CN105084406A - Hydrophilic nanometer erbium oxide suspension and preparation method thereof - Google Patents
Hydrophilic nanometer erbium oxide suspension and preparation method thereof Download PDFInfo
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- CN105084406A CN105084406A CN201410218777.5A CN201410218777A CN105084406A CN 105084406 A CN105084406 A CN 105084406A CN 201410218777 A CN201410218777 A CN 201410218777A CN 105084406 A CN105084406 A CN 105084406A
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Abstract
The invention relates to a hydrophilic nanometer erbium oxide suspension and a preparation method thereof. According to the invention, originally agglomerated nanometer erbium oxide powder is depolymerized through a high energy depolymerizer; and a proper amount of a dispersion medium, a surfactant, an aqueous disperser, etc. are added in the process of preparation so as to prepare the suspension with a secondary particle size D50 of 200 to 300 nm. The preparation method for the hydrophilic nanometer erbium oxide suspension is simple to operate, simplifies and shortens production process route, can prepare the hydrophilic nanometer erbium oxide suspension with the advantages of high suspension property, high dispersibility and convenience in addition, has low production cost, is favorable for industrial production and facilitates large scale popularization and application.
Description
Technical field
The present invention relates to a kind of nano-powder suspension, particularly relate to a kind of nano oxidized erbium hydrophilic suspensions and preparation method thereof.
Background technology
The specific function that nano-powder has in light, heat, electricity, magnetic etc. makes it create good condition widely using of every field.Many complete processings, production technique all need powder evenly and are stably scattered in liquid phase medium.But because superfine powder specific surface is large, surface energy is high makes particle attract each other and have unstable tendency, this tendency makes particle produce to reunite and affect its effect.Because the erbium of positive trivalent can be used for optical-fibre communications, erbium-doped fiber amplifier is absolutely necessary optics, the laser crystals of er-doped can be made into military upper portable laser stadimeter in addition, also can join in glass and make rare earth glass laserable material, also can be applicable to spectacle glass, the decolouring of crystal glass and painted etc.Along with the development in epoch, the new application of erbium will be opened up.But Erbium trioxide has gathering, the phenomenons such as flocculation, the nano oxidized erbium dispersion stability that ordinary method is made is poor, there will be muddiness, the phenomenons such as layering, have impact on the practical application of Erbium trioxide.
Summary of the invention
The object of the invention is the defect overcoming prior art existence, provide a kind of good dispersity, stability is high, and manufacture craft is simple, nano oxidized erbium hydrophilic suspensions that cost is low and preparation method thereof.
The technical scheme realizing the object of the invention is: a kind of nano oxidized erbium hydrophilic suspensions; Described suspension raw material composition and mass fraction as follows:
Wherein said dispersion medium is the one in water, ethanol, ethylene glycol, Virahol;
Wherein said tensio-active agent is the one in citric acid, oxysuccinic acid, acetic acid and oxalic acid;
Wherein said Hydrophilic dispersant is the one in sodium lauryl sulphate, silane coupling agent, hexadecyl brometo de amonio.
Technique scheme, described polyoxyethylene glycol is Macrogol 200, poly(oxyethylene glycol) 400 or cetomacrogol 1000.
Technique scheme, the solid content of described nano oxidized erbium hydrophilic suspensions is 2% ~ 30%.
Technique scheme, the solid content of described nano oxidized erbium hydrophilic suspensions is 5% ~ 25%.
Prepare a method for nano oxidized erbium hydrophilic suspensions, comprise the steps:
A, take raw material according to above-mentioned mass fraction, and powder Erbium trioxide is put into dispersion medium mix and stir, add the tensio-active agent of powder Erbium trioxide quality 1% ~ 10% again, being adjusted to PH is 3 ~ 7, and make powder complete wetting, and stir, churning time is 2 ~ 5 hours, obtains mixed slurry A;
B, in high energy depolymerizer, add depolymerizing media, and the mixed slurry A in step a is added in high energy depolymerizer, add Hydrophilic dispersant and polyoxyethylene glycol more subsequently, being adjusted to rotating speed is 2500 ~ 4000r/min, depolymerization, after 0.5 ~ 3 hour, obtains nano oxidized erbium hydrophilic suspensions B;
C, bottle obtaining nano oxidized erbium hydrophilic suspensions B in step b, sealing is preserved.
6, nano oxidized erbium hydrophilic suspensions according to claim 5, it is characterized in that: in described step a, the primary particle size of powder Erbium trioxide is 5 ~ 100nm, reunion state aggregate particle size is D50:3 ~ 7 μm.
Technique scheme, after depolymerization, the aggregate particle size of the suspension B of gained is D50:200 ~ 300nm.
Technique scheme, described dispersion medium is ethanol, and described tensio-active agent is citric acid.
Technique scheme, described depolymerizing media is the zirconium pearl of 0.3mm, and described zirconium pearl cumulative volume is 55 ~ 65% of high energy depolymerizer depolymerization chamber.
Technique scheme, the pH value of described nano oxidized erbium hydrophilic suspensions B is 5 ~ 8.
After adopting technique scheme, the present invention has following positive effect: (1) tensio-active agent optimization citric acid of the present invention, citric acid can regulate the pH value of mixed slurry, the hydroxide ion of citric acid modification particle surface can also be utilized, improve nano oxidized erbium surfactivity, also can play dispersion and suspension effect; (2) solid content of the present invention is selected between 2% ~ 30%, and preferably 5% ~ 25%, the too low Appropriate application being unfavorable for dispersion medium, causes the waste of dispersion medium and other added ingredientss, too high, and liquid can be caused to have and sink to the bottom precipitation, suspension property is poor; (2) because the Zeta potential of the nano powder surface in nano granule suspension has much relations with the pH value of the aqueous solution, can by ensureing that particle presents higher Zeta potential and obtains electrostatic stabilization effect, general nano-powder in media as well, when pH value is below or above 11, capital increases ionic strength, it is made to produce flocculation by compression double electric layer, and nano oxidized erbium hydrophilic suspensions, pass through great many of experiments, find that pH value has good dispersiveness in the scope of 3-7, when preferred pH value is 5, dispersiveness is best; (3) dispersion medium preferred alcohol, ethanol is as assistant for emulsifying agent synergistic surfactant granule for absorbing surface, infiltrate completely, through the depolymerization of high energy depolymerizer, add suitable tensio-active agent, overcome Van der Waals force and Coulomb's force, solve the problem of conventional nano dispersion stability difference, make nanotechnology be able to widespread use; (4) Hydrophilic dispersant and polyoxyethylene glycol is added during depolymerization, wherein polyoxyethylene glycol is as nonionic surface active agent, entropy repulsion can be produced between particle, make the strength degradation that tangles in particle cluster between microfracture, be conducive to particle cluster cracked, thus for obtaining polymolecularity, the suspension of high stability provides guarantee; (5) depolymerizing media of the present invention selects the zirconium pearl of 0.3mm, the main component of zirconium pearl is zirconium white, its hardness and wear resistance relatively good, other hardness can be avoided not high, the impurity that the bad depolymerizing media of wear resistance brings, thus affect the purity of the nano oxidized erbium of the present invention; Adopt the zirconium pearl of 0.3mm, granularity is less, thus after depolymerization, the granularity of nano oxidized erbium is also relatively little, and in conjunction with optimum revolution 3500r/min during high speed depolymerization, provides good basis for producing satisfactory nano oxidized erbium suspension.(6) the present invention not only easy to operate, simplify and shorten production process route, and can obtain uphanging buoyancy and polymolecularity, be convenient to the nano oxidized erbium hydrophilic suspensions added, production cost is low, be conducive to suitability for industrialized production, be convenient to large-scale promotion application.
Accompanying drawing explanation
In order to make content of the present invention more easily be clearly understood, below according to specific embodiment also by reference to the accompanying drawings, the present invention is further detailed explanation, wherein
Fig. 1 is the particle size distribution figure that second embodiment of the invention powder Erbium trioxide raw material is detected by Malvern;
Fig. 2 is the particle size distribution figure of second embodiment of the invention Erbium trioxide after depolymerization;
Fig. 3 is second embodiment of the invention nano oxidized erbium hydrophilic suspensions transmission electron microscope picture.
Embodiment
(embodiment 1)
Taking 20 grams of primary particle sizes is 5 ~ 100nm, and reunion state aggregate particle size is the nano oxidized erbium powder of D50:3 ~ 7 μm, stirs and soak with 400ml ethanol, add the citric acid of powder quality 2% again, regulate PH to 7, make it stir and complete wetting, churning time 2 hours.
Taking 1.5 kilograms of specifications is that the zirconium pearl of 0.3mm is first poured in the depolymerization chamber in high energy depolymerizer, zirconium pearl cumulative volume accounts for 55% of depolymerization cavity volume, again the Homogeneous phase mixing slip in above-mentioned is added in depolymerizer, and then add 1 gram of sodium lauryl sulphate and 2 grams of cetomacrogol 1000s, the rotating speed of depolymerizer is 2500r/min, depolymerization 3 hours, filter zirconium pearl, obtain pink not stratified, do not precipitate and the nano oxidized erbium hydrophilic suspensions be evenly distributed, recording pH value is without Precipitation after about 8,5 days, and the present embodiment gained suspension solid content is about about 5%.
(embodiment 2)
1. taking 40 grams of 20 grams of primary particle sizes is 5 ~ 100nm, reunion state aggregate particle size is the nano oxidized erbium powder of D50:3 ~ 4 μm, the size-grade distribution of nano oxidized erbium powder as shown in Figure 1, stir with 400ml ethanol and soak, add the citric acid of powder quality 3% again, regulate PH to 5, make it stir and complete wetting, churning time 2 hours.
2. taking 2 kilograms of specifications is that the zirconium pearl of 0.3mm is first poured in the depolymerization chamber in high energy depolymerizer, zirconium pearl cumulative volume accounts for 60% of depolymerization cavity volume, again the Homogeneous phase mixing slip in above-mentioned is added in depolymerizer, and then add the silane resin acceptor kh-550 of 5ml and the Macrogol 200 of 5ml, the rotating speed of depolymerizer is 3500r/min, depolymerization 1 hour, filter zirconium pearl, obtain pink not stratified, do not precipitate and the nano oxidized erbium hydrophilic suspensions be evenly distributed, recording the nano oxidized erbium aggregate particle size after depolymerization is D50:200 ~ 300nm, particle size distribution figure as shown in Figure 2, surveying pH value is about 7, without Precipitation after 7 days, the present embodiment gained suspension solid content is about about 10%, now the transmission electron microscope photo of suspension as shown in Figure 3.
(embodiment 3)
1. taking 100 grams of 20 grams of primary particle sizes is 5 ~ 100nm, and reunion state aggregate particle size is the nano oxidized erbium powder of D50:3 ~ 7 μm, stirs and soak with 400ml ethanol, add the citric acid of powder quality 8% again, regulate PH to 4, make it stir and complete wetting, churning time 5 hours.
2. taking 2.5 kilograms of specifications is that the zirconium pearl of 0.3mm is first poured in the depolymerization chamber of high energy depolymerizer, zirconium pearl cumulative volume accounts for 65% of depolymerization cavity volume, again the Homogeneous phase mixing slip in above-mentioned is added in depolymerizer, and then add 5 grams of hexadecyl brometo de amonios and 6ml poly(oxyethylene glycol) 400, the rotating speed of depolymerizer is 4000r/min, depolymerization 0.5 hour, filter zirconium pearl, obtain pink not stratified, do not precipitate and the nano oxidized erbium hydrophilic suspensions be evenly distributed, surveying pH value is without Precipitation after about 6,7 days, and the present embodiment gained suspension solid content is about about 25%.
Ethanol in above embodiment can substitute with the water of equal volume, ethylene glycol or Virahol, tensio-active agent also can adopt the one in oxysuccinic acid, acetic acid or oxalic acid to substitute, also can obtain suspension of the present invention, but the suspension of suspension and dispersion effect comparatively ethanol as the dispersion medium time difference.
The preferred 3500r/min of high speed depolymerizer rotating speed of the present invention, the faster depolymerization efficiency of rotating speed improves, but too fast meeting causes machine loss serious, also can cause the generation of security incident, and mixed slurry can be made to splash, cause the raw-material waste of rare earth; Rotating speed is crossed and then can be brought depolymerization inefficiency slowly, and particle diameter after depolymerization is comparatively thick, is difficult to meet customer need.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a nano oxidized erbium hydrophilic suspensions; It is characterized in that: described suspension raw material composition and mass fraction as follows:
Wherein said dispersion medium is the one in water, ethanol, ethylene glycol, Virahol;
Wherein said tensio-active agent is the one in citric acid, oxysuccinic acid, acetic acid and oxalic acid;
Wherein said Hydrophilic dispersant is the one in sodium lauryl sulphate, silane coupling agent, hexadecyl brometo de amonio.
2. nano oxidized erbium hydrophilic suspensions according to claim 1, is characterized in that: described polyoxyethylene glycol is Macrogol 200, poly(oxyethylene glycol) 400 or cetomacrogol 1000.
3. nano oxidized erbium hydrophilic suspensions according to claim 1 and 2, is characterized in that: the solid content of described nano oxidized erbium hydrophilic suspensions is 2% ~ 30%.
4. nano oxidized erbium hydrophilic suspensions according to claim 3, is characterized in that: the solid content of described nano oxidized erbium hydrophilic suspensions is 5% ~ 25%.
5. a preparation method for the nano oxidized erbium hydrophilic suspensions as described in any one of Claims 1 to 4 claim, is characterized in that: comprise the steps:
A, take raw material according to above-mentioned mass fraction, and powder Erbium trioxide is put into dispersion medium mix and stir, add the tensio-active agent of powder Erbium trioxide quality 1% ~ 10% again, being adjusted to PH is 3 ~ 7, and make powder complete wetting, and stir, churning time is 2 ~ 5 hours, obtains mixed slurry A;
B, in high energy depolymerizer, add depolymerizing media, and the mixed slurry A in step a is added in high energy depolymerizer, add Hydrophilic dispersant and polyoxyethylene glycol more subsequently, being adjusted to rotating speed is 2500 ~ 4000r/min, depolymerization, after 0.5 ~ 3 hour, obtains nano oxidized erbium hydrophilic suspensions B;
C, bottle obtaining nano oxidized erbium hydrophilic suspensions B in step b, sealing is preserved.
6. the preparation method of nano oxidized erbium hydrophilic suspensions according to claim 5, it is characterized in that: in described step a, the primary particle size of powder Erbium trioxide is 5 ~ 100nm, reunion state aggregate particle size is D50:3 ~ 7 μm.
7. the preparation method of nano oxidized erbium hydrophilic suspensions according to claim 5, is characterized in that: after depolymerization, the aggregate particle size of the suspension B of gained is D50:200 ~ 300nm.
8. the preparation method of nano oxidized erbium hydrophilic suspensions according to claim 5, it is characterized in that: described dispersion medium is ethanol, described tensio-active agent is citric acid.
9. the preparation method of nano oxidized erbium hydrophilic suspensions according to claim 5, is characterized in that: described depolymerizing media is the zirconium pearl of 0.3mm, and described zirconium pearl cumulative volume is 55 ~ 65% of high energy depolymerizer depolymerization chamber.
10. the preparation method of nano oxidized erbium hydrophilic suspensions according to claim 5, is characterized in that: the pH value of described nano oxidized erbium hydrophilic suspensions B is 5 ~ 8.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113842829A (en) * | 2021-10-13 | 2021-12-28 | 杭州晶祥新材料科技有限公司 | Preparation method of novel nano erbium oxide dispersion liquid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374882A (en) * | 1999-08-04 | 2002-10-16 | 罗狄亚稀土公司 | Organic colloidal dispersion of a rare earth compond monocrystalline particles |
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- 2014-05-22 CN CN201410218777.5A patent/CN105084406A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374882A (en) * | 1999-08-04 | 2002-10-16 | 罗狄亚稀土公司 | Organic colloidal dispersion of a rare earth compond monocrystalline particles |
Non-Patent Citations (1)
| Title |
|---|
| 陈雷等: "在纯水中高能球磨稀土氧化物制备超细纳米悬浮液", 《物理化学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113842829A (en) * | 2021-10-13 | 2021-12-28 | 杭州晶祥新材料科技有限公司 | Preparation method of novel nano erbium oxide dispersion liquid |
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