Water-adaptive cement self-healing system, preparation method and application thereof

Patent metadata

Field	Value
Publication number	US-12049425-B1
Application number	US-202318456661-A
Country	US
Kind code	B1
Filing date	Aug 28, 2023
Priority date	Aug 28, 2023
Publication date	Jul 30, 2024
Grant date	Jul 30, 2024

Abstract

A water-adaptive cement self-healing system, a preparation method and an application thereof are provided. A pH-triggered shell curing agent, an inorganic nano-emulsifier, and a polysaccharide shell material are added into deionized water to obtain an aqueous phase; an active diluent of epoxy is added to an epoxy to obtain a first oil phase; the aqueous phase is mixed with the first oil phase to obtain an oil/water emulsion; a surfactant is added into paraffin oil to obtain a second oil phase; the second oil phase is mixed with the oil/water emulsion to obtain an oil/water/oil emulsion; an acidic liquid is added into the oil/water/oil emulsion dropwise to obtain a solid, followed by centrifuging, washing, and freeze-drying to obtain a self-healing capsule; and then an epoxy curing agent is mixed with the self-healing capsule to obtain the water-adaptive cement self-healing system based on an oil/water/oil double-emulsion template.

First claim

What is claimed is:

1. A method for preparing a water-adaptive cement self-healing system, comprising the following steps:
step 1, preparation of a self-healing capsule, comprising the following steps:
step A1, preparation of an aqueous phase, comprising: adding a pH-triggered shell curing agent, an inorganic nano-emulsifier, and a polysaccharide shell material into deionized water, and then uniformly stirring to obtain the aqueous phase; wherein a mass fraction of the pH-triggered shell curing agent in the aqueous phase is 18.7%-37.4%, a mass fraction of the inorganic nano-emulsifier in the aqueous phase is 2.0%-8.0%, and a mass fraction of the polysaccharide shell material in the aqueous phase is 0.5%-2.0%; and the pH-triggered shell curing agent is a disodium calcium ethylenediaminetetraacetate, a calcium carbonate, or an aluminum hydroxide;
step A2, preparation of a first oil phase, comprising: adding an active diluent to an epoxy, and then uniformly stirring to obtain the first oil phase; wherein a mass fraction of the active diluent in the first oil phase is 10%-20%;
step A3, preparation of an oil/water emulsion, comprising: mixing the aqueous phase obtained in the step A1 and the first oil phase obtained in the step A2 according to a volume ratio of 80-50:20-50 to obtain a first mixture, and stirring the first mixture at 10,000-12,000 revolutions per minute (rpm) to obtain the oil/water emulsion;
step A4, preparation of a second oil phase, comprising: adding a surfactant into paraffin oil, and then uniformly stirring to obtain the second oil phase; wherein a mass fraction of the surfactant in the second oil phase is 50%-62.5%;
step A5, preparation of an oil/water/oil emulsion, comprising: mixing the second oil phase obtained in the step A4 and the oil/water emulsion obtained in the step A3 according to a volume ratio of 80-75:20-25 to obtain a second mixture, and stirring the second mixture at 600-800 rpm to obtain the oil/water/oil emulsion; and
step A6, preparing the self-healing capsule, comprising: dropwise adding an acidic liquid into the oil/water/oil emulsion obtained in the step A5 to obtain a mixed solution, stirring the mixed solution until the mixed solution is shaped to obtain a solid, centrifuging the solid, and then washing the centrifuged solid with deionized water, followed by freeze-drying the washed solid to obtain the self-healing capsule; wherein the self-healing capsule is of a core-shell structure, a shell material of the core-shell structure is the aqueous phase prepared in the step A1, and a core material of the core-shell structure is the first oil phase prepared in the step A2; and
step 2, mixing an epoxy curing agent with the self-healing capsule prepared in the step 1 according to a mass ratio of 0.5-1:1 to obtain the water-adaptive cement self-healing system based on an oil/water/oil double-emulsion template.

2. The method for preparing the water-adaptive cement self-healing system according to claim 1 , wherein in the step A1, the inorganic nano-emulsifier is a nano-silica, a bentonite, or a calcium silicate.

3. The method for preparing the water-adaptive cement self-healing system according to claim 1 , wherein in the step A1, the polysaccharide shell material is a sodium alginate or a xanthan gum.

4. The method for preparing the water-adaptive cement self-healing system according to claim 1 , wherein in the step A2, the active diluent is a benzyl glycidyl ether, a trimethylolpropane triglycidyl ether, or a 1,4-butanediol diglycidyl ether.

5. The method for preparing the water-adaptive cement self-healing system according to claim 1 , wherein in the step A4, the surfactant is a span 80, a polysorbate 20, or an op-10 surfactant.

6. The method for preparing the water-adaptive cement self-healing system according to claim 1 , wherein in the step A6, the acidic liquid is glacial acetic acid, diluted hydrochloric acid, or diluted sulfuric acid.

7. The method for preparing the water-adaptive cement self-healing system according to claim 1 , wherein in the step 2, the epoxy curing agent is a 4,4′-diaminodiphenylsulfone, a 4,4′-methylenedianiline, or a 3,3′-diethyl-4,4′-diaminodiphenylmethane.

Assignees

• Univ Tianjin

Inventors

• Guo Jintang
• Ying Yujie
• Hu Miaomiao
• Liu Ming

Classifications

• C04B22/10

  containing carbon in the anion, e.g. carbonates · CPC title

• C09K8/467

  containing additives for specific purposes · CPC title

• C04B28/04

  Portland cements · CPC title

• C04B2103/0035

  Type G · CPC title

• C04B20/1048 Primary

  Polysaccharides, e.g. cellulose, or derivatives thereof · CPC title