CN104709913A - Novel nano silica powder preparation method - Google Patents
Novel nano silica powder preparation method Download PDFInfo
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- CN104709913A CN104709913A CN201410852465.XA CN201410852465A CN104709913A CN 104709913 A CN104709913 A CN 104709913A CN 201410852465 A CN201410852465 A CN 201410852465A CN 104709913 A CN104709913 A CN 104709913A
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Abstract
The invention relates to a novel nano silica powder preparation method, and relates to an anode electrolytic deposition method for preparing the nano silica powder. The method can solve the problems of large powder particle size, easy agglomeration of particles, and nonuniform particle size during the preparation process. By employing a two-room electrolytic method, electrolytic current density of inert electrode is controlled in an anode chamber, under strong stirring environment, by reducing pH value of a sodium silicate solution in an anode chamber, ultrafine silicic acid deposition can be obtained, steps of filtering, washing by deionized water, washing with absolute ethyl alcohol and drying are carried out to obtain the ultrafine silicic acid powder, and nano level silica powder with granularity being 60-85nm can be obtained by pyrolysis at certain temperature. The method has the characteristics of simple process and convenient operation control.
Description
Technical field
The invention belongs to technical field prepared by nano material powder, be specifically related to a kind of novel nano silica powder preparation method.
Background technology
Nano silicon is that a kind of particle size is little, the ultrafine powder that specific surface area is large, there is quantum size, the effects such as quantum tunneling, show special light, electrical characteristic, high magnetic resistance, what still have under nonlinear resistance and high temperature is high-strength, high-ductility, the Strange properties such as good stability, nano silica powder is made to be widely used in electronic package material, polymer composite, plastics, coating, rubber, pigment, pottery, tackiness agent, glass reinforced plastic, pharmaceutical carrier, the field such as makeup and sterilization material, application for traditional silicon dioxide product brings epoch-making meaning.At present, there is nano-powder preparation difficulty, easily reunite between particle, particle size is large and homogeneity is poor and operative technique is complicated etc. problem in existing nano silica powder preparation method
Summary of the invention
The problems such as the present invention easily reunites between nano-powder preparation difficulty, particle for solving in existing nano silica powder preparation process, dimensional homogeneity is poor and operative technique is complicated, propose a kind of novel nano silica powder preparation method.The present invention includes following steps:
Steps A, choose and there is certain density sodium silicate solution (interpolation conducting material) join anolyte compartment in the two Room electrolyzers effectively separated by cation exchange ion film;
Step B, choose and there is certain density sodium chloride solution join cathode compartment in the two Room electrolyzers effectively separated by cation exchange ion film;
Step C, by controlling the rotation noble electrode surface current density be arranged in anolyte compartment on agitator, hydroxide ion in solution is oxidized, the solution ph of anolyte compartment reduces gradually, when reaching the pH value required for silicic acid precipitation, under violent stirring effect, ultra-fine silicic acid precipitation is constantly separated out, and by filtration, deionized water wash, absolute ethanol washing and vacuum, 100 DEG C ~ 120 DEG C dryings, obtains ultra-fine silicic acid powder;
Step D, by noble electrode surface current density in control cathode room, the hydrogen ion in solution is reduced, and the solution ph of cathode compartment raises gradually, and by adding the pH value of hydrochloric acid control solution, control ph is 7 ~ 9, the carrying out of stable electrical solution preocess;
Step e, ultra-fine silicic acid powder is placed in pyrolysis plant, control heat decomposition temperature 580 ~ 700 DEG C of scopes, the thermolysis of ultra-fine silicic acid powder obtains nano silica powder.
Beneficial effect: the present invention adopts the method for two Room electrolysis, ultra-fine silicic acid precipitation is obtained under agitator in the anode compartment and the effect of ultrasonic wave common distribution, through filtering, washing (deionized water and dehydrated alcohol) and the ultra-fine silicic acid powder of dry acquisition, pyrolysis at a certain temperature can obtain nano silica powder, to solve in existing nano silica powder preparation process between nano-powder preparation difficulty, particle problems such as easily reuniting, the poor and operative technique of dimensional homogeneity is complicated.This prepares the method for nano silica powder, and having the features such as sample making course is simple, convenient operation and control, is a kind of novel nano silica powder preparation method.
Accompanying drawing explanation
Fig. 1 realizes apparatus structure schematic diagram of the present invention.
Embodiment
See Fig. 1, present embodiment is made up of following steps:
Choosing concentration is 0.40mol/dm
3~ 1.10mol/dm
3sodium silicate solution join anolyte compartment in the two Room electrolyzers split by cation exchange ion film;
Step B, to choose concentration be 0.90mol/dm
3~ 2.50mol/dm
3sodium chloride solution join cathode compartment in the two Room electrolyzers split by cation exchange ion film;
Step C, be 0.50A/cm by controlling the current density on noble electrode surface in anolyte compartment
2~ 1.80A/cm
2carry out electrolysis, hydroxide ion in solution is oxidized, constantly overflow from system with oxygen form, the solution ph of anolyte compartment reduces gradually, when reaching the pH value required for silicic acid precipitation, under violent stirring effect (agitator and the effect of ultrasonic wave common distribution), ultra-fine silicic acid precipitation is constantly separated out, now the pH value of solution remains unchanged substantially, the hydrogen ion of new formation is all used for producing silicic acid precipitation at anode surface, after reaction terminates, be separated by precipitation in anolyte compartment is carried out filter method, the precipitation separated adopts deionized water more respectively, absolute ethanol washing, carry out water molecules displacement in ultra-fine silicic acid precipitation powder, in extracting vacuum, 100 DEG C ~ 120 DEG C conditions carry out drying, obtain ultra-fine silicic acid powder,
Step D, noble electrode surface current density 0.50A/cm by rotating in control cathode room
2~ 2.80A/cm
2, the hydrogen ion in solution is reduced, and the solution ph of cathode compartment raises gradually, and by adding hydrochloric acid, the pH value controlling solution is 7 ~ 9, the carrying out of stable electrical solution preocess;
Step e, ultra-fine silicic acid powder is placed in pyrolysis plant, control pyrolysis temperature at 580 ~ 700 DEG C, the thermolysis of ultra-fine silicic acid powder obtains the nano silica powder of grain graininess in 60 ~ 85nm scope.
The device (Fig. 1) completing the inventive method comprises direct supply 1, cathode compartment vapor pipe 2, cathode compartment 3, negative electrode 4, cationic exchange membrane 5, anode 6, the whipping appts 7 that anode is housed, ultrasonic unit 8, anolyte compartment 9 and anolyte compartment's vapor pipe 10 and forms, the electrolytic process closing two Room electrolyzers of cationic exchange membrane 5 is being housed, by controlling the current density on Anodic 6 surface, anolyte compartment 9, anode 6 surperficial oxygenous while, evenly discharge hydrogen ion, the degree of supersaturation of silicic acid precipitation is to a certain degree formed in anode surface region, contribute to the formation of ultra-fine silicic acid precipitation, by under the cavitation acting in conjunction of stirring action and ultrasonic unit 8 that the whipping appts 7 of anode 6 is housed, by the ultra-fine silicic acid sealed Belt of formation from corresponding precipitation zone, avoid depositing at anode surface, the precipitation formed enters solution bulk region, dispersed in bulk solution, along with the continuation of electrolytic process, new ultra-fine silicic acid precipitation is constantly had to be formed, by under agitator and ultrasonic acting in conjunction, leave anode 6 surface, enter solution bulk region, continue to the new ultra-fine silicate particle surface precipitation deposition formed in solution bulk region without corresponding hydrogen ion, now can keep the particle size stability that ultra-fine silicic acid precipitates, homogeneity.Obtain ultra-fine silicic acid precipitation, by filtering, by solid-liquid binary states separating substances, precipitated by deionized water wash, remove the silicate in precipitation, hetero-ion in the solution such as sodium ion, precipitated by absolute ethanol washing, replace water molecules in ultra-fine silicic acid precipitation, avoid water molecules in follow-up drying, hard aggregation effect is played in pyrolytic process, pass through extracting vacuum, 100 DEG C ~ 120 DEG C conditions carry out drying, the water molecules of absorption in the ultra-fine silicic acid precipitation of thorough removing, ultra-fine silicic acid is avoided to precipitate in high temperature pyrolysis process, the phenomenon of reuniting of putting up a bridge between nanometer silicon dioxide particle occurs.Because cationic exchange membrane 5 can effectively two tank rooms separately, only have sodium ion can enter cathode compartment 3 from anolyte compartment 9, by adding the sodium salt solution of Yi Rong in anolyte compartment 9, ensure the stable migration of sodium ion, effectively control the environment that anolyte compartment 9 forms ultra-fine silicic acid precipitation, the oxygen simultaneously produced is discharged by anolyte compartment's vapor pipe 10, and is collected.And negative electrode 4 surface constantly has hydrogen to produce in cathode compartment 3, discharged, collect by cathode compartment vapor pipe 2, along with the solution ph of cathode compartment 3 raises, by adding hydrochloric acid, the pH value of control cathode room solution is 7 ~ 9, ensures carrying out smoothly of electrolytic process.
Claims (9)
1. a novel nano silica powder preparation method, is characterized in that: its concrete preparation process is as follows:
Steps A, choose and there is certain density sodium silicate solution (interpolation conducting material) join anolyte compartment in the two Room electrolyzers effectively separated by cation exchange ion film;
Step B, choose and there is certain density sodium chloride solution join cathode compartment in the two Room electrolyzers effectively separated by cation exchange ion film;
Step C, by controlling inert anode electrode surface current density in anolyte compartment, hydroxide ion in solution is oxidized, the solution ph of anolyte compartment reduces gradually, when reaching the pH value required for silicic acid precipitation, under violent stirring effect, ultra-fine silicic acid precipitates constantly separates out, and by filtration, washing, drying, obtains ultra-fine silicic acid powder;
Step D, by inert cathode electrode surface current density in control cathode room, the hydrogen ion in solution is reduced, and the solution ph of cathode compartment raises gradually, by adding the pH value of hydrochloric acid control solution;
Step e, ultra-fine silicic acid powder is placed in pyrolysis plant, control pyrolysis temperature range, the thermolysis of ultra-fine silicic acid powder obtains nano silica powder.
2. a kind of novel nano silica powder preparation method according to claim 1, is characterized in that: steps A and the electrolyzer described in step B are the two Room electrolyzers that this electrolyzer is divided into anolyte compartment and cathode compartment by cationic exchange membrane effectively.
3. a kind of novel nano silica powder preparation method according to claim 1, is characterized in that: the conducting material described in steps A is sodium ion solution soluble in water and potassium ion solution.
4. a kind of novel nano silica powder preparation method according to claim 1, is characterized in that: the electrolytic current density of anode described in step B and step C is 0.50A/cm
2~ 1.80A/cm
2, the electrolytic current density of negative electrode is 0.50A/cm
2~ 2.80A/cm
2.
5. a kind of novel nano silica powder preparation method according to claim 1, it is characterized in that: the anolyte compartment's noble electrode described in step C is arranged on the stirring rake end of whipping appts, along with agitator rotates, anode electrode has netted (porous) structure, reduce and stir resistance, increase the turbulence of fluid, depositions settle can be avoided at anode surface, increase electrolysis area simultaneously, improve precipitation productive rate.
6. a kind of novel nano silica powder preparation method according to claim 1, it is characterized in that: the violent stirring environment of the anolyte compartment described in step C, for anode is arranged on agitator, it is in the ultrasonic unit of ultrasonic carrier that anolyte compartment is arranged on water.Under agitator stirring action and ultrasonic wave acting in conjunction, the electrolysis of solutions in anolyte compartment, silicic acid precipitation all complete in violent stirring environment, are conducive to ultra-fine silicic acid precipitation and are formed and high dispersing, avoid anode surface to precipitate between deposition, deposit seeds and reunite.
7. a kind of novel nano silica powder preparation method according to claim 1, it is characterized in that: the ultra-fine silicic acid sedimentation and filtration described in step C, washing, drying, washing adopts deionized water and dehydrated alcohol respectively, first adopt deionized water wash, after removing the anolyte compartment such as sodium ion and silicate ion hetero-ion, recycling dehydrated alcohol cleans ultra-fine silicic acid precipitation repeatedly, after water molecules in cementation, under extracting vacuum, 100 DEG C ~ 120 DEG C environment, carry out the drying of ultra-fine silicic acid precipitation.
8. a kind of novel nano silica powder preparation method according to claim 1, it is characterized in that: the NaCl electrolysis of cathode compartment described in step D process, because hydrogen ion constantly consumes, the pH value of solution raises, by adding hydrochloric acid, control ph is 7 ~ 9, the carrying out of stable electrical solution preocess.
9. a kind of novel nano silica powder preparation method according to claim 1, is characterized in that: ultra-fine silicic acid powder heat decomposition temperature described in step e controls, 580 ~ 700 DEG C of scopes, to obtain nano silica powder.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106191910A (en) * | 2016-09-19 | 2016-12-07 | 上海应用技术大学 | A kind of it is electrolysed the method that hexafluosilicic acid prepares fluosilicate |
| CN106191911A (en) * | 2016-09-19 | 2016-12-07 | 上海应用技术大学 | A kind of it is electrolysed the method that prodan prepares silicate fluoride solution |
| CN108977824A (en) * | 2018-08-31 | 2018-12-11 | 上海应用技术大学 | A kind of electrochemical preparation method of amorphous silica |
| CN110306201A (en) * | 2019-08-09 | 2019-10-08 | 刘光天 | A method of increasing modulus of water glass |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683594A (en) * | 2005-03-14 | 2005-10-19 | 新疆大学 | Process for preparing super fine metal oxide |
| CN102417186A (en) * | 2011-09-07 | 2012-04-18 | 黑龙江科技学院 | Novel method for preparing nano silica powder |
-
2014
- 2014-12-18 CN CN201410852465.XA patent/CN104709913A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683594A (en) * | 2005-03-14 | 2005-10-19 | 新疆大学 | Process for preparing super fine metal oxide |
| CN102417186A (en) * | 2011-09-07 | 2012-04-18 | 黑龙江科技学院 | Novel method for preparing nano silica powder |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106191910A (en) * | 2016-09-19 | 2016-12-07 | 上海应用技术大学 | A kind of it is electrolysed the method that hexafluosilicic acid prepares fluosilicate |
| CN106191911A (en) * | 2016-09-19 | 2016-12-07 | 上海应用技术大学 | A kind of it is electrolysed the method that prodan prepares silicate fluoride solution |
| CN106191911B (en) * | 2016-09-19 | 2018-12-04 | 上海应用技术大学 | A method of electrolysis prodan prepares silicate fluoride solution |
| CN108977824A (en) * | 2018-08-31 | 2018-12-11 | 上海应用技术大学 | A kind of electrochemical preparation method of amorphous silica |
| CN110306201A (en) * | 2019-08-09 | 2019-10-08 | 刘光天 | A method of increasing modulus of water glass |
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