# US 12,600,868 B2 · Organic-inorganic composite thermal insulation medium and preparation method thereof

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- Number: US 12,600,868 B2
- Document ID: US12600868B2
- Status: Granted
- Kind: B2
- Application number: 18/724,869
- Filed: 2023-04-28
- Published: 2025-05-08
- Granted: 2026-04-14
- Earliest claimed: 2022-07-06
- Assignees: Shanghai Huzheng Industry Co., Ltd
- Applicants: Shanghai Huzheng Industry Co., Ltd
- Inventors: Jiayi Li; Jiaxiao Xue
- Web page: https://patentgrep.com/patent/US12600868B2

## CPC

- C09D 5/18: Fireproof paints {including high temperature resistant paints}
- C09D 5/32: Radiation-absorbing paints {(protection against X-, gamma- or corpuscular radiation G21F)}
- C09D 7/62: modified by treatment with other compounds
- C09D 7/65: macromolecular (C09D7/41-C09D7/48 take precedence)
- C09D 7/67: {Particle size smaller than 100 nm}
- C09D 133/00: Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09K 3/00: Materials not provided for elsewhere
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE

## Abstract

Disclosed is an organic-inorganic composite thermal insulation medium, which is a nanoparticle having a structure of (Mx-Rn)WOy, where M represents a doped metal element, R represents an organic complex group, 0.3≤x≤0.7, 2<y<4, n represents a polymerization degree of the organic complex group, and n≥10; M is selected from the group consisting of an alkali metal, an alkaline earth metal, a transition metal, and a rare earth metal; and R is selected from the group consisting of pyrrole and a derivative thereof, aniline and a derivative thereof, and thiophene and a derivative thereof. In addition, also disclosed is a method for preparing the thermal insulation medium.

## Claims

### Claim 1

An organic-inorganic composite thermal insulation medium, which is a nanoparticle having a structure of (Mx-Rn)WOy, and having a particle size of 10 nm to 50 nm;
wherein M represents a doped metal element, R represents an organic complex group, 0.3≤x≤0.7, 2<y<4, n represents a polymerization degree of the organic group, and n≥10; the doped metal element is selected from the group consisting of an alkali metal, an alkaline earth metal, a transition metal, and a rare earth metal; and R is selected from the group consisting of pyrrole and a derivative thereof, aniline and a derivative thereof, and thiophene and a derivative thereof.

### Claim 2 (depends on 1)

A method for preparing the organic-inorganic composite thermal insulation medium according to claim 1, comprising the following steps:
(1) dispersing 1 part by mass of a tungstate in a water/ethanol (1/1, v/v) system to obtain a solution with a concentration of 0.05 mol/L to 0.5 mol/L, adding 0.05 to 0.5 parts by mass of a dilute acid solution with a concentration of 0.05 mol/L to 0.1 mol/L to the solution to obtain a solution system, and subjecting the solution system to ultrasonic treatment for 10 min to 30 min and aging for 12 h to 24 h to obtain a product;
(2) subjecting the product obtained in step (1) to filtering and then washing with water to obtain a washed product, dispersing the washed product and 0.1 to 0.5 parts by mass of a metal salt sequentially in 5 to 10 parts by mass of deionized water, then adding 0.5 to 3 parts by mass of a polyol thereto and stirring for 0.5 h to 2 h to obtain a mixture, and transferring the mixture to a pressure reactor and conducting a reaction for 12 h to 24 h at a pressure of 1 MPa to 5 MPa and a temperature of 100° C. to 150° C. to obtain a reaction product;
(3) subjecting the reaction product obtained in step (2) to filtering and then washing with water to obtain a washed reaction product, and dispersing the washed reaction product in 5 to 10 parts by mass of a solvent, then adding 0.05 to 0.2 parts by mass of an active monomer thereto to obtain a mixed system, adjusting the mixed system to a pH of 2 to 5 by using hydrochloric acid and conducting a pre-reaction for 1 h to 3 h to obtain a pre-reaction system, and adding 0.01 to 0.1 parts by mass of an oxidant to the pre-reaction system and conducting a reaction for 2 h to 5 h at a temperature of 50° C. to 80° C. to obtain a reaction system; and
(4) subjecting the reaction system obtained in step (3) to filtering and then washing with ethanol to obtain a washed reaction system, and vacuum-drying the washed reaction system for 24 h and conducting a treatment in a tube furnace at a temperature of 200° C. to 400° C. for 1 h to 5 h under a nitrogen atmosphere to obtain the stable organic-inorganic composite thermal insulation medium.

### Claim 3 (depends on 2)

The method for preparing the organic-inorganic composite thermal insulation medium according to claim 2, wherein in step (1), the tungstate is selected from the group consisting of sodium tungstate, potassium tungstate, and ammonium tungstate.

### Claim 4 (depends on 2)

The method for preparing the organic-inorganic composite thermal insulation medium according to claim 2, wherein in step (1), the dilute acid solution is selected from the group consisting of dilute hydrochloric acid and dilute nitric acid.

### Claim 5 (depends on 2)

The method for preparing the organic-inorganic composite thermal insulation medium according to claim 2, wherein in step (2), the polyol is selected from the group consisting of ethylene glycol, 1,3-propanediol, and glycerol.

### Claim 6 (depends on 2)

The method for preparing the organic-inorganic composite thermal insulation medium according to claim 2, wherein in step (3), the oxidant is selected from the group consisting of iron chloride and potassium chlorate.

### Claim 7 (depends on 2)

The method for preparing the organic-inorganic composite thermal insulation medium according to claim 2, wherein in step (2), the metal salt is selected from the group consisting of a soluble chloride of, sulfate of, and nitrate of the doped metal element.

### Claim 8 (depends on 2)

The method for preparing the organic-inorganic composite thermal insulation medium according to claim 2, wherein in step (3), the active monomer is selected from the group consisting of pyrrole and a derivative thereof, aniline and a derivative thereof, and thiophene and a derivative thereof.
