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WO-2026091774-A1 - PREPARATION METHOD FOR MONODISPERSE NANOMETER BERYLLIUM OXIDE

WO2026091774A1WO 2026091774 A1WO2026091774 A1WO 2026091774A1WO-2026091774-A1

Abstract

Provided in the present invention is a preparation method for monodisperse nanometer beryllium oxide, comprising the following steps: (S1) uniformly mixing urea and an aqueous formaldehyde solution, adjusting the pH with an organic amine to be weakly alkaline, and adding hydroxyalkyl (meth)acrylate, C12-16 alkyl (meth)acrylate and polyethylene glycol diacrylate to obtain a premix; (S2) adding a water-soluble beryllium salt to the premix, and under an inert atmosphere, adding a water-soluble initiator and slowly raising the temperature to 60-80°C for reaction to obtain a gel precursor; and (S3) after the gel precursor is dried, calcining same, washing same, and filtering same to obtain monodisperse nanometer beryllium oxide. The present invention involves a simple process and low costs, and the obtained beryllium oxide is nanoscale and has a monodisperse particle size.

Inventors

  • XIA, Weiguang
  • XU, XIAOFENG
  • KONG, Xiaoliang
  • GAO, Mingming
  • PENG, Jingpan

Assignees

  • 上海太洋科技有限公司

Dates

Publication Date
20260507
Application Date
20250813
Priority Date
20241031

Claims (10)

  1. A method for preparing monodisperse beryllium oxide nanoparticles, characterized by comprising the following steps: (S1) Mix urea and formaldehyde aqueous solution evenly, adjust the pH to weakly alkaline with organic amine, and add (meth)acrylate hydroxyalkyl ester, (meth)acrylate C12-16 alkyl ester and polyethylene glycol diacrylate to obtain a premixed solution; the molar ratio of urea to formaldehyde is 1:2-2.5; the molar ratio of urea, (meth)acrylate hydroxyalkyl ester, (meth)acrylate C12-16 alkyl ester and polyethylene glycol diacrylate is 1:0.6-0.8:2.2-3.4:0.2-0.3; (S2) Water-soluble beryllium salt is added to the premixed solution. Under an inert atmosphere, a water-soluble initiator is added, and the temperature is slowly raised to 60-80℃ to react and obtain the gel precursor. (S3) After drying the gel precursor, it was calcined, washed, and filtered to obtain monodisperse nano-beryllium oxide.
  2. According to the preparation method of claim 1, the concentration of the formaldehyde aqueous solution in step (S1) is 20-40 wt%; the weak alkalinity is achieved by adjusting the pH to 8-9.
  3. According to the preparation method of claim 1, the organic amine in step (S1) is selected from at least one of isopropylamine, n-butylamine, cyclohexylamine, diethylamine, triethylamine, diethylmethylamine, diethylisopropylamine, and diethylenetriamine.
  4. According to the preparation method of claim 1, the polyethylene glycol diacrylate has a number-average molecular weight of 200-400.
  5. According to the preparation method of claim 1, the water-soluble beryllium salt in step (S2) is selected from at least one of beryllium sulfate, beryllium chloride, and beryllium nitrate.
  6. According to the preparation method of claim 1, the water-soluble beryllium salt is added in such a way that the Be concentration in the system is 1-2 mol/L.
  7. According to the preparation method of claim 1, the inert atmosphere in step (S2) is at least one of nitrogen, helium, and argon; and the water-soluble initiator is selected from at least one of ammonium persulfate, potassium persulfate, and sodium persulfate.
  8. According to the preparation method of claim 1, the water-soluble initiator added in step (S2) is 1-3 wt% of the total mass of (meth)acrylate hydroxyalkyl ester, (meth)acrylate C12-16 alkyl ester and polyethylene glycol diacrylate.
  9. According to the preparation method of claim 1, the slow heating in step (S2) is characterized by a heating rate of 1-3℃/min.
  10. According to the preparation method of claim 1, the calcination in step (S3) is characterized by heating to 600-1000℃ at a heating rate of 1-5℃/min and holding at that temperature for 5-10 hours.

Description

A method for preparing monodisperse beryllium oxide nanoparticles Technical Field This invention belongs to the field of beryllium oxide preparation technology, specifically relating to a method for preparing monodisperse nano-beryllium oxide. Background Technology Beryllium oxide possesses high thermal conductivity, high melting point, high strength, high insulation, low dielectric constant, and low grafting loss, making it applicable in various fields such as microwave technology, electronic information, nuclear industry, and optoelectronics. Previous technologies primarily focused on manufacturing micron-sized beryllium oxide, but with current technological advancements, the demand for nano-sized beryllium oxide is gradually increasing, especially for nano-sized beryllium oxide materials with uniform particle size dispersion, which are highly sought after in the market. The main methods for manufacturing nano-sized beryllium oxide include deposition, emulsion, and sol-gel methods, but many of these methods suffer from insufficient particle size uniformity. The inventor's previous patent CN116553583A discloses a method for preparing nano-beryllium oxide, including the following steps: S1. Preparation of beryllium hydroxide suspension: In a beryllium sulfate aqueous solution, stir and add organic amine, control the pH value of the suspension, continue stirring, and allow to stand for aging to obtain a suspension; S2. Preparation of beryllium hydroxide gel: Stir the suspension evenly, filter and wash to obtain a gel; S3. Hydrothermal pretreatment of beryllium hydroxide gel: Dissolve the gel in deionized water, add polymers with different degrees of polymerization and ammonium persulfate, stir evenly, sonicate, and transfer the mixture to a hydrothermal synthesis reactor; S4. Hydrothermal treatment: Control the hydrothermal synthesis temperature and reaction time; S5. Formation of nano-beryllium oxide: After the hydrothermal treatment is completed, filter and wash the mixed solution, dry and calcine the obtained solid material to obtain nano-beryllium oxide material. This patent utilizes polymers with different degrees of polymerization. High-polymerization polymers facilitate the formation of stable three-dimensional network polymer chains, while low-polymerization polymers optimize dispersion performance, making the molecular chains in the three-dimensional structure easier to extend. This makes it difficult for beryllium oxide grains to aggregate, resulting in a more uniform particle size distribution of the final nano-beryllium oxide. CN116239133A discloses a method for preparing beryllium oxide, including the following steps: (1) Premixing: mixing beryllium salt with a eutectic solvent to obtain mixture A; (2) Ionic liquid coating: mixing mixture A from step (1) with an ionic liquid to obtain mixture B; (3) Carbonization: carbonizing mixture B obtained from step (2); (4) Calcination: calcining the carbonized product from step (3) to obtain beryllium oxide. This invention, through pre-coating with a eutectic solvent, can "bring closer" the interaction between beryllium salt and the outermost ionic liquid coating, improving the interaction force among the beryllium salt, eutectic solvent, and ionic liquid, thereby making the ionic liquid coating more compact and reducing the particle size range of beryllium oxide. CN114671444A discloses a beryllium oxide and its preparation method, including the following steps: (1) mixing beryllium salt and ionic liquid, with the ionic liquid coating the surface of the beryllium salt to obtain a mixture; (2) carbonizing the mixture to obtain a beryllium salt coated with a carbon layer; (3) calcining the beryllium salt coated with a carbon layer to obtain beryllium oxide with small particle size and concentrated particle size distribution, which not only prevents the aggregation of nanoparticles but also reduces the thermal decomposition temperature of the precursor beryllium salt, further reducing production costs. The above patents have all prepared nanoscale beryllium oxide with varying degrees of monodispersity. However, the preparation process is complex, costly, and uses reagents such as ionic liquids, and still needs improvement in large-scale industrial production. Existing technologies also include the preparation of nanoscale beryllium oxide via the sol-gel method, primarily using acrylamide polymers. The resulting three-dimensional network structure of polyacrylamide separates and blocks ions in the solution, yielding a gel containing salt solution within its fine spatial units. After drying and calcination, nanoparticles are obtained. However, acrylamide is neurotoxic, posing certain safety risks in large-scale industrial production. Furthermore, while nanoscale beryllium oxide can be obtained through experiments, the particle size uniformity needs improvement. Therefore, there is a need to develop a simple, low-cost, environmentally friendly, and low-toxicity