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Method for large-scale preparation of high-purity zinc oxide quantum dots

A large-scale preparation, zinc oxide technology, applied in chemical instruments and methods, zinc oxide/zinc hydroxide, nanotechnology and other directions, can solve the problems of low production efficiency, high production cost, easy agglomeration and precipitation, etc., to achieve high production efficiency , The effect of low production cost and no three waste emissions

Pending Publication Date: 2021-12-31
中科基创(成都)新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Due to the following disadvantages, the industrial production of zinc oxide quantum dots has not yet been popularized
[0006] 1. Zinc acetate is commonly used to prepare precursor solutions. Compared with inorganic zinc (zinc sulfate, zinc chloride), the production cost is higher; while zinc sulfate or zinc chloride is used to prepare precursor solutions, with the addition of alkali , affected by strong electronegative anions (sulfate, chloride), the resulting zinc oxide is easily agglomerated and precipitated during hydrolysis and polycondensation, and a clear zinc oxide sol with good dispersion cannot be obtained.
[0007] 2. The by-product acetate will be generated and dissolved in ethanol. It needs to be washed with a large amount of ethanol, which is not easy to clean. The product often contains acetate impurities.
[0008] 3. The reaction is carried out at normal temperature. Under normal temperature, the solubility of zinc acetate in ethanol is not high, and the output is very low. To expand the output, the only way to expand the scale of equipment is to increase the investment in equipment, and the production efficiency is low

Method used

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  • Method for large-scale preparation of high-purity zinc oxide quantum dots
  • Method for large-scale preparation of high-purity zinc oxide quantum dots

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Step 1: Dissolving zinc chloride in an ethanol solution with a volume fraction of 95%, the mass ratio of zinc chloride and ethanol solution is 1:6, and adding an appropriate amount of water to form a zinc precursor solution as solution A;

[0030] Step 2: Add propylene oxide to solution A, the molar ratio of propylene oxide to zinc chloride is 2:1, and react for 30 minutes to generate a clear and transparent zinc oxide sol as solution B;

[0031] Step 3: Mix the surface modifier polyethylene glycol 400 with pure water for hydrolysis, the mass ratio of polyethylene glycol 400 and zinc chloride is 1:5, mix the hydrolyzate evenly, add it to solution B, stir for 10 minutes, and react Generate white zinc oxide quantum dot gel;

[0032] Step 4: Centrifuge the zinc oxide gel obtained in step 3, and dry the sediment to obtain a zinc oxide quantum dot xerogel. The dry tail gas is collected and enters a rectification tower together with the supernatant for separation.

Embodiment 2

[0034] Step 1: Dissolving zinc chloride in an ethanol solution with a volume fraction of 95%, the mass ratio of zinc chloride and ethanol solution is 1:7, and adding an appropriate amount of water to form a zinc precursor solution as solution A;

[0035] Step 2: Add propylene oxide to solution A, the molar ratio of propylene oxide to zinc chloride is 2:1, and react for 20 minutes to generate a clear and transparent zinc oxide sol as solution B;

[0036] Step 3: Mix the surface modifier polyethylene glycol 400 with pure water for hydrolysis, the mass ratio of polyethylene glycol 400 and zinc chloride is 1:5, mix the hydrolyzate evenly, add it to solution B, stir for 10 minutes, and react Generate white zinc oxide quantum dot gel;

[0037] Step 4: Centrifuge the zinc oxide gel obtained in step 3, and dry the sediment to obtain a zinc oxide quantum dot xerogel. The dry tail gas is collected and enters a rectification tower together with the supernatant for separation.

Embodiment 3

[0039] Step 1: Dissolving zinc chloride in an ethanol solution with a volume fraction of 95%, the mass ratio of zinc chloride and ethanol solution is 1:10, and adding an appropriate amount of water to form a zinc precursor solution as solution A;

[0040] Step 2: Add propylene oxide to solution A, the molar ratio of propylene oxide to zinc chloride is 3:1, and react for 10 minutes to generate a clear and transparent zinc oxide sol as solution B;

[0041] Step 3: Mix the surface modifier polyethylene glycol 400 with pure water for hydrolysis, the mass ratio of polyethylene glycol 400 and zinc chloride is 1:5, mix the hydrolyzate evenly, add it to solution B, stir for 20 minutes, and react Generate white zinc oxide quantum dot gel;

[0042] Step 4: Centrifuge the zinc oxide gel obtained in step 3, and dry the sediment to obtain a zinc oxide quantum dot xerogel. The dry tail gas is collected and enters a rectification tower together with the supernatant for separation.

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Abstract

The invention relates to the technical field of preparation of high-purity zinc oxide quantum dots, and particularly discloses a large-scale preparation method of high-purity zinc oxide quantum dots, which comprises the following steps: dissolving zinc chloride in an ethanol solution to form a zinc precursor solution as a solution A; adding an epoxy compound into the solution A to generate clear and transparent zinc oxide sol as a solution B; mixing and hydrolyzing a surface modifier and pure water, uniformly mixing a hydrolysis product, adding the hydrolysis product into the solution B, and reacting the solution B to generate white zinc oxide quantum dot gel. According to the invention, the epoxy compounds such as ethylene oxide or epoxypropane are added into a zinc precursor solution, the reaction activity is high, the epoxy compounds can react with protons in the solution, the acidity of the solution is reduced, the pH value of the solution is increased, and hydrolysis and condensation polymerization of the zinc precursor are promoted; meanwhile, an epoxy compound is subjected to ring-opening reaction and is combined with chlorine in the precursor, and irreversible reaction is carried out to generate low-boiling-point chloroethanol or chloropropanol, so that the agglomeration phenomenon of zinc oxide caused by anions is avoided.

Description

technical field [0001] The invention relates to the technical field of preparation of high-purity zinc oxide quantum dots, and the specific field is a method for large-scale preparation of high-purity zinc oxide quantum dots. Background technique [0002] When the radius of a certain semiconductor material is smaller than or close to the Bohr radius of excitons, the material will have a strong quantum confinement effect. Such materials are called quantum dots (QDs). The size of quantum dots is usually less than 10nm, and the smaller size Bring about changes in its surface physical and chemical properties. ZnO quantum dots have attracted widespread attention due to their excellent optical properties and biological activity. They are a new functional material with potential applications and are considered to be one of the most commercially valuable materials in the 21st century. [0003] The preparation methods of zinc oxide quantum dots are various, which can be generally di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/54C01G9/02B82Y20/00B82Y40/00
CPCC09K11/54C01G9/02B82Y20/00B82Y40/00
Inventor 万宇吴兵陈永坡王显祥邵勇杰王来泉吕宗良
Owner 中科基创(成都)新材料科技有限公司