A method for preparing monodisperse spherical yttrium oxide with controllable particle size

By preparing specific surfactants and high-temperature and high-pressure reactions, the problem of difficult control of nano-yttrium oxide particle size distribution was solved, the uniformity and dispersion of spherical yttrium oxide were achieved, and the stability and application effect of the material were ensured.

CN120348968BActive Publication Date: 2025-09-09JIANGSU GUOSHENG RARE EARTH CO LTD
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Patent Information

Application Number
CN202510820434.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-06-19
Publication Date
2025-09-09
Estimated Expiration
2045-06-19

AI Technical Summary

Technical Problem

In the existing technology for preparing nano-yttrium oxide, it is difficult to precisely control the particle size distribution, which causes the nanoparticles to easily agglomerate and affects their application performance.

Method used

Specific surfactants are used to prepare monodisperse spherical yttrium oxide with controllable particle size through electrostatic interaction and steric hindrance. The specific steps include preparing ester double bond compounds, epoxy compounds, tetraimidazole compounds and surfactants, combining high temperature and high pressure reaction and roasting process to form a confined space for the growth of nanomaterials.

Benefits of technology

The uniform morphology and good dispersibility of spherical yttrium oxide are achieved, the particle size distribution is narrow, the particle size is controllable, the agglomeration of nanoparticles is avoided, and the dispersion performance of the material is improved.

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Abstract

The present invention discloses a method for preparing monodisperse spherical yttrium oxide with controllable particle size, and relates to the field of rare earth materials. The method for preparing monodisperse spherical yttrium oxide with controllable particle size comprises the following steps: S1: stirring and mixing an alcoholic solution of triethanolamine and aqueous ammonia to prepare a mixed precipitant solution; S2: slowly adding an yttrium nitrate solution to the mixed precipitant solution at 60-80°C, aging the solution after addition, filtering, and washing with deionized water to obtain a precursor precipitate; S3: stirring and mixing 1,2-propylene glycol, the precursor precipitate, and a surfactant, reacting the mixture under high temperature and high pressure, filtering, washing, drying, and calcining to obtain spherical yttrium oxide. The spherical yttrium oxide particles prepared by the present invention have good dispersibility and no agglomeration; the particle size is uniform and controllable, and the particle size distribution range is narrow.
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Description

Technical Field

[0001] The present invention relates to the field of rare earth materials, and in particular to a method for preparing monodisperse spherical yttrium oxide with controllable particle size. Background Art

[0002] Nano-yttrium oxide (Y2O3) is an important rare earth nanomaterial with unique physical and chemical properties compared to traditional materials, making it widely applicable in fields such as fluorescent materials and advanced ceramics. Yttrium oxide nanospheres possess higher specific surface area, surface atomic number, surface energy, and improved dispersibility, significantly enhancing their optical, electrical, magnetic, mechanical, and chemical properties. The main methods for preparing nano-yttrium oxide include sol-gel, hydrothermal synthesis, combustion, electrochemical, and precipitation methods.

[0003] Due to their large surface energy, nanoparticles are unstable and prone to agglomeration, losing their inherent properties and severely impacting the application of nanomaterials. By designing a synthesis method and combining different surfactants, we achieve controlled synthesis of yttrium oxide powder morphology while ensuring good dispersion and uniformity. This customized preparation of powder morphology has important scientific significance and application value.

[0004] Chinese invention patent application publication number CN118145693A discloses a method for preparing yttrium oxide powder. The invention involves a precipitation reaction between an aqueous yttrium salt solution and an alkali metal hydroxide at a pH of 7-14; a hydrothermal reaction of the reaction mixture at a temperature of 160-200°C to produce a precursor; and preheating the precursor at 200-300°C before calcining it at 800-900°C to produce the yttrium oxide powder. This method allows the preparation of yttrium oxide powders of varying morphologies and crystal structures by controlling the pH of the reaction system. However, the invention has limitations in precisely controlling the particle size distribution. Summary of the Invention

[0005] In view of the shortcomings of the prior art, the object of the present invention is to provide a method for preparing monodisperse spherical yttrium oxide with controllable particle size.

[0006] To achieve the above object, the present invention is implemented through the following technical solutions:

[0007] A method for preparing monodisperse spherical yttrium oxide with controllable particle size comprises the following steps:

[0008] S1: stirring and mixing the alcohol solution of triethanolamine and aqueous ammonia to prepare a mixed precipitant solution;

[0009] S2: Slowly add the yttrium nitrate solution to the mixed precipitant solution at 60-80°C, age it, filter it, and wash it with deionized water to obtain a precursor precipitate;

[0010] S3: mixing 1,2-propylene glycol, the precursor precipitate and the surfactant, reacting at high temperature and high pressure, filtering, washing, drying and calcining to obtain spherical yttrium oxide;

[0011] The surfactant is prepared by the following method:

[0012] N1: 2,6-nonadien-1-ol reacts with n-octylsuccinic anhydride to form an ester double bond compound; the reaction equation is as follows:

[0013]

[0014] N2: Ester double bond compound generates epoxy compound under the action of formic acid and 30wt% H2O2; the reaction equation is as follows:

[0015]

[0016] N3: The epoxy compound reacts with 1-(2-hydroxyethyl)imidazole to form a tetraimidazole compound; the reaction equation is as follows:

[0017]

[0018] N4: Tetraimidazole compound reacts with 1-bromododecane to form a surfactant; the reaction equation is as follows:

[0019]

[0020] In step N1, the molar ratio of the 2,6-nonadien-1-ol to n-octylsuccinic anhydride is 2:1; in step N2, the mass ratio of the ester double bond compound, formic acid, and 30wt% H2O2 is 10:6:9; in step N3, the molar ratio of the epoxy compound to 1-(2-hydroxyethyl)imidazole is 1:5; in step N4, the molar ratio of the tetraimidazole compound to 1-bromododecane is 1:4.5.

[0021] In step S1, the solvent in the alcoholic solution of triethanolamine is one of ethanol, n-butanol and n-hexanol.

[0022] In step S1, the concentration of the triethanolamine alcohol solution is 1-2 mol / L, and the volume ratio of the ammonia water to the triethanolamine alcohol solution is (5-10):1.

[0023] In step S2, the concentration of the yttrium nitrate solution is 0.1-0.2 mol / L.

[0024] In step S2, the molar ratio of triethanolamine in the mixed precipitant solution to yttrium nitrate in the yttrium nitrate solution is 10:(1-2).

[0025] In step S3, the mass ratio of the precursor precipitate, surfactant, and 1,2-propylene glycol is 50:(5-15):(300-600).

[0026] In step S3, the high temperature and high pressure reaction temperature is 100-150° C., the time is 12-24 hours, and the pressure is 0.5-8.0 MPa.

[0027] In step S3, the calcination temperature is 700-800° C. and the calcination time is 3-5 hours.

[0028] Due to the adoption of the above technical solution, the beneficial effects of the present invention include:

[0029] The surfactant prepared by the present invention is adsorbed on the surface of the nanoparticles through electrostatic action, and forms micelles under the action of the hydrophobic long chain, providing a confined space for the growth of the nanomaterial. The steric hindrance of the imidazole ring and the electrostatic repulsion of the quaternary ammonium salt limit the growth space of the nanomaterial, so that the prepared spherical nano yttrium oxide powder has uniform morphology, good dispersibility and narrow particle size distribution, and the nano yttrium oxide powder with a size of less than 1000 nm can be prepared in a controllable manner. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 This is a high-resolution mass spectrum of the surfactant prepared in Example 1;

[0031] Figure 2 This is a scanning electron microscope image of spherical yttrium oxide prepared in Example 2;

[0032] Figure 3 This is a scanning electron microscope image of spherical yttrium oxide prepared in Example 3;

[0033] Figure 4 This is a scanning electron microscope image of spherical yttrium oxide prepared in Example 4;

[0034] Figure 5 This is a scanning electron microscope image of spherical yttrium oxide prepared in Example 5;

[0035] Figure 6 This is a scanning electron micrograph of spherical yttrium oxide prepared in Example 6;

[0036] Figure 7 This is a scanning electron microscope image of spherical yttrium oxide prepared in Example 7. DETAILED DESCRIPTION

[0037] The present invention will be further described below with reference to the embodiments, but the present invention is not limited to these embodiments.

[0038] Example 1 Preparation of surfactant:

[0039] N1: Add 400 ml of toluene, 0.1 mol of n-octylsuccinic anhydride, 0.2 mol of 2,6-nonadien-1-ol, and 5 g of p-toluenesulfonic acid to a reaction flask, stir and mix thoroughly, heat to 100°C, react for 7 h, separate the water produced during the reaction through a water separator, cool to room temperature, adjust the pH to 7 with saturated sodium bicarbonate solution, allow to stand and separate, wash the organic phase with deionized water three times (200 ml each time), dry with 40 g of anhydrous magnesium sulfate, filter, and distill the organic phase under reduced pressure at 60°C for 3 h to obtain an ester double bond compound; its H NMR spectrum data are as follows: 1 H NMR (300 MHz, Chloroform- d ) δ 5.76 - 5.55 (m, 4H), 5.55 - 5.28 (m, 4H), 4.76 - 4.58 (m, 4H), 2.93 - 2.67 (m, 2H), 2.56 - 2.42(m, 1H), 2.21 - 1.97 (m, 12H), 1.78 (dq, J = 13.8, 8.4 Hz, 1H), 1.62 - 1.16 (m, 13H), 1.02 - 0.79 (m, 9H);

[0040] N2: 300 ml of DMF, 50 g of an ester double bond compound, and 5 g of a strong acid cation exchange resin were sequentially added to a reaction kettle, stirred, and heated to 60°C. A mixed solution of 30 g of formic acid and 45 g of 30 wt% H2O2 was added dropwise over 30 min. The reaction was continued for 6 h, and the mixture was distilled under reduced pressure at 60°C for 3 h. The mixture was washed three times with deionized water (300 ml each time), and dried under vacuum at 50°C for 10 h to obtain an epoxy compound. The H NMR spectrum data are as follows: 1 H NMR (300 MHz, Chloroform- d) δ 4.40 (dt, J = 11.4, 3.5 Hz, 2H), 4.15 (dt, J = 11.4, 3.5 Hz, 2H), 3.63 (dq, J = 4.7, 3.2 Hz, 2H), 3.34(q, J = 4.7 Hz, 2H), 3.25 (q, J = 4.4 Hz, 2H), 3.13 - 3.02 (m, 2H), 2.94 -2.67 (m, 2H), 2.48 (dd, J = 16.6, 8.7 Hz, 1H), 2.02 - 1.48 (m, 14H), 1.47 -1.14 (m, 12H), 0.98 - 0.82 (m, 9H);

[0041] N3: Under nitrogen protection, 600 ml of isopropanol, 0.1 mol of the epoxy compound, and 0.5 mol of 1-(2-hydroxyethyl)imidazole were added to the reactor in sequence, stirred and mixed, and 10 g of tetraethylammonium bromide was added. The temperature was raised to 70°C and the reaction was carried out for 4 h. The mixture was cooled and distilled under reduced pressure at 50°C for 2 h. The mixture was washed three times with deionized water (300 ml each time) and dried under vacuum at 70°C for 12 h to obtain the tetraimidazole compound. Its H NMR spectrum data are as follows: 1 H NMR (300 MHz, Chloroform-d) δ 7.80 (tt, J = 1.7, 0.8 Hz, 4H), 7.16 - 7.02 (m, 8H), 4.32 (ddd, J = 11.7, 7.4, 5.7 Hz, 2H), 4.17 - 4.01(m, 10H), 3.97 - 3.72 (m, 12H), 3.67 - 3.52 (m, 4H), 3.27 (d, J = 6.4 Hz, 2H), 2.94 - 2.65 (m, 4H), 2.48 (dd, J = 16.6, 8.7 Hz, 1H), 1.93 - 1.14 (m,26H), 1.00 - 0.82 (m, 9H);

[0042] N4: Add 800 ml of anhydrous ethanol and 0.1 mol of tetraimidazole compound to a reaction kettle, stir and mix, heat to 60°C, and under nitrogen protection, dropwise add 0.45 mol of 1-bromododecane over 30 minutes. Reflux for 48 hours, cool to room temperature, and distill under reduced pressure at 60°C for 2 hours. Wash twice with acetone (500 ml each time), and dry under vacuum at 50°C for 6 hours to obtain a surfactant. Its H NMR spectrum data are as follows: 1 H NMR (300 MHz, Chloroform-d ) δ 10.13 (tt, J = 1.7, 0.9 Hz, 4H), 7.88 (ddt, J = 4.2, 1.7, 0.9 Hz, 4H), 7.71 (ddt, J = 4.3, 1.7, 0.9 Hz, 4H), 4.91 (tt, J = 5.6, 0.9 Hz, 8H), 4.39 - 4.26 (m, 2H), 4.24 - 4.02 (m, 10H), 3.97 - 3.71 (m, 12H), 3.68 - 3.53 (m, 4H), 3.27 (d, J = 6.4 Hz, 2H), 2.93 -2.67 (m, 4H), 2.48 (dd, J = 16.7, 8.7 Hz, 1H), 2.08 (tt, J = 7.8, 5.6 Hz, 8H), 1.94 - 1.16 (m, 98H), 1.01 - 0.81 (m, 21H).

[0043] Example 2 Preparation of spherical yttrium oxide:

[0044] S1: 100 ml of triethanolamine alcohol solution (the concentration of triethanolamine is 1 mol / L, the solvent is ethanol) and 500 ml of ammonia water (28 wt%) are stirred and mixed to prepare a mixed precipitant solution;

[0045] S2: Using the reverse feeding method, 100 ml of 0.1 mol / L yttrium nitrate solution was slowly added to 600 ml of the mixed precipitant solution at 60°C via a peristaltic pump. The addition was completed over 1.5 h. The mixture was aged for 2 h, filtered, washed twice with deionized water (500 g each time), and dried under vacuum at 60°C for 10 h to obtain a precursor precipitate.

[0046] S3: 300 g of 1,2-propylene glycol, 50 g of the precursor precipitate, and 5 g of the surfactant (prepared in Example 1) were stirred and mixed, and reacted at 0.5 MPa and 100°C under high temperature and high pressure for 24 h. The mixture was filtered, washed twice with deionized water (500 g each time), vacuum dried at 60°C for 10 h, and calcined at 700°C for 5 h to obtain spherical yttrium oxide.

[0047] Example 3 Preparation of spherical yttrium oxide:

[0048] S1: 100 ml of triethanolamine alcohol solution (the concentration of triethanolamine is 1.5 mol / L, and the solvent is n-butanol) and 800 ml of ammonia water (25 wt%) are stirred and mixed to prepare a mixed precipitant solution;

[0049] S2: Using the reverse feeding method, 150 ml of 0.15 mol / L yttrium nitrate solution was slowly added to 900 ml of the mixed precipitant solution at 70 °C via a peristaltic pump over 1.5 h. The addition was completed, aged for 1.5 h, filtered, washed twice with deionized water (500 g each time), and dried under vacuum at 60 °C for 10 h to obtain a precursor precipitate.

[0050] S3: 450 g of 1,2-propylene glycol, 50 g of the precursor precipitate, and 5 g of the surfactant (prepared in Example 1) were stirred and mixed, and reacted at 5 MPa and 130°C under high temperature and high pressure for 20 h. The mixture was filtered, washed twice with deionized water (500 g each time), vacuum dried at 60°C for 10 h, and calcined at 750°C for 4 h to obtain spherical yttrium oxide.

[0051] Example 4 Preparation of spherical yttrium oxide:

[0052] S1: 100 ml of triethanolamine alcohol solution (the concentration of triethanolamine is 2 mol / L, and the solvent is n-hexanol) and 1 L of ammonia water (20 wt%) are stirred and mixed to prepare a mixed precipitant solution;

[0053] S2: Using the reverse feeding method, 200 ml of 0.2 mol / L yttrium nitrate solution was slowly added to 1100 ml of 80°C mixed precipitant solution via a peristaltic pump. The addition was completed over 1.5 h. The mixture was aged for 1 h, filtered, washed twice with deionized water (500 g each time), and dried under vacuum at 60°C for 10 h to obtain a precursor precipitate.

[0054] S3: 600 g of 1,2-propylene glycol, 50 g of the precursor precipitate, and 5 g of the surfactant (prepared in Example 1) were stirred and mixed, and reacted at 8.0 MPa and 150°C for 12 h. The mixture was filtered, washed twice with deionized water (500 g each time), vacuum dried at 60°C for 10 h, and calcined at 800°C for 3 h to obtain spherical yttrium oxide.

[0055] Example 5 Preparation of spherical yttrium oxide:

[0056] The raw material composition and preparation method of spherical yttrium oxide are basically the same as those in Example 2, except that the amount of surfactant added in step S3 (prepared in Example 1) is replaced from 5 g to 8 g.

[0057] Example 6 Preparation of spherical yttrium oxide:

[0058] The raw material composition and preparation method of spherical yttrium oxide are basically the same as those in Example 2, except that the amount of surfactant added in step S3 (prepared in Example 1) is replaced from 5 g to 10 g.

[0059] Example 7 Preparation of spherical yttrium oxide:

[0060] The raw material composition and preparation method of spherical yttrium oxide are basically the same as those in Example 2, except that the amount of surfactant added in step S3 (prepared in Example 1) is replaced from 5 g to 15 g.

[0061] In Comparative Example 1, the raw material composition and preparation method of spherical yttrium oxide are basically the same as those in Example 5, except that the surfactant in step S3 (prepared in Example 1) is replaced by an equal weight of a surfactant prepared by the following method:

[0062] The preparation method of the surfactant is substantially the same as that of Example 1, except that the 2,6-nonadien-1-ol in step N1 is replaced by an equal molar amount of cis-6-nonen-1-ol.

[0063] In Comparative Example 2, the raw material composition and preparation method of spherical yttrium oxide are basically the same as those in Example 5, except that the surfactant in step S3 (prepared in Example 1) is replaced by an equal weight of a surfactant prepared by the following method:

[0064] The preparation method of the surfactant is basically the same as that of Example 1, except that the 1-(2-hydroxyethyl)imidazole in step N3 is replaced by an equimolar amount of 3-dimethylamino-1-propanol.

[0065] In Comparative Example 3, the raw material composition and preparation method of spherical yttrium oxide are basically the same as those in Example 5, except that the surfactant in step S3 (prepared in Example 1) is replaced by an equal weight of surfactant prepared by the following method:

[0066] N1: Under nitrogen protection, add 400 ml of anhydrous THF, 0.3 mol of potassium carbonate, and 0.2 mol of 2,6-nonadien-1-ol into a reaction kettle, stir for 30 min, cool to 0°C, and add 100 ml of a tetrahydrofuran solution containing 0.1 mol of 1,12-dichlorododecane dropwise for 30 min. Warm the mixture to room temperature and react for 5 h. Wash with saturated brine three times (200 ml each time), and distill under reduced pressure at 30°C for 2 h to obtain a double bond compound.

[0067] N2: 300 ml of DMF, 50 g of a double bond compound, and 5 g of a strong acid cation exchange resin were sequentially added to a reactor, stirred, and heated to 60°C. A mixed solution of 30 g of formic acid and 45 g of 30 wt% H2O2 was added dropwise for 30 min. The reaction was continued for 6 h, and the mixture was distilled under reduced pressure at 60°C for 3 h. The mixture was washed three times with deionized water (300 ml each time), and dried under vacuum at 50°C for 10 h to obtain an epoxy compound.

[0068] N3: Under nitrogen protection, 600 ml of isopropanol, 0.1 mol of the epoxy compound, and 0.5 mol of 1-(2-hydroxyethyl)imidazole were added to the reactor in sequence, stirred and mixed, and 10 g of tetraethylammonium bromide was added. The temperature was raised to 70°C and the reaction was carried out for 4 h. The mixture was cooled and distilled under reduced pressure at 50°C for 2 h. The mixture was washed three times with deionized water (300 ml each time) and dried under vacuum at 70°C for 12 h to obtain the tetraimidazole compound.

[0069] N4: Add 800 ml of anhydrous ethanol and 0.1 mol of tetraimidazole compound to the reactor, stir and mix, heat to 60°C, and under nitrogen protection, add 0.45 mol of 1-bromododecane dropwise for 30 minutes. Reflux for 48 hours, cool to room temperature, and distill under reduced pressure at 60°C for 2 hours to obtain a white solid. Wash with acetone twice (500 ml each time), and vacuum dry at 50°C for 6 hours to obtain a surfactant.

[0070] In Comparative Example 4, the raw material composition and preparation method of spherical yttrium oxide are basically the same as those in Example 5, except that the surfactant in step S3 (prepared in Example 1) is replaced by an equal weight of a surfactant prepared by the following method:

[0071] The preparation method of the surfactant is basically the same as that of Example 1, except that the 1-bromododecane in step N4 is replaced by an equal molar amount of 1-bromohexane.

[0072] In Comparative Example 5, the raw material composition and preparation method of spherical yttrium oxide are basically the same as those in Example 5, except that the surfactant in step S3 (prepared in Example 1) is replaced by an equal weight of PEG2000.

[0073] In Comparative Example 6, the raw material composition and preparation method of spherical yttrium oxide are basically the same as those in Example 5, except that the surfactant in step S3 (prepared in Example 1) is replaced by an equal weight of CTAB.

[0074] The yttrium oxide prepared in Examples 2-7 of the present application was morphologically characterized; the particle size distribution of the yttrium oxide prepared in Examples 2-7 of the present application and Comparative Examples 1-6 was tested using a laser particle size analyzer (using sodium hexametaphosphate as a dispersant and then dispersed in an ultrasonic oscillator for 5 minutes). The test results are shown in Table 1.

[0075] Table 1 Particle size distribution of spherical yttrium oxide

[0076]

[0077] Note: The particle size distribution values ​​in the above table are rounded off.

[0078] It can be seen from Examples 2, 5, 6, and 7 in Table 1 that the spherical yttrium oxide particles prepared by the present invention have good dispersibility and no agglomeration; the particle size is uniform and controllable, and the particle size distribution range is narrow. Spherical yttrium oxide of several hundred nanometers can be prepared by controlling the amount of surfactant added.

[0079] The imidazole N, ester group (-COO-), and ether bond in the surfactant prepared in this application possess high polarity, resulting in strong chemical adsorption or chemical bonding on the nanoparticles. The imidazole quaternary ammonium salt cations adsorb onto the nanoparticle surface through electrostatic interactions, interacting with the hydrophobic long-chain alkyl groups to form micelles with a tendency to aggregate, providing a confined space for the growth of the nanomaterial. The surfactant prepared in this application can form a molecular film on the surface of the nanoparticles, hindering contact between the particles and improving dispersion performance. Furthermore, the steric hindrance of the imidazole ring and the electrostatic repulsion of the quaternary ammonium salt can prevent further growth of the nanoparticles. The surfactant used in Comparative Example 1 contained only two quaternary ammonium salts, resulting in uneven adsorption and dispersion, leading to larger yttrium oxide nanoparticles and a wider particle size distribution. The surfactant used in Comparative Example 4 had a shorter hydrophobic chain, resulting in poor nanoparticle dispersibility and uncontrollable particle size growth.

[0080] pass Figure 2-7 It can be seen that the yttrium oxide prepared in this application is spherical particles.

[0081] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. However, any equivalent changes, modifications and evolutions made by ordinary technicians in this field without departing from the scope of the technical solution of the present invention by using the technical content disclosed above are all equivalent embodiments of the present invention. At the same time, any equivalent changes, modifications and evolutions made to the above embodiments based on the essential technology of the present invention are still within the scope of protection of the technical solution of the present invention.

Claims

1. A method for preparing monodisperse spherical yttrium oxide with controllable particle size, characterized in that: The following steps are involved: S1: stirring and mixing the alcohol solution of triethanolamine and aqueous ammonia to prepare a mixed precipitant solution; S2: Slowly add the yttrium nitrate solution to the mixed precipitant solution at 60-80°C, age it, filter it, and wash it with deionized water to obtain a precursor precipitate; S3: mixing 1,2-propylene glycol, the precursor precipitate and the surfactant, reacting at high temperature and high pressure, filtering, washing, drying and calcining to obtain spherical yttrium oxide; The surfactant is prepared by the following method: N1: 2,6-nonadien-1-ol reacts with n-octylsuccinic anhydride to form an ester double bond compound; N2: Ester double bond compounds generate epoxy compounds under the action of formic acid and 30wt% H2O2; N3: The epoxy compound reacts with 1-(2-hydroxyethyl)imidazole to form a tetraimidazole compound; N4: Tetraimidazole compound reacts with 1-bromododecane to form a surfactant.

2. The method for preparing monodisperse spherical yttrium oxide with controllable particle size according to claim 1, wherein: In step N1, the molar ratio of the 2,6-nonadien-1-ol to n-octylsuccinic anhydride is 2:

1.

3. The method for preparing monodisperse spherical yttrium oxide with controllable particle size according to claim 1, wherein: In step N2, the mass ratio of the ester double bond compound, formic acid, and 30 wt% H2O2 is 10:6:

9.

4. The method for preparing monodisperse spherical yttrium oxide with controllable particle size according to claim 1, wherein: In step N3, the molar ratio of the epoxy compound to 1-(2-hydroxyethyl)imidazole is 1:

5.

5. The method for preparing monodisperse spherical yttrium oxide with controllable particle size according to claim 1, characterized in that: In step N4, the molar ratio of the tetraimidazole compound to 1-bromododecane is 1:4.

5.

6. The method for preparing monodisperse spherical yttrium oxide with controllable particle size according to claim 1, characterized in that: In step S1, the solvent in the alcoholic solution of triethanolamine is one of ethanol, n-butanol and n-hexanol.

7. The method for preparing monodisperse spherical yttrium oxide with controllable particle size according to claim 1, characterized in that: In step S1, the concentration of the triethanolamine alcohol solution is 1-2 mol / L, and the volume ratio of the ammonia water to the triethanolamine alcohol solution is (5-10):

1.

8. The method for preparing monodisperse spherical yttrium oxide with controllable particle size according to claim 1, characterized in that: In step S2, the concentration of the yttrium nitrate solution is 0.1-0.2 mol / L.

9. The method for preparing monodisperse spherical yttrium oxide with controllable particle size according to claim 1, characterized in that: In step S2, the molar ratio of triethanolamine in the mixed precipitant solution to yttrium nitrate in the yttrium nitrate solution is 10:(1-2).

10. The method for preparing monodisperse spherical yttrium oxide with controllable particle size according to claim 1, characterized in that: In step S3, the mass ratio of the precursor precipitate, surfactant, and 1,2-propylene glycol is 50:(5-15):(300-600).

11. The method for preparing monodisperse spherical yttrium oxide with controllable particle size according to claim 1, characterized in that: In step S3, the high temperature and high pressure reaction temperature is 100-150° C., the time is 12-24 hours, and the pressure is 0.5-8.0 MPa.

12. The method for preparing monodisperse spherical yttrium oxide with controllable particle size according to claim 1, characterized in that: In step S3, the calcination temperature is 700-800° C. and the calcination time is 3-5 hours.

Citation Information

Patent Citations

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    CN118145693A

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  • Preparation method of nano yttrium oxide

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