US 11,691,043 B2
Multi-functional plugging agent for coal mine and preparation method thereof
Xiangming Hu, Qingdao (CN); Weimin Cheng, Qingdao (CN); Bingrui Yan, Qingdao (CN); Yanyun Zhao, Qingdao (CN); Di Xue, Qingdao (CN); Mingyue Wu, Qingdao (CN); Zhenglong He, Qingdao (CN); Guangxing Bai, Qingdao (CN); and Zonglei Mou, Qingdao (CN)
Assigned to SHANDONG UNIVERSITY OF SCIENCE AND TECHNOLOGY, Qingdao (CN)
Filed by SHANDONG UNIVERSITY OF SCIENCE AND TECHNOLOGY, Qingdao (CN)
Filed on Jul. 19, 2022, as Appl. No. 17/868,037.
Application 17/868,037 is a continuation of application No. PCT/CN2021/076121, filed on Feb. 9, 2021.
Claims priority of application No. CN202110010867.5 (CN), filed on Jan. 6, 2021.
Prior Publication US 2022/0362599 A1, Nov. 17, 2022
Int. Cl. A62D 1/00 (2006.01); B01D 11/02 (2006.01); C09K 21/02 (2006.01); C09K 21/06 (2006.01); E21F 15/00 (2006.01)
CPC A62D 1/005 (2013.01) [B01D 11/0288 (2013.01); C09K 21/02 (2013.01); C09K 21/06 (2013.01); E21F 15/005 (2013.01)] 1 Claim
OG exemplary drawing
 
1. A multi-functional plugging agent for a coal mine based on an Ecklonia Kurome Okam biological extract, wherein the multi-functional plugging agent for the coal mine contains the Ecklonia Kurome Okam biological extract; and
a preparation method of the multi-functional plugging agent for the coal mine comprises:
(1) soaking Ecklonia Kurome Okam in fresh water in a light-proof tank for 3 hours to 4 hours, taking out and then washing the soaked Ecklonia Kurome Okam with running water for 2 times to 3 times, then putting the washed Ecklonia Kurome Okam in a drying oven for drying at 90° C. to 100° C. for 50 minutes to 60 minutes, crushing the dried Ecklonia Kurome Okam in a pulverizer for 3 minutes to 5 minutes, and screening Ecklonia Kurome Okam powder with a particle size less than 120 meshes;
(2) putting the Ecklonia Kurome Okam powder into a reaction container for mixing with water to obtain an Ecklonia Kurome Okam suspension, heating the Ecklonia Kurome Okam suspension to 45° C. to 55° C., stirring the Ecklonia Kurome Okam suspension in an air atmosphere and adding phosphorus pentoxide, stirring the mixture for reaction for 30 minutes and then adding a complex enzyme for continuous stirring for 30 minutes, standing the mixture for reaction for 50 hours to 55 hours, and filtering the mixture to obtain the Ecklonia Kurome Okam biological extract;
(3) adding urea into the Ecklonia Kurome Okam biological extract obtained in step (2) for neutralizing and stirring for 20 minutes, heating the mixture to 60° C. and then stirring the mixture in a nitrogen atmosphere, and sequentially adding 0.5% to 2% by mass fraction of inorganic catalyst and 1% to 3% by mass fraction of melamine for full reaction and mixing to obtain a bio-based plugging synergist solution; and
(4) after cooling the bio-based plugging synergist solution obtained in step (3), uniformly stirring and mixing the solution with pentaerythritol and ammonium polyphosphate to obtain the multi-functional plugging agent for the coal mine based on the Ecklonia Kurome Okam biological extract;
a mixing ratio of the Ecklonia Kurome Okam powder to water in step (2) is 1:35 to 1:45 in a mass ratio; a mass ratio of the added phosphorus pentoxide to water is 1:13 to 1:42; and the complex enzyme is one or more of endoglucanase, cellobiase, carboxypeptidase and beta-glucosidase, with an addition amount of 0.5% to 1.5% by mass fraction;
the inorganic catalyst in step (3) is a layered metal composite hydroxide; and a mass ratio of an addition amount of the urea to the phosphorus pentoxide is 1:1 to 1:3; and
after cooling the bio-based plugging synergist solution obtained in step (4), 100 parts to 105 parts by weight of the solution are uniformly stirred and mixed with 3 parts to 5 parts by weight of the pentaerythritol and 2 parts to 5 parts by weight of the ammonium polyphosphate.