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Process for producing vanadium-dioxide-containing particles

A technology of vanadium dioxide, manufacturing method, applied in vanadium oxide, chemical instruments and methods, methods of chemically changing substances by atmospheric pressure, etc. Issues such as mentioning, disclosing, etc., to achieve the effect of high thermochromic

Active Publication Date: 2019-01-11
KONICA MINOLTA INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] However, the hydrothermal synthesis method using a flow-through reaction device disclosed in Patent Document 3 has the following problems: If a flow-type reaction device is used to hydrothermally synthesize metal-containing particles, the particle size distribution becomes wider due to aggregation, and the transparency of the film becomes weaker. get lower
[0015] Then, in the above-mentioned Patent Document 3 and Patent Document 4, the use of a flow-through reaction device to produce a compound containing vanadium dioxide (VO 2 ) and other metal oxide particles, there is a problem that due to the dissolved oxygen dissolved in the water used in the production, the raw material and the formed vanadium dioxide are excessively oxidized during synthesis, and the metal oxidation of the desired valence cannot be obtained. In addition, a decrease in the monodispersity of the formed metal oxide particles, a decrease in thermochromism
The hydrothermal synthesis method using a flow-through reaction device disclosed in Patent Document 5 is a method for controlling the particle diameter of functional nanoparticles by supplying an aqueous alkali solution to the reaction field to adjust the pH during microparticle synthesis. During the particle formation process, excessive salts and the like are not removed, and the particle formation is carried out in an intact environment. Therefore, it is difficult to control the crystallite diameter and particle diameter of the particles to desired conditions. As a result, there are particles Widening the diameter distribution, causing a decrease in thermochromic properties, or causing a decrease in transparency (haze) when applied to an optical film
[0017] In addition, in Patent Document 3 and Patent Document 4, regarding the application of a flow-through reaction device to thermochromic vanadium dioxide (VO 2 ) particles, and obtained vanadium dioxide (VO 2 ) methods and specific heat treatment conditions are not mentioned or disclosed at all, requiring the establishment of manufacturing conditions as soon as possible

Method used

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  • Process for producing vanadium-dioxide-containing particles
  • Process for producing vanadium-dioxide-containing particles
  • Process for producing vanadium-dioxide-containing particles

Examples

Experimental program
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Effect test

Embodiment approach 1A

[0122] Embodiment 1A, which is one of the applicable manufacturing processes of manufacturing condition 1, is the following method: Figure 1A As shown, add 1) the raw material liquid containing the vanadium-containing compound (A) and degassed water, 2) the compound (B) that reacts with the vanadium-containing compound to the raw material liquid container one 5, for example, dissolve it in the degassed Alkali or reducing agent for water, add degassed water as water in another raw material liquid container 2, and make the degassed water in a supercritical or subcritical state by using a heating medium 13 at a specified temperature and pressure. After gas and water, the two are combined at the confluence point (MP) to make a reaction solution, and then hydrothermal treatment is performed on the heating part piping 17 in the hydrothermal reaction part 16 constituting the hydrothermal reaction part to prepare particles containing vanadium dioxide. .

Embodiment approach 1B

[0124] Embodiment 1B, which is one of the applicable manufacturing processes of manufacturing condition 1, is the following method: Figure 1B As shown, in raw material liquid container one 5, add 1) the raw material liquid that contains vanadium-containing compound (A) and degassed water, in another raw material liquid container two 2, add and contain 2) compound (B) that contains vanadium-containing compound reaction ) degassed water, the degassed water containing the compound (B) that reacts with the vanadium-containing compound is made into degassed water in a supercritical or subcritical state by using a heating medium 13 at a specified temperature and pressure, and then the two After they meet at the confluence point (MP) to form a reaction solution, hydrothermal treatment is performed on the heating section piping 17 in the hydrothermal reaction section 16 constituting the hydrothermal reaction section to prepare vanadium dioxide-containing particles.

[0125] 〔Flow-thr...

Embodiment approach 2

[0253] Embodiment 2 is characterized in that, after preparing a slurry raw material liquid containing at least a vanadium-containing compound and water and a compound reacting with the vanadium-containing compound using a flow-through reaction device having a hydrothermal reaction part, the reaction liquid is The hydrothermal reaction is performed in the hydrothermal reaction section for performing the hydrothermal synthesis constituting the above-mentioned flow-type reaction device with a passage time in the range of 3 to 1000 seconds.

[0254] In the hydrothermal reaction part, the values ​​of the average particle diameter (D) and the polydispersity index (PDI) of the particles containing vanadium dioxide can be made extremely small by carrying out under high pressure and in the presence of supercritical or subcritical water. , particularly excellent thermochromism of the vanadium dioxide-containing particles and transparency of an optical film containing the vanadium dioxide...

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Abstract

The present invention addresses the problem of providing a process for producing vanadium-dioxide-containing particles which have a small average particle diameter and a narrow particle diameter distribution, are excellent in terms of monodispersity and dispersion stability, and have excellent thermochromic properties. The process for producing vanadium-dioxide-containing particles of the presentinvention comprises using a flow-through type reactor including a hydrothermal reaction part and using a liquid reaction mixture obtained by mixing a raw-material slurry, the slurry comprising a vanadium-containing compound and water, and a compound that reacts with the vanadium-containing compound, with water in a supercritical or subcritical state. The production process is characterized in that1) the water is degassed water, 2) the time over which the liquid reaction mixture passes through the hydrothermal reaction part is 3-1,000 seconds, 3) the raw-material slurry is subjected, before the hydrothermal synthesis, to a desalting treatment for salt removal therefrom and hence the particles have an average particle diameter of 15-40 nm and an average crystallite diameter of 15-40 nm, or4) prior to the step of producing vanadium-dioxide-containing particles, the raw-material slurry is subjected to a dispersing treatment.

Description

technical field [0001] The present invention relates to a method for producing vanadium dioxide-containing particles that do not aggregate, have a narrow particle size distribution, and have excellent thermochromic properties by a hydrothermal synthesis method using a flow-through reaction device. Background technique [0002] In places where a large heat exchange occurs between the internal environment of a building such as a house and a building, and a mobile body such as a vehicle, and the external environment (for example, building window glass, car body window glass, etc.), in order to Considering both energy saving and comfort, the application of thermochromic materials is being actively studied. [0003] The "thermochromic material" referred to here is a material whose optical characteristics represented by light transmittance can be controlled by temperature, for example. For example, when a thermochromic material is applied to window glass of a building, it can ref...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02B01J3/00C02F1/20C09K9/00
CPCB01J3/00C01G31/02C02F1/20C09K9/00Y02P20/54
Inventor 工藤智广千叶隆人高向保彦林健司
Owner KONICA MINOLTA INC
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