# US 12,110,449 B1 · Bio-enzyme degradable temporary plugging material and preparation method and application thereof

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- Number: US 12,110,449 B1
- Document ID: US12110449B1
- Status: Granted
- Kind: B1
- Application number: 18/391,726
- Filed: 2023-12-21
- Granted: 2024-10-08
- Earliest claimed: 2023-09-12
- Assignees: China University of Petroleum (East China)
- Applicants: China University of Petroleum (East China)
- Inventors: Jintang Wang; Bo Liao; Xiaohui Sun; Jiaqi Xu; Yingrui Bai; Jian Li; Xianbin Huang; Jiafeng Jin; Meichun Li; Shenglong Shi; Kaihe Lv; Jingping Liu; Jinsheng Sun
- Web page: https://patentgrep.com/patent/US12110449B1

## CPC

- C04B 20/12: Multiple coating or impregnating
- C09K 8/426: {for plugging}
- C09K 8/035: Organic additives
- C09K 8/50: Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls (compositions for consolidating loose sand or the like around wells C09K8/56)
- C09K 8/5045: {containing inorganic compounds}
- C09K 8/506: containing organic compounds
- C09K 8/5086: {obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds}
- C09K 8/514: of natural origin, e.g. polysaccharides, cellulose (C09K8/512 takes precedence)
- C09K 8/516: characterised by their form or by the form of their components, e.g. encapsulated material
- C09K 8/52: Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE

## Abstract

Disclosed is a bio-enzyme degradable temporary plugging material and a preparation method and application thereof in the technical field of natural gas hydrate drilling and production; the preparation method of the bio-enzyme degradable temporary plugging material includes the following steps: mixing the ceramsite with an aqueous solution of 3-aminopropyl trimethoxysilane before a stirring reaction and drying to obtain modified ceramsite; and fully dispersing the modified ceramsite, ethyl cellulose, and epoxy resin in dichloromethane to obtain an oil phase; adding the oil phase into a gelatin aqueous solution and mixing uniformly; after a stirring reaction, evaporating an organic solvent, filtering, washing, and drying, to obtain the bio-enzyme degradable temporary plugging material.

## Claims

### Claim 1

A process of applying a bio-enzyme degradable temporary plugging material in a well when drilling natural gas in sea areas comprising the following steps:
(1) preparing a modified ceramsite by:
mixing ceramsite with an aqueous solution of 3-aminopropyl trimethoxysilane, stirring, and drying to obtain the modified ceramsite;
(2) preparing a bio-enzyme degradable temporary plugging material by:
fully dispersing the modified ceramsite, ethyl cellulose, and an epoxy resin in dichloromethane to obtain an oil phase; adding the oil phase into a gelatin aqueous solution and mixing uniformly; stirring, evaporating the dichoromethane, filtering, washing, drying, and obtaining the bio-enzyme degradable temporary plugging material, wherein
a mass ratio of the modified ceramsite, the ethyl cellulose, and the epoxy resin is (1-4):1:1;
(3) plugging a reservoir during drilling of the reservoir by applying the bio-enzyme degradable temporary plugging material into the reservoir to maintain stability of well walls; and
(4) contacting the bio-enzyme degradable temporary plugging material in the reservoir with a bio-enzyme when the drilling is completed to degrade the bio-enzyme degradable temporary plugging material.

### Claim 2 (depends on 1)

The process according to claim 1, wherein in the step (1), one or more of the following conditions are met:
i. a particle size of the ceramsite is 20 to 40 μm;
ii. a mass ratio of the ceramsite to the 3-aminopropyl trimethoxysilane is (4 to 20):1;
iii. a mass concentration of the aqueous solution of 3-aminopropyl trimethoxysilane is 0.5% to 10%; and
iv. a stirring temperature is room temperature, a stirring time is 30 to 50 minutes, and a stirring rate is 200 to 300 r/min.

### Claim 3 (depends on 1)

The process according to claim 1, wherein in the step (2), one or more of the following conditions are met:
i. a mass ratio of the modified ceramsite and the dichloromethane is 1:(4 to 6);
ii. a mass concentration of the gelatin aqueous solution is 0.5% to 10%; and
iii. a mass ratio of dichloromethane in the oil phase to water in the gelatin aqueous solution is 1:1.

### Claim 4 (depends on 1)

The process according to claim 1, wherein in the step (2), one or more of the following conditions are met:
i. a stirring temperature is room temperature, a stirring time is 4 to 6 hours, and a stirring rate is 200 to 300 r/min; and
ii. the organic solvent is evaporated at an evaporation temperature of 45 to 55° C. for 1 to 3 hours under stirring conditions.

### Claim 5 (depends on 1)

The process according to claim 1, wherein the bio-enzyme is a low-temperature complex enzyme, cellulase, or amylase.