CN106495227B - A kind of preparation method of oil-soluble dispersed nano manganese dioxide powder - Google Patents
A kind of preparation method of oil-soluble dispersed nano manganese dioxide powder Download PDFInfo
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Abstract
A kind of preparation method of oil-soluble dispersed nano manganese dioxide powder, it is related to a kind of nano-manganese dioxide raw powder's production technology.It is not oil-soluble the invention aims to solve the manganese dioxide of existing method preparation, the manganese dioxide size of preparation is big, the problem of easily reunion.Method：First, liquor potassic permanganate is prepared；2nd, hydrogenperoxide steam generator is prepared；3rd, hydrogenperoxide steam generator is added dropwise into liquor potassic permanganate, sedimentation agent is added after stirring reaction, is stirred for reacting；Cooled again, stood, cleaned, dried, ground, obtain oil-soluble dispersed nano manganese dioxide powder.The particle diameter of oil-soluble dispersed nano manganese dioxide powder prepared by the present invention is 1nm~80nm, and the present invention can obtain the crystal formation and pattern that size is small, mono-dispersed nano manganese dioxide is stable.The present invention is applied to prepare oil-soluble dispersed nano manganese dioxide powder.
Description
Technical field
The present invention relates to a kind of nano-manganese dioxide raw powder's production technology.
Background technology
Manganese dioxide is a kind of quite varied inorganic amphoteric oxide of purposes, due to there is the physicochemical characteristics of uniqueness,
Preparation technology is simple, and the reasons such as cost is relatively low, abundant raw materials, environmental pollution are low are widely used.Such as：Used in chemical reaction
Make catalyst, serve as polarization agent, biological molecular sieve, energy storage medium, lithium ion battery, ultracapacitor, glass in the battery
Good decolorising agent in glass industry etc., can be also used for pyrotechnics, the iron purification of water, medicine, fertilizer and fabric printing, paint and
The drier of ink.Therefore the preparation technology of research manganese dioxide has been applied to vital effect.And nanoscale dioxy
Change manganese because of the granular of its particle size, specific surface area increases severely and generates the effect of the surface not available for conventional manganese bioxide material
Should, the increase of size dimension effect, i.e. surface area, activity centre increase, reacting environment increases, and can increase electric discharge in electrode reaction
Capacity.More preferable catalytic action may also be played in chemical reaction.
Therefore, the scientists numerous studies preparation technology of manganese dioxide.But manganese dioxide prepared by existing method is not
It is oil-soluble, size is big, and manganese dioxide is easily reunited.
The content of the invention
It is not oil-soluble, the manganese dioxide of preparation the invention aims to solve the manganese dioxide of existing method preparation
Size is big, the problem of easily reunion, and provides a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder.
A kind of preparation method of oil-soluble dispersed nano manganese dioxide powder, is completed according to the following steps：
First, potassium permanganate is dissolved into distilled water, obtains liquor potassic permanganate；
The mass fraction of liquor potassic permanganate described in step 1 is 3%~10%；
2nd, the hydrogenperoxide steam generator that mass fraction is 30% is diluted, obtains the mistake that mass fraction is 2%~5%
Hydrogen peroxide solution；
3rd, the liquor potassic permanganate obtained in step 1 is heated to 35 DEG C~50 DEG C, then to temperature be 35 DEG C~50 DEG C
Liquor potassic permanganate in using 5 drops/min~15 drops/min rate of addition be added dropwise mass fraction that step 2 obtains as 2%~
5% hydrogenperoxide steam generator；Obtain reaction solution；Reaction solution is warming up to 75 DEG C~85 DEG C, then temperature be 75 DEG C~85 DEG C and
Mixing speed is stirring reaction 5min~15min under 300r/min~800r/min, then sedimentation agent is added into reaction solution, then
Temperature is 75 DEG C~85 DEG C and mixing speed is stirring reaction 40min~60min under 300r/min~800r/min；
The mol ratio of potassium permanganate and hydrogen peroxide is 1 in reaction solution described in step 3:(1.5~2.5)；
The quality of sedimentation agent described in step 3 and the volume ratio of reaction solution are (0.1g~1g):100mL；
4th, low whipping speed is that will be reacted with 2 DEG C/min~5 DEG C/min cooling rate under 300r/min~800r/min
The temperature of liquid is down to 30 DEG C~35 DEG C from 75 DEG C~85 DEG C, then stops stirring, and stands 10min~20min；By the upper strata after standing
Clear liquid is poured out, and filters the MnO of lower floor2, the solid matter after being filtered；After the water that temperature in use is 85 DEG C~95 DEG C is to filtering
Solid matter clean 3 times~5 times, reuse methanol clean 2 times~4 times, the MnO after being cleaned2Powder；
5th, by the MnO after cleaning2Powder dries 2h~5h at being 25 DEG C~35 DEG C in temperature, then is ground, and obtains oil
Dissolubility dispersed nano manganese dioxide powder；
The particle diameter of oil-soluble dispersed nano manganese dioxide powder described in step 5 is 1nm~80nm.
The principle and advantage of the present invention：
First, reaction equation of the invention is：
2MnO4 -+4H2O2→2MnO2+2H2O+5O2(g)+2OH-；
2nd, on the one hand the sedimentation agent that the present invention adds can make MnO2Little particle is easily separated from the aqueous solution, another
Aspect, the reunion of nano particle is prevented, particle size distribution can narrow, and improve the stability of powder, expand its application neck
Domain；
3rd, oil-soluble dispersed nano manganese dioxide powder prepared by the present invention and existing manganese dioxide powder body phase ratio, system
Standby technique is simple, and cost is low, and particle size distribution is narrow, due to the stability for the powder that the cladding of oleic acid improves, becomes its application
Obtain more extensive；
4th, the particle diameter of oil-soluble dispersed nano manganese dioxide powder prepared by the present invention is 1nm~80nm, present invention side
Method can obtain the crystal formation and pattern that size is small, mono-dispersed nano manganese dioxide is stable；
5th, method technique of the invention is simple, so that the application field of nano-manganese dioxide is wider, makes its performance whole
Show.
The present invention is applied to prepare oil-soluble dispersed nano manganese dioxide powder.
Brief description of the drawings
Fig. 1 is the SEM figures of the oil-soluble dispersed nano manganese dioxide powder prepared in the step 5 of embodiment one.
Embodiment
Embodiment one：Present embodiment is a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder
Complete according to the following steps：
First, potassium permanganate is dissolved into distilled water, obtains liquor potassic permanganate；
The mass fraction of liquor potassic permanganate described in step 1 is 3%~10%；
2nd, the hydrogenperoxide steam generator that mass fraction is 30% is diluted, obtains the mistake that mass fraction is 2%~5%
Hydrogen peroxide solution；
3rd, the liquor potassic permanganate obtained in step 1 is heated to 35 DEG C~50 DEG C, then to temperature be 35 DEG C~50 DEG C
Liquor potassic permanganate in using 5 drops/min~15 drops/min rate of addition be added dropwise mass fraction that step 2 obtains as 2%~
5% hydrogenperoxide steam generator；Obtain reaction solution；Reaction solution is warming up to 75 DEG C~85 DEG C, then temperature be 75 DEG C~85 DEG C and
Mixing speed is stirring reaction 5min~15min under 300r/min~800r/min, then sedimentation agent is added into reaction solution, then
Temperature is 75 DEG C~85 DEG C and mixing speed is stirring reaction 40min~60min under 300r/min~800r/min；
The mol ratio of potassium permanganate and hydrogen peroxide is 1 in reaction solution described in step 3:(1.5~2.5)；
The quality of sedimentation agent described in step 3 and the volume ratio of reaction solution are (0.1g~1g):100mL；
4th, low whipping speed is that will be reacted with 2 DEG C/min~5 DEG C/min cooling rate under 300r/min~800r/min
The temperature of liquid is down to 30 DEG C~35 DEG C from 75 DEG C~85 DEG C, then stops stirring, and stands 10min~20min；By the upper strata after standing
Clear liquid is poured out, and filters the MnO of lower floor2, the solid matter after being filtered；After the water that temperature in use is 85 DEG C~95 DEG C is to filtering
Solid matter clean 3 times~5 times, reuse methanol clean 2 times~4 times, the MnO after being cleaned2Powder；
5th, by the MnO after cleaning2Powder dries 2h~5h at being 25 DEG C~35 DEG C in temperature, then is ground, and obtains oil
Dissolubility dispersed nano manganese dioxide powder；
The particle diameter of oil-soluble dispersed nano manganese dioxide powder described in step 5 is 1nm~80nm.
The principle and advantage of present embodiment：
First, the reaction equation of present embodiment is：
2MnO4 -+4H2O2→2MnO2+2H2O+5O2(g)+2OH-；
2nd, on the one hand the sedimentation agent that present embodiment adds can make MnO2Little particle is easily separated from the aqueous solution,
On the other hand, the reunion of nano particle is prevented, particle size distribution can narrow, and improve the stability of powder, and expanding it should
Use field；
3rd, oil-soluble dispersed nano manganese dioxide powder prepared by present embodiment and existing manganese dioxide powder body phase
Than preparation technology is simple, and cost is low, and particle size distribution is narrow, due to the stability for the powder that the cladding of oleic acid improves, makes it should
With becoming more extensive；
4th, the particle diameter of oil-soluble dispersed nano manganese dioxide powder prepared by present embodiment is 1nm~80nm, this reality
The crystal formation and pattern that size is small, mono-dispersed nano manganese dioxide is stable can be obtained by applying methods；
5th, the method technique of present embodiment is simple, so that the application field of nano-manganese dioxide is wider, makes its performance
All show.
Present embodiment is applied to prepare oil-soluble dispersed nano manganese dioxide powder.
Embodiment two：Present embodiment is with the difference of embodiment one：Gao Meng described in step 1
The mass fraction of sour potassium solution is 3%~5%.Other steps are identical with embodiment one.
Embodiment three：Present embodiment is with one of embodiment one or two difference：Institute in step 1
The mass fraction for the liquor potassic permanganate stated is 5%~10%.Other steps are identical with embodiment one or two.
Embodiment four：Present embodiment is with one of embodiment one to three difference：Will in step 2
The hydrogenperoxide steam generator that mass fraction is 30% is diluted, and obtains the hydrogenperoxide steam generator that mass fraction is 2%~3%.Its
His step is identical with embodiment one to three.
Embodiment five：Present embodiment is with one of embodiment one to four difference：Will in step 2
The hydrogenperoxide steam generator that mass fraction is 30% is diluted, and obtains the hydrogenperoxide steam generator that mass fraction is 3%~5%.Its
His step is identical with embodiment one to four.
Embodiment six：Present embodiment is with one of embodiment one to five difference：Institute in step 3
The mol ratio of potassium permanganate and hydrogen peroxide is 1 in the reaction solution stated:2.Other steps are identical with embodiment one to five.
Embodiment seven：Present embodiment is with one of embodiment one to six difference：Institute in step 3
The sedimentation agent stated is oleic acid or oleyl amine.Other steps are identical with embodiment one to six.
Embodiment eight：Present embodiment is with one of embodiment one to seven difference：Will in step 3
The liquor potassic permanganate obtained in step 1 is heated to 40 DEG C, then into the liquor potassic permanganate that temperature is 40 DEG C with 10 drops/min
Rate of addition the hydrogenperoxide steam generator that the obtained mass fraction of step 2 is 3% is added dropwise；Obtain reaction solution；Reaction solution is heated up
To 80 DEG C, then the stirring reaction 10min in the case where temperature is 80 DEG C and mixing speed is 500r/min, then sedimentation is added into reaction solution
Agent, then the stirring reaction 60min in the case where temperature is 80 DEG C and mixing speed is 500r/min.Other steps and embodiment one
It is identical to seven.
Embodiment nine：Present embodiment is with one of embodiment one to eight difference：In step 4
Mixing speed is that the temperature of reaction solution is down into 30 DEG C from 80 DEG C with 3 DEG C/min cooling rate under 500r/min, then stops stirring
Mix, stand 10min；Supernatant liquor after standing is poured out, filters the MnO of lower floor2, the solid matter after being filtered；Use
The water that temperature is 90 DEG C cleans 3 times to the solid matter after filtering, reuses methanol and cleans 2 times, the MnO after being cleaned2Powder
End.Other steps are identical with embodiment one to eight.
Embodiment ten：Present embodiment is with one of embodiment one to nine difference：Institute in step 5
The particle diameter for the oil-soluble dispersed nano manganese dioxide powder stated is 20nm.Other steps and the phase of embodiment one to nine
Together.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：A kind of preparation method of oil-soluble dispersed nano manganese dioxide powder, is to complete according to the following steps
's：
First, potassium permanganate is dissolved into distilled water, obtains liquor potassic permanganate；
The mass fraction of liquor potassic permanganate described in step 1 is 5%；
2nd, the hydrogenperoxide steam generator that mass fraction is 30% is diluted, obtains the hydrogen peroxide that mass fraction is 3%
Solution；
3rd, the liquor potassic permanganate obtained in step 1 is heated to 40 DEG C, then it is molten to the potassium permanganate that temperature is 40 DEG C
Mass fraction that step 2 obtains is added dropwise as 3% hydrogenperoxide steam generator using 10 drops/min rate of addition in liquid；Reacted
Liquid；Reaction solution is warming up to 80 DEG C, then the stirring reaction 10min in the case where temperature is 80 DEG C and mixing speed is 500r/min, then to
Sedimentation agent, then the stirring reaction 60min in the case where temperature is 80 DEG C and mixing speed is 500r/min are added in reaction solution；
The mol ratio of potassium permanganate and hydrogen peroxide is 1 in reaction solution described in step 3:2.5；
The quality of sedimentation agent described in step 3 and the volume ratio of reaction solution are 1g:100mL；
4th, low whipping speed is to be down to the temperature of reaction solution from 80 DEG C with 3 DEG C/min cooling rate under 500r/min
30 DEG C, then stop stirring, stand 10min；Supernatant liquor after standing is poured out, filters the MnO of lower floor2, after being filtered
Solid matter；The water that temperature in use is 90 DEG C cleans 3 times to the solid matter after filtering, reuses methanol and cleans 2 times, obtains clear
MnO after washing2Powder；
5th, by the MnO after cleaning2Powder dries 4h at being 30 DEG C in temperature, then is ground, and obtains oil-soluble single dispersing
Nano-manganese dioxide powder；
The particle diameter of oil-soluble dispersed nano manganese dioxide powder described in step 5 is 20nm.
Fig. 1 is the SEM figures of the oil-soluble dispersed nano manganese dioxide powder prepared in the step 5 of embodiment one, from Fig. 1
Understand, the particle diameter of oil-soluble dispersed nano manganese dioxide powder prepared by embodiment one is about 20nm, and size is small, and pattern is equal
One.
Oil-soluble dispersed nano manganese dioxide powder prepared by embodiment one can be applied makees depolarizing agent in the battery,
Decolorising agent in glass industry, the drier, fabric printing agent etc. of the catalyst of organic synthesis, paint and ink；Due to
Size is small, and shape is homogeneous, and the effect of repid discharge is can reach when being applied in the battery after surface treatment；Catalysis in organic synthesis
Efficiency also has very high lifting；Applied in coating and printing and dyeing is to have good organic dispersiveness.
Claims (9)
1. a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder, it is characterised in that a kind of oil-soluble single dispersing is received
The preparation method of rice manganese dioxide powder is completed according to the following steps：
First, potassium permanganate is dissolved into distilled water, obtains liquor potassic permanganate；
The mass fraction of liquor potassic permanganate described in step 1 is 3%~10%；
2nd, the hydrogenperoxide steam generator that mass fraction is 30% is diluted, obtains the peroxidating that mass fraction is 2%~5%
Hydrogen solution；
3rd, the liquor potassic permanganate obtained in step 1 is heated to 35 DEG C~50 DEG C, then to the height that temperature is 35 DEG C~50 DEG C
The mass fraction obtained in potassium manganate solution using 5 drops/min~15 drops/min rate of addition dropwise addition step 2 is 2%~5%
Hydrogenperoxide steam generator；Obtain reaction solution；Reaction solution is warming up to 75 DEG C~85 DEG C, then for 75 DEG C~85 DEG C and stirred fast in temperature
Spend for stirring reaction 5min~15min under 300r/min~800r/min, then sedimentation agent is added into reaction solution, then be in temperature
75 DEG C~85 DEG C are stirring reaction 40min~60min under 300r/min~800r/min with mixing speed；
Sedimentation agent described in step 3 is oleic acid or oleyl amine；
The mol ratio of potassium permanganate and hydrogen peroxide is 1 in reaction solution described in step 3:(1.5~2.5)；
The quality of sedimentation agent described in step 3 and the volume ratio of reaction solution are (0.1g~1g):100mL；
4th, low whipping speed is by reaction solution under 300r/min~800r/min with 2 DEG C/min~5 DEG C/min cooling rate
Temperature is down to 30 DEG C~35 DEG C from 75 DEG C~85 DEG C, then stops stirring, and stands 10min~20min；By the supernatant liquor after standing
Pour out, filter the MnO of lower floor2, the solid matter after being filtered；Temperature in use is 85 DEG C~95 DEG C of water to consolidating after filtering
Body material cleans 3 times~5 times, reuses methanol and cleans 2 times~4 times, the MnO after being cleaned2Powder；
5th, by the MnO after cleaning2Powder dries 2h~5h at being 25 DEG C~35 DEG C in temperature, then is ground, and obtains oil-soluble
Dispersed nano manganese dioxide powder；
The particle diameter of oil-soluble dispersed nano manganese dioxide powder described in step 5 is 1nm~80nm.
2. a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The mass fraction of liquor potassic permanganate described in step 1 is 3%~5%.
3. a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The mass fraction of liquor potassic permanganate described in step 1 is 5%~10%.
4. a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The hydrogenperoxide steam generator that mass fraction is 30% is diluted in step 2, obtains the peroxide that mass fraction is 2%~3%
Change hydrogen solution.
5. a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The hydrogenperoxide steam generator that mass fraction is 30% is diluted in step 2, obtains the peroxide that mass fraction is 3%~5%
Change hydrogen solution.
6. a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The mol ratio of potassium permanganate and hydrogen peroxide is 1 in reaction solution described in step 3:2.
7. a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The liquor potassic permanganate obtained in step 1 is heated to 40 DEG C in step 3, then to the liquor potassic permanganate that temperature is 40 DEG C
In mass fraction that step 2 obtains is added dropwise as 3% hydrogenperoxide steam generator using 10 drops/min rate of addition；Obtain reaction solution；
Reaction solution is warming up to 80 DEG C, then the stirring reaction 10min in the case where temperature is 80 DEG C and mixing speed is 500r/min, then to reaction
Sedimentation agent, then the stirring reaction 60min in the case where temperature is 80 DEG C and mixing speed is 500r/min are added in liquid.
8. a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
Low whipping speed is that the temperature of reaction solution is down into 30 from 80 DEG C with 3 DEG C/min cooling rate under 500r/min in step 4
DEG C, then stop stirring, stand 10min；Supernatant liquor after standing is poured out, filters the MnO of lower floor2, consolidating after being filtered
Body material；The water that temperature in use is 90 DEG C cleans 3 times to the solid matter after filtering, reuses methanol and cleans 2 times, is cleaned
MnO afterwards2Powder.
9. a kind of preparation method of oil-soluble dispersed nano manganese dioxide powder according to claim 1, its feature exist
The particle diameter of oil-soluble dispersed nano manganese dioxide powder described in step 5 is 20nm.
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| CN1515632A (en) * | 2003-08-26 | 2004-07-28 | 武汉理工大学 | Preparation method of inorganic-organic composite particle and its special-purpose equipment |
| CN105032404A (en) * | 2015-07-28 | 2015-11-11 | 福州大学 | Calcination-free MnO2/CNTs low-temperature denitration catalyst and preparation method thereof |
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| CN1515632A (en) * | 2003-08-26 | 2004-07-28 | 武汉理工大学 | Preparation method of inorganic-organic composite particle and its special-purpose equipment |
| CN105032404A (en) * | 2015-07-28 | 2015-11-11 | 福州大学 | Calcination-free MnO2/CNTs low-temperature denitration catalyst and preparation method thereof |
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