CN112964798A - Analysis method of nano zirconia dispersion liquid - Google Patents
Analysis method of nano zirconia dispersion liquid Download PDFInfo
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- CN112964798A CN112964798A CN202110163926.2A CN202110163926A CN112964798A CN 112964798 A CN112964798 A CN 112964798A CN 202110163926 A CN202110163926 A CN 202110163926A CN 112964798 A CN112964798 A CN 112964798A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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Abstract
The invention provides an analysis method of a nano zirconia dispersion liquid, which comprises a pretreatment step of the nano zirconia dispersion liquid, wherein a dispersion medium of the nano zirconia dispersion liquid is an organic solvent system, and the pretreatment step comprises a step of adding inorganic base to precipitate nano zirconia powder after mixing the nano zirconia dispersion liquid and a polar solvent. The analysis method of the nano zirconia dispersion liquid provided by the invention is beneficial to realizing the separation of nano zirconia powder and a dispersion medium at room temperature, and does not damage the modified group of the nano zirconia, so that the detection result is more accurate than that of the existing method, and the analysis method can be combined with infrared, nuclear magnetism and GC-MS comprehensive analysis, and has high accuracy; convenient operation and wide application range.
Description
Technical Field
The invention relates to the technical field of analysis methods, in particular to an analysis method of a nano zirconia dispersion liquid.
Background
The nano zirconia dispersion liquid is generally composed of a dispersion medium (monomer, solvent), an auxiliary agent (defoamer, dispersant, etc.) and nano zirconia powder (wherein zirconia is generally modified), and is used for preparing a brightness enhancement film or an anti-reflection film. Wherein the dispersion medium is organic solvent such as alcohols, esters, ethers, etc., or UV monomer, or water; the assistant is mostly an oily dispersant with high refractive index; the grain size range of the nano zirconia is 3-10 nm.
The nano zirconia dispersion is used for a brightness enhancement film, and a part of components such as acetic acid and the like corrode equipment, and the components need to be analyzed to confirm the influence. Currently, IR or GC-MS is mostly adopted for the qualitative determination of the nano zirconia dispersion liquid, and the monomer, the dispersant, the modified group of the nano zirconia and the like in the dispersion liquid are judged through characteristic peaks.
However, the above qualitative analysis method often causes great interference in the judgment of characteristic peaks due to the complex components of the nano zirconia dispersion liquid, thereby affecting the accurate qualitative analysis. Therefore, a method for accurately determining the nano zirconia dispersion is urgently needed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an analysis method of a nano zirconia dispersion liquid.
The invention adopts the following technical scheme:
the invention provides an analysis method of a nano zirconia dispersion liquid, which comprises a pretreatment step of the nano zirconia dispersion liquid, wherein a dispersion medium of the nano zirconia dispersion liquid is an organic solvent system, and the pretreatment step comprises a step of adding inorganic alkali to precipitate nano zirconia powder after mixing the nano zirconia dispersion liquid and a polar solvent.
The nano zirconia dispersion liquid has good stability, the dispersion characteristic of nano particles is not easy to be damaged, solid-liquid separation is difficult to realize even high-speed centrifugal separation is adopted, and particularly, under the condition that a dispersion medium is an organic solvent system, the separation of nano zirconia powder and the dispersion medium is more difficult to realize. The method of the invention is beneficial to realizing the separation of the nano zirconia powder and the dispersion medium at room temperature, and the modified group of the nano zirconia is not damaged. The polar solvent is added in the pretreatment process, so that a rich solution environment can be provided, and inorganic alkali is dissolved to separate out the zirconia powder.
In actual practice, when the components of the nano zirconia dispersion are unknown, it is possible to easily distinguish whether the dispersion medium is water or an organic solvent system, and when the dispersion medium is water, it is conceivable to obtain a dispersant by directly performing extraction separation. The specific distinguishing method can be as follows: and adding white anhydrous copper sulfate powder into the nano zirconia dispersion liquid, and if the white copper sulfate powder is not changed in color in a large amount, judging that the nano zirconia dispersion liquid medium is an organic solvent system.
Preferably, the polar solvent is ethanol or propylene glycol.
Preferably, the volume ratio of the nano zirconia dispersion to the polar solvent is 1: (1-2).
Preferably, the inorganic base is sodium bicarbonate.
Preferably, the solid-to-liquid ratio of the sodium bicarbonate to the nano zirconia dispersion is 0.5 g: (3-5) ml.
Further, the pretreatment also comprises the step of carrying out centrifugal treatment on a sample after the nano zirconia powder is separated out, and separating supernate and the nano zirconia powder.
Preferably, the rotation speed of the centrifugal treatment is 6000-8000 rpm.
Preferably, the nano zirconia powder obtained after the centrifugation is washed with the polar solvent for a plurality of times and then washed with distilled water.
In a preferred embodiment of the present invention, the specific operation of obtaining the sample after the precipitation of the nano zirconia powder is as follows: taking a proper amount of sample, centrifuging the sample in a centrifuge tube at the rotating speed of 8000rpm for 10 minutes, and pouring out supernatant liquor for later use;
adding a proper amount of polar solvent (ethanol, propylene glycol and the like) into the centrifuge tube again, shaking and cleaning the bottom powder, centrifuging for 10 minutes, and pouring out the supernatant for later use; repeating the step for 1-2 times, collecting supernatant liquid after multiple times of centrifugation for later use, taking out powder at the bottom, cleaning the powder with distilled water for multiple times, and drying the powder in vacuum.
Further, the analysis method further comprises the step of carrying out infrared test on the nano zirconia powder obtained through pretreatment so as to determine the modified group of the nano zirconia powder.
And performing GC-MS analysis on the supernatant obtained by the pretreatment to determine a dispersion medium and/or a dispersion auxiliary agent of the nano zirconia dispersion liquid.
Preferably, in the GC-MS analysis, the GC instrument tests parameters: a chromatographic column: DB-5, 60m 0.25mm 0.25 um; sample inlet temperature: 280 ℃; the split ratio is as follows: 20: 1; the sample volume is 1 mu L; initial temperature: keeping at 50 deg.C for 5min, heating to 220 deg.C at 10 deg.C/min, keeping for 5min, heating to 300 deg.C at 20 deg.C/min, and keeping for 20 min;
testing parameters of an MS instrument: transmission line: 300 ℃, ionization energy: 70V, ion source temperature: 230 ℃, four bar temperature: 150 ℃, scan range: 10-550m/z, solvent retardation: and 7 min.
The invention provides an analytical method of nano zirconia dispersion, which is beneficial to realizing the separation of nano zirconia powder and dispersion medium at room temperature without damaging the modified group of the nano zirconia, so that the detection result is more accurate than the prior method, and the method can be combined with infrared, nuclear magnetism and GC-MS comprehensive analysis, and has high accuracy; convenient operation and wide application range.
Drawings
FIG. 1 is an IR spectrum obtained by measuring dried powder in example 1 of the present invention;
FIG. 2 is a GC-MS spectrum obtained by measuring the supernatant in example 1 of the present invention;
FIG. 3 is a GC-MS spectrum of pure 3-phenoxybenzyl acrylate;
FIG. 4 is an IR spectrum obtained by measuring dried powder in example 2 of the present invention;
FIG. 5 is a GC-MS spectrum obtained by measuring the supernatant in example 2 of the present invention;
FIG. 6 is a GC-MS spectrum of pure benzyl acrylate;
FIG. 7 is an infrared spectrum obtained by directly measuring the dispersion in comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides an analysis method of a nano zirconia dispersion liquid (self-made: hydroxyl modified zirconia powder is dispersed in 3-phenoxyl benzyl acrylate), which comprises the following specific steps:
pretreatment: taking 3ml of nano zirconium oxide dispersion liquid, adding 5ml of ethanol, and shaking uniformly; then adding 0.5g of sodium bicarbonate, stirring once every 10 minutes for three times, and standing for 3 hours to gradually separate out powder; transferring the mixed solution into a centrifuge tube, centrifuging at 8000rpm for 10 minutes, and pouring out supernatant for later use; adding a proper amount of ethanol into the centrifugal tube again, shaking to clean the powder at the bottom, centrifuging for 10 minutes, and pouring out the supernatant for later use; repeating the steps twice, collecting supernatant after 4 times of centrifugation, taking out powder at the bottom, washing for 3 times by using distilled water, and then drying in vacuum.
And (3) determination: the dried powder was subjected to infrared measurement, and FIG. 1 shows the infrared spectrum of the measurement, from which it was seen that the peak of hydroxyl group characteristics was 3400cm-1And the left and right parts are matched with the hydroxyl modified zirconia powder body.
Performing GC-MS detection on the supernatant under the following detection conditions:
GC instrument test parameters: a chromatographic column: DB-5, 60m 0.25mm 0.25 um; sample inlet temperature: 280 ℃; the split ratio is as follows: 20: 1; the sample volume is 1 mu L; initial temperature: keeping at 50 deg.C for 5min, heating to 220 deg.C at 10 deg.C/min, keeping for 5min, heating to 300 deg.C at 20 deg.C/min, and keeping for 20 min;
testing parameters of an MS instrument: transmission line: 300 ℃, ionization energy: 70V, ion source temperature: 230 ℃, four bar temperature: 150 ℃, scan range: 10-550m/z, solvent retardation: and 7 min.
The result is shown in figure 2 as the GC-MS spectrogram of the supernatant and figure 3 as the GC-MS spectrogram of pure 3-phenoxyl benzyl acrylate, and the testing method is accurate and reliable.
Example 2
The embodiment provides an analysis method of a nano zirconia dispersion liquid (self-made: hydroxyl modified zirconia powder is dispersed in benzyl acrylate), which comprises the following specific steps:
pretreatment: taking 3ml of nano zirconium oxide dispersion liquid, adding 5ml of ethanol, and shaking uniformly; then adding 0.5g of sodium bicarbonate, stirring once every 10 minutes for three times, and standing for 3 hours to gradually separate out powder; transferring the mixed solution into a centrifuge tube, centrifuging at 8000rpm for 10 minutes, and pouring out supernatant for later use; adding a proper amount of ethanol into the centrifugal tube again, shaking to clean the powder at the bottom, centrifuging for 10 minutes, and pouring out the supernatant for later use; repeating the above steps twice, collecting supernatant after 4 times of centrifugation, taking out powder at the bottom, washing with distilled water for 3 times, and vacuum drying.
And (3) determination: the dried powder was subjected to infrared measurement, and FIG. 4 shows an infrared spectrum of the measurement, from which a characteristic peak of hydroxyl group at 3400cm was observed-1And the left and right parts are matched with the hydroxyl modified zirconia powder body.
Performing GC-MS detection on the supernatant under the following detection conditions:
GC instrument test parameters: a chromatographic column: DB-5, 60m 0.25mm 0.25 um; sample inlet temperature: 280 ℃; the split ratio is as follows: 20: 1; the sample volume is 1 mu L; initial temperature: keeping at 50 deg.C for 5min, heating to 220 deg.C at 10 deg.C/min, keeping for 5min, heating to 300 deg.C at 20 deg.C/min, and keeping for 20 min;
testing parameters of an MS instrument: transmission line: 300 ℃, ionization energy: 70V, ion source temperature: 230 ℃, four bar temperature: 150 ℃, scan range: 10-550m/z, solvent retardation: and 7 min.
The result is shown in figure 5 as the GC-MS spectrogram of the supernatant liquid and figure 6 as the GC-MS spectrogram of pure benzyl acrylate, and the testing method is accurate and reliable.
Comparative example 1
This comparative example provides an analytical method for a nano zirconia dispersion (same as example 1) in order to directly subject the dispersion to infrared testing.
The result is shown in fig. 7, which is a measured infrared image, and the spectral peaks in the image have serious mutual interference and can not be accurately determined.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. An analysis method of a nano zirconia dispersion, comprising a pretreatment step of the nano zirconia dispersion, characterized in that a dispersion medium of the nano zirconia dispersion is an organic solvent system, and the pretreatment step comprises a step of mixing the nano zirconia dispersion with a polar solvent, and then adding an inorganic base to precipitate nano zirconia powder.
2. The method for analyzing a nano zirconia dispersion according to claim 1, wherein the polar solvent is ethanol or propylene glycol.
3. The method for analyzing a nano zirconia dispersion according to claim 1 or 2, wherein the volume ratio of the nano zirconia dispersion to the polar solvent is 1: (1-2).
4. The method for analyzing a nano zirconia dispersion according to any one of claims 1 to 3, wherein the inorganic base is sodium hydrogen carbonate.
5. The method for analyzing the nano zirconia dispersion according to claim 1, wherein the solid-to-liquid ratio of the sodium bicarbonate to the nano zirconia dispersion is 0.5 g: (3-5) ml.
6. The method for analyzing a nano zirconia dispersion according to any one of claims 1 to 5, wherein the method for judging whether the dispersion medium of the nano zirconia dispersion is an organic solvent system comprises: and adding white anhydrous copper sulfate powder into the nano zirconia dispersion liquid, and if the white copper sulfate powder is not changed in color in a large amount, judging that the nano zirconia dispersion liquid medium is an organic solvent system.
7. The method for analyzing a nano zirconia dispersion according to any one of claims 1 to 6, wherein the pretreatment further comprises centrifuging a sample from which the nano zirconia powder has been precipitated, and separating the supernatant from the nano zirconia powder.
8. The method for analyzing a nano zirconia dispersion liquid according to claim 7, wherein the nano zirconia powder is subjected to an infrared test to determine a modified group of the nano zirconia powder.
9. The method for analyzing a nano zirconia dispersion according to claim 7, wherein the supernatant is subjected to GC-MS analysis to determine a dispersion medium and/or a dispersion aid of the nano zirconia dispersion.
10. The method for analyzing a nano zirconia dispersion according to claim 9, wherein in the GC-MS analysis, GC instrument test parameters: a chromatographic column: DB-5, 60m 0.25mm 0.25 um; sample inlet temperature: 280 ℃; the split ratio is as follows: 20: 1; the sample volume is 1 mu L; initial temperature: keeping at 50 deg.C for 5min, heating to 220 deg.C at 10 deg.C/min, keeping for 5min, heating to 300 deg.C at 20 deg.C/min, and keeping for 20 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113912792A (en) * | 2021-11-08 | 2022-01-11 | 东莞市光志光电有限公司 | Preparation method and application of high-refractive-index nano-zirconia composite resin |
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| CN113912792A (en) * | 2021-11-08 | 2022-01-11 | 东莞市光志光电有限公司 | Preparation method and application of high-refractive-index nano-zirconia composite resin |
| CN113912792B (en) * | 2021-11-08 | 2023-12-15 | 东莞市光志光电有限公司 | Preparation method and application of high-refractive-index nano zirconia composite resin |
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