IP Library Granted Patent US 11,905,352
Granted Patent B2
US 11,905,352 · App. 17/275,998 · Granted Feb 20, 2024

Expansive polymer grouting material for treating high-pressure large-flow-rate karst water inrush and preparation method thereof

Inventors: Shucai Li (Jinan, CN); Rentai Liu (Jinan, CN); Chenyang Ma (Jinan, CN); Mengjun Chen (Jinan, CN); Yankai Liu (Jinan, CN); Zhenjun Wang (Jinan, CN); Chunyu Zhang (Jinan, CN); Xiuhao Li (Jinan, CN); Shaolong Duan (Jinan, CN)
Assignee: SHANDONG UNIVERSITY
C08F220/06C08K3/36E21D11/38
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Quick Facts
Patent No.
US 11,905,352
App. No.
17/275,998
Granted
Feb 20, 2024
Kind
B2
Abstract

A preparation method of an expansive polymer grouting material for treating high-pressure large-flow-rate karst water inrush includes: 1) adding a crosslinking agent to acrylic acid; then adding a polymer water-absorbent resin comonomer and performing a polymerization reaction to obtain a precursor; 2) adding an initiator to the precursor obtained in step 1), heating the mixture, performing a reaction to obtain a hydrogel, and grinding the hydrogel to obtain a primary polymer water-absorbent resin; 3) spraying a surface crosslinking agent onto a surface of the primary polymer water-absorbent resin obtained in step 2), and drying the product; and 4) preparing a suspension from an inorganic water conducting agent, spraying the suspension onto the product obtained in step 3), and performing drying to obtain the expansive polymer grouting material.

Claims (33)

1. A preparation method of an expansive polymer grouting material for treating high-pressure large-flow-rate karst water inrush, comprising the following steps:

(1) adding a crosslinking agent to acrylic acid; then adding a polymer water-absorbent resin comonomer and performing a polymerization reaction to obtain a precursor;

(2) adding an initiator to the precursor of step (1), heating the mixture, performing a reaction to obtain a hydrogel, and grinding the hydrogel to obtain a primary polymer water-absorbent resin;

(3) spraying a surface crosslinking agent onto a surface of the primary polymer water-absorbent resin of step (2), and drying the obtained product for later use; and

(4) preparing a suspension from an inorganic water conducting agent, spraying the suspension onto the dried product of step (3), and performing drying to obtain the expansive polymer grouting material;

wherein the polymer water-absorbent resin comonomer comprises polyvinyl alcohol, acrylamide, methacrylamide or acrylonitrile;

the crosslinking agent comprises one or a combination of more of N,N-methylenebisacrylamide, dipentaerythritol hexaacrylate, pentaerythritol tetraester, pentaerythritol triallyl ether, pentaerythritol triacrylate, polyethylene glycol diglycidyl ether, ethoxylated glycerol triacrylate and ethylene glycol dimethacrylate;

the surface crosslinking agent comprises one or a combination of more of water, polylol, glycidyl ether, ethylene carbonate, propylene carbonate and a polyvalent metal compound; and

the inorganic water conducting agent comprises fumed silica, nano titania or activated alumina powder.

2. A preparation method of an expansive polymer grouting material for treating high-pressure large-flow-rate karst water inrush, wherein in the preparation method according to claim 1 , when a precursor is prepared in step (1), firstly, acrylic acid is incompletely neutralized with lye to obtain an incompletely neutralized solution containing acrylic acid, then the incompletely neutralized solution and a crosslinking agent are mixed and subjected to a polymerization reaction with a polymer water-absorbent resin comonomer to obtain the precursor, and the subsequent steps are the same as steps (2)-(4) in the preparation method according to claim 1 .

3. The preparation method according to claim 2 , wherein a degree of neutralization of the incompletely neutralized solution is maintained at 40%-90%.

4. The preparation method according to claim 2 , wherein the lye comprises sodium hydroxide, calcium hydroxide or a mixture of both.

5. The preparation method according to claim 2 , wherein a mass concentration of the lye is 20-50%.

6. The preparation method according to claim 1 , wherein in step (1), a mass concentration of the acrylic acid is 25-45%.

7. The preparation method according to claim 6 , wherein in step (1), the polymer water-absorbent resin comonomer is added in a proportion of 0.5-20% by mass of the acrylic acid in step (1).

8. The preparation method according to claim 6 , wherein in step (1), the crosslinking agent is added in a proportion of 0.5-2% by mass of the acrylic acid in step (1).

9. The preparation method according to claim 6 , wherein in step (2), the initiator is added in a proportion of 0.1-0.7% by mass of the acrylic acid in step (1).

10. The preparation method according to claim 6 , wherein in step (3), the surface crosslinking agent is added in a proportion of 3-6% by mass of the primary polymer water-absorbent resin in step (2).

11. The preparation method according to claim 6 , wherein in step (4), the inorganic water conducting agent is added in a proportion of 0.5-1.5% by mass of the primary polymer water-absorbent resin.

12. The preparation method according to claim 1 , wherein

in step (2), the initiator comprises: an inorganic peroxide initiator, an azo initiator and redox initiators.

13. The preparation method according to claim 12 , wherein the inorganic peroxide initiator comprises potassium persulfate, sodium persulfate and ammonium persulfate;

the azo initiator comprises azobisisobutyronitrile, azobisisoheptonitrile and dimethyl azobisisobutyrate; and

the redox initiators comprise ammonium persulfate/sodium bisulfite, hydrogen peroxide/ferrous sulfate, ammonium persulfate/ferrous sulfate and potassium persulfate/ferrous chloride; wherein the substance before “/” indicates an oxidation initiator, the substance after “/” indicates a reduction initiator, and each couple of redox initiators are used at the same time; and a mass ratio of the oxidation initiator to the reduction initiator is 1:3-8.

14. The preparation method according to claim 1 , wherein

the polylol comprises ethylene glycol, propylene glycol or glycerol; and the polyvalent metal compound comprises silver nitrate and cupric chloride.

15. The preparation method according to claim 1 , wherein in step (2), the heating means: gradually increasing a reaction temperature from 0 to 85° C., and the initiator is a combination of an inorganic peroxide initiator, an azo initiator and redox initiators.

16. The preparation method according to claim 15 , wherein a mass ratio of the inorganic peroxide initiator to the azo initiator to the redox initiators is 1-2:1-2:1-7.

17. The preparation method according to claim 1 , wherein in step (1), the time of the polymerization reaction is 1-1.5 h; and in steps (3) and (4), the drying conditions are: aeration-drying at 100-120° C. for 20-60 min.

18. An expansive polymer grouting material prepared by the method according to claim 1 , wherein the grouting material has a core-shell structure, wherein the primary polymer water-absorbent resin obtained in step (2) is a core, and the surface crosslinking agent and the water conducting agent respectively added in step (3) and step (4) are a shell.

19. An expansive polymer grouting material composition, wherein the composition is composed of an expansive polymer grouting material and a carrying fluid; and the expansive polymer grouting material is the expansive polymer grouting material obtained by the preparation method according to claim 1 .

20. The composition according to claim 19 , wherein the carrying fluid comprises one or both of glycerol and ethanol.

21. The composition according to claim 19 , wherein a mass ratio of the expansive polymer grouting material to the carrying fluid is 1-2:1-5.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 12, 2021
From: LI, SHUCAI; LIU, RENTAI; MA, CHENYANG; CHEN, MENGJUN; LIU, YANKAI; WANG, ZHENJUN; ZHANG, CHUNYU; LI, XIUHAO; DUAN, SHAOLONG
To: SHANDONG UNIVERSITY
Reel/Frame 055578/0913 →
Priority Claims (1)
CN 201811378133.7 · Nov 19, 2018 · national
Continuity (1)
Related Publication 20220064347A1 · Mar 3, 2022
Cited By (1)
US 12,276,076