invention is to overcome above Problems existing and the preparation method that a kind of high-purity magnesium stannate powder is provided, magnesium stannate powder obtained by this method, purity is high, and particle diameter is little, can meet the industries such as dielectric ceramic, architectural pottery, fire retardant to the requirement of magnesium stannate.
For realizing above object, the preparation method of high-purity magnesium stannate powder of the present invention, sodium stannate and magnesium chloride are mixed with respectively sodium stannate solution that tin ion content is 22.25 ~ 44.45g/L and magnesium ion content is the magnesium chloride solution of 4.55 ~ 9.11g/L, be incubated after first sodium stannate solution being heated to 60 ~ 80 DEG C, get the magnesium chloride solution with molar masss such as sodium stannate solutions again, drop in sodium stannate solution under the condition stirred, the rate of addition controlling magnesium chloride makes the pH value of reaction solution remain on 9.8 ~ 10.8, by reaction solution ageing after magnesium chloride dropwises, sedimentation, washing, three hydrated stannic acid magnesium are obtained after solid-liquid separation and oven dry, the three hydrated stannic acid magnesium calcined dehydration at 700 ~ 850 DEG C will obtained again, cooling obtains anhydrous magnesium stannate finished product, above-mentioned sodium stannate is the three hydrated agent level sodium stannate crystal of free alkali at 0.1-0.5%, and magnesium chloride is SILVER REAGENT Magnesium dichloride hexahydrate or Magnesium Chloride Anhydrous.
Above-mentioned free alkali is at the three hydrated agent level sodium stannate crystal of 0.1-0.5%, commercially available analytically pure sodium stannate is added pure water and is dissolved to the solution that sodium stannate concentration is 50-100g/L by preferred employing, then SILVER REAGENT hydronium(ion) stannic oxide is added, free naoh concentration to 5 ~ 20g/L in adjustment solution, refilters, condensing crystal, centrifugal and obtained, SILVER REAGENT hydronium(ion) stannic oxide is Jiang Xihua, sodium hydroxide, pure water is respectively put in reactor, be warming up to 90 ~ 110 DEG C, pass into ozone, reaction to the free sodium hydroxide concentration in reaction solution is 50 ~ 90g/L, obtain stanniferous basic solution, stanniferous filtration of alkaline solution is fallen unreacted scruff completely, filtrate is put into synthesis reaction vessel, open whipping appts, pass into carbon dioxide, when the pH value of reaction solution is 9.0-10.0, stop passing into carbon dioxide, by reacting liquid filtering, washing, centrifugal and obtained, wherein tin flower controls at 1 ︰ 1-1.4 with the mass ratio that feeds intake of sodium hydroxide, the add-on of pure water controls make the concentration of sodium hydroxide be 100g/L ~ 160g/L.
Above-mentioned free alkali, at the three hydrated agent level sodium stannate crystal of 0.1-0.5%, is preferably adopted and is prepared with the following method:
(1) Jiang Xihua, sodium hydroxide, pure water are respectively put in reactor, be warming up to 90 ~ 110 DEG C, pass into ozone, reaction to the free sodium hydroxide concentration in reaction solution is 50 ~ 90g/L, obtain stanniferous basic solution, wherein tin flower controls at 1 ︰ 1-1.4 with the mass ratio that feeds intake of sodium hydroxide, and the add-on of pure water controls make the concentration of sodium hydroxide be 100g/L ~ 160g/L;
(2) add SILVER REAGENT hydronium(ion) stannic oxide in the stanniferous basic solution obtained in step (1), free naoh concentration to 5 ~ 20g/L in adjustment solution, again passing into ozone to solution is water white transparency, filters to obtain sodium stannate stoste;
(3) the sodium stannate stoste that step (2) obtains is joined in concentration response still, low whipping speed is under the condition of 10 ~ 30 revs/min, when having most of crystallization in evaporation concentration to solution, stops concentrated, blanking is to whizzer, and centrifugal gained crystallization is finished product sodium stannate;
Wherein the SILVER REAGENT hydronium(ion) stannic oxide of step (2) is that the stanniferous filtration of alkaline solution that step (1) obtains is fallen unreacted scruff completely, filtrate is put into synthesis reaction vessel, open whipping appts, pass into carbon dioxide, when the pH value of reaction solution is 9.0-10.0, stop passing into carbon dioxide, by reacting liquid filtering, washing, centrifugal and obtained.
In order to reduce the absorption of impurity in precipitation surface, in above-mentioned magnesium stannate raw powder's production technology, the aging condition of reaction solution is 60 ~ 80 DEG C of insulated and stirred more than 1 hour, then standing sedimentation more than 1 hour.
In order to better removing does not have magnesium chloride and the sodium stannate of complete reaction, in above-mentioned magnesium stannate raw powder's production technology, washing washs 30 minutes, standing sedimentation 3 hours, preferred 3-6 time of washing times by the deionized water and stirring of 60-80 DEG C.
In order to control the content of three hydrated stannic acid magnesium crystal water, in above-mentioned magnesium stannate raw powder's production technology, the preferred 90-100 DEG C of bake out temperature.
In order to better control the purity of anhydrous magnesium stannate, in above-mentioned magnesium stannate raw powder's production technology, calcining temperature preferably 750 ~ 800 DEG C, calcination time is 2 ~ 6 hours.
In the preparation method of above-mentioned low free alkali sodium stannate, the tin of step (1) spends preferred 0# tin, sodium hydroxide preferred reagent sodium hydroxide.
The preparation method of high-purity magnesium stannate powder of the present invention, by adopting the sodium stannate of low free alkali and SILVER REAGENT Magnesium dichloride hexahydrate or Magnesium Chloride Anhydrous as raw material, the pH value simultaneously controlling reaction system remains on 9.8 ~ 10.8, the generation of stannic oxide and metastannic acid can be avoided, ensure that the magnesium stannate foreign matter content obtained is few, and react again after sodium stannate and magnesium chloride are first mixed with certain density solution, be conducive to the control of speed of response, ensure the even of product cut size.Preparation method of the present invention, material composition is single, reaction process inclusion-free generates, operational path is short, and simple to operate, processing parameter easily controls, the product magnesium stannate of acquisition, inorganic, organic impurity content is low, purity is high, and particle diameter is little, is suitable for the use of gas sensor, fire retardant and ceramic industry.
Embodiment
Here is the several specific embodiment of the present invention, and these embodiments are illustrating high-purity magnesium stannate powder preparation method of the present invention just, and be not used to limit the scope of the invention.
Embodiment 1
Commercially available analytical pure sodium stannate being added the concentration that pure water is dissolved to sodium stannate is the solution of 200g/L, add analytical pure hydronium(ion) stannic oxide, in adjustment sodium stannate solution, the concentration of free sodium hydroxide is 5g/L, then by reacting liquid filtering, condensing crystal, centrifugally the three hydration analytical pure sodium stannate crystal that free alkali is 0.1% are obtained, with pure water, sodium stannate is configured to the solution that tin concentration is 22.25g/L, get 500ml sodium stannate solution heating in water bath to 60 DEG C, separately get SILVER REAGENT Magnesium dichloride hexahydrate, be configured to the solution that magnesium density is 4.55g/L, magnesium chloride solution is dripped in sodium stannate solution under the condition stirred, the rate of addition controlling magnesium chloride makes the pH value of reaction solution remain on 9.8, wait drip with the magnesium chloride solution of the molar masss such as sodium stannate after, by reaction solution insulated and stirred 1.5 hours at 65 DEG C, then standing sedimentation 1.5 hours, obtain white solid, with 80 DEG C of deionized waters to white solids wash 4 times, centrifugation, at 90 DEG C of oven dryings, obtain three hydrated stannic acid magnesium, analyzing its content is 99%.
Embodiment 2
Commercially available analytical pure sodium stannate being added the concentration that pure water is dissolved to sodium stannate is the solution of 200g/L, add analytical pure hydronium(ion) stannic oxide, in adjustment sodium stannate solution, the concentration of free sodium hydroxide is 20g/L, then condensing crystal, centrifugally obtains the three hydration analytical pure sodium stannate crystal that free alkali is 0.5%, with pure water, sodium stannate is configured to the solution that tin concentration is 44.5g/L, get 500ml sodium stannate solution heating in water bath to 80 DEG C, separately get SILVER REAGENT Magnesium dichloride hexahydrate, be configured to the solution that magnesium density is 9.11g/L, magnesium chloride solution is dripped in sodium stannate solution under the condition stirred, the rate of addition controlling magnesium chloride makes the pH value of reaction solution remain on 10.5, wait drip with the magnesium chloride solution of the molar masss such as sodium stannate after, by reaction solution insulated and stirred 2 hours at 75 DEG C, then standing sedimentation 1.5 hours, obtain white solid, with 60 DEG C of deionized waters to after white solids wash 6 times, centrifugation, solid is dried at 110 DEG C, obtain three hydrated stannic acid magnesium, three hydrated stannic acid magnesium are calcined 5h in the tunnel furnace of 700 DEG C, obtained anhydrous magnesium stannate powder, analyzing its content is 99.1%.
Embodiment 3
1, the preparation of hydronium(ion) stannic oxide:
Tin is spent with sodium hydroxide in mass ratio for 1:1 is fed in reactor, in reactor, add pure water again makes naoh concentration be 100g/L, then 95 DEG C are warming up to, pass into ozone, and keep the pressure in reactor to be 0.1Mpa, the concentration of reaction solution free sodium hydroxide in the coronite detection reaction still of limit, when free sodium hydroxide reaction solution in reactor being detected is 50g/L, take out stanniferous basic solution, filter out unreacted scruff completely, then stanniferous basic solution is put into synthesis reaction vessel, open whipping appts, pass into carbon dioxide, when pH value reaction solution being detected is 9.0, stop passing into carbonic acid gas, by reacting liquid filtering, obtain white solid, be that 4:1 wash 3 time to white solid with liquid-solid ratio with pure water, the hydronium(ion) stannic oxide of solid-liquid separation white,
2, the preparation of low free alkali sodium stannate
Tin is spent with sodium hydroxide in mass ratio for 1:1.4 is fed in reactor, in reactor, add pure water again makes naoh concentration be 140g/L, then be warming up to 100 DEG C, pass into ozone, and keep the pressure in reactor to be 0.2Mpa, the concentration of reaction solution free sodium hydroxide in the coronite detection reaction still of limit, when detecting that the free sodium hydroxide of reaction solution in reactor is 80g/L, take out stanniferous basic solution, progressively add above-mentioned obtained hydronium(ion) stannic oxide, the free sodium hydroxide concentration adjusting to reaction solution is 5g/L, continuing to pass into ozone to reaction solution is water white transparency, then by reacting liquid filtering, add in concentration response still by filtering the solution obtained, the stirring velocity of adjustment agitator is 10 revs/min, evaporation concentration is separated out to there being mass crystallization, crystallization is put into centrifuge dehydration, obtain three hydrated stannic acid sodium crystals, test by analysis, indices is as shown in the table, meet analytical pure standard,
3, the preparation of magnesium stannate
With pure water, above-mentioned low free alkali sodium stannate crystal is configured to the sodium stannate solution that tin ion concentration is 44.5g/L, get 500ml sodium stannate solution heating in water bath to 70 DEG C, separately get SILVER REAGENT Magnesium dichloride hexahydrate, be configured to the magnesium chloride solution that magnesium density is 6g/L, slowly join in sodium stannate solution, magnesium chloride solution is dripped in sodium stannate solution under the condition stirred, the rate of addition controlling magnesium chloride makes the pH value of reaction solution remain on 10, wait drip with the magnesium chloride solution of the molar masss such as sodium stannate after, by reaction solution insulated and stirred 2 hours at 80 DEG C, then standing sedimentation 2 hours, obtain white solid, with 70 DEG C of deionized waters to after white solids wash 5 times, centrifugation, solid is put into baking oven to dry at 100 DEG C, obtain three hydrated stannic acid magnesium powders, detecting its content is 99.2%, , by three hydrated stannic acid magnesium powders in 800 DEG C of calcinings, obtain anhydrous magnesium stannate powder, detected result: the content of anhydrous magnesium stannate is 99%.
product checking:
Tested by the three hydrated stannic acid magnesium that obtain embodiment 1,2,3 and anhydrous sodium stannate powder, all technical is as following table:
Three hydrated stannic acid magnesium quality and technical index: %
Anhydrous magnesium stannate quality and technical index: %
| MgSnO 3 | Cu | Fe | Pb | Sb | Vitriol | Nitrate | Particle diameter≤20um |
| ≥99% | ≤15ppm | ≤25ppm | ≤15ppm | ≤15ppm | ≤0.01% | ≤0.01% | ≥98% |
Claims (8)
1. the preparation method of a high-purity magnesium stannate powder, it is characterized in that: sodium stannate and magnesium chloride are mixed with sodium stannate solution that tin ion content is 22.25 ~ 44.45g/L and magnesium ion content is the magnesium chloride solution of 4.55 ~ 9.11g/L by described preparation method respectively, be incubated after first sodium stannate solution being heated to 60 ~ 80 DEG C, get the magnesium chloride solution with molar masss such as sodium stannate solutions again, drop in sodium stannate solution under the condition stirred, the rate of addition controlling magnesium chloride makes the pH value of reaction solution remain on 9.8 ~ 10.8, by reaction solution ageing after magnesium chloride dropwises, sedimentation, washing, three hydrated stannic acid magnesium are obtained after solid-liquid separation and oven dry, again by three hydrated stannic acid magnesium calcined dehydration at 700 ~ 850 DEG C, cooling obtains anhydrous magnesium stannate finished product, wherein sodium stannate is the three hydrated agent level sodium stannate crystal of free alkali at 0.1-0.5%, and magnesium chloride is SILVER REAGENT Magnesium dichloride hexahydrate or Magnesium Chloride Anhydrous.
2. the preparation method of high-purity magnesium stannate powder according to claim 1, it is characterized in that: described free alkali is at the three hydrated agent level sodium stannate crystal of 0.1-0.5%, adopt commercially available analytically pure sodium stannate is added pure water to be dissolved to the solution that sodium stannate concentration is 50-100g/L, then SILVER REAGENT hydronium(ion) stannic oxide is added, free naoh concentration to 5 ~ 20g/L in adjustment solution, refilters, condensing crystal, centrifugal and obtained, SILVER REAGENT hydronium(ion) stannic oxide is Jiang Xihua, sodium hydroxide, pure water is respectively put in reactor, be warming up to 90 ~ 110 DEG C, pass into ozone, reaction to the free sodium hydroxide concentration in reaction solution is 50 ~ 90g/L, obtain stanniferous basic solution, stanniferous filtration of alkaline solution is fallen unreacted scruff completely, filtrate is put into synthesis reaction vessel, open whipping appts, pass into carbon dioxide, when the pH value of reaction solution is 9.0-10.0, stop passing into carbon dioxide, by reacting liquid filtering, washing, centrifugal and obtained, wherein tin flower controls at 1 ︰ 1-1.4 with the mass ratio that feeds intake of sodium hydroxide, the add-on of pure water controls make the concentration of sodium hydroxide be 100g/L ~ 160g/L.
3. the preparation method of high-purity magnesium stannate powder according to claim 1, is characterized in that: described free alkali, at the three hydrated agent level sodium stannate crystal of 0.1-0.5%, is adopt to prepare with the following method:
(1) Jiang Xihua, sodium hydroxide, pure water are respectively put in reactor, be warming up to 90 ~ 110 DEG C, pass into ozone, reaction to the free sodium hydroxide concentration in reaction solution is 50 ~ 90g/L, obtain stanniferous basic solution, wherein tin flower controls at 1 ︰ 1-1.4 with the mass ratio that feeds intake of sodium hydroxide, and the add-on of pure water controls make the concentration of sodium hydroxide be 100g/L ~ 160g/L;
(2) add SILVER REAGENT hydronium(ion) stannic oxide in the stanniferous basic solution obtained in step (1), free naoh concentration to 5 ~ 20g/L in adjustment solution, again passing into ozone to solution is water white transparency, filters to obtain sodium stannate stoste;
(3) the sodium stannate stoste that step (2) obtains is joined in concentration response still, low whipping speed is under the condition of 10 ~ 30 revs/min, when having most of crystallization in evaporation concentration to solution, stops concentrated, blanking is to whizzer, and centrifugal gained crystallization is finished product three hydrated stannic acid sodium crystal;
Wherein the SILVER REAGENT hydronium(ion) stannic oxide of step (2) is that the stanniferous filtration of alkaline solution that step (1) obtains is fallen unreacted scruff completely, filtrate is put into synthesis reaction vessel, open whipping appts, pass into carbon dioxide, when the pH value of reaction solution is 9.0-10.0, stop passing into carbon dioxide, by reacting liquid filtering, washing, centrifugal and obtained.
4. the preparation method of the high-purity magnesium stannate powder according to claim 1,2 or 3, it is characterized in that: in described magnesium stannate raw powder's production technology, the aging condition of reaction solution is 60 ~ 80 DEG C of insulated and stirred more than 1 hour, then standing sedimentation more than 1 hour.
5. the preparation method of high-purity magnesium stannate powder according to claim 4, it is characterized in that: in described magnesium stannate raw powder's production technology, washing washs 30 minutes, standing sedimentation 3 hours by the deionized water and stirring of 60-80 DEG C, and washing times is 3-6 time.
6. the preparation method of high-purity magnesium stannate powder according to claim 5, is characterized in that: in described magnesium stannate raw powder's production technology, and bake out temperature is 90-100 DEG C.
7. the preparation method of high-purity magnesium stannate powder according to claim 6, is characterized in that: in described magnesium stannate raw powder's production technology, and calcining temperature is 750 ~ 800 DEG C, and calcination time is 2 ~ 6 hours.
8. the preparation method of high-purity magnesium stannate powder according to claim 3, it is characterized in that: described free alkali is in the preparation method of the three hydrated agent level sodium stannate crystal of 0.1-0.5%, the tin flower of step (1) is 0# tin, and sodium hydroxide is reagent grade sodium hydroxide.
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| GB2552840A (en) * | 2016-08-12 | 2018-02-14 | William Blythe Ltd | Synthesis of and uses of alkaline earth metal stannates |
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| CN105800672B (en) * | 2016-03-02 | 2017-05-24 | 广东光华科技股份有限公司 | Preparation method of zinc hydroxystannate ultrafine powder and zinc stannate ultrafine powder |
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| EP2644723A1 (en) * | 2012-03-26 | 2013-10-02 | Umicore AG & Co. KG | Composite material |
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| EP2644723A1 (en) * | 2012-03-26 | 2013-10-02 | Umicore AG & Co. KG | Composite material |
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