US 11,786,880 B2
Preparation method of the microcapsules for low-temperature well cementation to be used to control cement hydration heat
Chunmei Zhang, Chengdu (CN); Jingxuan Cai, Chengdu (CN); Jia Wang, Chengdu (CN); Xiaowei Cheng, Chengdu (CN); Kaiqiang Liu, Chengdu (CN); Ping Wang, Chengdu (CN); Hao Xu, Chengdu (CN); Bibo Dai, Chengdu (CN); Baoyang Ke, Chengdu (CN); Xiaoyang Guo, Chengdu (CN); Mingze Li, Chengdu (CN); Song Yang, Chengdu (CN); and Zheng Xi, Chengdu (CN)
Assigned to SOUTHWEST PETROLEUM UNIVERSITY, Chengdu (CN); and YAO BAI SPECIAL CEMENT TECHNOLOGY RESEARCH AND DEVELOPMENT CO., LTD., Xi'an (CN)
Filed by Southwest Petroleum University, Chengdu (CN); and Yao Bai Special Cement Technology Research and Development Co., Ltd., Xi'an (CN)
Filed on May 20, 2022, as Appl. No. 17/750,054.
Claims priority of application No. 202110661829.6 (CN), filed on Jun. 15, 2021.
Prior Publication US 2022/0395796 A1, Dec. 15, 2022
Int. Cl. B01J 13/04 (2006.01); C04B 20/00 (2006.01); C09K 5/06 (2006.01); C09K 8/467 (2006.01)
CPC B01J 13/043 (2013.01) [C04B 20/0004 (2013.01); C09K 5/06 (2013.01); C09K 8/467 (2013.01)] 2 Claims
OG exemplary drawing
 
1. A preparation method of the microcapsules for low-temperature well cementation to be used to control cement hydration heat, comprising the following steps in proper order:
S1: a shell material being weighted with 10-20 g, and added into 50-100 mL of deionized water, then the resultant mixture being stirred in a thermostat water bath at 45° C. so as to completely dissolve it into a homogeneous and stable shell material solution, said shell material being sodium silicate NaSiO3·9H2O;
S2: 10-20 g of a core material and 0.02-0.1 g of an emulsifier being put into a three-necked flask and stirred in a thermostat water bath at 45° C. for 30-60 min so as to uniformly emulsify and disperse them, forming a stable oil-in-water core material emulsion, while adjusting the pH value of said emulsion to descend below 5.5 with a pH adjuster, where said core material is a binary composite phase-change material prepared by n-decanoic acid and lauryl alcohol, the preparation process of said binary composite phase-change material includes mixing n-decanoic acid with lauryl alcohol by mass ratio of 1:1, and stirring them evenly; said emulsifier is a mixture of alkylphenol polyoxyethylene ether-10 and cetyl trimethyl ammonium bromide, the mass ratio of the cetyl trimethyl ammonium bromide is 20-80%;
S3: said three-necked flask containing said core material emulsion being transferred to a water bath at 50-90° C., and then said shell material solution being dropwise added into it with stirring, after reacting for 2-3 hours, a solid-liquid mixture being poured out so as to naturally cool it to room temperature, thus said cooled solid-liquid mixture being processed by suction filtration, washed with ethanol and deionized water, respectively, to remove impurities, and finally being processed by freeze-drying.