A method for simply preparing a high-refractive transparent nano-zirconium oxide dispersion liquid

Abstract

The application relates to the technical field of nano zirconium oxide preparation, in particular to a method for simply preparing high-refractive transparent nano zirconium oxide dispersion liquid; the zirconium salt solution is weighed, directly poured into water or an organic solvent or a mixed solution of water and the organic solvent, and subjected to hydrothermal treatment, so that nano zirconium oxide particles are directly obtained and washed, thereby obtaining a nano zirconium oxide liquid dispersion body; compared with the method for preparing the nano dispersion liquid of zirconium oxide in the prior art, the steps are simpler, and other complicated procedures are not needed. The refractive index of the nano zirconium oxide liquid dispersion body manufactured by the application is about 1.7-1.8, while the refractive index of the nano zirconium oxide dispersion liquid in the prior art is about 1.6, the refractive index is improved, the light transmittance of the zirconium oxide dispersion liquid when preparing a lower-level product is improved, and the downstream process is facilitated.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of nano zirconium oxide preparation, in particular to a method for simply preparing high-refractive transparent nano zirconium oxide dispersion liquid. BACKGROUND

[0002] Nano zirconium oxide has many excellent properties, such as wear resistance, high hardness, good toughness, small thermal expansion coefficient, low thermal conductivity and good biocompatibility. These excellent properties make zirconium oxide widely used in abrasive materials, structural ceramics, electronic ceramics and biological ceramics. In recent years, with the development of the optical field, higher requirements are put forward for the optical properties of materials, especially materials with high refractive index. Zirconium oxide has been widely concerned in the academic field due to its excellent optical properties. However, how to realize the stable dispersion of nano zirconium oxide ceramic and ensure that its optical properties and transparency are not affected has become a major pain point in the industry.

[0003] At present, most of the methods for preparing zirconium oxide are as follows: organic zirconium salt is hydrolyzed to prepare zirconium oxide precursor, impurity ions are removed through washing and centrifugation to obtain relatively pure zirconium hydroxide precursor, then the zirconium hydroxide precursor is placed in a hydrothermal kettle with a hydrothermal solvent to react, and after the reaction is completed, the nano zirconium oxide powder is obtained through washing again, then the obtained nano zirconium oxide powder is modified in a series of ways, and finally the modified nano powder is dispersed in a solvent to obtain a nano zirconium oxide dispersion liquid.

[0004] However, the theoretical refractive index of the zirconium oxide dispersion liquid is about 2.2, and the actual refractive index of the zirconium oxide dispersion liquid obtained by using the preparation method in the related art is about 1.6, such as the patent CN112499678A nano zirconium oxide powder, a preparation method thereof and a dispersion liquid obtained therefrom and an optical film. The refractive index of the nano zirconium oxide powder prepared in the patent is 1.549-1.649, the refractive index is low, and the process is relatively complicated.

[0005] Therefore, the application discloses a method for simply preparing high-refractive transparent nano zirconium oxide dispersion liquid, which realizes a simple process, improves the refractive index of the obtained zirconium oxide dispersion liquid, and further improves the light transmission level of the downstream product. SUMMARY

[0006] The purpose of the application is to provide a method for simply preparing high-refractive transparent nano zirconium oxide dispersion liquid to solve the problems in the background art.

[0007] In order to solve the above technical problems, the application provides the following technical scheme:

[0008] A method for simply preparing high-refractive transparent nano zirconium oxide dispersion liquid, the specific steps are as follows:

[0009] Step 1: mix the zirconium salt and solvent, stir until uniform, to obtain a zirconium salt solution;

[0010] Step 2: add the surfactant and organic acid to the zirconium salt solution, heat and react for a period of time, centrifuge to collect the product, to obtain nano-zirconium oxide;

[0011] Step 3: wash the nano-zirconium oxide obtained in Step 2, disperse into a liquid medium, to obtain a nano-zirconium oxide dispersion, and adjust the pH of the nano-zirconium oxide dispersion to 2-7.

[0012] In a more preferred embodiment, the solubility of the zirconium salt solution in Step 1 is 5wt%-30wt%.

[0013] In a more preferred embodiment, the liquid medium in Step 3 is any one or a mixture of several of toluene, methanol, ethanol, n-heptane, ethyl acetate.

[0014] In a more preferred embodiment, the surfactant in Step 2 is any one or a mixture of several of caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, oleic acid, petroselinic acid, erucic acid, linoleic acid, 2,4-decadienoic acid, linolenic acid, chaulmoogric acid, stearic acid, α-eleostearic acid, ricinoleic acid, polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone.

[0015] In a more preferred embodiment, the organic acid in Step 2 is any one or a mixture of several of formic acid, acetic acid, oxalic acid, propionic acid, propiolate acid, butyric acid, succinic acid, benzoic acid, phenylacetic acid, phthalic acid, terephthalic acid, valeric acid, hexanoic acid, capric acid, maleic acid, tartaric acid, malic acid, citric acid, ascorbic acid, salicylic acid, coffee acid.

[0016] In a more preferred embodiment, the solid content of the nano-zirconium oxide dispersion is 50-60wt%; the pH of the nano-zirconium oxide dispersion is adjusted to 2-4.

[0017] In a more preferred embodiment, the addition amount of the surfactant is 3wt%-7wt% of the total mass of the system; the addition amount of the organic acid is 3wt%-15wt% of the total mass of the system.

[0018] In a more preferred embodiment, the solvent in Step 1 is any one or a mixture of two of deionized water, an organic solvent; the organic solvent is any one or a mixture of several of toluene, xylene, n-pentane, isopentane, hexane, cyclohexane, cyclohexanone, methanol, ethanol, ethylene glycol, benzyl alcohol, isopropyl alcohol, diethyl ether, propyl ether, n-heptane, butyl acetate, ethyl acetate.

[0019] More preferably, in step 1, the zirconium salt is any one or a mixture of several of zirconium hydroxycarbonate, zirconium nitrate, zirconium oxychloride, zirconium acetate, zirconium propionate, zirconium n-propyl alcohol, zirconium isopropyl alcohol, zirconium phosphate, zirconium citrate, zirconium iso-octanoate, zirconium hydroxide, and zirconium hexafluoride.

[0020] More preferably, in step 2, the temperature is raised to 170-230°C, and the reaction time is 10-72 hours.

[0021] More preferably, the nano-zirconium oxide dispersion liquid is prepared by the method according to any one of the above.

[0022] Compared with the prior art, the present application has the following beneficial effects:

[0023] (1) In the present application, the zirconium salt solution is directly poured into water or an organic solvent or a mixed solution of water and an organic solvent, and then hydrothermally treated to directly obtain nano-zirconium oxide particles and wash them to obtain a nano-zirconium oxide liquid dispersion. Compared with the related art, the method for preparing the nano-zirconium oxide dispersion liquid is simpler and does not require other complicated procedures.

[0024] (2) According to the experimental data, the refractive index of the nano-zirconium oxide liquid dispersion prepared by the method of the present application is about 1.7-1.8, while the refractive index of the nano-zirconium oxide dispersion liquid in the related art is about 1.6. The refractive index is improved, and the light transmittance of the zirconium oxide dispersion liquid in the preparation of downstream products is improved, which facilitates the processing of downstream processes.

[0025] (3) The technical point of the present application is the dispersion system of nano-zirconium oxide and liquid medium. By adjusting the solid content and pH of the dispersion system, the dispersion is maintained under acidic conditions to improve the refractive index of the nano-zirconium oxide dispersion liquid to 1.7-1.8. BRIEF DESCRIPTION OF DRAWINGS

[0026] The accompanying drawings are included to provide a further understanding of the present application, and constitute a part of the specification, illustrate the present application and are used to explain the present application, and do not constitute a limitation on the present application. In the drawings:

[0027] Figure 1 is an electron microscope diagram of the nano-zirconium oxide powder of Example 3 of the present application Figure One .

[0028] Figure 2 is an electron microscope diagram of the nano-zirconium oxide powder of Example 3 of the present application Figure Two . DETAILED DESCRIPTION

[0029] With reference to the accompanying drawings, the technical solutions in the embodiments of the present application will be clearly and completely described below, obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work belong to the protection scope of the present application.

[0030] Embodiment 1

[0031] A method for simply preparing a high-refractive transparent nanometer zirconium oxide dispersion liquid, and the specific steps are as follows:

[0032] Step 1: 3.08 g of zirconium carbonate and 48 g of benzyl alcohol are mixed and stirred uniformly to obtain a zirconium salt solution;

[0033] Step 2: 2 g of a surfactant and 1.8 g of an organic acid are added to the zirconium salt solution prepared in step 1, the temperature is raised to 230 DEG C, and the solution is subjected to a solvothermal reaction for 36 h; the product is collected by centrifugation at 5000 r / min for 5 min to obtain nanometer zirconium oxide; the surfactant is lauric acid, and the organic acid is butyric acid.

[0034] Step 3: The nanometer zirconium oxide obtained in step 2 is washed with ethanol for 3 times, and is dispersed in toluene to obtain a clear and transparent nanometer zirconium oxide dispersion liquid. The solid content of the nanometer zirconium oxide dispersion liquid is 60 wt%, and the pH of the solution is adjusted to 4 by an organic acid.

[0035] The detection result is that no visible precipitate is observed after standing for 6 months at room temperature. The obtained dispersion is observed by transmission electron microscopy, and the refractive index of the nanometer zirconium oxide dispersion liquid is about 1.693. At this time, the refractive index of the nanometer zirconium oxide dispersion liquid is generally, and it can be seen that the one-dimensional size of the particles of the obtained nanometer zirconium oxide / toluene phase dispersion is 7 nm, and the particles are uniformly dispersed.

[0036] Embodiment 2

[0037] A method for simply preparing a high-refractive transparent nanometer zirconium oxide dispersion liquid, and the specific steps are as follows:

[0038] Step 1: 6.16 g of zirconium carbonate and 48 g of benzyl alcohol are mixed and stirred uniformly to obtain a zirconium salt solution;

[0039] Step 2: 2 g of a surfactant and 3.6 g of an organic acid are added to the zirconium salt solution prepared in step 1, the temperature is raised to 230 DEG C, and the solution is subjected to a solvothermal reaction for 36 h; the product is collected by centrifugation at 5000 r / min for 5 min to obtain nanometer zirconium oxide; the surfactant is lauric acid, and the organic acid is butyric acid.

[0040] Step 3: The nano-zirconium oxide obtained in Step 2 is washed with ethanol for 3 times, and dispersed in toluene to obtain a clear and transparent nano-zirconium oxide dispersion. The solid content of the nano-zirconium oxide dispersion is 60wt%, and the pH of the solution is adjusted to 4.

[0041] The detection result is that there is no visible precipitate after standing for 6 months at room temperature. The obtained dispersion is observed by transmission electron microscopy, and the refractive index of the nano-zirconium oxide dispersion is about 1.789. At this time, the refractive index of the obtained nano-zirconium oxide dispersion is better, and it can be seen that the one-dimensional size of the obtained nano-zirconium oxide / toluene phase dispersion particles is 7nm, and the particles are uniformly dispersed.

[0042] Example 3

[0043] A simple method for preparing a high-refractive transparent nano-zirconium oxide dispersion, the specific steps are:

[0044] Step 1: Mix 6.16g of zirconium carbonate and 48g of benzyl alcohol, and stir uniformly to obtain a zirconium salt solution;

[0045] Step 2: Add 4g of a surfactant and 5.4g of an organic acid to the zirconium salt solution prepared in Step 1, heat to 230℃, and solvothermal reaction for 36h, centrifuge at 5000r / min for 5min, collect the product to obtain nano-zirconium oxide; the surfactant is lauric acid, and the organic acid is butyric acid.

[0046] Step 3: The nano-zirconium oxide obtained in Step 2 is washed with ethanol for 3 times, and dispersed in toluene to obtain a clear and transparent nano-zirconium oxide dispersion. The solid content of the nano-zirconium oxide dispersion is 60wt%, and the pH of the solution is adjusted to 4.

[0047] The detection result is that there is no visible precipitate after standing for 6 months at room temperature. The obtained dispersion is observed by transmission electron microscopy, and the refractive index of the nano-zirconium oxide dispersion is about 1.789. At this time, the refractive index of the obtained nano-zirconium oxide dispersion is better, and it can be seen that the one-dimensional size of the obtained nano-zirconium oxide / toluene phase dispersion particles is 7nm, and the particles are uniformly dispersed.

[0048] Comparative Example 1: Comparative Example 1 and Example 3 are control experiments. In Comparative Example 1, the pH of the nano-zirconium oxide dispersion is adjusted to 7.

[0049] A simple method for preparing a high-refractive transparent nano-zirconium oxide dispersion, the specific steps are:

[0050] Step 1: Mix 6.16g of zirconium carbonate and 48g of benzyl alcohol, and stir uniformly to obtain a zirconium salt solution;

[0051] Step 2: 4 g of surfactant and 5.4 g of organic acid were added to the zirconium salt solution prepared in Step 1, and the temperature was raised to 230°C, and the solvothermal reaction was carried out for 36 h. The product was collected by centrifugation at 5000 r / min for 5 min, and the nanometer zirconium oxide was obtained. The surfactant was lauric acid, and the organic acid was butyric acid.

[0052] Step 3: The nanometer zirconium oxide obtained in Step 2 was washed with ethanol for 3 times, and dispersed in toluene to obtain a clear and transparent nanometer zirconium oxide dispersion liquid. The solid content of the nanometer zirconium oxide dispersion liquid was 60 wt%, and the pH of the solution was adjusted to 7.

[0053] Comparative Example 2: Comparative Example 2 and Example 3 are control experiments. In Comparative Example 2, the solid content of the nanometer zirconium oxide dispersion liquid was adjusted to 70 wt%.

[0054] A simple method for preparing a high-refractive transparent nanometer zirconium oxide dispersion liquid, the specific steps are as follows:

[0055] Step 1: 6.16 g of zirconium carbonate and 48 g of benzyl alcohol were mixed and stirred uniformly to obtain a zirconium salt solution;

[0056] Step 2: 4 g of surfactant and 5.4 g of organic acid were added to the zirconium salt solution prepared in Step 1, and the temperature was raised to 230°C, and the solvothermal reaction was carried out for 36 h. The product was collected by centrifugation at 5000 r / min for 5 min, and the nanometer zirconium oxide was obtained. The surfactant was lauric acid, and the organic acid was butyric acid.

[0057] Step 3: The nanometer zirconium oxide obtained in Step 2 was washed with ethanol for 3 times, and dispersed in toluene to obtain a clear and transparent nanometer zirconium oxide dispersion liquid. The solid content of the nanometer zirconium oxide dispersion liquid was 70 wt%, and the pH of the solution was adjusted to 4.

[0058] Example 4

[0059] A simple method for preparing a high-refractive transparent nanometer zirconium oxide dispersion liquid, the specific steps are as follows:

[0060] Step 1: 3.22 g of zirconium oxychloride and 48 g of benzyl alcohol were mixed and stirred uniformly to obtain a zirconium salt solution;

[0061] Step 2: 2 g of surfactant and 0.7 g of organic acid were added to the zirconium salt solution prepared in Step 1, and the temperature was raised to 230°C, and the solvothermal reaction was carried out for 36 h. The product was collected by centrifugation at 5000 r / min for 5 min, and the nanometer zirconium oxide was obtained. The surfactant was lauric acid, and the organic acid was butyric acid.

[0062] Step 3: The nanometer zirconium oxide obtained in Step 2 was washed with ethanol for 3 times, and dispersed in toluene to obtain a clear and transparent nanometer zirconium oxide dispersion liquid. The solid content of the nanometer zirconium oxide dispersion liquid was 60 wt%, and the pH of the solution was adjusted to 2.

[0063] The detection result is that no visible precipitate is observed at room temperature for 6 months. The obtained dispersion is observed by transmission electron microscopy, and the refractive index of the nano-zirconium oxide dispersion is about 1.687. At this time, compared with Example 3, the refractive index of the nano-zirconium oxide dispersion is general, and it can be seen that the one-dimensional size of the obtained zirconium oxide / toluene phase dispersion particles is 7 nm, and the particles are uniformly dispersed.

[0064] Example 5

[0065] A simple method for preparing a high-refractive transparent nano-zirconium oxide dispersion is provided, and the specific steps are as follows:

[0066] Step 1: 6.16 g of zirconium oxychloride octahydrate and 48 g of benzyl alcohol are mixed and stirred uniformly to obtain a zirconium salt solution;

[0067] Step 2: 2 g of a surfactant and 0.7 g of an organic acid are added to the zirconium salt solution prepared in Step 1, and the temperature is raised to 230°C. Solvothermal reaction is performed for 36 h, and the product is collected by centrifugation at 5000 r / min for 5 min to obtain nano-zirconium oxide. The surfactant is lauric acid, and the organic acid is butyric acid.

[0068] Step 3: The nano-zirconium oxide obtained in Step 2 is washed with ethanol for 3 times, and dispersed in toluene to obtain a clear and transparent nano-zirconium oxide dispersion. The solid content of the nano-zirconium oxide dispersion is 60 wt%, and the pH of the solution is adjusted to 2 by hydrochloric acid.

[0069] The detection result is that no visible precipitate is observed at room temperature for 6 months. The obtained dispersion is observed by transmission electron microscopy, and the refractive index of the nano-zirconium oxide dispersion is about 1.705. At this time, compared with Example 3, the refractive index of the nano-zirconium oxide dispersion is lower than that of Example 3, and it can be seen that the one-dimensional size of the obtained zirconium oxide / toluene phase dispersion particles is 7 nm, and the particles are uniformly dispersed.

[0070] In Comparative Example 3, the pH of the nano-zirconium oxide dispersion is adjusted to 9.

[0071] A simple method for preparing a high-refractive transparent nano-zirconium oxide dispersion is provided, and the specific steps are as follows:

[0072] Step 1: 3.22 g of zirconium oxychloride octahydrate and 48 g of benzyl alcohol are mixed and stirred uniformly to obtain a zirconium salt solution;

[0073] Step 2: 2.4 g of a surfactant and 0.8 g of sodium hydroxide are added to the zirconium salt solution prepared in Step 1, and the temperature is raised to 230°C. Solvothermal reaction is performed for 36 h, and the product is collected by centrifugation at 5000 r / min for 5 min to obtain nano-zirconium oxide. The surfactant is lauric acid.

[0074] Step 3: The nano-zirconium oxide obtained in Step 2 is washed with ethanol for 3 times, dispersed in toluene to obtain a clear and transparent nano-zirconium oxide dispersion. The solid content of the nano-zirconium oxide dispersion is 60wt%, and the pH of the solution is adjusted to 9.

[0075] Test result: No visible precipitate is observed after standing at room temperature for 6 months. Dispersion phenomenon occurs in the solution, so the alkaline condition is not conducive to dispersion.

[0076] Comparative Example 4: Comparative Example 4 is a control experiment of Example 4. In Comparative Example 4, the pH of the nano-zirconium oxide dispersion is adjusted to 7.

[0077] A simple method for preparing a high-refractive transparent nano-zirconium oxide dispersion includes the following steps:

[0078] Step 1: 3.22g of zirconium oxychloride octahydrate and 48g of benzyl alcohol are mixed and stirred uniformly to obtain a zirconium salt solution.

[0079] Step 2: 2g of a surfactant and 0.7g of an organic acid are added to the zirconium salt solution prepared in Step 1, and the temperature is raised to 230°C. Solvothermal reaction is performed for 36h, and the product is collected by centrifugation at 5000r / min for 5min to obtain nano-zirconium oxide. The surfactant is lauric acid, and the organic acid is butyric acid.

[0080] Step 3: The nano-zirconium oxide obtained in Step 2 is washed with ethanol for 3 times, dispersed in toluene to obtain a clear and transparent nano-zirconium oxide dispersion. The solid content of the nano-zirconium oxide dispersion is 60wt%, and the pH of the solution is adjusted to 7.

[0081] Comparative Example 5: In Comparative Example 5, the pH of the nano-zirconium oxide dispersion is adjusted to 9, and the organic solvent is selected as ethylene glycol.

[0082] A simple method for preparing a high-refractive transparent nano-zirconium oxide dispersion includes the following steps:

[0083] Step 1: 6.45g of zirconium oxychloride octahydrate and 48g of ethylene glycol are mixed and stirred uniformly to obtain a zirconium salt solution.

[0084] Step 2: 2.4g of a surfactant and 0.8g of sodium hydroxide are added to the zirconium salt solution prepared in Step 1, and the temperature is raised to 230°C. Solvothermal reaction is performed for 36h, and the product is collected by centrifugation at 5000r / min for 5min to obtain nano-zirconium oxide. The surfactant is lauric acid.

[0085] Step 3: The nano-zirconium oxide obtained in Step 2 is washed with ethanol for 3 times, dispersed in toluene to obtain a clear and transparent nano-zirconium oxide dispersion. The solid content of the nano-zirconium oxide dispersion is 60wt%, and the pH of the solution is adjusted to 9.

[0086] Comparative Example 6: In Comparative Example 6, the pH of the nano-zirconium oxide dispersion liquid is adjusted to 9, and the organic solvent is selected as n-heptane.

[0087] A method for simply preparing a high-refractive transparent nano-zirconium oxide dispersion liquid, the specific steps are:

[0088] Step 1: 6.45 g of zirconium oxychloride octahydrate and 48 g of n-heptane are mixed and stirred uniformly to obtain a zirconium salt solution;

[0089] Step 2: 2.4 g of a surfactant and 0.8 g of sodium hydroxide are added to the zirconium salt solution prepared in Step 1, the temperature is raised to 230°C, and the solvent is heated for 36 h; centrifugation is performed at 5000 r / min for 5 min, and the product is collected to obtain nano-zirconium oxide; the surfactant is lauric acid.

[0090] Step 3: The nano-zirconium oxide obtained in Step 2 is washed with ethanol for 3 times, and dispersed in toluene to obtain a clear and transparent nano-zirconium oxide dispersion liquid. The solid content of the nano-zirconium oxide dispersion liquid is 60 wt%, and the pH of the solution is adjusted to 9.

[0091] Comparative Example 7: Comparative Example 7 is a control experiment with Example 3. In Comparative Example 7, the solid content of the nano-zirconium oxide dispersion liquid is adjusted to 40 wt%.

[0092] A method for simply preparing a high-refractive transparent nano-zirconium oxide dispersion liquid, the specific steps are:

[0093] Step 1: 6.45 g of zirconium oxychloride octahydrate and 48 g of n-heptane are mixed and stirred uniformly to obtain a zirconium salt solution;

[0094] Step 2: 2.4 g of a surfactant and 0.8 g of sodium hydroxide are added to the zirconium salt solution prepared in Step 1, the temperature is raised to 230°C, and the solvent is heated for 36 h; centrifugation is performed at 5000 r / min for 5 min, and the product is collected to obtain nano-zirconium oxide; the surfactant is lauric acid.

[0095] Step 3: The nano-zirconium oxide obtained in Step 2 is washed with ethanol for 3 times, and dispersed in toluene to obtain a clear and transparent nano-zirconium oxide dispersion liquid. The solid content of the nano-zirconium oxide dispersion liquid is 40 wt%, and the pH of the solution is adjusted to 4.

[0096] Comparative Example 8: Comparative Example 8 is a control experiment with Example 3. In Comparative Example 8, the amount of the surfactant added is adjusted.

[0097] A method for simply preparing a high-refractive transparent nano-zirconium oxide dispersion liquid, the specific steps are:

[0098] Step 1: 6.45 g of zirconium oxychloride octahydrate and 48 g of n-heptane are mixed and stirred uniformly to obtain a zirconium salt solution;

[0099] Step 2: 4 g of surfactant and 5.4 g of organic acid were added to the zirconium salt solution prepared in step 1, and the temperature was raised to 230°C for solvent thermal reaction for 36 h, and then centrifuged at 5000 r / min for 5 min, and the product was collected to obtain nano-zirconia; the surfactant was lauric acid, and the organic acid was butyric acid.

[0100] Step 3: The nano-zirconia obtained in step 2 was washed with ethanol for 3 times, and then dispersed in toluene to obtain a clear and transparent nano-zirconia dispersion liquid. The solid content of the nano-zirconia dispersion liquid was 70 wt%, and the pH of the solution was adjusted to 4.

[0101] Comparative Example 9: Comparative Example 9 and Example 3 were control experiments, and the amount of organic acid added in Comparative Example 9 was adjusted.

[0102] A simple method for preparing a high-refractive transparent nano-zirconia dispersion liquid, the specific steps are as follows:

[0103] Step 1: 6.16 g of zirconium carbonate and 48 g of benzyl alcohol were mixed and stirred uniformly to obtain a zirconium salt solution;

[0104] Step 2: 4 g of surfactant and 5.4 g of organic acid were added to the zirconium salt solution prepared in step 1, and the temperature was raised to 230°C for solvent thermal reaction for 36 h, and then centrifuged at 5000 r / min for 5 min, and the product was collected to obtain nano-zirconia; the surfactant was lauric acid, and the organic acid was butyric acid.

[0105] Step 3: The nano-zirconia obtained in step 2 was washed with ethanol for 3 times, and then dispersed in toluene to obtain a clear and transparent nano-zirconia dispersion liquid. The solid content of the nano-zirconia dispersion liquid was 70 wt%, and the pH of the solution was adjusted to 4.

[0106] The raw material usage and parameters of the above examples and comparative examples are shown in the following table:

[0107]

[0108] It should be noted that, in this document, relational terms such as first and second and the like can be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises", "comprising", or any other variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but can include other elements not expressly listed or inherent to such process, method, article, or apparatus.

[0109] Finally, it should be noted that the above only describes the preferred embodiments of the present application and is not intended to limit the present application. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art will appreciate that the technical solutions described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalent ones. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A simple method for preparing a high-refractive-index transparent nano-zirconia dispersion, characterized in that: The specific steps are: Step 1: Mix the zirconium salt and the solvent, stir evenly, and obtain a zirconium salt solution; Step 2: Add a surfactant and an organic acid to the zirconium salt solution, heat the solution to react for a period of time, and collect the product by centrifugation to obtain nano zirconium oxide; Step 3: washing the nano-zirconia obtained in step 2, dispersing it into a liquid medium to obtain a nano-zirconia dispersion, and adjusting the pH of the nano-zirconia dispersion to 2-7; The surfactant is any one of caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, oleic acid, petroselinic acid, erucic acid, linoleic acid, 2,4-decadienic acid, linolenic acid, calendula acid, oleic acid, α-eleostearic acid, vernolic acid, ricinoleic acid, polyvinyl alcohol, polyethylene glycol, and polyvinyl pyrrolidone, or a mixture thereof; The organic acid is any one of formic acid, acetic acid, oxalic acid, propionic acid, acrylic acid, butyric acid, succinic acid, benzoic acid, phenylacetic acid, phthalic acid, terephthalic acid, valeric acid, hexanoic acid, capric acid, maleic acid, tartaric acid, malic acid, citric acid, ascorbic acid, salicylic acid, and caffeic acid, or a mixture thereof; The solid content of the nano-zirconia dispersion is 50-60 wt %; the pH of the nano-zirconia dispersion is adjusted to 2-4; The added amount of the surfactant is 3wt%~7wt% of the total mass of the system; the added amount of the organic acid is 3wt%~15wt% of the total mass of the system.

2. The method for preparing a high-refractive-index transparent nano-zirconia dispersion according to claim 1, characterized in that: In step 1, the solubility of the zirconium salt solution is 5wt%~30wt%.

3. The method for preparing a high-refractive-index transparent nano-zirconia dispersion according to claim 1, characterized in that: In step 3, the liquid medium is any one of toluene, methanol, ethanol, n-heptane, and ethyl acetate, or a mixture of several of them.

4. The method for preparing a high-refractive-index transparent nano-zirconia dispersion according to claim 1, characterized in that: In step 1, the solvent is any one of deionized water and an organic solvent, or a mixture of two of them; the organic solvent is any one of toluene, xylene, n-pentane, isopentane, hexane, cyclohexane, cyclohexanone, methanol, ethanol, ethylene glycol, benzyl alcohol, isopropanol, diethyl ether, propyl ether, n-heptane, butyl acetate, and ethyl acetate, or a mixture of several of them.

5. The method for preparing a high-refractive-index transparent nano-zirconia dispersion according to claim 1, characterized in that: In step 1, the zirconium salt is any one of basic zirconium carbonate, zirconium nitrate, zirconium oxychloride, zirconium acetate, zirconium propionate, zirconium n-propoxide, zirconium isopropoxide, zirconium phosphate, zirconium citrate, zirconium isooctanoate, zirconium hydroxide, and hexafluorozirconic acid, or a mixture of several of them.

6. The method for preparing a high-refractive-index transparent nano-zirconia dispersion according to claim 1, characterized in that: In step 2, the temperature is raised to 170°C to 230°C, and the reaction time is 10 to 72 hours.

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